EP4672972A1

EP4672972A1 - Method and apparatus for preparing flakes

Info

Publication number: EP4672972A1
Application number: EP24712948.9A
Authority: EP
Inventors: Guy Fefferman; Aleksey Elisha LEVIN
Original assignee: Landa Labs 2012 Ltd
Current assignee: Lot Foodtech Ltd
Priority date: 2023-02-27
Filing date: 2024-02-26
Publication date: 2026-01-07
Also published as: IL322572A; CN120826162A; AU2024229394A1; MX2025010110A; WO2024180459A1; KR20250154478A; JP2026509774A

Abstract

There is disclosed a method of manufacturing flakes, comprising: a) providing a liquid stock comprising at least one solid material dissolved or dispersed in a liquid; b) applying the liquid stock to a first movable surface, so as to form thereon a thin film of liquid stock; c) cyclically i) evaporating at least a part of the liquid from the thin film, so as to increase the concentration of solid particles, and ii) applying pressure to the film by passing it through at least one nip formed by urging opposed surfaces towards one another, so as to progressively form a layer comprised of relatively dry flakes consisting of agglomerated and/or compacted solid particles. Flakes made thereby and an apparatus for producing the same are also disclosed, as well as uses and advantages of such flakes.

Description

METHOD AND APPARATUS FOR PREPARING FLAKES

CROSS-REFERENCE TO RELATED APPLICATIONS

This application claims Paris Convention priority from Great-Britain patent applications Nos. GB 2302788.1 filed on February 27, 2023, and GB 2316241.5 filed on October 24, 2023. The contents of these applications are incorporated by reference in their entirety as if fully set forth herein.

FIELD

The present disclosure relates to a method for manufacturing flakes out of materials disposed in a liquid and to an apparatus enabling the implementation of the method.

BACKGROUND

Modifying the morphology of materials has long been known to affect their properties or behaviors in a variety of ways too numerous to list extensively. One of the many properties that can be affected by changing the dimensions and shapes of a material, and inter alia their specific surface area (ANA), is their solubility in any particular liquid. Increasing the specific surface area of a material, and their rate of dissolution, has far reaching application in a wide range of fields, including for example, the agricultural industry, the cosmetic industry, the manufacturing industry, the water treatment industry, the fire suppression industry, the pharmaceutical industry, and the food industry, to name but a few.

As the latter fields, which ultimately involve ingestion of products by living subjects, can be more readily appreciated, the benefits of the following disclosure shall be illustrated inter alia with respect to constituents of such goods.

Flavor perception is a complex process that involves smell, taste, and chemical sensations (e.g., pungency, astringency, irritation, etc.). Regarding taste, it is perceived through dedicated taste receptors located within the taste buds found on the tongue, the side of the mouth, the soft palate, the cheeks, the back of the throat and even in the oesophagus. The five main tastes perceivable are sweet, sour, salt, bitter and umami, as can be detected when eating, for instance, sugar, vinegar, salt, caffeine and monosodium glutamate, respectively. The compounds or compositions that may induce or elicit taste perception of one or more of the taste categories or other taste sensation are referred to as tastants. Tastants may be added to food products to improve the overall taste. The tastants need to be in solution to be perceived as a taste, which is one of the reasons that animals salivate. Once the tastant molecules are dissolved in the saliva, they can suitably contact the taste receptor nerve located within each taste bud and stimulate it so as to accordingly transmit the perception of the relevant taste to the brain.

While the importance of taste is not limited to food consumed by humans and may similarly impact the compliance of other animals to ingest, for instance, medications, it may be easier to discuss the present problems in the former context. Considering for example table salt (sodium chloride, often referred to simply as salt) and sugar (e.g., glucose, fructose, sucrose, lactose, etc.), both are significant ingredients of food stuff that we may eat or drink, their relatively high presence being even notified as a health concern on packaging in view of their long-term effects. Too much salt in the diet, through its sodium part, can lead to high blood pressure, heart disease, and stroke, among other ailments. Too much sugar can also lead to weight gain, eye, kidney or nerve damages, and diabetes, if the insulin endogenously produced by the subjects is insufficient to eliminate such excess sugar. On the other hand, too little of them is also undesired, insufficient salt levels leading for instance to weakness, nausea, or muscle cramps; and insufficient sugar levels (e.g., hypoglycemia) being capable of causing headaches, dizziness or confusion. If salt or sugar levels are too low or too high for a prolonged period of time, the medical consequences may worsen and be lethal, if untreated. For some individuals, having access to food products with reduced amounts of some tastants is medically warranted.

In recent years, the food industry has made efforts to reduce the contents of salt and sugar in their products, such decrease in their amounts being sometimes compensated by the addition of substances potentiating their taste effect. Additional approaches include replacing these leading tastants by substances providing a similar taste while being deemed less deleterious to the health; or manufacturing them as hollow structures (e.g., spheres, cubes, or pyramids) or as thin coatings over an edible core, the increased surface provided by such methods enhancing the perceived taste. The simple grinding of tastants into granular particles of smaller sizes which could achieve an increase in specific surface area, to some extent a better adhesion to dry food products, and an enhanced taste perception was ruled out at as a viable solution, this approach yielding new problems of flowability, tiny particles having a higher tendency to stick one to the other into chunky aggregates, this clogging and clumping leading to difficult handling, transportation and storage, or leading to adverse dust-ability, tiny particles becoming airborne during their processing. Tiny granular particles may also more readily be swamped in oil layers, slowing their dissolution and decreasing the intensity of the taste they may provide. Wellbeing of consumers, their compliance to ingest materials having a favorable morphology, advantages such morphologies may provide to the effectiveness of the material during processes for manufacturing products including the same and/or to the efficacy of said products following their administration are not the sole improvements one may seek. Materials suitably improved may in turn enable reducing their relative amounts in the intended products, leading to cost reduction.

There remains a need to modify the morphology of materials so as to improve at least one of their properties as can be desired for their future intended uses. In the context of ingested goods, such as food products or medicaments, such a morphology-derived improvement may be exemplified by maintaining the satisfactory organoleptic sensation associated with the tastants or achieving a desired dissolution of active ingredients, while advantageously reducing their presence in the articles respectively manufactured therewith.

SUMMARY

The present disclosure is directed to answer at least some of the foregoing needs for materials having a morphology advantageously adapted to overcome the limitations currently observed in the field, so as to allow, for instance, reducing the presence of such materials and/or increasing their efficacy for their respective intended uses.

In a first aspect, the disclosure provides a method of manufacturing flakes as set forth in more detail hereinafter and as claimed in Claim 1 of the appended claims and in claims depending therefrom.

In a second aspect, the disclosure provides an apparatus for producing flakes as set forth in more detail hereinafter and as claimed in Claim 15 of the appended claims and in claims depending therefrom.

Further aspects of the disclosure are set out in the clauses set out below following the description of the embodiments.

These aspects and additional benefits and features of the disclosure will be better understood with reference to the following detailed description taken in conjunction with the figures and non-limiting examples.

BRIEF DESCRIPTION OF THE DRAWINGS

Some embodiments of the disclosure will now be described further, by way of example, with reference to the accompanying figures, where like reference numerals or characters (or last digits thereof) indicate corresponding or like components. The description, together with the figures, makes apparent to a person having ordinary skill in the art how some embodiments of the disclosure may be practiced. The figures are for the purpose of illustrative discussion and no attempt is made to show structural details of an embodiment in more detail than is necessary for a fundamental understanding of the disclosure. For the sake of clarity and convenience of presentation, some objects depicted in the figures are not necessarily shown to scale.

In the Figures:

Figure 1 depicts a flowchart of a method for preparing (e.g., tastant) flakes according to embodiments of the present teachings.

Figures 2-7 each schematically illustrates a nip or series of nips, as may be used according to one embodiment of a method or an apparatus of the present teachings.

Figures 8A and 8B are pictures captured by scanning electron microscopy (SEM) having furthermore focused ion beam (FIB) capacity. Fig. 8A shows a tastant before being processed by a method or using an apparatus according to one embodiment of the present teachings; whereas Fig. 8B shows the same tastant after being processed thereby. In this particular case, the tastant is fed to the nip as a dry powder.

Figures 9A and 9B are pictures similarly captured by SEM-FIB microscopy. Fig. 9A shows a tastant before being processed by a method or using an apparatus according to another embodiment of the present teachings; whereas Fig. 9B shows the same tastant after being processed thereby. In this particular case, the tastant is fed to the nip as a paste consisting of a dry powder dispersed in a viscous medium.

Figures 10A and 10B are pictures similarly captured by SEM-FIB microscopy. Fig. 10A shows a tastant before being processed by a method or using an apparatus according to a further embodiment of the present teachings; whereas Fig. 10B shows the same tastant after being processed thereby. In this particular case, the tastant is fed to the nip as a solution.

Figures 11 A and 1 IB are pictures similarly captured by SEM-FIB microscopy. Fig. 11 A, which is identical to Fig. 10A, shows a tastant before being processed by a method or using an apparatus according to another further embodiment of the present teachings; whereas Fig. 1 IB shows the same tastant after being processed thereby. In this particular case, the tastant is fed to the nip as a dispersion in a liquid in which it can be soluble at a lower concentration. Figures 12A and 12B are pictures similarly captured by SEM-FIB microscopy. Fig. 12A, which is identical to Figs. 10A and 11 A, shows a tastant before being processed by a method or using an apparatus according to an additional embodiment of the present teachings; whereas Fig. 12B shows the same tastant after being processed thereby. In this particular case, the material is fed to the nip as a dispersion in a liquid in which it is not soluble.

Figures 13 A and 13B are pictures similarly captured by SEM-FIB microscopy. Fig. 13 A shows a water-soluble material before being processed by a method or using an apparatus according to yet another embodiment of the present teachings; whereas Fig. 13B shows the same material after being processed thereby. In this particular case, the water-soluble material, which can be an active ingredient in various products, is fed to the nip as a solution.

Figures 14A and 14B are pictures similarly captured by SEM-FIB microscopy. Fig. 14A shows a water-insoluble material before being processed by a method or using an apparatus according to yet a further embodiment of the present teachings; whereas Fig. 14B shows the same material after being processed thereby. In this particular case, the water-insoluble material, which can be an active ingredient in various products, is fed to the nip as a dispersion.

Figures 15A and 15B are pictures similarly captured by SEM-FIB microscopy. Fig. 15 A shows a water-insoluble material before being processed by a method or using an apparatus according to the present teachings; whereas Fig. 15B shows the same material after being processed thereby. In this particular case, the material is fed to the nip as a solution in a nonaqueous solvent.

Figures 16A to 16F are pictures similarly captured by SEM-FIB microscopy. Fig. 16A to 16E show different commercially available particles of sodium chloride as conventionally prepared; whereas Fig. 16F shows flakes of the same material as prepared according to the present teachings.

DETAILED DESCRIPTION

In order to address some of the drawbacks of the prior art, the present invention seeks to modify the morphology of materials, whether inactive or active ingredients such as tastants, so as to obtain flakes thereof. The methods and apparatuses designed for this purpose can be accordingly referred to as “flaking” processes and devices.

While the disclosed invention is not limited to tastants and may similarly apply to additional water-soluble or water-insoluble materials (e.g., detergents or any other active ingredients), which may elicit different morphology-derived advantages once flaked as herein described, for simplicity of illustration, the present technology will be mainly exemplified with these particular types of materials which inter alia may improve a taste of a food product. Hence, reference in the following for brevity to tastant(s) should be understood to refer more generally to any materials that may be similarly processed as herein demonstrated in a non- limitative manner.

Before explaining at least some embodiments in detail, some general introductions shall be provided.

Water-soluble materials can dissolve (e.g., form a clear solution) in water. A water- soluble material would at least dissolve in water at a concentration of 10 g/1 (in other words, at 1 wt.% or more), the water-soluble materials used in the preparation of flakes of the present compositions being in some embodiments water-soluble by 2 wt.% or more, 4 wt.% or more, 6 wt.% or more, 8 wt.% or more, or 10 wt.% or more. Water-solubility is typically assessed at room temperature (between 20°C and 25°C), but a material suitable for the present method may alternatively, or additionally, be water-soluble at an elevated temperature (e.g., at which flaking may be performed). While solubility is often referring to water, similar rules may apply to the solubility of a material in any other solvent of interest and similar rules may apply. Solubility (or lack thereof) in any liquid can be assessed by the naked eye, a composition in which a material is soluble at a particular concentration (and/or at a particular temperature) being typically clear, while an insoluble material would form a turbid dispersion.

While many tastants are water-soluble materials, this is not essential for the performance of the present teachings and some ingredients known to provide a taste and including waterinsoluble constituents (e.g., cacao, coffee) can also be flaked. For avoidance of a doubt, the present method is suited for both water-soluble and water-insoluble materials, regardless of their intended use. Moreover, the materials can be either dissolved in a single phase in a liquid (forming a solution) or suspended as solids in a different phase (forming a suspension or a dispersion) for their successful flaking.

For illustration, the materials, even if water-soluble, can be flaked at a concentration higher than their solubility in an aqueous liquid carrier being considered or can be dispersed in a liquid carrier other than pure water in which they might be insoluble (/.< ., dissolve at less than 1 wt.%). In such cases, the water-soluble materials would be suspended rather than dissolved. Alternatively, the materials, even if water-insoluble, can be flaked in a liquid carrier other than pure water in which they might be soluble (/.< ., dissolve at more than 1 wt.%). In such cases, the water-insoluble materials would be dissolved rather than suspended in the liquid acting as a solvent.

The present teachings may not necessarily modify the absolute water-solubility of a material (e.g., transform a water-insoluble material into a water-soluble version of the same) but may nevertheless sufficiently improve the rate of dissolution to obtain a detectable upgrade of practical significance. For illustration, a quasi-insoluble material (e.g., dissolving in water at less than 100 ppm) may not turn highly soluble, but can progress thanks to the present teachings to become sparingly soluble. Moreover, the solubility might not be the property sought to be modified by the change in morphology of the material.

In some embodiments, the rate of dissolution of the flakes made from the flaked material is at least 20% higher than the dissolution rate of the unflaked counterpart, at least 30% higher, at least 40% higher, at least 50% higher, or at least 60% higher. The improvement in the rate of dissolution between an unflaked and a flaked version of the same material can also be in some embodiments of 2-fold or more, 3-fold or more, 4-fold or more, 5-fold or more, or 6-fold or more. In particular embodiments, the improvement in rate of dissolution conveyed by the implementation of the present method can be measured in order of magnitude and be of 10-fold or more.

While the materials have been characterized by their solubility in water (or lack thereof), this need not be the only liquid of relevance to the assessment of the improved rate of dissolution. For illustration, if the material is to be used in a manufacturing process in which the intended liquid of the reaction is an alcohol, then the improvement in dissolution rate can be assessed in said alcohol. Furthermore, the liquid of interest for the sake of dissolution assessment can be a blend of liquids and/or a liquid supplemented with any agent of relevance (e.g., a pH modifying agent) to the conditions under which solubilization would be sought. The rate of dissolution of a material can be assessed by routine experimentation using standard methods, known to skilled persons.

As the rate of dissolution can be assessed by the time it takes (e.g., in seconds) to dissolve a predetermined amount of material (e.g., 100 mg) in a particular volume (e.g., 100 ml) of the liquid of interest at any pertinent temperature and/or pressure, under any particular agitation conditions, and/or in any equipment adapted for such measurements, an increase in the rate of dissolution corresponds to a decrease in the time needed to achieve complete solubilization of the tested sample under test conditions. For illustration, if flaked material is said to have a rate of dissolution 2-fold higher than its an unflaked precursor, it corresponds to the duration of time necessary for full dissolution being halved under similar test conditions.

Due to their size and morphology, traditionally prepared tastants only partially dissolve in the mouth during consumption so that a major portion of the tastant is swallowed without contributing to the perceived taste of the product. Without wishing to be bound by any particular theory, it is believed that the morphology according to the present teachings facilitates the dissolution of the tastants, accordingly increasing the taste that would be perceived, as compared to a same amount of a less soluble counterpart of the tastant. In other words, for a similar taste, flavor intensity and duration of perception of the taste, a tastant having a morphology according to the present teachings would be required in a lesser amount than the same tastant having a conventional morphology.

While tastants can be conventionally provided in a variety of forms, shapes and dimensions, they are traditionally available as small granules which can have a grain size of 2- 5 mm, or even up to about 10 mm if coarse and/or flaky, the grains being typically in the range of 1-2 mm, some tastants being available as fine powders of 0.2-1 mm, or even less for particular applications (e.g., sugar powder). Some tastants, for which reduced consumption is sufficiently critical to afford substantive research, have been developed to even be in the micrometer (pm) range, generally having at least one dimension greater than 20 pm, greater than 30 pm, or greater than 40 pm. Many of them have remained of anecdotal interest, since such exceedingly small particles do not generally readily flow and cannot be applied using conventionally available equipment. Materials, other than tastants can exist as much larger pellets in the range of centimeters (cm), or as small granules in the range of a few millimeters (mm) which can have a grain size of up to 10 mm. Yet, for the implementation of the method, it might be advantageous to use elements of reduced sizes, as starting materials.

The dimensions of particles (e.g. , before or after being processed as herein disclosed) may be estimated by scanning electron microscope (SEM), transmission electron microscope (TEM) focused ion beam (FIB), by confocal laser scanning microscopy techniques, and/or by light microscopy. For instance, light microscopy can be used for particles of several microns or down to estimated dimensions of about 200 nm, scanning electron microscopy may be used for assessment of planar dimensions for particles having dimensions of less than 200 nm, while thickness or length of particles can be determined by focused ion beam FIB technique. Such dimensions can be assessed, for instance, by image analysis of at least one instrumental field of view obtained by suitable microscopic technique and magnification, and the microscopic measurements being repeated on several particles to gain statistical significance, the representative particles being in one or more fields of view. Certain microscopes incorporate image analyser able to readily provide metrics of relevance to the population of particles captured in the relevant field of view. Depending on the microscopy technique, the magnification and the size of the particles under investigation, a field of view may include at least 5 particles, at least 10 particles, or at least 20 particles; and optionally, at most 200 particles, or at most 100 particles, or at most 50 particles. In some embodiments, a field of view includes a number of particles within a range of 5 to 200, 10 to 100 or 20 to 50. In some embodiments, two or more distinct fields of view are being considered to reach the number of particles deemed sufficient to reasonably represent the population. As used herein, an average dimension reflects the mean value of such dimension as estimated on at least 10 particles, at least 20 particles, at least 30 particles, at least 40 particles, or at least 50 particles. Selecting a representative particle, or a group of representative particles, that may characterize with sufficient accuracy a population (e.g., by diameter, longest dimension, thickness, aspect ratio and like characterizing measures of the particles, or average values thereof) can be within the skills of a trained operator.

According to one aspect of the disclosure, there is provided a material (e.g., a tastant or any other compound having a desired activity and/or providing any manufacturing advantage) the material having the shape of a thin flake, which can be referred to herein as a flake or a tastant flake. The (tastant) flake can be defined by its thickness (or average thickness across its planar dimension; f) and by its longest dimension (Z) in the plane, and further characterized by a dimensionless aspect ratio between the two (Asp=L/t). Taking tastants as one example of active ingredients contributing to an efficacy of an end-product (e.g., the taste of a food product), in clear contrast with conventional tastants, the present flakes have at least their thickness being in the low micrometer range (e.g., being thinner than 200 pm), the thickness of the tastant flakes being optionally in the submicron range (e.g., being thinner than 1 pm), or in the nanometer (nm) range (e.g., being thinner than 200 nm, 150 nm or 100 nm). Flakes (of tastant) having an average thickness between 1 and 200 pm can also be referred to as (tastant) micro flakes, flakes (of tastant) having an average thickness between 0.2 and 1 pm can also be referred to as (tastant) sub-micro flakes, and flakes (of tastant) having an average thickness smaller than 0.2 pm can also be referred to as (tastant) nano flakes.

In some embodiments, the average thickness t of the (e.g., tastant) flakes is at most 200 pm, 175 pm, 150 pm, 125 pm, 100 pm, 90 pm, 80 pm, 70 pm, 60 pm, 50 pm, 40 pm, or 30 pm. In some embodiments, the average thickness t of the flakes is at most 20 pm, 18 pm, 16 pm, 14 pm, 12 pm, or 10 pm. In some embodiments, the average thickness t of the flakes is at most 9 pm, 8 gm, 7 gm, 6 gm, 5 gm, 4 gm, 3 gm, or 2 gm. In some embodiments, the average thickness t of the flakes is at most 1 gm, 0.9 gm, 0.8 gm, 0.7 gm, 0.6 gm, 0.5 gm, 0.4 gm, or 0.3 pm.

In some embodiments, the average thickness t of the (e.g., tastant) flakes is at least 50 nm, at least 100 nm, at least 150 nm, or at least 175 nm.

In some embodiments, the average thickness of the (e.g., tastant) flakes t is between 50 nm and 200 gm, between 50 nm and 150 gm, between 50 nm and 100 gm, between 50 nm and 50 pm, between 50 nm and 20 gm, between 100 nm and 18 gm, between 100 nm and 16 gm, between 150 nm and 14 gm, between 150 nm and 12 gm, between 200 nm and 10 gm, between 200 nm and 5 gm, between 100 nm and 4 gm, between 100 nm and 2 gm, or between 100 nm and 1 pm.

In some embodiments, the longest planar dimension of the (e.g., tastant) flakes L is on average at most 10,000 pm, at most 7,500 pm, at most 5,000 pm, at most 4,500 pm, at most 3,000 pm, at most 2,500 pm, at most 2,000 pm, at most 1,500 pm, at most 1,000 pm, at most 500 pm, at most 400 pm, at most 300 pm, at most 200 pm, at most 100 pm, or at most 50 pm.

In some embodiments, the longest planar dimension of the (e.g., tastant) flakes L is on average at least 5 pm, at least 7.5 pm, at least 10 pm, at least 12.5 pm, or at least 15 pm.

In some embodiments, the longest planar dimension of the (e.g., tastant) flakes L is on average between 5 pm and 10,000 pm, between 5 pm and 7,500 pm, between 5 pm and 5,000 pm, between 5 pm and 500 pm, between 7,5 pm and 4,000 pm, between 7.5 pm and 300 pm, between 10 pm and 2,000 pm, between 10 pm and 1,000 pm, between 10 pm and 200 pm, or between 10 pm and 100 pm.

The ranges each of the thickness and the longest planar dimension the present flakes may respectively fall in are generally correlated, so that they may additionally, or alternatively, be characterized by their relationship, as can be determined by calculating a dimensionless aspect ratio between the two. In some embodiments, the aspect ratio between the longest planar dimension of (e.g., tastant) flakes and their thickness (Asp= L/f) is on average at least 5, at least 10, at least 15, at least 20, at least 25, at least 30, at least 35, at least 40, at least 45, or at least 50. In some embodiments, the aspect ratio Asp is on average at most 200, at most 150, at most 125, at most 100, or at most 75. In some embodiments, the aspect ratio Asp is on average between 5 and 200, between 5 and 150, between 10 and 100, between 10 and 50, between 50 and 150, or between 20 and 75.

As shall be further detailed hereinbelow, the present method and apparatus allow controlling to some extent the dimensions of the flakes to be obtained thereby. While usually the majority of the flakes have the afore-said sizes and aspect ratios, conforming to the specified ranges, in some embodiments it may be desired to achieve distinct values (e.g., narrower size distribution) as may be sought for particular intended uses. In such a case, the flakes originally obtained can be further classified by a suitable separation step or device (e.g., sieves) into subpopulations, each having sizes conforming or not the desirable ranges. In such a case, the non-conforming particles can be, if so desired, recycled back into the process (e.g., dissolved or dispersed to be part of a liquid stock to be subsequently applied). Such a recycling can be performed at a post-flaking station, following the collection of the flakes and their desirable sorting.

Advantageously, tastant flakes having the afore-mentioned dimensions are expected to display good blendability in the food products, good adherence to food surfaces (and in turn more uniform coverage of the surface) and less dusting problems than their conventional counterparts. The foregoing may be considered manufacturing advantages of the flakes, this terminology additionally encompassing steps preceding and/or following (e.g., storage, transportation, packaging, etc.) actual manufacturing of a product. The dimensions they can be prepared at might also be elected to provide a desired texture (e.g. , crunchy) or appearance (e.g. , visual aspect of toppings), or any other benefit depending on the size of the flakes and the properties (e.g., rate of dissolution) derivable therefrom. Such effects, more directly linked to the activity expected from the tastant or flakes thereof in the first place may be considered efficiency advantages, the usefulness of tastant flakes encompassing in some cases both types of advantages which are not mutually exclusive.

As the tastant flakes have a higher specific surface area than their standard counterparts they can dissolve faster, providing a more intense taste for a same amount of tastant or a same taste with a lower amount, allowing to reduce the contents of the tastant in the food product. The food product can have any conventional consistency and be, for instance, a liquid, a semisolid (e.g., a spread, a paste, a gel) or a solid at their usual temperature of storage or use. The tastant flakes can be either apposed on external surfaces of the food product (e.g., salt on snacks, sugar on cereals, spices on biscuits or croutons), dispersed therein, or both. When the tastant flakes are due to remain dispersed in the food product until its consumption, the tastant is usually made of a material having poor solubility or being insoluble in the food product. For instance, a water-soluble tastant (e.g., salt) can be dispersed as flakes into a hydrophobic liquid (e.g., an oil), a semi-solid emulsion (e.g., a mayonnaise or oil-containing sauce) or any product relatively solid under normal storage conditions (e.g., butter). Similar considerations regarding relative viscosity of the product and localization of the flakes on and/or in said products apply to any other goods that may benefit from the presence of flakes prepared as herein taught.

Having a higher specific surface area may not only accelerate the rate of dissolution of any specific material in any particular liquid, but may also increase any other desirable interactions between molecules. Taking chemical reactions as an example, and materials serving as catalysts in such reactions, catalysts having a relatively higher surface area are expected to stimulate more swiftly the rate of the chemical reaction they usually promote than their counterparts having a relatively smaller surface area.

The tastant flakes are capable of imparting a sweet, salty, sour, bitter or umami taste and can be made of any tastant known or being developed to provide such tastes, or of their combinations. In some embodiments the tastant flakes comprise one or more of acetic acid, citric acid, lactic acid, malic acid, ascorbic acid, tartaric acid, succinic acid, hydrochloric acid, phosphoric acid, sulphuric acid, sucrose, arabinose, ribose, xylose, glucose, galactose, mannose, fructose, lactose, maltose, raffinose, stachyose, sucralose, trehalose, glycerol, erythritol arabitol, xylitol, sorbitol, mannitol, lactitol, malitol, corn syrups, aspartame, low molecular weight maltodextrins, bitter peptides, amino acids, alkaloids, amides, thioureas, polyphenols, sodium bicarbonate, monosodium glutamate, disodium 5’-inosate, and disodium 5’-guanylate, sodium chloride, iodized sodium chloride, calcium chloride, potassium chloride, iodized potassium chloride, or mixtures thereof; the foregoing list being exemplary of materials capable of providing a taste and non-limitative.

As the present approach does not rely on the presence of taste modulating compounds to alter the perception of the taste provided by a tastant, the tastant flakes (which can consist of a pure compound or a blend of natural tastants) are devoid of aftertaste. This may also increase compliance with customers seeking clean alternatives as close as possible to their natural source of tastants. This would certainly be the case when the tastant flakes are made of a single material (e.g., salt).

But tastants are only provided as examples and additional materials can be flaked as herein taught. Such materials are generally selected in view of the efficacy they may provide to a product comprising them or consisting of these materials, the flakes enabled by the present teachings providing an improvement over the traditional shapes (e.g., increasing efficacy (optionally allowing to reduce a presence of the material required to obtain a specific effect), facilitating manufacturing, reducing the costs, etc.). When the materials contribute to or generate the chemical, physical and/or biological effect of the manufactured article, they can generally be defined as “active ingredients”, catalysts, reinforcing materials and active pharmaceutical ingredients being respective examples of such effects. However, as the improvement provided by the flaked material is not limited to the chemical, physical and/or biological effect they may at least contribute to, “inactive ingredients” which may “just” ease in any way the manufacturing of the article are also encompassed. Inactive ingredients may be said to provide a manufacturing advantage, this terminology including all technical aspects of steps preceding or following manufacturing. The efficacy of active ingredients prepared according to the present teachings pertains at least to the usually desired effectiveness of the ingredients as-is or in its end products but optionally further includes a manufacturing advantage.

Suitable materials (active or inactive ingredients) can be water-soluble or water-insoluble, organic (e.g., plastics or other non-polar compounds) or inorganic (e.g., ceramics, minerals, metal -based, etc.) and be found in a variety of chemical families serving a wide range of industries.

Water-soluble materials other than tastants, or used in context other than providing a taste or otherwise improving an ingested product, include, for instance, sodium chloride (NaCl), which is commonly known as table salt as used in food seasoning, can also be used as a deicing agent, a reagent or a catalyst in the manufacturing of chemicals. A non-limiting list of water- soluble materials include for illustration: Ammonium nitrate (NH4NO3) which can be used on fertilizers, as an explosive, and in the production of nitric acid; Calcium carbonate (CaCCh) which can be used as a dietary supplement in human and animal food, as an antacid both in medicine and more agricultural/industrial settings, as a filler in the production of adhesives, sealants, paints, coatings, papers and plastics, and in the manufacturing of cement and concrete; Calcium chloride (CaCh) which in addition to its uses in food processing can be used as a deicing agent and in the production of cement and concrete; Copper sulfate (CuSCh) which can be used as a algaecide, bactericide, fungicide, herbicide, molluscicide and root killer, in addition to being a catalyst; Ferric chloride (FeCh) which can be used to treat sewage, industrial waste, to purify water, as an etching agent for engraving circuit boards, and in the manufacture of other chemicals; Magnesium sulfate (MgSCh) which can be used in agriculture as a fertilizer, in medicine as a laxative, in the production of paper and textiles, and as a catalyst; Manganese sulfate (MnSO₄) which can be used as a fertilizer and as livestock supplement where soils are deficient in manganese, then in some glazes, varnishes, ceramics, and fungicides; Nicotine salt which can be used in smoking replacement products (e.g., e-cigarettes or vaping devices) or in pharmaceutical product targeting nicotine-specific withdrawal symptoms; Potassium chloride (KC1) which can be used as a fertilizer and in the manufacturing of potassium hydroxide (KOH) itself used in the production of soaps and detergents; Potassium hydroxide which in addition to its uses as a pH adjuster in food processing can be used in the manufacturing of soap and detergents and in the production of biodiesel; Potassium iodide (KI) which can be used as dietary supplement, as a medication for treating hyperthyroidism, in radiation emergencies, and for protecting the thyroid gland when certain types of radiopharmaceuticals are used, and as a catalyst; Potassium nitrate (KNO3) which in addition to its uses in food preservation can be used in fertilizers and in the manufacturing of gunpowder; Sodium bicarbonate (NaHCOs) which in addition to its uses in food processing can be used in medicine as antacid, or combined with organic acids such as citric and tartaric acid to provide the effervescent effect to active pharmaceutical ingredients, and in fire extinguishers; Sodium hydroxide (NaOH) which can be used in the manufacturing of soap and detergents, as a drain cleaner and in the production of paper; and Zinc chloride (ZnCl₂) which can be used in dry cells as an electrolyte, as a catalyst, a condensing agent, a dehydrating agent, a deodorant, a disinfectant, or a wood preservative.

Water-insoluble materials which may benefit from the present method comprise carbonates, phosphates, sulfides, and oxides, said chemical families also including relatively soluble exceptions being known or readily ascertainable. Taking, for illustration, materials including a metal such as calcium, then Calcium carbonate (CaCO₃), Calcium phosphate (Ca₃(PO₄)₂), Calcium sulfate (CaSO₄), Bone meal ((Ca(PO₄)2)₃CaF₂), Rock phosphate (Ca₃(PO₄)2CaF2), and other such phosphate minerals can be cited as water-insoluble materials of widespread uses. Other common water-insoluble materials include Barium carbonate (BaCO₃), Barium sulfate (BaSO₄), Copper carbonate (CuCO₃), Iron oxide (Fe2O₃), Lead chromate (PbCrO₄), Lead chloride (PbCL), Lead sulfate (PbSO₄), Silicon dioxide (SiO₂), Silver chloride (AgCl), Magnesium hydroxide (Mg(0H)₂), Magnesium stearate (Mg/CixHxsOi)?) and Zinc oxide (ZnO).

As readily appreciated from the foregoing non-exhaustive list of exemplary materials, many are salts which exist in various forms of hydrates and/or crystals, some forms having different roles, but all supporting that a wide variety of industries may benefit from the present teachings and all forms being encompassed as materials (e.g., active ingredients) adapted to the present flaking method.

Regardless of the types of materials constituting the flakes, they can be considered as made of a pure material, if this material constitutes at least 95% of the flakes by weight, the degree of purity as assessed by weight contents being advantageously of at least 96 wt.%, at least 97 wt.%, at least 98 wt.%, at least 99 wt.%, or at least 99.5 wt.%. The purity of the material (or of a blend of materials) in the flakes can be determined by any analytical method adapted to measure a definite property (e.g., elemental composition, physico-chemical property, etc.) of the material(s) under consideration.

As already mentioned, the present method is suitable for the preparation of flakes constituted of two or more materials. This can be advantageous when the materials of the blend can additionally or synergistically act one with the others(s) when in close proximity, and/or when the effect sought from the materials may benefit from their overall distribution being relatively uniform. Taking for illustration a food product to be coated with different flakes, each type of flakes providing a distinct savor (e.g., salt and pepper), if the flakes are not distributed relatively evenly on the surface of the food product, a subject eating the food may perceive different tastes in different regions (e.g., bites) of the product. Though not essential for all products, in some cases it can be beneficial to have flakes made of two or more materials to impart an even effect (e.g., a similar taste profile, aroma, color etc.) to each portion of the (e.g., food) product to which it is applied or in which it is incorporated.

By way of non-limiting example, if one of the materials is a tastant (e.g., a salt such as sodium chloride or a sugar such as sucrose), the additional materials that can be combined therewith in flakes prepared according to the present teachings can be selected from a group comprising flavoring agents, seasoning agents, aroma agents, spices (e.g., basil, cardamom, chili, cinnamon, coriander, cumin, garlic, ginger, nutmeg, oregano, paprika, pepper, rosemary, sage, thyme, turmeric, etc.), extracts, coloring agents, masking agents, enhancing agents, nutrients, minerals, vitamins, emulsifying agents, stabilizing agents, anti-caking agents, dietary supplements, antioxidants, and combinations thereof. One material may serve as carrier to the other.

In some embodiments, the (e.g., tastant) flakes have a specific surface area of at least 0.001 m²/g, at least 0.005 m²/g, at least 0.01 m²/g, at least 0.05 m²/g, at least 0.1 m²/g, at least 0.2 m²/g, at least 0.3 m²/g, at least 0.4 m²/g, or at least 0.5 m²/g. Generally, the tastant flakes have a specific surface area not exceeding 10 m²/g, their specific surface area being usually of at most 8 m²/g, at most 6 m²/g, at most 4 m²/g, or at most 2 m²/g. Thus, in some cases, the specific surface area of the present flakes is between 0.001 m²/g and 10 m²/g, between 0.01 m²/g and 8 m²/g, between 0.1 m²/g and 6 m²/g, between 0.2 m²/g and 4 m²/g, or between 0.5 m²/g and 2 m²/g.

For reference, materials (e.g., tastants) having a same density but a granular shape which could be approximated to a sphere, and having an average diameter of 50 pm, might have a specific surface area of no more than about 0.2 m²/g. The surface area of a material can be routinely determined by any suitable method, such as by nitrogen sorption as can be analyzed by the Brunauer-Emmett-Teller (BET) or Langmuir procedures, in any adequate instrument, and the specific surface area calculated based on the weight of the measured sample.

The (e.g., tastant) flakes may additionally, or alternatively, be characterized in that their bulk density (/>«), also referred to as their apparent density, /.< ., the ratio of the mass to the bulk volume (Eg) of an untapped (hence, including interparticulate void volume) powder sample, is relatively lower than the bulk density of their standard counterparts. In other words, for a same volume of tastant particles (e.g. , a tablespoon), the weight of tastant would be relatively reduced when the tastant is flaked as herein disclosed. If the taste provided to the food product is not compromised by the reduced bulk density, this allows to diminish the weight contents of the tastant accordingly. However, if a taste to be provided by the tastant flakes is affected by the reduction in bulk density, the reduction in weight of tastant being added to the food product would no longer be analogous to the decrease in bulk density, as additional volume of tastant would probably be added to compensate for the initial “weight loss” induced taste impairment.

In some embodiments, the bulk density of the (e.g, tastant) flakes is at least 20% lower than the bulk density of the standard counterpart, at least 30% lower, at least 40% lower, or at least 50% lower. Taking table salt for illustration, standard granulated salt typically has a bulk density of about 1.25 g/cm³, in which case the reduced bulk densities of tastant flakes would be of at most 1.00 g/cm³ (80% of 1.25 g/cm³), at most 0.88 g/cm³, at most 0.75 g/cm³, or at most 0.62 g/cm³. Bulk density of tastant flakes can be even lower, if desired, such as being of at most 0.50 g/cm³, at most 0.40 g/cm³, or at most 0.30 g/cm³, but it generally needs not being lower than 1% or even 5% of the original bulk density of the conventional tastant. Thus, in some embodiments, the bulk density of the tastant flakes is between 0.01 g/cm³ and 1.00 g/cm³, between 0.01 g/cm³ and 0.80 g/cm³, between 0.05 g/cm³ and 0.50 g/cm³, between 0.10 g/cm³ and 0.75 g/cm³, between 0.10 g/cm³ and 0.70 g/cm³, between 0.05 g/cm³ and 0.65 g/cm³, or between 0.20 g/cm³ and 0.62 g/cm³. The apparent bulk density of a particulated matter can be assessed by routine experimentation using standard methods, such as described in ASTM B527. When the (e.g., tastant) flakes are to be mixed with other dry powders (e.g., other flakes) for their intended use, it may be advantageous for all powders being mixed to have a relatively similar bulk density so as to reduce the separation of the powders and maintain a homogenous mix. The bulk density would be considered relatively similar, if the bulk density of an individual component of the mixture were within 20% deviation from the bulk density of the mixture.

The (e.g., tastant) flakes may additionally, or alternatively, be characterized in that their tap density (pi) is relatively lower than the tap density of their standard counterparts. In contrast with the bulk density, the measurement of the tap density involves tapping of the sample to reduce interparticulate voids and assess the packing ability of the powder. For a defined mass of powder, the bulk density is calculated by measuring the bulk volume VB occupied by the mass of the powder whereas the tap density is calculated by measuring the tapped VT volume typically shrank by the rearrangement of the powder during the application of tapping. Usually, unless the powder is perfectly free flowing, the tap density of a powder is higher than its bulk density but the differences between the two values depend on the intrinsic properties of the particles (e.g., size, shape, porosity, etc.), on the particle size distribution (e.g., homogeneity, ability to segregate, etc.) and on inter particle interactions, as may also result from their environment (e.g., moisture, temperature, etc.).

In some embodiments, the tap density of the (e.g., tastant) flakes is at least 20% lower than the tap density of the standard counterpart, at least 30% lower, at least 40% lower, or at least 50% lower, but it generally needs not being lower than 5% of the original tap density of the conventional material. Taking a tastant and specifically salt for illustration, standard granulated salt typically has a tapped density of about 1.45 g/cm³, in which case the reduced tapped densities of tastant flakes would be of at most 1.16 g/cm³ (80% of 1.45 g/cm³), at most 1.02 g/cm³, at most 0.87 g/cm³, or at most 0.73 g/cm³. Tapped density of tastant flakes can be even lower, if desired, such as being of at most 0.50 g/cm³, at most 0.40 g/cm³, or at most 0.30 g/cm³, but it generally needs not being lower than 5% of the original tap density of the conventional tastant. Thus, in some embodiments, the tap density of the tastant flakes is between 0.07 g/cm³ and 1.02 g/cm³, between 0.07 g/cm³ and 0.87 g/cm³, between 0.10 g/cm³ and 0.73 g/cm³, between 0.07 g/cm³ and 0.50 g/cm³, or between 0.20 g/cm³ and 0.73 g/cm³.

A relatively low bulk and/or tap density, as can be displayed by the present tastant flakes, is deemed advantageous, in particular when the tastant is to be applied to the surface of dry snack foods, such as crisps or nuts. For such foods, the conventionally applied tastants generally suffer from relatively high lost during processing due to their relatively poor adhesion and/or their relatively high tendency to detach and fall off the food product by the time it is to be consumed. Such phenomenon leads to unnecessary wastage of the tastant.

While having a tastant shaped as a flake may by itself increase the likelihood of sufficient contact to promote adhesion during the application of the tastant to the food product, as compared to a more granular form of the tastant, this is but a first requirement. The tastant flakes should also remain on the product, during the remaining processing steps, and any subsequent handling of the food product such as its packaging, transport and storage. It has been reported that tastants having a relatively lower bulk density are less prone to detach from the food surface than tastants having a relatively higher bulk density. This can be explained in part by the fact that particles having a lower bulk density and accordingly a smaller mass are less affected by gravity than particles having a higher bulk density / larger mass, thus such tastant flakes could better maintain their adhesion to the food product until it is ingested.

In some cases, the dimensions of the flakes and their relatively high aspect ratio as compared to conventional products provide for a relatively higher compressibility of the particles which can facilitate their packaging, storage or transport. The compressibility of the flakes can be determined by calculating a unit-less ratio between the density of the particles after and before compression. This ratio may further serve to assess the correlation between the aspect ratio of the flakes and their compressibility. Such factors (e.g., F5 and F6) and measurements made to estimate them can, for instance, be determined as illustrated in Example 10 hereinbelow, which also provides ranges of values that may, alone or in combination with other features, characterize the present flakes.

In some embodiments, the (e.g., tastant) flakes may be made of a water-soluble or waterinsoluble material having a crystalline structure. In such a case, the flakes may, for some materials, be additionally, or alternatively, characterized by a particular crystallographic structure as detectable by X-ray diffraction (XRD), the XRD detectable structure being selected from a group consisting of a position of a diffraction peak, a relative intensity of a diffraction peak at a particular position, a ratio between any two diffraction peaks at two particular positions, a diffraction peak width, a crystallite size, a microstrain value and a dislocation density at any particular diffraction peak or over the spectrum of scanning, and like parameters indicative of a crystallographic structure.

In some embodiments, at least one of the afore-said crystallographic parameters as measurable by XRD or other suitable method on the (e.g., tastant) flakes diverge by at least 20% as compared to the same parameter as measured in the reference (e.g., unflaked or alternatively prepared) crystalline material. In some cases, the value of the parameter measured in the flakes can be diverging by being at least 20% lower or at least 20% higher than the same parameter as measured in the standardly grown / prepared crystal. In some embodiments, at least one of these crystallographic parameters as measurable on the flakes diverge by at least 30%, by at least 40%, or by at least 50%, as compared to a corresponding parameter in a reference standard unflaked crystal. For some crystallographic parameters, the difference between a measurement made in the flakes as compared to a measurement made in the relevant reference crystal can even be of at least 2-fold, at least 3 -fold, or at least 4-fold.

For illustration, crystallite size and microstrain values, which can be indicative of relatively high compression perceived during the crystal growth and the compaction and agglomeration of the precipitated material(s) by passage(s) through the nip(s) can be respectively at least 2-fold smaller or 2-fold larger in tastant flakes made of salt, as compared to standard salt.

An XRD structure detectable in the original unflaked material (e.g., tastant) before being processed according to the present method and/or using an apparatus as herein taught, can be referred to as an XRD detectable first structure, whereas a corresponding structure detectable in the (e.g., tastant) flakes following their preparation may be referred to as an XRD detectable second structure. The structures in the (e.g., unflaked) original material and the flaked version of the same are deemed corresponding if relating to a similar parameter as analyzed at about a similar position or along a similar spectrum span, since understandingly a modification in the crystallographic structure of a crystalline material as may occur in some embodiments, may in itself cause minor shifts in the diffraction peaks. Thus, corresponding structures need not be identical but the parameters being asserted should in essence be of the same kind.

While in the foregoing the (e.g., tastant) flakes have been characterized by one parameter at a time, such as by i) their thickness, ii) their length, iii) their aspect ratio, iv) their specific surface area, v) their bulk density, their tap density, or any ratios between the two densities, or vi) any crystallographic specification adapted to a material, if crystalline, the skilled persons can readily appreciate that flakes, as can be produced by the present method, may be characterized by any combination of two or more of these parameters. For illustration, a tastant flake may have both a bulk density and a crystallographic behavior as herein disclosed. In some embodiments, the tastant flakes displaying the afore-said characteristic parameters are furthermore made of a pure tastant (e.g., constituting more than 95 wt.% of the flakes). For example, tastant flakes according to the present teachings can be a) made of a pure salt, such as containing more than 95 wt.% of sodium chloride for instance; b) having a relatively low bulk density not exceeding 0.60 g/cm³, being optionally of at most 0.55 g/cm³, at most 0.50 g/cm³, at most 0.45 g/cm³, at most 0.40 g/cm³, at most 0.35 g/cm³, at most 0.30 g/cm³, at most 0.25 g/cm³, at most 0.20 g/cm³, at most 0.15 g/cm³, or at most 0.10 g/cm³; and c) having an XRD detectable structure being at least one of i) a microstrain value of at least 0.050%, at least 0.075%, at least 0.100%, at least 0.125%, at least 0.150%, or at least 0.175%; and ii) a crystallite size of at most 1,000 Angstroms (A), at most 750 A, at most 625 A, or at most 500 A.

When the term salt is used herein to refer to sodium chloride, the raw materials that can be used for the preparation of salt flakes include all sources of salt available, whether naturally obtainable (e.g., sea salt, ocean salt, mineral salt, etc.) or further processed (e.g., smoked salt, flavored salt, supplemented salt such as iodized salt, etc.) and the flakes made therefrom can have similar denominations.

The present flakes can be characterized by additional features, which in turn may serve to calculate relationships between two or more structural features. The aspect ratio of a flake is but one example of how the ratio between two measurable features (longest planar dimension and thickness) can provide supplementary valuable and distinctive information. Alternative or additional calculated ratios are exemplified by factors Fl to F6 as described in Examples 7, 9 and 10.

For conciseness, only the mathematical expressions of the afore-mentioned exemplary factors are reproduced in the following paragraph. Fl is the ratio between the aspect ratio of the flakes ASP and their rate of dissolution (Z)T), which can be mathematically expressed by F1=ASP/ DT (having units of seconds'¹). F2 is a unit-less ratio between the tap density / and the bulk density pp> of the flakes, which can be mathematically expressed by F2=pr/pB. F3 is the ratio between the aspect ratio ASP of the flakes and their bulk density pp>, which can be mathematically expressed by F3=ASP/ PB (having units of cubic centimeters per gram). F4 is the ratio between the aspect ratio ASP of the flakes and their tap density pr, which can be mathematically expressed by F4=ASP/ pr (having units of cubic centimeters per gram). F5 is the ratio between the compressed density pc and the initial bulk density pp, of the flakes before being compressed, which can be mathematically expressed by F5=pc /ps. F6 is the ratio between the aspect ratio ASP of the flakes and their compressibility as estimated by 5, which can be mathematically expressed by F6=ASP /F5. As for the measurable features, the present factors may be combined amongst themselves and/or with measured features (e.g., i) thickness t, ii) longest planar dimension L, iii) specific surface area SSA, iv) dissolution rate DT, v) bulk density ps, vi) tap density pr, vii) compressed density pc, viii) any crystallographic specification, etc.) to characterize and distinguish the present flakes.

For illustration, the present flakes may have at least two, at least three, at least four, or at least five of the following features, which for conciseness are illustrated in this paragraph by only one of the various limitations they may each fulfill as set in more details hereinbelow: 1) an average thickness t not exceeding 200 pm; 2) an aspect ratio ASP of at least 10; 3) a Fl factor of at least 5; 4) a F2 factor of at least 1.25; 5) a F3 factor of at least 25; 6) a F4 factor of at least 20; 7) a F5 factor of at least 1.6; and 8) a F6 factor of at least 6.

In some embodiments, the two or more features characterizing the present flakes include above listed items 1) and 2), 2) and 3), 2) and 4), 2) and 5), 2) and 6), 2) and 7), and 2) and 8), and any of their respective limitations as described herein. In some embodiments, the three or more features include above listed items 1), 2) and 3); 2), 3) and 4); 3), 4) and 5); 3), 5) and 7);

3), 5) and 8), to name a few combinations, and any of their respective limitations as described herein. In some embodiments, the four or more features include above listed items 1), 2), 3) and

4); 2), 3), 4) and 5); 3), 4), 5) and 7); 2), 3), 5) and 7); 2), 3), 5) and 8), to name a few combinations, and any of their respective limitations as described herein.

According to another aspect of the disclosure, there is provided a method for manufacturing flakes (e.g., tastant flakes), the method comprising: a) providing a liquid stock comprising at least one solid material dissolved or dispersed in a liquid; b) applying the liquid stock to a first movable surface, so as to form thereon a thin film of liquid stock; c) cyclically i) removing at least a part of the liquid from the thin film of liquid stock, so as to increase the concentration of solid particles in the film, and ii) applying pressure to the film by passing the film through at least one nip formed by urging opposed nip-forming surfaces towards one another, so as to progressively form a layer including flakes consisting of compacted and/or agglomerated solid particles, said cycles being repeated until the flakes contain less than 5wt.% of the liquid. The flakes manufactured by said method can have an average thickness t of at most 200 pm, not exceeding the thickness of the layer, and can have in further embodiments an average aspect rati oASP between the longest planar dimension Z and the thickness t of the (e.g. , tastant) flakes of at least 10.

The values recited in the above introduction to the present method are exemplary and can be substituted by any additional ones associated herein with the feature being monitored to set the termination of the flaking method.

As used herein, the layer from which the flakes are ultimately formed need not be a continuous layer and can refer to discrete clusters of otherwise scattered particles that can be assembled and held together by any suitable force. Without wishing to be bound by any particular theory, it is believed that in the present method the particles of solid materials progressively separating from the liquid stock, as the liquid is removed, can be agglomerated by pressure agglomeration, partial sintering or fusion, and/or by build-up crystallization, depending on the materials being considered.

As agglomeration does not require a definite pattern for the gathering of the particles into a solid mass, such assembly could have assumed any shape and size, if naturally forming. As the solid particles in the present method agglomerate whilst being periodically subjected to compaction, at least the thickness of the layer once substantially dry (e.g, containing less than 5 wt.% liquid) can be (e.g, empirically) predetermined, for instance according to the size of the solid particles that may be present in the liquid stock, or progressively separate therefrom, their hardness, and the force to which they are subjected at the nip(s). As flakes can be viewed as portions of the layer initially comprising them, separated from adjacent flakes and/or from an underlying surface either progressively or upon termination, they too may be considered as agglomerates of solid particles. Since the present process also involves compaction, the particles forming a flake (or a layer from which they are separable) can be said to be agglomerated and compacted, or vice versa compacted and agglomerated, both effects probably taking place concomitantly and their order in any particular sentence not implying any particular sequence of events with respect to the particles.

As readily appreciated, layers comprising flakes constituted of agglomerated and compacted particles need not be one particle thick, the number of strata of particles stacked one on the other depending on the material and the operating conditions. Taking, for illustration, crystals of solid materials capable of progressively separating from a liquid stock, an agglomerated layer of crystals can be formed of a plurality of crystals adjacent to one another in all three dimensions.

It is appreciated that while two cylinders urged into contact (e.g., by pneumatic or hydraulic pistons, the latter optionally including an accumulator which can be a spring loaded or a gas loaded accumulator compensating for the lack of compressibility of the hydraulic fluid to provide some spring-like behavior to the piston) are due to be at an essentially null distance one from the other (e.g., 1 pm or less) in absence of any material fed to the nip, this spacing may increase in the presence of the material. The extent of actual spacing between the two cylinders at the nip therebetween may depend upon the volume and/or size of the material being fed, its concentration, the speed of rotation, the pressure applied to achieve contact, the time having passed since initial application and like factors. In some embodiments, the initial spacing at a nip formed between two rotating cylinders upon application of the material to be flaked can be of up to 400 pm, up to 300 pm, up to 200 pm, up to 100 pm, up to 80 pm, up to 60 pm, up to 40 pm, up to 20 pm, up to 10 pm, or up to 5 pm, this distance being required to gradually decrease as the liquid is removed whilst the cylinders are urged into contact in presence of the material being flaked (e.g., the concentration of solid particles increasing, allowing for the agglomeration and compaction of said particles into flakes).

The dynamic adjustment of the gap dimensions at the nip in response to the process conditions and the degree of completion of each of its steps or cycles is naturally taking place as the flaking proceeds, no dedicated device being used to controllably directly adjust nip spacing (e.g., by fixing the cylinders at a predetermined distance one from the other). The cyclical closing of the gap as the material in the liquid stock is being flaked (and the liquid removed) and its widening as new liquid stock is presented to the nip is therefore viewed as a spontaneous springlike process, and the nip or the gap between the nip-forming surfaces facing one another at the nip can be called “dynamic” to reflect this continuous phenomenon.

If a hydraulic system is employed to urge the cylinders into contact, it may include an accumulator to provide the desired spacing variations in absence or presence of a material being thinned. Rotating cylinders being transiently separated at the nip by no more than 400 pm at the beginning of the process are deemed urged into contact one with the other, even if said “contact” is mediated by the presence of the material or liquid stock therebetween.

Dry flakes that can be obtained from such initial nip gaps are thinner, usually having at most the thickness corresponding to the solid content of the liquid stock being applied and being sometimes thinner. Considering for illustration a stock solution comprising 25 wt.% of sodium chloride, the operating conditions being such that the initial spacing between the cylinders urged to contact at the nip is 400 pm, then the resulting flakes would have at most a thickness of about 100 pm.

In some embodiments, the recycling of the material being progressively thinned into collectible flakes, is to the same nip to which the material was first fed. In other embodiments, the recycling can be to one or more nips different from the nip of first feeding, which may be called the first nip. While in case of multiple nips, each nip may be constituted of a pair of cylinders having no contact with any of the cylinders of another nip, it may be preferred in some embodiments to have the multiple nips sharing common cylinders. The rotating cylinders of each nip, and a fortiori of different nips, need not be the same. While for efficiency they typically have a similar axial length, they may have different diameters, and/or be made of different matters, and/or be coated with different substances, and/or be heated or cooled to different temperatures, etc.

In one embodiment, the material (e.g., tastant) is provided in dry parti culated form. While this method is appropriate for any tastant existing in dry form (e.g., plant spices derived from roots, stems, bark, leaves, flowers, or seeds) it is particularly indicated for tastants which cannot be dispersed or dissolved in a medium from which they might be efficiently isolated with relative ease. This “dry method” typically enables an at least 5-fold thinning of the tastant from an initial dimension (e.g., diameter, edge, thickness) to its final thickness, following an ultimate recycling of the thinned tastant through the nip. This method is generally suitable for the preparation of micro flakes.

In one embodiment, the material (e.g., tastant) is provided as a relatively viscous paste (e.g., having a dynamic viscosity of more than 5,000 milliPascal-seconds (mPa.s) at room temperature circa 23°C). The viscosity of the paste can be achieved by dispersing a relatively high quantity of tastant in a relatively low quantity of liquid, and/or by using a liquid relatively viscous by itself. The dispersing medium should preferably be compatible with the material to be flaked (e.g., if a tastant, not affecting its taste), and if necessary or desired, it should be separatable therefrom. The dispersing medium, which can itself be relatively viscous, can be selected in accordance with a future use of the (e.g., tastant) flakes. For instance, the tastant can be cacao and the viscous medium cacao butter (both water-insoluble) or sugar and molasses (both water-soluble), at least one of the rotating cylinders being optionally heated or cooled to maintain a desired viscosity to the paste. This example is non-limiting and the dispersing (e.g., viscous) medium need not be of a similar source or type as the tastant. This “paste method” typically enables an at least 10-fold thinning of the tastant from an initial dimension (before forming the paste) to its final thickness, following an ultimate recycling of the thinned tastant through the nip. This method is generally suitable for the preparation of micro flakes and submicro flakes.

A dispersing medium adapted to form with the material a relatively viscous paste can be an intrinsically viscous product, such as honey for a tastant, or be prepared by increasing the viscosity of a non-viscous liquid. Such increased viscosity allowing the paste to display a dynamic viscosity of at least 5,000 mPa.s at room temperature can be achieved by using a relatively high amount of material (e.g., tastant) and/or by including a thickening agent in the dispersing medium. If the material to be flaked is intended to provide a taste or be used in a product to be ingested, the thickening agent should preferably be tasteless by itself and advantageously, but not necessarily, approved for food consumption, to the extent that residual amounts are not eliminated from the surface of the tastant flakes. Such thickening agents, which can be natural or synthetic, are known and can, for instance, be selected from a group comprising alginic acid (E400), sodium alginate (E401), potassium alginate (E402), ammonium alginate (E403), calcium alginate (E404), propylene glycol alginate (E405), agar (E406), carrageenan (E407), furcelleran (E408), locust bean gum (E410), oat gum (E411), guar gum (E412), tragacanth (E413), gum Arabic (E414), xanthan gum (E415), karaya gum (E416), tara gum (E417), gellan gum (E418), pectin (E440), gelatin (E441), cellulose (E460), methyl cellulose (E461), ethyl cellulose (E462), hydroxypropyl cellulose (E463), hydroxy-propyl- methyl cellulose (E464), methyl-ethyl cellulose (E465), carboxymethyl cellulose (E466), natural or modified starches (E1400 series), and combinations thereof.

In one embodiment, the material (e.g., tastant) is provided dispersed or dissolved in a liquid relatively non-viscous having at room temperature a dynamic viscosity of less than 1,000 mPa.s, less than 100 mPa.s, or less than 10 mPa.s or less (e.g., water). The liquid should be compatible with the material (e.g. , not affecting its taste, if a tastant), and if necessary or desired, it should be separatable therefrom. Tastants suitable for such a method are typically, but not necessarily, solvable in the liquid, even if fed at a concentration higher than their limit of solubility, the tastants being accordingly dispersed rather than fully dissolved in the liquid. This “liquid method” typically enables an at least 15-fold thinning of the tastant from an initial dimension (before mixing in the liquid) to its final thickness, following an ultimate recycling of the thinned tastant through the nip. This method is generally suitable for the preparation of micro flakes, sub-micro flakes and nano flakes. As mentioned, it is stressed that the selection of liquid carriers, additives thereto, matters of which parts of the apparatus are made or coated with, with respect to any material to be flaked by the present method and/or with the apparatus herein described, is guided by principles of compatibility. The materials should be chemically compatible with one another. Fundamentally, a material or a chemical composition is compatible with another (or inert with respect thereto, if so desired) if it does not prevent its activity or does not reduce it to an extent that would significantly affect the intended purpose. For instance, a liquid carrier would not be compatible if, among other things, affecting the taste of a material being a tastant intended for ingestion, or affecting the potency or reactivity of materials intended for manufacturing processes. The materials should also be physically compatible with one another. For illustration, the liquid carrier should preferably be sufficiently volatile at a temperature not affecting the material(s) to be flaked. Thus, the materials should also be compatible with the manufacturing method and its operating conditions and vice versa. For illustration, the liquid stock in which the materials to be flaked are dissolved or dispersed should not be corrosive to the surfaces to be applied thereto or the surfaces should be inert with respect to the stock and the flakes to be produced therefrom. Such general considerations shall not be further detailed herein, as known to persons skilled in the field of chemical manufacturing.

However, in some embodiments, the liquid can be selected to intentionally trigger a reaction with the material being flaked. In such a case, the chemical composition of the material before and after its flaking may differ. Hence, the term “flakes made from the material(s)” encompasses both flakes having retained the original chemical composition of the material treated by the present flaking method, as well as flakes including a modified version of the material. For illustration, if calcium carbonate is flaked in neutral water, the flakes obtained therefrom will consist of calcium carbonate. However, if calcium carbonate is flaked in acetic acid, the flakes obtained therefrom may consist of calcium acetate, the reaction between the carbonate salt and the acetic acid also producing water and carbon dioxide.

Regardless of the form in which the material (e.g., tastant) is fed to one or both surfaces forming any particular nip (e.g., in dry form, in a paste, or dissolved or dispersed in a liquid), its application can be continuous or intermittent.

Considering in a particular aspect the latter manufacturing of flakes from a material fed dispersed or dissolved in a non-viscous liquid, in one embodiment the method comprises: a) providing at least one material (e.g., tastant or any other active or inactive ingredient) dispersed or dissolved in a liquid so as to form a liquid (e.g., tastant(s)) stock; b) applying the liquid (e.g., tastant(s)) stock to a movable surface so as to form a thin film of liquid (e.g., tastant(s)) stock; c) removing at least a part of the liquid from the thin film of liquid (e.g. , tastant(s)) stock so as to form a thin coat of solid particles (e.g., of precipitated tastant(s)), the thin coat optionally having a thickness of no more than 400 pm; and d) agglomerating and compacting the particles of the thin coat, so as to obtain once most of the liquid is removed from the coat its constituting (e.g., tastant(s)) substantially dry flakes (e.g., containing less than 5 wt.% of liquid and optionally having a thickness of 200 pm or less and an average aspect ratio between their longest planar dimension and their thickness of at least 10: 1).

While in theory the liquid stock can be applied at any initial thickness, a relatively thicker film being expected to require a longer duration of process than a relatively thinner one under otherwise similar conditions, in some embodiments, the thin film of the liquid stock has an initial thickness of 400 pm or less, 325 pm or less, or 250 pm or less, the material(s) being preferably homogenously dispersed or dissolved (or both) in the liquid at the time of their application. A liquid stock in which the material to be flaked is dissolved can also be referred to as a stock solution. A liquid stock in which the material to be flaked is dispersed can also be referred to as a stock dispersion.

For similar reasons, while in theory the liquid stock can be applied at any initial concentration of the material, it may be advantageous to use relatively concentrated ones which are expected to require a shorter duration of process than a relatively dilute stock under otherwise similar conditions. Understandingly, a relatively high proportion of a material in a liquid may affect its viscosity. It is therefore stressed that while the liquid carrier used to form the liquid stock can by itself be non-viscous (e.g., having a dynamic viscosity of less than 1,000 mPa.s), the liquid stock can on the contrary be slightly viscous. Thus, while the liquid stock may also be non-viscous, in some embodiments, the liquid stock can have a dynamic viscosity of up to 5,000 mPa.s, up to 4,000 mPa.s, up to 3,000 mPa.s, up to 2,000 mPa.s, up to 1,500 mPa.s, or up to 1,250 mPa.s, as measured at room temperature. As appreciated by persons skilled in the assessment of rheological properties of materials, the dynamic viscosity of the liquid stock may also depend on the probe of the equipment intended for analysis and upon its frequency of oscillation and/or shear rate, if operated under continuous rotation. These parameters may need to be adjusted according to the behavior of the tested material and are therefore typically screened for suitable settings over a range, e.g., between 0.1 and 100 Hz for the frequency of oscillation, typically used for more viscous materials, and between 1 and 1,000 s'¹ for the shear rate of relatively non-viscous products, the shear rate range for more viscous paste like products being usually from about 1 to 100 s'¹. The viscosity values reported herein can be measured within said ranges of operation as suitable for their determination using a suitable rheometer, parts thereof and operating conditions. In some embodiments, the dynamic viscosity (e.g., of a liquid carrier or of a liquid stock prepared therewith) is determined at a shear rate in a range of about 10 to 250 s'¹ or in a range of about 50 to 150 s'¹.

In some cases, it may be desired to pre-treat the liquid stock and/or its constituents before applying it to the intended nip-forming surface. The pre-treatment can be at least one of a) the size reduction of the particles of materials to be dispersed, b) the heating of the liquid to facilitate dissolution or dispersion of the materials, c) the homogenization of the stock dispersion, and d) the heating of the liquid stock prior to its application. From the viewpoint of an apparatus, a device configured to provide such a pre-treatment can be referred to as a pretreating station.

In some embodiments, the surface to which the liquid stock is applied is wettable by said liquid stock, the liquid being able to evenly spread over the surface.

In some embodiments, the thin film of the (e.g., tastant(s) liquid stock is obtained by intermittently or continuously applying the liquid stock to the (e.g., wettable) surface, the surface being movable, and inter alia by passing the applied stock through a nip formed by urging into contact the movable surface and a counter surface one against the other. The portions of the movable surface and counter surface facing one another at the nip formed therebetween, can also be referred to as nip-forming surfaces. When both opposed surfaces are in motion, for instance the nip being formed at the line of contact between counter-rotating cylinders, all portions of the outer surface of the cylinders may periodically (cyclically) constitute a nip-forming surface.

The applicator of the liquid stock of material(s), which serves as a dosing device, and the first movable surface are typically in relative motion one with respect to the other. As used herein, the terms “tastant(s) stock”, “liquid stock”, “tastant(s) liquid stock”, or even “stock” can be interchangeably used to refer to the liquid containing the dispersed or dissolved material(s) (e.g., tastant(s)). The liquid carrier of the stock can be constituted of one or more fluids (and additives therein, if desired), the liquid carrier being relatively non-viscous (/.< ., having a dynamic viscosity of less than 1,000 mPa.s at room temperature) and the liquid stock having therefore a viscosity not exceeding 5,000 mPa.s upon its application to the movable surface. In some embodiments, the compaction of the thin coat of precipitated material(s) e.g., tastant(s) or any other solid particles progressively leaving the stock) is obtained by passing the thin coat through a same or at least one different nip than the one used inter alia to level the liquid stock into a thin liquid film, the material(s) gradually precipitating out of the liquid in the progressively drying coat, and the solid particles consolidating into larger assemblies (e.g., agglomerates) such that the (e.g., tastant(s)) flakes obtained thereby have a thickness of at most 200 pm, at most 150 pm, at most 100 pm, at most 50 pm, at most 20 pm, at most 10 pm, at most 5 pm, or at most 1 pm and an aspect ratio between the longest planar dimension of the (e.g., tastant) flakes and their thickness being on average of at least 10: 1, at least 20: 1, or at least 30: 1 (also referred to for brevity as at least 10, at least 20, or at least 30). Repeated passage of the thin coat including the solid particles progressively concentrating as liquid is evaporated ultimately results in a layer of flakes, each flake being constituted of agglomerated and/or compacted solid particles. This semantic distinction may however be sometimes arbitrary as areas of a thin coat may be capable of forming flakes before being sufficiently dry as a whole for the solid particles to be compacted into the highest number of flakes possibly manufactured by the process.

Importantly, the spacing at the nip need not be constant during the flaking process. On the contrary, the nip advantageously displays a dynamic spacing as the steps or cycles proceed and/or are completed. While the nips of the present flaking method can be viewed as “dynamic nips” more preferably having spacings inherently varying in response to process conditions and status, for brevity they shall be referred to as nips.

As appreciated from the above exemplary illustration, the compaction of the thin liquid film and of the coat of material(s) resulting therefrom by one or more passages through one or more dynamic nips between cylinders urged into contact may also provide a “crushing” step transforming into flakes the material(s) precipitated in the coat and the dry layer resulting therefrom. Thus, the crushing step can naturally result from the previously described steps, not requiring any dedicated actions. Crushing may additionally, or alternatively, require active separation or breaking of the dry layer containing the aggregated particles into distinct flakes of the precipitated materials consolidated by cyclic compaction. The crushing or breaking of the coat or dry layer devoid of most of the liquid (e.g., containing less than 5 wt.%) into flakes of compacted solid particles typically involves the natural detachment of flakes from the thin coat from and/or the assisted detachment of the layer comprising the flakes from the movable surface, and the inherent or forced break-down of the relatively dry layer into individual flakes. As the formation of the flakes encompasses different mechanisms that may each be viewed as a separation, either from an underlying surface or material, or from neighboring portions of the coat turning into flakes, the thin coat of precipitating solid particles and the layer in which their vast majority would be agglomerated and compacted, can be viewed as separable into flakes or comprised of flakes.

For the sake of efficiency, the material (e.g., tastant) can be provided with dimensions facilitating its dispersion or dissolution in the liquid, and for example can be grinded to have a largest dimension not exceeding 5 mm (e.g., if the material is soluble and the size reduction aiming to accelerate dissolution) or any other size desired as a pre-treatment to the preparation of the liquid stock to be applied (e.g., reducing the size of the material to 10 pm or less, 7.5 pm or less, or 5 pm or less, if the material is insoluble in the liquid, such a size reduction aiming to facilitate initial passages of the dispersion through the nip. A grinding pre-treatment of raw material can be performed with any standard equipment such as with a coffee grinder, a mortar and pestle, a hammer mill, a ball mill, a jet mill, and like known devices. Similarly, the liquid stock may be pretreated before being applied to a nip by any device adapted for the sought pretreatment (e.g., with a heater to heat the liquid, with a sonicator to accelerate dissolution, etc.). Alternatively, an apparatus for implementing the present method can be modified to allow for in-line pre-treatment of the material to be flaked, either as solid raw material or as liquid stock.

When the material is solvable in the liquid carrier of the stock, the process can be alternatively, or additionally, accelerated by using a saturated or near saturated solution. A saturated solution is a solution in which there is so much solute that if there was any more, it would not dissolve and would for instance precipitate out of solution as a solid. The maximum amount of any material (e.g., tastant) in a saturated solution thereof depends inter alia on the material, on its initial specific surface area, on the liquid in which it is dissolved, on the temperature of the solution, on pressure applied thereto and any other conditions (e.g., stirring) maintaining a homogenous concentration of the material in the solution. Therefore, a solution that can be saturated, for instance, at a relatively elevated temperature can be supersaturated (containing a higher-than-expected amount of soluble material) at a relatively lower temperature. Near saturated solutions comprise less than the maximum amount of material that may dissolve under the conditions set for the preparation of the solution. Such amounts (e.g., between 70% and 90% of the maximum amount) may suffice to render the solution saturated under different conditions to which the near saturated solution may be subjected during the process of preparing the flakes. In other words, while a solution can be prepared to be near saturated, saturated, or supersaturated upon completion of its preparation, such classification may evolve during the process. For illustration, a near saturated solution may become a saturated solution as liquid is removed therefrom and may even turn into a dispersion once the material (e.g., tastant) starts to precipitate out of solution (e.g., by crystallization of the material). In this context, a dispersion of a material being otherwise solvable in the liquid, indicates that the material is present at a concentration higher than tolerable for the formation of a supersaturated solution. Alternatively, the material may be dispersed in a liquid in which it is not solvable. For illustration, a material soluble in water need not be soluble in alcohol.

As used herein, “precipitate”, “precipitation”, and grammatical variants are not used to exclusively refer to a process resulting in the formation of a substance permanently insoluble in the liquid from which it precipitated out. On the contrary, these terms are meant to also include any processes resulting in the concentration or formation of an insoluble substance to an extent enabling its separation from a liquid as a solid, typically in the form of discrete solid particles, the solid so extracted being optionally soluble in the liquid under different conditions. Hence, materials being precipitated out of a liquid could have been previously dissolved or dispersed therein. Crystallization is a particular kind of precipitation process in which the structure of the substance rendered solid by loss of solubility becomes organized. A particular material (e.g., tastant) being a crystalline material may have a number of polymorphs, all being herein encompassed.

In some embodiments, the dispersion or the dissolution of the material (e.g., tastant) in the liquid is performed at a temperature above room temperature, this temperature not exceeding the boiling temperature of the liquid. Considering water as an exemplary liquid, the dispersing or dissolving step can be performed at a temperature of at least 30°C, at least 40°C or at least 50°C; and at most 95°C, at most 90°C or at most 85°C. If the liquid is an alcohol or contains enough alcohol or any other material having a boiling point lower than water, then the upper limits of the afore-said ranges should be reduced according to the relative proportions of such volatile fluids in the liquid, the dispersing or dissolving step being performed for illustration at a temperature between 30°C and 75°C. The temperature not to be exceeded during this step should also consider the heat resistance of the material (or the heat resistance of the most sensitive material, if more than one), and in the case of a tastant should preferably be lower than a temperature at which the taste of the tastant would be detectably impaired, as can be determined by organoleptic testing. Regardless of the temperature at which the dispersing or dissolving step can be performed, it may also be performed at a pressure other than ambient atmospheric pressure. Furthermore, and regardless of temperature and/or pressure conditions, the dispersing or dissolving step can be performed under ongoing agitation of the liquid while dispersing or dissolving the material(s) therein and/or while maintaining the liquid stock homogeneous for the formation of the continuous film (/.< ., during its application to a surface). Regardless of the conditions elected for the preparation of the liquid stock, it may be applied on the movable surface at a temperature above ambient temperature. This could be the case in particular if the surface is itself being heated at a same or different temperature above ambient temperature.

In some embodiments the removal of at least part of the liquid out of the (e.g., tastant) liquid stock forming a thin continuous film on the surface is expeditious. Without wishing to be bound by any particular theory, it is believed that, if sufficiently rapid, the liquid removal (e.g., evaporation) can take place while the material (e.g., tastant) is still relatively homogeneously dispersed or dissolved in the thin film. Quick removal of the liquid at such a stage enables the formation of a relatively homogenous coat of precipitated material (e.g, tastant or any other solid particles), which in turn may facilitate the compacting of the coat (by agglomeration of the solid) and its crushing into flakes having a relatively uniform thickness. A liquid film, a dry coat, a population of flakes or of nano flakes have a relatively uniform thickness if the ratio between their respective largest and smallest thickness, or their respective largest and smallest average thicknesses, is 10 or less, 8 or less, 6 or less, 5 or less, 4 or less, 3 or less, or 2 or less.

Advantageously, the rate of liquid removal in the present method is such that the formation of a coat of precipitated material (e.g, tastant) can take place in less than 1 minute from the time the thin film of (e.g., tastant) liquid stock is formed. In some embodiments, the liquid removal step takes 50 seconds or less, 40 seconds or less, or 30 seconds or less. If the method of liquid removal alternatively or further includes heating the surface upon which the liquid stock was applied to form a thin film, the liquid removal step can also be referred to as an accelerated evaporation step. In some particular embodiments, the liquid removal or evaporation step takes 20 seconds or less, 15 seconds or less, or 10 seconds or less. The liquid removal or evaporation step can be performed while blowing or aspiring away at least part of the liquid being removed or its vapors.

While any liquid could be used based on its ability to satisfactorily dissolve or disperse the material and on its relative ease of removal for the sake of process efficiency, it may be advantageous in the case of tastants or materials to be ingested by living subjects to select liquids also approved for animal (e.g., human) consumption. Such liquids are known and need not be detailed but for illustration can be selected from a group consisting of water, alcohols, fatty alcohols, glycerol (also called glycerine), propylene glycol, and combinations thereof. When the water-soluble material is not a tastant, or to be used for animal ingestion (e.g., dietary supplement, medicine, etc.), the liquid may additionally be selected from a wider range of fluids, which nevertheless may also take into account the intended use of the flaked material. For illustration, if the flakes are to be used in a manufacturing process, the liquid can be compatible with the process (e.g., not inhibiting an intended reaction).

Advantageously, but not necessarily, the liquid selected for the preparation of the liquid stock, whether pure or blended, should enable the dissolution of the material (e.g., tastant) to a concentration of at least 1 g per 100 g of the liquid (1 wt.%), or of at least 5 g of tastant per 100 g of the liquid (5 wt.%), at least 10 g of tastant per 100 g of the liquid (10 wt.%), at least 20 g of tastant per 100 g of the liquid (20 wt.%), as measurable at room temperature. To the extent that the flakes may retain residual liquid on their outer surface, the liquid should preferably be selected to be compatible to the intended use of the material, for instance, for tastants, not exceeding a content that would be deemed toxic for consumption. In other words, the liquid should preferably be Generally Recognized as Safe (GRAS), food-grade, and/or labelled with any other like denomination indicating its suitability for oral consumption when the material is intended for ingestion.

Alternatively, the liquid, whether pure or blended, should only enable the dispersion of the material (e.g., tastant), in other words the material dissolving at a concentration of less than 1 g per 100 g of the dispersing liquid (< 1 wt.%).

In some embodiments, the movable surface (e.g., wettable by the liquid stock) is the surface of a rotating cylinder. In such a case, and assuming a single nip, the liquid removal step configured to remove at least a part of the dissolving or dispersing liquid can preferably take place during no more than 60 cycles of the rotating cylinder, the number of cycles necessary to enable sufficient removal of at least a part of the liquid depending on the initial concentration of the material (e.g., tastant) in the liquid, the rotational speed of the cylinder, the temperature of the surface of the cylinder, the number of nips positioned along the rotating cylinder and like factors. In some embodiments, the liquid removal or evaporation step takes 50 cycles or less, 40 cycles or less, 30 cycles or less, 20 cycles or less, or 10 cycles or less. Preferably, the liquid removal or evaporation step should take 8 cycles or less, 6 cycles or less, 4 cycles or less, or 2 cycles or less, and ideally 1 cycle or less.

For avoidance of a doubt, it is stressed that the typically progressive removal of the liquid from a liquid film of stock need not be complete for material(s) (e.g., tastant(s)) to start precipitating. Consequently, the compacting of a coat of precipitated material(s) and its crushing into flakes can also initiate before complete liquid removal following one or more cycles of compaction. In other words, the removal of a first part of the liquid may cause the precipitation of a first part of solid particles, and while this first part would be compacted (e.g., leading to the agglomeration of the particles), the removal of a second part of the liquid could cause the precipitation of a second part of solid particles of the material(s), and so on. Thus, while the steps of liquid stock application, partial liquid removal till partial precipitation, and compaction leading to partial crushing of the precipitated material(s) into flakes are sequentially correct, a subsequent step does not require the full completion of a previous step to initiate, and some steps may coexist each for a different part of the film of liquid stock, precipitated coat, and layer of agglomerated particles compacted therefrom. Based on the same rational of a process allowing for concomitant coexistence of various phases, it can be appreciated that if all steps were to be ideally carried out in a single cycle through the nip, then different sections of the movable surface (e.g., rotatable cylinder) may display relative enrichment in products of the various phases.

When the surface upon which the film of (e.g., tastant) liquid stock is turning into a thin coat of precipitated material (e.g., tastant) and into a layer of flakes is the outer surface of a rotatable cylinder, compaction of the particles can be performed at a nip between the rotating cylinder and a counter surface urged into contact one with the other by a force mechanism, by passage(s) through the nip. The counter surface can be static, in which case, the surface coated with the precipitated material(s) and the counter surface are in relative motion. The counter surface may alternatively be movable and can for instance be a second rotating cylinder. In such a case, the two surfaces may enter the nip at the same or a different speed, the two cylinders being either rotating in the same direction or more typically in opposite directions.

While the nip (e.g., formed between two rotating cylinders urged into contact) is being described as providing for the confinement of the thin film of liquid stock, for the compaction of the coat of precipitated material (e.g. , tastant), and optionally for the crushing of the coat into flakes, this may not be its sole role in the present method. Without wishing to be bound by any particular theory, the pressure applied at the nip upon the film of liquid stock is believed to contribute to the removal of at least part of the liquid from the film, even at ambient temperature, without further heating of the surface of the cylinder. Regardless of the mechanisms of action that may be relevant to the restricted volumes of liquid stock, thinning film thereof, coat of precipitated material, and/or flakes crushed therefrom, that can be passed once or more times through the nip, it is believed that controlling the nip (e.g., by its operational parameters, such as speed of rotation, temperature, contact pressure, etc.) can inter alia dictate some characteristics of the (e.g., tastant) flakes being manufactured therethrough (e.g., size, morphology, etc.) and/or of the process efficacy (e.g., production rate).

In some embodiments, the pressure applied at the nip is at least 10 MPa, at least 50 MPa, or at least 100 MPa. Typically, the pressure applied at an ideal line of contact between surfaces involved in one or more nips in the present method does not exceed 1,500 MPa, being sometimes no higher than 1,250 MPa, or no higher than 1,000 MPa. If more than one nip is employed in the present method, the pressure applied at a first nip need not be the same as a pressure applied at another nip. This may be the case if the series of nips is formed radially around a common central cylinder, each externally rotating cylinder being urged into contact therewith at a different pressure. In some embodiments, the pressure applied at each nip can independently be between 10 MPa and 1,500 MPa, between 50 MPa and 1,250 MPa, or between 100 MPa and 1,000 MPa. The afore-said pressures are the maximum Hertzian contact pressure values calculated based on the forces that can be applied to urge the various nip-forming surfaces into contact.

The force / pressure applied to urge surfaces of the method / apparatus into contact for the formation of at least one nip need not be constant during the performance of any of the steps herein disclosed. Taking for clarity of illustration a material (e.g., tastant) being fed as a dry powder to a single nip, the thinning of the powder into flakes requiring more than one passage through the nip, the force applied by the compression mechanism and the pressure perceived at the nip may be gradually increased until reaching a peak or plateau value in the afore-said ranges of suitable pressures. Alternatively, the force applied by the compression mechanism could be constant, but the pressure perceived at different nips in a series of nip compressed by the same mechanism could be distinct. For illustration, considering a series of nips linearly aligned and formed by a series of rotatable cylinders having a gradually decreasing diameter, the pressure perceived at a nip between relatively smaller cylinders would be higher that the pressure perceived at a nip between relatively smaller cylinders, so that for a same force the pressure would be increasing as the diameter is decreasing. Interestingly, a same force mechanism can be used to simultaneously apply a force on two or more series of rotating cylinders / nips, each series forming an independent module capable of producing same or different (e.g., tastant) flakes, as herein taught. For illustration, a same compression mechanism can be applying a force on a first series of rotating cylinders forming a first series of nips (e.g., to produce flakes of a first material), and on a second series of rotating cylinders forming a second series of nips (e.g., to produce flakes of a second material). The first and second series are physically separated one from the other and can be arranged in parallel or serially one with the other.

Such configurations, enabling the simultaneous preparation of flakes of two or more different materials on separate series of nips, can be advantageous when preparing flaked materials to be mixed one with the other. In such a case, the second material need not provide any taste by itself if the first material is a tastant intended for that purpose. For illustration, a first material to be flaked on a first series of nip can be sodium bicarbonate, its flaking according to the present teachings being expected to reduce the presence of sodium that might be required for this agent to be sufficiently effective in a food product. As sodium bicarbonate may require, for products deprived of natural acids, the addition of an acidifying agent to react therewith for the release of carbon dioxide which ultimately leavens the product when entrapped in the batter, it can be suitable to flake an appropriate second material at the same time. For example, acetic acid (CH3CO2H; E260), acid calcium phosphate (ACP; Ca(H2PO4)2; E341), acidic sodium aluminium phosphate (SALP; E541), citric acid (HOC(CO2H)(CH2CO2H)2; E330), tartaric acid (C4H6O6; E334), or sodium acid pyrophosphate (SAPP; Na2H2P2O?; E450), to name a few weak acids which exist in crystal forms, can be flaked on a second series of nip the mixture of the two materials enabling the preparation of baking powders, or other food products (e.g., flours) typically including such agents. Similarly, when none of the materials to be flaked is a tastant, they may be two or more materials adapted for a same manufacturing process, the prospective “contamination” of flakes of a first material with flakes of a second (or third etc.) material having no deleterious effect on the intended manufacturing process.

In view of the relatively high pressures that can be applied at a nip, the rotating cylinder(s) and counter surface are advantageously made of materials having sufficient hardness, or any other property providing mechanical resistance, adapted to resist such pressures without significant deformation and/or wear. The rotating cylinder(s) and counter surface may be made of or coated with a metal (e.g., stainless steel), a ceramic (e.g., tungsten carbide (WC)), or a polymer (e.g., Kevlar®), so has to have on their outer surfaces contacting one another a Vickers hardness of at least 50 HV, at least 100 HV, at least 150 HV, or at least 200 HV. While the hardness of the materials need not be limited, it typically does not exceed 10,000 HV (e.g., if coated with a diamond like carbon (DLC) film), being often less than 5,000 HV, less than 3,500 HV, less than 2,000 HV, or less than 1,500 HV. The hardness desired for any surface may decrease as the pressure to be applied thereto is relatively reduced.

The hardness of the cylinders or their outer surface depends on a) the exact composition of each cylinder and coating, if present, and b) whether the bulk material was further treated (e.g., annealed, cold worked, hardened, heat treated or tempered), and in the affirmative to what extent (e.g., stainless steel can be tempered to be 1/16, %, 14, Yi, ³/4, or Full Hard). While the relative resilience of the rotating cylinders is expressed above in terms of their hardness, a person skilled in materials and their physical properties can readily “translate” such requirements in other terms, such as strength, yield point and the like, all such alternative, or additional, parameters being likewise selected to avoid or minimize deformation and/or wear of the surface of the cylinders under the operational conditions of the method or apparatus.

In some embodiments, the rotating cylinder(s) and counter surface are not only made of sufficiently hard and resilient materials, but additionally have a desirable surface topography (e.g., being smooth or textured, whether or not randomly). In some embodiments, the surfaces to be pressed one against the other are relatively smooth. In such a case, they may have a surface roughness (1?«) of 500 nm or less, 400 nm or less, 300 nm or less, 200 nm or less, or 100 nm or less. While a perfectly smooth surface may ideally display a null average surface roughness, typically R_a is greater than 20 nm.

The temperature of the rotating cylinder(s) and counter surface can be adjusted as desired, by using any suitable internal or external heating or cooling device. The temperature of the rotating cylinder(s) and counter surface can be selected according to principles similar to those described for the preparation of the (e.g., tastant) liquid stock. However, following the application of the liquid stock, it is no longer essential to avoid exceeding the boiling temperature of the liquid, the only consideration remaining being the heat sensitivity of the material.

The heating may take different forms depending on the temperature to be reached and can be by conduction, convection and/or radiation. Conduction can be achieved by positioning heating elements underneath a surface or liquid to be heated; or by circulating a hot liquid (e.g., heated oil or water) in pipes, chambers or jackets suitably located for that effect. Heating by convection can be achieved by blowing a hot gas (typically air) towards the surface to be heated. Heating by radiation can be achieved with microwaves, if in a suitable chamber, but more typically infrared lamps directed to radiate towards the relevant surface or material.

As appreciated by a skilled person, the rate at which the liquid (e.g., tastant(s)) stock is applied to the movable (e.g., wettable) surface depends inter alia on the surface tension of the liquid stock and the surface energy of the surface, the desired thickness of the thin film, the rate of removal (e.g., evaporation) of the liquid under operating temperature and pressure conditions, the speed of the surface at the nip, the dimensions of the nip, and like factors. The flow rate, or the metering of doses intermittently applied, can be empirically determined and adapted as desirable.

The thin film can be formed by running the surface to be coated trough a bath of the (e.g., tastant) liquid stock, by dripping or spraying the liquid stock on the surface through one or more nozzles disposed in parallel to the line of contact of the nip / the axial length of the rotatable cylinder, the nozzles being for instance arranged across the width of the movable surface, by providing the liquid stock upstream of a device configured to level it (e.g., a doctor blade, an air knife, a squeegee, etc.) or by any other method adapted to form a liquid film of minute thickness on a surface. As can be appreciated, in some embodiments, the liquid need not be applied as a thin film upstream of a nip, the nip itself serving to level an excess volume of liquid stock forming an initial, optionally transient, upstream pool into a downstream thin film.

As readily appreciated, for a predetermined concentration of material (e.g., tastant) in the liquid, a relatively thinner film of (e.g., tastant) liquid stock enables a relatively faster removal of the liquid, or at least a part thereof, than a relatively thicker film, all other conditions of the method being similar. In some embodiments, the thin film has an initial thickness at the time of application to the surface (prior to any significant removal of liquid) of 400 pm or less, 325 pm or less, 250 pm or less, 125 pm or less, 70 pm or less, or 35 pm or less. Typically, the thin film is applied to have an initial thickness of at least 250 nm, at least 500 nm, at least 750 nm, or at least 1 pm.

The above values refer to an initial thickness, as the present method is intended to remove parts of the liquid over time, so that the thickness of the (e.g., tastant) liquid stock gradually diminishes until the material precipitates into a thin coat, first partially then totally upon essentially complete removal of the liquid in the ultimate layer of separable flakes. The thickness of the thin coat of precipitating materials may also diminish over time and repeated compaction. As appreciated “complete removal” of the liquid as deemed obtained at the end of the flaking process does not mean that the resulting layer of flakes constituted of agglomerated and/or compacted particles, nor the flakes separable therefrom, would be totally devoid of liquid which could remain in the “drying” coat or adsorbed on the flake surfaces in relatively minute amounts. Any residual amount of liquid in the layer comprising, upon termination of the process, the particles in compacted and agglomerated form allowing for their crushing into commercially significant flakes could be tolerated. In some embodiments, the at least partial removal of liquid (e.g., partial evaporation) would enable the production of a dry layer and/or crushed (e.g., tastant) flakes having a liquid content of 5 wt.% or less, as can be determined by monitoring weight loss under conditions (e.g., temperature and duration of time) adapted to eliminate essentially all of the liquid without affecting the remaining solids. In some embodiments, the flakes contain less than 4 wt.%, less than 3 wt.%, or less than 2 wt.% of liquid per weight of the flakes. In other embodiments, the liquid content is deemed insignificant (or the flakes are deemed substantially dry) when the liquid content is of 1 wt.% or less, 0.8 wt.% or less, 0.6 wt.% or less, 0.4 wt.% or less, 0.2 wt.% or less, 0.1 wt.% or less, or 0.05 wt.% or less, by weight of the (e.g., tastant) flakes. The same upper limits of liquid contents apply to the layer of compacted and/or agglomerated particles prior to its crushing into flakes, which can be considered as representative samples of the dry layer.

While the process for preparing (e.g., tastant) flakes by the present method could ideally be continuous, generally when relying on more than one nip, it may alternatively be performed in an alternating “Stop and Go” manner. In such case, a dose of liquid is applied, and only once this first dose has been transformed into flakes, a second dose is applied, and so on and so forth. When a number of nips are involved in the process, a second dose can be applied before the flakes are collected at the last nip. It is therefore believed that a higher number of nips may shorten the time between application of separated doses or may even render the process continuous.

The (e.g., tastant) flakes can be naturally collected into a collector, the flakes spontaneously detaching from the thin coat disposed on the surface as it is compacted by passage(s) through the nip(s) and progressively forms the layer comprising the flakes; the flakes crushed out at the nip being funneled by gravitation to the collector. The flakes can be additionally, or alternatively, actively collected, using for instance a blade, a propelled jet of gas (e.g., air or heated air), or any other means suitable to detach the flakes from the layer of compacted particles or its underlying surface. Typically, flakes that spontaneously detached from the rotating surface upon which they were formed are relatively larger and/or thicker than flakes actively detached with the assistance of a detaching device. Generally, spontaneously detaching flakes are made of materials more friable.

The (e.g., tastant) flakes obtained by such method may not be sufficiently thinned after a single passage through the nip to form micro flakes, sub-micro flakes or nano flakes of desired dimensions. In such a case, the flaked product collected from the nip of first compaction can be advanced towards one or more additional nips until the collected product displays the properties desired for the flakes. It is believed that passing the flakes through additional nips, once most of the liquid has been removed or evaporated after cyclic passage through the first nip, can assist in removing residual liquid that might be absorbed on the surface of the flakes.

Alternatively, or additionally, the (e.g., tastant) flakes obtained by such method may contain a residual amount of liquid that may be incompatible with intended use and/or storage stability. Regardless of the reason for its desirable elimination, the method may further include a step dedicated to the removal of residual liquid, if any. For illustration, the flakes may be dried.

As the (e.g., tastant) flakes prepared according to the methods herein disclosed have a relatively high specific surface area as compared to their conventional unflaked counterparts, some may display an increased tendency to absorb ambient moisture. This phenomenon may lead to the caking of the flakes, impeding their flowability and making their transport, handling, storage, and application more difficult. In such a case, the flakes may be treated with additives capable of inhibiting caking, and the present method may further comprise a step to this effect. Alternatively, or additionally, the treatment can be physical, the flakes being for instance dried before being stored in an environment free of an otherwise deleterious factor (e.g., the dried flakes being stored in vacuum or under inert gas conditions or in a liquid in which they are stable (not soluble), the liquid being impermeable to adverse agents). For illustration, flakes made of water-soluble tastants can be preserved in an edible oil (or in a semi-solid or essentially solid similarly lipophilic product) in which they are substantially insoluble, the (e.g., plant) oil serving to deliver the dispersed tastant to the food products upon their preparation or ahead of their consumption.

In some embodiments, the method may further comprise sorting of the (e.g., tastant) flakes according to size so as to increase the size uniformity of each sub-population sorted thereby. By way of example, the flakes may be sieved through meshes of desired aperture size. A population of flakes having relatively uniform particle dimensions is expected to provide for a relatively more consistent effect, as may be required when standardized performance is expected from the flakes or the products incorporating them. All optional steps that may be performed following the collection of the flakes, not being limited to the ones above exemplified, can be referred to as post-processing steps, or postflaking steps. Devices or sub-systems enabling their performance in an apparatus for manufacturing such flakes, can accordingly be referred to as post-processing stations, or postflaking stations.

While the method has been described with respect to a single material (e.g., tastant), it can similarly be used to prepare flakes of two or more materials. For illustration, if each material is a crystal, the method can be used to achieve their co-crystallization, their compaction enabling the preparation of flakes of a mixture of the materials (e.g., tastants). The terms “material(s) or “tastant(s)” can be used herein to indicate that one or more materials or tastants could be used in the step, device or product being described.

A flake prepared as herein described, regardless of the number of distinct materials (e.g., tastants) being used for their preparation, generally contains more than one individual element of precipitated material(s), for illustration more than a single crystal of a tastant precipitating with a crystallographic structure. A flake is usually constituted of several such elements typically forming a continuous mosaic of precipitated material(s) (e.g., a plurality of salt or sugar crystals, if the material is a crystalline tastant), the coat of agglomerated elements not being itself necessarily continuous. Advantageously, in some embodiments, the mosaic of precipitated material(s) appears in the resulting flake as substantially merged / essentially devoid of voids between the various elements forming the flake.

Some embodiments of the present method and its various steps are depicted in Figure 1 in which a box having a dashed contour indicates an optional step.

In a first step SOI, one or more materials (e.g., tastants) to be manufactured as flakes are provided. Typically, the material(s) are provided as dry powders of various shapes and dimensions. If the material(s) is/are provided as a paste or a liquid, the method may start from step S03 to obtain a concentration of material(s) and/or a viscosity of liquid stock as desired or may even start from step S04 if the material(s) have a desirable concentration (e.g., adapted to form at least a near saturated solution) and/or if the liquid stock has a desirable viscosity (e.g., not exceeding 5,000 mPa.s at the temperature of dispersion, dissolution or application).

If the materials (e.g., tastants) are provided as dry powders and one of the materials has a relatively large initial size, for instance having at least one dimension larger than 5 mm, the material can be size reduced by any suitable method to have preferably all dimensions not exceeding 5 mm or being even smaller and in the micrometer range, if so desired. For illustration, this second step S02 can consist of optionally grinding the at least one material provided in SOI.

In a third step S03, the at least one material (e.g. , tastant) (which may have been optionally size reduced to any desirable grain size in the low millimeter range (e.g., between 0.5 and 5 mm) or in the low micrometer range (e.g., between 0.5 and 10 pm)) is dissolved or dispersed into a liquid (the number of phases in the liquid stock depending on relative amounts and/or on the nature of the liquid and the capacity of the material to dissolve therein). This step can be performed under agitation, heat, and/or pressure, as previously described and adapted to the liquid stock to be obtained.

In a fourth step S04, the (e.g., tastant(s)) liquid stock is applied to a movable surface (which may optionally be wettable by the liquid stock). Typically, the applicator of the liquid stock and the surface to be coated therewith as a thin liquid film are in relative movement. The applied liquid can be leveled to form a thin film using a dedicated leveling device setting a desirable initial thickness or/and by displacing the applied liquid (or liquid film having a first thickness) towards a nip formed between the movable surface and a counter surface.

The nip between the two surfaces is formed by urging one against another in a step illustrated as S05 in Fig. 1. The nip can be a single nip, or a series of nips as shall be further detailed with reference to Figures 2 to 7. It is stressed that in contrast with traditional levelling or thinning devices which are set to maintain a constant distance about the material processed thereby, the present nips formed under the ongoing application of urging pressure are on the contrary configured to assume spacings fluctuating between gaps of up to 400 pm upon application of a liquid stock down to 1 pm or less before feeding or once all flakes have detached from the surface upon which they were formed.

While the optional heating of at least one of the movable surface and counter surface is illustrated as S06 apparently following S05, this is not the sole possible sequence of events, and the optional heating of the surfaces (or one of them) may alternatively, or additionally, take place before the application of the liquid stock (before S04) and/or before the liquid stock reaches the nip (before S05).

In a seventh step S07, at least a part of the liquid is removed from the thin film of (e.g., tastant(s)) liquid stock so as to increase the relative concentration of the material(s) in the liquid phase and their progressive separation therefrom as solid particles. While ideally, the liquid should be removed rapidly enough to ensure the formation of a thin coat of entirely precipitated material(s) (e.g., tastant(s)) in a single passage through a single nip, to permit continuous application of the liquid stock, this is not essential. The method can be alternatively continuously carried out by running the thinning film of liquid stock in which the concentration of solid particles of the materials(s) progressively increases through a series of nips, the thin coat of precipitated material(s) turning into a dry layer of agglomerated particles generally after the last or the penultimate nip. The method can also be carried out in an alternative mode with respect to the application of the liquid stock being batch-wise, the thinning film of liquid stock passing more than one time through a same nip or through a series of nips, the thin coat of progressively precipitated material(s) generally turning into a dry layer of agglomerated particles after the last or the penultimate passage through the (last or penultimate) nip. The progressive removal of the liquid (e.g., by evaporation, which can be accelerated by heating the nip-forming surfaces) leads to the precipitation of the material(s), which can also be an ongoing event until all liquid is essentially removed. Considering for illustration a tastant made of a crystalline material, the precipitation of a first part of the tastants can result in the formation of initial crystals constituting in turn nucleation centers for tastants subsequently precipitating out of the film of liquid stock.

In an eighth step S08, the thin coat of precipitated material(s) (e.g., tastant(s)) is compacted (and optionally crushed down in the process to flakes naturally detaching from areas of the coat sufficiently compacted). As for the gradual removal of the liquid, this progressive compaction of the solid particles ongoingly separating from the liquid may occur in one or more passages through a same or different nips. While for simplicity referred to as “compacting”, this step may achieve several effects that could be synchronous and not necessarily distinguishable, nor all taking place. Advantageously, the compaction of the solid particles progressively separating from the liquid stock as the liquid evaporates, regardless of methods or means to implement it, is believed to achieve a consolidation of the particles of precipitated material(s) into agglomerates, the individual elements of precipitant having a relatively high cohesion among themselves and the thin coat of agglomerated particles and the layer of flakes emerging therefrom being relatively more uniform (e.g., in thickness, etc.) than a layer resulting from a “pressure-deprived” precipitation of same materials. Thus, while conventional precipitation could form relatively friable agglomerates of individual precipitated elements, the present repeated passage of the liquid stock through the nip(s) and the cyclic compaction of the materials precipitated therefrom is believed to initially include an amalgamation in which individual precipitated elements could be considered as merging one with the other. Flakes obtained by the present method may therefore have a relatively low porosity and/or a relatively high transparency. In some embodiments, the (e.g., tastant) flakes have a porosity of at most 30%, at most 25%, at most 20%, or at most 15%. In some embodiments, the flakes have a porosity of at least 1%, at least 2%, or at least 5%.

While in the present figures, the removal of the liquid (S07) is presented as preceding the compaction of the particles separating from the liquid stock as solid elements (S08), in practice as both steps are typically cyclically repeated, they may take place concomitantly. Taking a rotating cylinder for illustration of a movable surface upon which flakes would form, compaction may take place in the nip-forming region of the cylinder engaged with the counter surface, while its surface upstream and downstream of the nip may be exposed and allows the evaporation of the liquid.

In a ninth step S09, the (e.g., tastant(s)) flakes can be collected from the last surface upon which the thin coat of precipitated material(s) was disposed. When the method is carried out in a series of nips, the collection can be performed at different nips. If the collected fractions have similar properties (e.g., similar dimensions), the different nips can serve to increase the productivity of the method. If the fractions collected at the different nips have distinct properties (e.g., different dimensions, aspect ratios, etc. , the different nips may serve to sort the flakes produced by the method.

Exemplary different nips of relevance to the present method, and following apparatus, shall be briefly described with reference to their schematic illustrations, as depicted in Figs. 2 to 7. For clarity of these non-limiting nip configurations, some devices of the apparatus or enabling the herein disclosed method steps shall not be represented in these figures. The omitted devices might be essential and include, for illustration, a compression mechanism for urging at least one pair of surfaces into contact so as to constitute a nip, a drive mechanism (e.g., motor, connector, etc.) for driving the rotation of at least one rotatable cylinder, and a dosing device capable of periodically providing to an applicator a desired dose of a liquid stock or a desired continuous flow rate of a liquid stock. The omitted devices might be optional and include, for illustration, a levelling device capable of forming a thin layer of liquid having a desired thickness; a heating device capable of heating the surfaces being coated during the process (the heat being applied from the rear and/or the front side of the surfaces); and a detaching device capable of “scratching away” a thin coat of precipitated material(s) (e.g., tastant(s)) breaking the last formed such layer into the flakes constituting it, such a device being optionally retractable, depending on the nip configuration being elected. Such devices, as well as optional driers, chambers, flake sorters, and like equipment as may be used in the conventional preparation of flakes, are known and need not be detailed herein. Furthermore, all may be arranged on and supported by a suitable structure or support frame.

For brevity, principles of operation common to all nip configurations are not necessarily repeated in the following descriptions. For the avoidance of a doubt, while in these figures the various nip configurations are illustrated upon engagement of the surfaces forming the respective nips, in an apparatus including such nip configurations the surfaces can be disengaged to permit maintenance (e.g., cleaning) or replacement of the surfaces when desired. Moreover, while in some illustrated embodiments, the plane including the axes of rotation of the rotating cylinders is depicted with a horizontal orientation, this should not be construed as limiting. For illustration, a pair of counter rotating cylinders can be angled with respect to the horizon, the liquid stock being applied at an upper end of the tilted nip and the flakes being collected at a lower end of the nip. Conceivably, if the cylinders have suitable dimensions (e.g., are long enough), under appropriate operating conditions (e.g., flow rate of the liquid stock, rotational speed and temperature of the cylinders, pressure applied thereto as perceived at the nip, etc.) such an arrangement may advantageously permit continuous application of the stock and collection of the flakes made therefrom.

Figure 2 schematically depicts a nip 200 formed by urging a rotating cylinder 210 having an (e.g., wettable) outer surface 210’ against a counter surface 220 being planar (and typically, though not necessarily static) and having an outer surface 220’ facing the cylinder. In this figure the applicator of the (e.g., tastant(s)) liquid stock is illustrated by arrow 260 and the collector of the (e.g., tastant(s)) flakes is illustrated by vessel 270.

While an applicator 260 could be any device capable of dispensing a liquid (e.g., a nozzle) or applying it to a surface (e.g., a brush) so as cover the surface, this term is often used herein to also refer to a dosing device capable of intermittently applying controllable quantities of the liquid stock at predetermined rates of repeated application (e.g., 1 ml every minute) or capable of applying the liquid stock as a continuous stream at predetermined flow rates (e.g., 1 ml per minute), the quantities being repeatedly applied or the flow rate of continuous application being selected to avoid excess liquid stock spilling out from the surfaces forming the nip.

While the collector 270 is for simplicity depicted downstream of nip 200, it may alternatively be at any other position along the path followed by the rotating surface 210’. As cylinder 210 may not only rotate around its axis, but also move along the counter surface 220 (up and down in the illustrated figure) the counter surface being static, the collection of the flakes into collector 270 may also take place from a thin coat formed on surface 220’. A similar effect of having the thin coat of precipitated material formed on surface 220’ can be achieved conversely by having the axis of rotation of cylinder 210 static, the counter surface 220 being in relative motion therewith (up and down in the illustrated figure) or by having both the axis of rotation of 210 and the counter surface 220 being displaced in the Z-direction in the present illustration, contact between the two surfaces (hence, nip 200) being maintained at all times. The collection of the flakes can result from spontaneous detachment of the flakes, as the thin coat of precipitated material(s) is generated from the progressive removal of the liquid or at least part thereof and is compacted by passage through the nip, each said step lasting one or more rotations of cylinder 210 and passages through nip 200. The collection of the flakes can also involve a detaching device, which may be controllably operated following the formation of the relatively dry layer comprising the flakes of precipitated and agglomerated material(s), the flakes at this stage typically containing no more than 5 wt.% of liquid. For example, detachment can be facilitated by directing, when desired, a jet of gas onto the layer comprised of the flakes or by approaching a suitable mechanical obstacle (e.g., a blade) towards it, to scrape it away from its underlying surface as individual flakes.

Figure 3 schematically depicts a nip 300 formed by urging a first rotating cylinder 310 having an (e.g., wettable) outer surface 310’ against a counter surface being a second rotating cylinder 320 having an (e.g., wettable) outer surface 320’. In this figure the two cylinders are rotated in the same (e.g., clockwise) direction generating slippage at the line of contact. The applicator of the (e.g., tastant(s)) liquid stock is illustrated by arrow 360 and the collector of the (e.g., tastant(s)) flakes is illustrated by vessel 370, arbitrarily depicted downstream of nip 300, though it may alternatively be at any other position along the path followed by the rotating surface 310’ and advantageously by the rotating surface 320’.

Figure 4 schematically depicts a nip 400 formed by urging a first rotating cylinder 410 having an (e.g., wettable) outer surface 410’ against a counter surface being a second rotating cylinder 420 having an (e.g., wettable) outer surface 420’. In this figure, in contrast with Fig. 3, the two cylinders are counter-rotated (e.g., one being in a clockwise direction and the other counterclockwise). If the two cylinders have the same speed, slippage at the line of contact can ideally be avoided, this however is not essential. The applicator of the (e.g., tastant(s)) liquid stock is illustrated by arrow 460 and the collector of the (e.g., tastant(s)) flakes is illustrated by vessel 470, arbitrarily depicted downstream of nip 400, though it may alternatively be at any other position along the path followed by the rotating surface 410’ and advantageously by the rotating surface 420’.

Figure 5 schematically depicts a series of nips 500a, 500b and 500c which are linearly aligned. Nip 500a is formed by urging a first rotating cylinder 510 having an (e.g., wettable) outer surface 510’ against a counter surface being a second rotating cylinder 520 having an (e.g., wettable) outer surface 520’. Nip 500b is formed by urging the second rotating cylinder 520 against a counter surface being a third rotating cylinder 530 having an (e.g., wettable) outer surface 530’. Nip 500c is formed by urging the third rotating cylinder 530 against a counter surface being a fourth rotating cylinder 540 having an (e.g., wettable) outer surface 540’. The applicator of the (e.g., tastant(s)) liquid stock is illustrated by arrow 560 and the collector of the (e.g., tastant(s)) flakes is illustrated by vessel 570, arbitrarily depicted downstream of nip 500c, though it may alternatively be at any other position along the path followed by the rotating surfaces 510’, 520’, 530’ and advantageously by the rotating surface 540’. If desired, more than one collector can be used along a series of nips as schematically illustrated, for example, in Figs. 5-7. While a linear alignment of nips has been illustrated in this figure with four cylinders of similar dimensions, each pair of cylinders being counter rotating, this need not be the case. Linear alignment of nips can be achieved with any other number of cylinders being equal or greater than three, the cylinders being same or different, being rotated in same or different direction, and/or at same or different speed. In a linear alignment of cylinders, in which a single compression system and/or a single motor can be used to urge and/or rotate any two cylinders into rolling contact, each pair of cylinders may conceivably be separated from nearby pairs.

In some cases, the series of nips (whether or not as schematically illustrated in Figs. 5-7) includes a number of nips sufficiently great under the operating conditions elected for the preparation of the (e.g., tastant) flakes to allow for the presence of more than one applicator (e.g., dosing device) capable of feeding (e.g., tastant) liquid stocks on more than one of the outer surfaces of the cylinders constituting the series of nips. The liquid stocks fed by all applicators can be the same and such configuration can be appropriate for continuous application of the liquid stock and collection of the flakes produced therefrom.

Figure 6 schematically depicts a series of nips 600a, 600b, 600c and 600d which are radially aligned towards a common central rotating cylinder 610 having an (e.g., wettable) outer surface 610’ (not marked on the figure). Nip 600a is formed by urging against the first rotating cylinder 610 a counter surface being a second rotating cylinder 620 having an (e.g., wettable) outer surface 620’ (not marked on the figure). Nip 600b is formed by urging against the first rotating cylinder 610 a counter surface being a third rotating cylinder 630 having an (e.g., wettable) outer surface 630’ (not marked on the figure). Nip 600c is formed by urging against the first rotating cylinder 610 a counter surface being a fourth rotating cylinder 640 having an (e.g., wettable) outer surface 640’ (not marked on the figure). Nip 600d is formed by urging against the first rotating cylinder 610 a counter surface being a fifth rotating cylinder 650 having an (e.g., wettable) outer surface 650’ (not marked on the figure). The applicator of the (e.g., tastant(s)) liquid stock is illustrated by arrow 660 and the collector of the (e.g., tastant(s)) flakes is illustrated by vessel 670, arbitrarily depicted downstream of nip 600c, though it may alternatively be at any other position along the path followed by the rotating surfaces 610’, 620’, 630’, 640’, and advantageously by the rotating surface 650’. For instance, collector 670 can be located downstream of nip 600d. While a radial alignment of nips has been illustrated in this figure with four cylinders of similar dimensions dispose on diametrically opposed side of a common central cylinder, each outer cylinder being counter rotating with respect to the central one, this need not be the case. Radial alignment of nips can be achieved with any other number of outer cylinders being equal or greater than three, the cylinders being same or different, being rotated in same or different direction, and/or at same or different speed.

Notably, while in Fig. 6, rotating cylinders 620, 630, 640 and 650 are disposed to contact the outer surface of a centrally rotating cylinder 610 upon which the liquid stock is applied to be processed by the present method, they can alternatively face the cylindric wall of 610 from the inner side. In such a case, rotating cylinder 610 shall be a hollow cylinder or a drum, and the liquid stock shall be applied on the inner surface of the hollow cylinder. Similarly, the collector 670 would be located within the hollow plenum of 610.

Whether located internally or externally to the centrally rotating cylinder 610, the presence of a number of cylinders (e.g., 620, 630, 640 and 650) disposed to rotate in contact therewith enables a different mode of application of the liquid stock. Namely, instead of applying the liquid stock towards a first nip in the series, for instance, by way of one or more nozzles disposed in parallel to the nip and adapted to jet the liquid as required, the stock can be applied by dipping a portion of the cylinder of the first nip through a bath filled with the liquid stock. In the latter case, the proper dosing of the liquid stock applied to the surface is governed by the surface energy of the surface of the cylinder dipping into the bath and the surface tension of the liquid stock, excess liquids typically dripping back to the bath by gravitation prior to the remaining thin film entering a downstream nip.

Figure 7 schematically depicts a configuration of a series of nips combining the principles of linear and radial alignment of the nips. The nips between rotating cylinders 710, 720, 730, 740 and 74B form a linear alignment, whereas the nips between 71A, 71B and 710, or 72A, 72B and 720, or 73A, 73B and 730, or 74A, 74B and 740, are deemed to form radial alignments with respect to rotating cylinders 710, 720, 730, and 740, respectively. The applicator of the (e.g., tastant(s)) liquid stock is illustrated by arrow 760 and the collector of the (e.g., tastant(s)) flakes is illustrated by vessel 770, arbitrarily depicted downstream of the nip formed by rotating cylinders 740 and 74C.

In some of the above-described configurations, in particular in those including a series of nips, essential or optional devices which for clarity are not illustrated in the figures may be included more than once. For instance, each rotating cylinder may be independently driven by a different motor. Considering a levelling and/or a detaching device, they need not to be exclusively disposed on the first and the last cylinder, respectively, and they may each be repeatedly disposed along the series of nips. Taking Fig. 6 for illustration, a first levelling device could be disposed to face cylinder 610 downstream of the applied liquid stock and upstream of cylinder 620, whereas a second levelling device may be found adjacent cylinder 620, or again adjacent cylinder 610 but downstream of nip 600a. Likewise, a last detaching device may be found to detach flakes from the surface of cylinder 650, but may be preceded by an upstream positioned detaching device which may for illustration be removing the (e.g., tastant) flakes from the surface of cylinder 610 in the section between nips 600c and 600d. An additional collector could be required besides 670, depending on its particular architecture and mode of action, as well as on the exact relative positioning of the detaching devices.

In particular embodiments, regardless of the type of alignment(s) followed by a series of nips (e.g., linear and/or radial), the number of nips and the rotating cylinders forming them are selected to enable a continuous application of (e.g., tastant(s)) liquid stock and collection of (e.g., tastant(s)) flakes upon completion of the process under the operating conditions set therefor.

According to another aspect of the disclosure, there is provided an apparatus for making flakes from a liquid stock comprising a material dissolved or dispersed in a liquid, the apparatus comprising: a) a support frame, b) at least two cylinders mounted in the frame with at least one of the cylinders movable relative to the support frame, c) a force mechanism for applying a force to urge the cylinders into contact with one another so as to form at least one nip, and d) a drive motor for rotating at least one of the cylinders, characterized by e) a dosage device for applying the liquid stock onto at least one of the cylinders so as only to apply thin films to the surfaces of the cylinders, the concentration of solid material in the films increasing with repeated passage of the films through the at least one nip resulting in the formation of flakes of the material, and f) a controller for regulating the rate at which liquid stock is applied onto at least one of the cylinders to match the rate at which liquid is lost from the films during continued passage of the films through the at least one nip.

As the two or more rotatable cylinders of the present apparatus are urged into contact whilst the flaking system is operating, the nips respectively formed between any two adjacent cylinders can vary in spacing during the process. Even if a constant force is applied by the force mechanism urging the cylinders into contact, the nips may assume a larger gap (separation) upon feeding of a material to be flaked as compared to the gap, if any, that would exist under similar condition in absence of applied liquid stock (e.g. , before application of the stock or upon completion of flaking).

In some embodiments, the apparatus further comprises a levelling device adapted to level the (e.g., tastant) liquid stock into a thin film prior to passage through the nip. As opposed to the nips herein preferred, the levelling device can be set at a fixed distance from the surface upon which the liquid is to be levelled.

In some embodiments, the apparatus further comprises at least one heating device to heat at least one of the (e.g., tastant) liquid stock to be dispensed by the dosing device and any of the surfaces of the two or more rotatable cylinders.

In some embodiments, the apparatus further comprises a detaching device adapted to detach the (e.g., tastant) flakes from the films being deprived of the liquid, in other words from the thin coats or layers of precipitated, agglomerated and compacted solid material forming the flakes, for their collection by the collector.

In some embodiments, the apparatus further comprises a controller serving to control constantly or periodically at least one of: a- the quantity of liquid stock being dispensed and/or the periodicity or rate of liquid stock being applied by the dosing device; b- the force or pressure applied by the force mechanism (also referred to as the compression mechanism); c- the speed of rotation of at least one of the two or more rotating cylinders; and d- the temperature of the liquid stock and/or the temperature of any surface of the two or more rotating cylinders.

Such controlling systems are known and need not be further detailed herein. They can be based on feed forward proactive control, setting predetermined target values to be met, and/or on feedback control, responsive to a signal relevant to the parameter being controlled. For illustration, the Inventors have found that the torque of the motor rotating a cylinder engaged at a nip with materials being flaked could predict the timing at which a new dose of material can be applied if the flaking process is discontinuous. Therefore, liquid applicators or dosing devices (e.g., illustrated by arrows 260, 360, 460, 560, 660, and 760 in the previously described figures) can be controlled by such a feedback mechanism to release a new dose of liquid at one or more sites along the respective (e.g., first) nips (e.g., 200, 300, 400, 500a, 600a, and nip between rotating cylinders 710 and 720) once the torque of the motor, as measured by a torque measuring device, reaches its lowest value (corresponding a lowest proportion of liquid in the layer comprising the flakes). Other suitable controllers may monitor the progression of the flaking process and accordingly regulate the dosing device. Other types of control can relate to the force or pressure applied by the force mechanism, which can be for instance monitored via strain gauges disposed adjacent to the nip being controlled proximally to the compression mechanism.

In some embodiments, the outer surface of each of the two or more rotatable cylinders of the apparatus is made of, or coated with, a material wettable by the (e.g., tastant(s)) liquid stock.

In some embodiments, the outer surface of each of the two or more rotatable cylinders of the apparatus is made or, or coated with, a material having an average surface roughness (Rd) of 500 nm or less, 400 nm or less, or 300 nm or less.

In some embodiments, the outer surface of each of the two or more rotatable cylinders of the apparatus is made of, or coated with, a material having a Vickers hardness between 50 HV and 10,000 HV, between 100 HV and 5,000 HV, between 150 HV and 3,500 HV, or between 200 HV and 2,000 HV.

According to another aspect of the disclosure, there is provided a product (which can also be referred to as a manufactured article) comprising flakes of water-soluble or water-insoluble material(s) as herein disclosed, and/or prepared by the present methods, and/or prepared by using the present apparatus.

According to another aspect of the disclosure, there is provided a food comprising tastant flakes as herein disclosed, and/or prepared by the present methods, and/or prepared by using the present apparatus.

According to another aspect of the disclosure, there is provided a method for improving a manufactured article, the method comprising incorporating into the article flakes as herein disclosed, and/or prepared by the present methods, and/or prepared by using the present apparatus, the flakes comprising or consisting of at least one active or inactive ingredient. The improvement of the manufactured article can be in its chemical efficacy, its physical efficacy, its biological efficacy, its quality, its ease of preparation, storage or transportation, or its cost of preparation, storage or transportation, to name a few fields in which an article of manufacture can be improved by the present flakes.

According to another aspect of the disclosure, there is provided a method for improving a food, the method comprising incorporating into the food or beverage flakes as herein disclosed, and/or prepared by the present methods, and/or prepared by using the present apparatus, the flakes optionally being of a tastant. The improvement of the food can be in its taste, its odor, its preservation, its texture, its appearance, or its ease of preparation, to name a few fields in which food improvement can be required and achieved by the present flakes.

The food improvement can alternatively, or additionally, be in the prolonged retention or delayed reduction in the properties of the food as displayed when freshly prepared and expected from a consumer using all senses typically involved in the appreciation of a food product. Therefore, in a broader sense, a tastant need not necessarily provide a taste but assist in the perception of a quality of a food product and can be for non-limiting illustration an emulsifier, a thickener, a binder, a gelling agent, a texturizer, a firming agent, a leavening agent, a stabilizer, a preservative agent, an anti-caking agent, an humectant, a pH controlling agent, a color additive, a flavor enhancer, a vitamin, a mineral nutrient, and any like food additive expected to positively affect the characteristics of the food, whether for the sake of its consumption, production, processing, treatment, packaging, transportation or storage.

According to another aspect of the disclosure, there is provided a method for reducing the amount of a material in a manufacturing process or in a manufactured product, the method comprising replacing at least a part of the material in said process or product by flakes as herein disclosed, and/or prepared by the present methods, and/or prepared by using the present apparatus.

According to another aspect of the disclosure, there is provided a method for reducing the amount of a tastant adapted to provide a desired taste to a food, the method comprising replacing at least a part of the tastant in said food or beverage by tastant flakes as herein disclosed, and/or prepared by the present methods, and/or prepared by using the present apparatus.

While for brevity the present methods and apparatus have been predominantly described as suitable for the preparation of tastant flakes, as relevant to the food industry or any other industry relying on oral administration or use of products inter alia having a taste and/or contributing to a quality of the (e.g., food) product, they may similarly serve for the preparation of flakes of any other active or inactive ingredient intended for any other purpose. The raw material to be flaked need not provide a taste, nor be suited for animal consumption or use, nor be intended for the food industry. For illustration the product being flaked can be any product for which this particular morphology could be beneficial, such as to facilitate dissolution, dispersion, decomposition, release into the surroundings, uptake by relevant organisms, or any such process in which a relatively increased specific surface area can be beneficial to the product efficiency.

EXAMPLES

Example 1 : Dry Flaking of Tastants

In this example, tastants selected from sugar, salt and ground coffee, as commercially available, were flaked while being fed as dry powders. Sugar and salt represent water-soluble materials, whereas coffee despite containing water-soluble constituents is considered as a water-insoluble material. The dry samples were fed to an apparatus having a nip as schematically illustrated in Fig. 5 and consisting of three rotating cylinders. Both rotating cylinders 510 and 530 were made of stainless steel 17-4 PH® (having a Vickers hardness of 240 HV and an average surface roughness R_a of less than 1,600 nm), and had a diameter of 30 cm. Rotating cylinder 520, positioned between cylinders 510 and 530, was made of tungsten carbide and had a diameter of 1 cm. All three cylinders shared a similar axial length of 25 cm. They were counter-rotated at a similar speed of 20 rounds per minute (rpm), while being urged into contact by a calculated Hertz contact pressure of up to 750 MPa, using a compressing mechanism providing a force of 1.5 ton-force, in the present case a hydraulic piston. The granulated sugar was fed to the nip, the surfaces of the rotating cylinders being at ambient temperature of about 23°C. After a single application of 1 g of sugar and 6 passages through the nip (reported below as number of cycles), flaked sugar was collected using a doctor blade coated with a ceramic material, the blade being suitably positioned and oriented to detach the flakes from their underlying surface. This experiment and the resulting flakes were named DF-1. SEM-FIB micrographs were taken by placing the particles being studied on an aluminium pin type SEM mount covered in double sided adhesive carbon tape, the images were captured at a magnification of XI 00 with an electron high tension (EHT) voltage of 1.2 kV and an aperture size of 30 pm (using a Crossbeam 340 microscope of Zeiss). The samples were measured at the beginning and end of the flaking process, and their average dimensions were assessed on at least 10 individual grains or flakes detectable in the field of view, usually on 20-30 discrete particles in one or more fields of view. All initial grains were approximated to spheres, even if slightly more cubic in shape, so that the original size of the tastants is presented as an average diameter. Figure 8A is a picture of sugar grains, before being fed to the apparatus, while Figure 8B is a picture of sugar flakes as obtained under the afore-described conditions.

The conditions and results obtained by the afore-detailed and similar dry flaking methods are summarized in Table 1 for all tastants accordingly prepared and fed in the same quantity. In this and following tables, SS stands for stainless steel 17-4 PH®, WC stands for tungsten carbide, and 0 stands for the average diameter of the grains being fed or for the diameter of the rotating cylinders.

Table 1

Example 2: Paste Flaking of Tastants

In this example, granulated coffee having an average diameter of about 500 pm was flaked while being fed as a paste of dry powders dispersed in a viscous medium to an apparatus having a nip as schematically illustrated in Fig. 4. The first and second rotating cylinders 410 and 420 were identical and made of stainless steel 17-4 PH® (having a Vickers hardness of 240 HV and an average surface roughness R_a of less than 1,600 nm), and had a diameter of 30 cm for an axial length of 25 cm. They were counter-rotated at a similar speed of 60 rpm, while being urged into contact by a calculated pressure of 370 MPa, using a compressing mechanism providing a force of 7.5 ton-force, in the present case using a hydraulic piston. The granulated coffee was mixed at a weight ratio of 1 : 10 into a viscous medium made of 20 wt.% xanthan gum in water, this medium having a dynamic viscosity of about 10,000 mPa.s as measured at room temperature in an appropriate rheometer (Thermo Scientific (Germany) Haake Mars III) with a C20/1⁰ spindle, a gap of 0.052 mm, a volume of 0.04 ml and a shear rate - oscillation frequency sweep of 0.1-100 Hz, Gamma 1%. The resulting paste was fed to the nip, the surfaces of the rotating cylinders being at ambient temperature. After a single application of 0.5 g of paste and 20 passages through the nip, flaked coffee at least partially enrobed with the viscous medium was collected from the surface of the cylinder using a suitably oriented doctor blade as previously detailed. This experiment and the resulting flakes were named PF-1. SEM-FIB micrographs were taken, as previously described, at the beginning and end of the flaking process, and average dimensions were assessed on at least 10 individual grains or flakes detectable in the field of view. Figure 9A is a picture of coffee grains, before being fed to the apparatus, while Figure 9B is a picture of coffee flakes as obtained under the afore-described conditions, both being at a magnification of XI 00.

The conditions and results obtained by the afore-detailed flaking method are summarized in Table 2.

Table 2

Example 3: Liquid Flaking of Materials Including Tastants

In this example, materials, whether water-soluble or water-insoluble, were flaked while being fed as a solution or a dispersion in a non-viscous liquid to an apparatus having a nip as schematically illustrated in Fig. 4 or in Fig. 5. The materials tested, which may serve as tastants and/or other purposes in additional industries, included A: salt, citric acid, potassium chloride, sodium bicarbonate, and sodium phosphate monobasic and dibasic, which are considered water- soluble materials; and B: calcium carbonate, a dye, magnesium stearate, silica and zinc oxide, which are considered water-insoluble materials.

Regarding non-limiting prospective uses of the water-soluble materials flaked in the present example, both salt and citric acid (E330) are known for their dual roles as flavor enhancers and food preservatives, but both may fulfill many additional functions in other industries. Potassium chloride can serve in the food industry as a substitute to sodium chloride, and as a thickener, a flavor enhancer and a pH regulator. It may also serve as an electrolyte replenisher in medicine, a fertilizer in agriculture, and as a water softening agent in any industry of relevance. While sodium bicarbonate (E500) can provide for a slightly bitter and salty taste, it is better known for its use as leavening agent for baked goods, while having a variety of additional uses in other industries (e.g., as an antacid used in medicine to relieve heartburn and acid indigestion, as a stain remover in personal care or cleaning products, etc.). Sodium phosphate monobasic (E339(i)) and dibasic (E339(ii)), also known as monosodium phosphate (MSP) and disodium phosphate (DSP), are considered relatively tasteless, but can be used as food emulsifiers, thickeners, leavening agents, anti-caking agents or pH controlling agents. In other industries they can be used in detergents and cleaning products, while in medicine they are used as a laxative (e.g., prior to a colonoscopy).

Regarding, non-limiting prospective uses of the water-insoluble materials flaked in the present example, silicon dioxide, also known as silica, can be used for a variety of purposes such as in the construction industry to produce concrete, in hydraulic fracturing (when in its crystalline form), in the production of glass, as a sedative, in the production of elemental silicon, as an anti-caking agent in powdered foods like spices, as a fining agent in juice, beer, and wine, in pharmaceuticals for making tablets and in toothpaste to remove tooth plaque, to name a few. Zinc oxide is used very widely as a bulking agent or filler, and as a white pigment. It is found in some rubber, glass and ceramic products, and finds use in the chemical industry as a catalyst. It is also used in paints as a corrosion inhibitor and for mildew control. As zinc is an essential trace element, zinc oxide is also added to fertilizers, animal feed, and vitamin supplements. It is also used in cosmetic and medical products for its antibacterial and deodorant properties. Its strong absorption of ultra-violet (UV) light has led to its use in sunscreen products. Near Infra- Red (NIR) dyes, such as NIR983A of QCR Solutions Corp, can served in the preparation of images to be read by specialized infrared detectors, such as serving in security solutions from QR codes to semi-disappearing pictures, or in chemical biology or medicine as research tool or diagnostic imaging. Tumor-specific imaging by NIR dyes may open the way to photothermal, and photodynamic therapies. Magnesium stearate can serve in the food industry, as well as in the pharmaceutical one, typically as an emulsifier, a binder, a thickener, as well as an anticaking, lubricant, release, and antifoaming agent. The many uses of calcium carbonate have been previously illustrated and shall not be repeated.

As to the procedure, regular table salt (sodium chloride, NaCl) having an average diameter of about 500 pm was first briefly ground in a coffee grinding machine to produce a finer salt with grains having an average diameter of about 50 pm. The extra fine salt was mixed at room temperature at a weight ratio of 1 :3 into water until complete dissolution. For reference, this solution is considered nearly saturated, the weight percent concentration of the sodium chloride per total weight of the solution being 25 wt.%, while a solution would be saturated at about 35 g of sodium chloride per 100 g pure water (/.< ., at about 26.5 wt.% of salt per total weight of the solution) at the same temperature. The resulting liquid stock was fed to the nip of an apparatus as schematically illustrated in Fig. 4. Both rotating cylinders 410 and 420 were made of stainless steel 17-4 PH® (having a Vickers hardness of 240 HV and an average surface roughness R_a of less than 1,600 nm), had a diameter of 30 cm and an axial length of 25 cm. They were counter-rotated at a similar speed of 60 rpm, while being urged into contact by a calculated Hertz contact pressure of 370 MPa using a compressing mechanism (hydraulic piston) providing a force of 7.5 ton-force, the surfaces of the rotating cylinders being at ambient temperature. After a single application of 0.5 ml of liquid at about the middle of the cylinder so it may extend along the nip in both opposite directions parallel to its axis and 38 passages through the nip, salt flakes were collected using a suitably oriented doctor blade as previously detailed. This experiment and the resulting flakes were named LF-1. SEM-FIB micrographs were taken, as previously described, at the beginning and end of the flaking process, and average dimensions were assessed on at least 10 individual grains or flakes detectable in the field of view. Figure 10A is a picture at a magnification of X100 of salt grains, before being dissolved and fed to the apparatus, while Figure 10B is a picture at a magnification of XI, 000 of salt flakes as obtained under the afore-described conditions.

The conditions and results obtained by the afore-detailed and similar liquid flaking methods are summarized in Table 3 A and following paragraphs, when the materials were water- soluble, and in Table 3B, when the materials were water-insoluble. In each part of this table and example, water stands for pure double distilled water and Citric Ac. stands for citric acid. For the sake of LF-2 and LF-3, the surfaces of rotating cylinders 410 and 420 were pre-heated to the desired temperature by blowing hot air towards the rotating surfaces. Furthermore, the liquid stocks of salt solution and salt dispersion were applied at the same temperature (as obtained by stirring the liquid stocks on a hot plate). For the sake of LF-4 and LF-5, the apparatus included a series of nips as schematically illustrated in Fig. 5. For LF-4, rotating cylinders 510, 520 and 530 were as described in Example 1. For LF-5, a series of six identical cylinders linearly aligned was used, allowing for a single passage through any of the nips, continuous application of liquid stocks on the first cylinder and continuous collection of tastant flakes on the sixth cylinder. For LF-6, the configuration was similar to the one described for LF-1, except for the nearly saturated stock of tastant being made of citric acid (HOC(CO2H)(CH₂CO2H)2). Table 3A

Figure 11A is a picture at a magnification of XI 00 of salt grains, before being dispersed and fed to the apparatus, while Figure 11B is a picture at a magnification of XI, 000 of salt flakes as obtained under the conditions above described for LF-3. As for LF-1 to LF-6, in the following experiments not reported in previous table, 0.5 ml of liquid stock was applied as a single dose at about the center of the length of the cylinder to facilitate an even distribution of the liquid along the nip.

In LF-7, the configuration was similar to the one described for LF-1, except that instead of feeding a solution, the liquid stock was fed as a dispersion. The stock was prepared by dispersing salt into a liquid in which it is not soluble. Fine salt grounded to have an average diameter of about 50 pm was dispersed at 3 g in 100 ml of isopropyl alcohol. It was found that after 10 passages through the nip, flakes of sodium chloride having an average thickness t of about 3 pm, an average longest planar dimension L of about 400 pm, with an aspect ratio ASP of approximately 133. The thickness is comparable to LF-1, the planar dimension of the flakes (and the aspect ratio) being relatively larger. Notably, as isopropyl alcohol is more volatile than water, in particular at room temperature in which the experiment was carried out, the flakes were obtained more rapidly from the dispersion in the alcohol than from the solution in water. Figures 12A and 12B are pictures at a magnification of X100 of salt, respectively as grains before being dispersed and fed to the apparatus in a liquid improper for their solubilization, and as flakes obtained under the conditions above described for LF-7.

For LF-8 to LF-10, the configuration was similar to the one described for LF-1, except that the cylinders were rotated at room temperature at a speed of 120 rpm, instead of 60 rpm.

In LF-8, the nearly saturated stock of water-soluble material was made by dissolving sodium bicarbonate (NaHCOs) at a 1 : 10 weight ratio in water. It was found that after 40 passages through the nip, the sodium bicarbonate which was globular with an average diameter of about 70 pm before being dissolved yielded by this method flakes having an average thickness t of about 1.5 pm, an average longest planar dimension L of about 40 pm, with an aspect ratio ASP of approximately 27.

In LF-9, the nearly saturated stock of water-soluble material was made by dissolving sodium phosphate dibasic (NaiHPCL) at a 1 : 10 weight ratio in water. It was found that after 10 passages through the nip, the sodium phosphate dibasic which was globular with an average diameter of about 200 pm before being dissolved yielded by this method flakes having an average thickness t of about 4 pm, an average longest planar dimension L of about 60 pm, with an aspect ratio ASP of approximately 15.

In LF-10, the stock of water-soluble material was made by dissolving sodium phosphate monobasic (NaELPCh) at a 1 : 14 weight ratio in water. It was found that after 10 passages through the nip, the sodium phosphate monobasic which was globular with an average diameter of about 400 pm before being dissolved yielded by this method flakes having an average thickness t of about 6 pm, an average longest planar dimension L of about 150 pm, with an aspect ratio ASP of approximately 25. Figures 13A and 13B are pictures at a magnification of XI 00 respectively of grains of sodium phosphate, before being dispersed and fed to the apparatus, and of flakes as obtained under the conditions above described for LF-10.

In LF-11, the cylinders were made of zirconia (having a Vickers hardness of 1300 HV and an average surface roughness R_a of about 250 nm) instead of stainless steel and each cylinder of the pair had a diameter of 6 cm instead of 30 cm, their axial length being of 6 cm. A liquid stock made of a solution of extra fine salt prepared as described in LF-1 was applied at room temperature to a cylinder while rotating at 300 rpm. The cylinders of zirconia were urged into contact by a calculated Hertz contact pressure of 350 MPa using a suitably set compressing mechanism, in the present case a pneumatic piston. The flakes obtained after 150 passages through the nip had an average thickness t of about 5 pm, an average longest planar dimension L of about 400 pm, with an aspect ratio ASP of approximately 80.

In LF-12, the cylinders were made of zirconia, each cylinder having a diameter of 11 cm and an axial length of 25 cm. A liquid stock made of an aqueous solution of 25 wt.% of potassium chloride (KC1) having an initial grain size of about 500 pm was applied to a cylinder heated to 70°C while rotating at 100 rpm. The cylinders of zirconia were urged into contact by a calculated Hertz contact pressure of 225 MPa using a suitably set pneumatic compressing mechanism. The flakes obtained after 35 passages through the nip had an average thickness t of about 25 pm, an average longest planar dimension L of about 450 pm, with an aspect ratio ASP of approximately 18.

Salt flakes LF-13 were prepared in a setup similar to the one described for LF-12, except that the cylinders were heated to 65°C while rotating at 250 rpm. Moreover, the liquid stock was not applied as a single dose of 0.5 ml at a single central site along the nip, as for LF-1 to LF-12, but as a larger dose at multiple points to facilitate an even distribution of the liquid along the nip. In LF-13 an aqueous solution of 25 wt.% of sodium chloride having an initial grain size of about 500 pm before dissolution was synchronously applied at three sites along the nip, each site receiving a dose of about 1.2 ml. The flakes obtained after 40 passages through the nip had an average thickness t of about 25 pm, an average longest planar dimension L of about 800 pm, with an aspect ratio ASP of approximately 32.

The materials and conditions for the preparation of LF-14 to LF-18, relating to the flaking of water-insoluble materials whether dispersed or dissolved, and the flakes obtained thereby are summarized in Table 3B, in which Mg Ste. Stands for magnesium stearate. For all samples, the configuration of the nip was according to Fig. 4, wherein two cylinders of stainless steel each having a diameter of 30 cm and an axial length of 25 cm were rotated at 60 rpm, and the liquid stocks and surfaces were at room temperature. Furthermore, since the pressure applied by a hydraulic piston was of 370 MPa for each sample of this series, this information is omitted from the following table. In all cases, 0.5 ml of liquid stock was applied as a single dose at a central position along the nip. Table 3B

LF-14 to LF-17 represent dispersions, the water-insoluble materials not dissolving in water at their added concentration, whereas in LF-18 the non-aqueous liquid (namely acetone) was adapted to dissolve the NIR dye. As can be deduced from the dimension of the flakes obtained in this series of experiments, flakes are typically composed of solid particles compacted in the present process by cyclically passing through the nip. Moreover, in view of the planar dimension of the flakes, it is anticipated that agglomeration of particles is also taking place. This latter assumption was confirmed by applying liquid stocks containing much smaller dispersed particles, the flakes formed thereby having in some instances a thickness exceeding the size of a single particle, and certainly of a single compacted particle, if subjected to appropriate operational conditions. For illustration, ZnO particles having a ten-fold smaller initial diameter of about 0.5 pm were shown to produce flakes having a thickness larger than 2 pm.

Figures 14A and 14B are pictures of calcium carbonate at a magnification of XI, 000 and XI 00, respectively of grains, before being dispersed and fed to the apparatus, and of flakes as obtained under the conditions above described for LF-14.

Figures 15A and 15B are pictures of NIR dye NIR983A at a magnification of XI, 000, respectively of grains, before being dissolved and fed to the apparatus, and of flakes as obtained under the conditions above described for LF-18.

Example 4: Improved Dissolution Rate of Flakes

In this example, flakes prepared according to Example 3 were tested for their rates of dissolution in water at room temperature, as compared to the rate of dissolution of different types of unflaked references. Unless otherwise stated, all experiments reported in this and following examples were performed on flakes actively detached from the surface of the rotating cylinders upon which they were formed using a suitably oriented doctor blade.

The dissolution rates of flakes made of salt were determined by measuring the electrical conductivity of various salt compositions prepared from sample tastants or references dissolved in water, the dissolution of the salt changing the ionic conductivity of the solution. 40 mg of salt samples previously dried for at least two hours at 120°C and kept thereafter at room temperature in a dessicator, were added to 80 ml of double distilled water at room temperature under ongoing stirring at 400 rpm. Conductivity was measured using a Keithley 2750 Multimeter, by applying an alternating voltage via electrodes immersed in the solution samples and measuring the resulting current. Conductivity, hence measured current, increased as long as the salt was dissolving, then reached a plateau. The time that lapsed between the addition of the salt and plateau values of current was recorded. Each conductivity measurement was repeated at least three times and the duration of dissolution till current stabilized to plateau values, as measured with a chronometer in seconds, before and after flaking is reported as an average of all repeats in Table 4.

Table 4

The rate of dissolution was also qualitatively assessed by placing a known amount of a sample on a glass slide and adding at a distance therefrom a known volume of a solvent, in an amount sufficient to dissolve the solid by capillarity once a liquid bridge is formed by the operator while observing the outcome using a confocal microscope under a magnification of x228. For each material, two samples were tested, first the unflaked raw material, then the flaked version of the same. Observations were made in repeats for all samples. By this method it was found that the rates of dissolution of sodium phosphate monobasic monohydrate and sodium phosphate dibasic in water were visibly faster when these materials were flaked as described in LF-10 and LF-9, respectively.

Example 5: Density of Tastants

In this example, tastant flakes made of sodium chloride or potassium chloride and prepared according to Example 3 were tested for their bulk and tap densities, as compared to the bulk and tap densities of unflaked standard powders which served for their preparation, as references.

The flakes of sodium chloride and potassium chloride were prepared as described for LF- 11 and LF-12, respectively. The bulk density pp, of each sample was measured by weighing the mass of a previously dried sample filling in a known bulk volume VB as measured in a finely graduated cylinder. Then the vessel was repeatedly tapped until the volume no longer contracted, the final constant value serving to estimate the tapped volume VT from which the tapped density pr was calculated. Typically, the tapping lasted up to one minute at a pace of two taps per second. Flaked tastants were collected from two sources, first when spontaneously detaching from the surface of the rotating cylinder, secondly when actively detached by placing a blade on the surface of the rotating cylinder, the blade being oriented to peel away the flakes. The results are presented in Table 5 in which spontaneously detached flakes are annotated by an S superscript and actively detached flakes are annotated by an A superscript. Additional information and factors calculated therewith are also presented.

Table 5

As can be seen from the above table, the flakes prepared as presently taught tend to a have a lower bulk density pp, and a lower tapped density pr than the corresponding values of a reference (unflaked) material. Moreover, the F2 ratio (F2= pr/pp>) of the flaked samples was greater than the same ratio as calculated for their respective reference material, which suggests a better packing ability.

Taking into consideration the respective aspect ratios of the flaked samples as compared to their granular source, the factors calculated based on the above measurements led to even greater divergences between flakes prepared as herein taught and their source. For instance, the F3 ratio (F3=ASP/ pp>) of the flakes was at least 60 cm³/g as compared to values between 0.85 and 1.25 cm³/g and the F4 ratio (F4=ASP/ pr) of the flakes was at least 40 cm³/g as compared to values between 0.74 and 0.79 cm³/g.

Example 6: Crystallographic Analysis of Crystalline Tastants

Analysis of the crystallographic structure of salt flakes by X-ray powder diffraction (XRPD) was performed on pellets of compressed flakes. The data were collected on a Panalytical Empyrean III multi-purpose diffractometer (K_a radiation, k=l .541 A) equipped with a pixCEL 3D detector in ID line-detector mode, and with an X-ray tube operated at v=45 kV, I = 40 mA. Each sample was mounted directly in a stainless-steel, ring, back-filled sample holder. The sample was rotated at 8 rotations/min during the measurement, which was run from 5-140° 29. Phase identification and Size-Strain analysis by Reitveld refinement was performed using the HighScore Plus powder diffraction data analysis suite (version 5.1), coupled with the ICDD (International Centre for Diffraction Data) Powder Diffraction File (PDF-4+) database (2022).

Pellet 1 was made of grains of standard table salt having an average diameter of about 500 pm (which served when grounded to form the extra fine salt), pellet 2 was made of grains of extra fine salt having an average diameter of about 50 pm (which served when dissolved to form the flakes of LF-1) and pellet 3 was made of the resulting salt flakes LF-1 prepared as described in Example 3.

The diffraction peaks obtained from the analyzed samples appeared to be relatively similar with respect to their respective positions and included known characteristic peaks of sodium chloride such as detected at about 31.7°, 45.4°, 66.2°, and 75.3°, to name a few. The diffraction peaks of the flaked sample seemed mildly broader than their counterparts as obtained from the reference granular sample. Phase identification indicated that all samples contained more than 99.5 wt.% of NaCl. The microstrain values only (in percentage) and the crystallite size of each sample are reported in Table 6.

Table 6

As can be seen from the above-table, thin flakes prepared by the present method display a crystallite size about 4-fold smaller than the original material from which they were prepared, the microstrain values being at least 3 -fold higher. Similar results showing a crystallite size smaller than starting material was observed with additional samples of salt flakes prepared according to the present teaching. To understand whether these significant changes were due to the shape of the manufactured material as flakes or to their method of preparation, a similar analysis was performed on conventionally prepared flakes of salt commercially available under the trade name Cargill Alberger® Shur-Flo® Fine Flake Salt. The crystallite size of this control was found to be 2,513 A with a microstrain of 0.017%, closer to the results observed with Pellet 1 than with Pellet 3. It is therefore believed that the values monitored on flakes freshly prepared by the present method result from the manufacturing process which involves repeated compaction, rather than from the mere shape of the material as a flake. Thus, the crystallographic analysis of flakes made of crystalline material, when displaying a smaller crystallite size and/or a larger microstrain value than a same material conventionally prepared, suggest that such flakes were prepared by the present method. Such identification is facilitated when the flakes have not yet been subjected to environmental conditions deleterious to their crystalline structure. For example, if the material is hygroscopic, such as salt, exposure to humidity may affect the flakes. It is therefore preferable to perform such analysis on freshly prepared flakes, or on flakes suitably preserved from agents capable of affecting their crystallographic behavior.

Example 7: Flakes Made of a Blend of Materials Including Tastants

Flakes can be prepared from a liquid stock comprising more than one material, allowing for instance to combine two or more tastants. The following mixtures were prepared according to Example 3 with the modifications indicated below and summarized in part in Table 7.

In a first series of experiments, the materials being mixed to jointly form flakes were tastants individually supplied. The first tastant was table salt made of grains having an initial diameter of about 500 pm which was dissolved at a weight per weight ratio of 1 :3 in water (i.e. , at 25 wt.%). 34g of this solution of NaCl were used to grind and homogenize 16g of fresh hot red peppers in a Ninja blender (Model Nutri-Blender Plus BN303) operated at a power of 700 Watt for about 20 seconds till a smoothie-like mixture was obtained. The mixture was filtered by decantation through a cloth to separate the pulp. The brownish liquid stock so separated was then fed to a nip according to Fig. 4, formed between two identical cylinders of stainless steel on which a sleeve made of zirconia was mounted, each cylinder with the sleeve mounted thereon having a diameter of 11 cm and an axial length of 20 cm. The cylinders were heated to 65°C and rotated at 250 rpm, while being urged into contact one with the other at a calculated Hertz contact pressure of 365 MPa using a pneumatic piston. 1.5 ml of the liquid containing the salt and the hot pepper extracted in the blending process was synchronously applied at two sites along the nip, each dose being of 0.75 ml. After 45 passages through the nip, flakes containing a mix of salt and fresh hot pepper savor were collected by gravitation, the flakes detaching from the cylinders over time. This experiment and the resulting flakes were named LF-19 and their average dimensions were assessed by microscopy as previously detailed through analysis of 20-30 individual particles. The conditions and results obtained by the afore-detailed liquid flaking methods for preparing flakes of mixed materials, such as flavored or colored salt, are summarized in Table 7 in which the description of the nip and its operating settings are not repeated.

Table 7

As can be seen, all flakes so prepared achieved an aspect ratio of at least 55. Besides assessing their dimensions, they were tested for their savor and/or color. LF-19 and LF-20 flakes provided a hot spicy taste in addition to the salty base. LF-19 flakes were slightly brownish, LF-20 flakes were faintly red tinted and LF-21 flakes more strongly red tinted without any change in taste.

In a second series of experiments, the materials jointly forming the flakes prepared according to the present teachings were detergents supplied as a mixture. As appreciated, powdered detergents, as used for laundry, can be problematic if they do not dissolve properly during the washing process. For instance, they may leave solid residues that can cause white stains on clothes and/or a buildup in the washing machine’s drain, especially when used with cold or hard water. The laundry powders typically contain a complex mixture of agents including surfactants (non-ionic, anionic and/or cationic) to remove the stains, chelating agents (e.g., to stabilize other agents, ensuring the effectiveness of the detergent under broad conditions, to remove malodors, etc.), polymers (e.g., to prevent the stains from returning to the garment they have been removed from), builders (e.g., to soften the water, buffer its pH, facilitate emulsification of oily stains, etc.), bleaching agents, oxidizing agents, fabric conditioners, pH buffering agents, enzymes, solubilizers, pigments, and fragrances, some of the foregoing materials constituting the mix suffering from poor solubility in water, under particular conditions.

A commercially available laundry powder (Ariel, manufactured by Procter & Gamble) with relatively coarse grains of detergent having on average an initial diameter of about 500 pm was suspended at a weight per weight ratio of 1 :9 in water (i.e., at 10 wt.%). The liquid stock suspension was then fed to a nip according to Fig. 4, formed between two identical cylinders of stainless steel having a diameter of 30 cm and an axial length of 25 cm. The cylinders were rotated at 120 rpm, in absence of any heating, while being urged into contact one with the other at a calculated Hertz contact pressure of 370 MPa using a hydraulic piston. After a single application of 1 ml of the liquid stock at a relatively central position along the nip and 40 passages through the nip, flakes containing the detergent mix were detached from the cylinders’ surfaces using a suitable scraper. This experiment and the resulting flakes were named LF-22 and their average dimensions were assessed by microscopy as previously detailed through analysis of 20-30 individual particles. The average thickness t of the flakes of detergents was found to be of about 10 pm, for a longest planar dimension L of about 600 pm on average and a calculated aspect ratio of about 60.

In an additional experiment, the “coarse” grains of detergent were briefly ground in a coffee grinding machine to produce a finer detergent with grains having an average diameter of about 50 pm. The finer detergent was suspended at a weight per weight ratio of 1 : 1 in water (i.e., at 50 wt.%), all other parameters of the process being as described for LF-22. This experiment and the resulting flakes were named LF-23, the flakes having dimensions similar to the ones previously measured for LF-22 flakes.

The respective rates of dissolution of LF-22 and LF-23 detergent flakes in water as compared to the detergent coarse granular powders they were directly or indirectly prepared from, DT determined in seconds, were assessed according to the method previously detailed in Example 4. 110 mg of samples (LF-22 or LF-23 flakes, or the native crude grains) were added to 80 ml of water under stirring at 970 rpm. While it took 13.27 seconds for the reference powder to dissolve, the flakes prepared as aforesaid achieved a similar solubilization about 10- times faster in only 1.34 and 1.49 seconds, respectively.

The bulk and tap density of LF-22 detergent flakes was compared to the corresponding densities of the detergent coarse powders they were prepared from, the pp, and pr densities of each being assessed according to the method previously detailed in Example 5 and provided in grams per cubic centimeter. The bulk density decreased from 0.80 g/cm³ for native grains of detergent to 0.40 g/cm³ for flakes of the same, while the tap density decreased from 0.93 g/cm³ for the reference to 0.64 g/cm³ for LF-22 flakes.

The factors that were calculated based on these measurements led to even greater divergences between flakes prepared as herein taught and their reference material. For instance, the present flakes displayed an Fl ratio (F1=ASP/ DT) of about 44.78 sec'¹ as compared to 0.08 sec'¹ for native grains of detergent, an F2 ratio (F2= pr/pp,) of about 1.60 as compared to 1.16, which suggests a better packing ability, an F3 ratio (F3=ASP/ pp>) of 150 cm³/g as compared to 1.25 cm³/g and an F4 ratio (F4=ASP/ pr) of 93.75 cm³/g as compared to about 1.08 cm³/g.

The above results further support that materials other than tastants, and mixtures as well as pure compounds, may benefit from the present teachings. In the case of detergents, the improved dissolution of the active ingredients (being approximately 10-fold more rapid) is expected to increase their efficacy in a manufactured article (e.g., a laundry powder) comprising or consisting of the same. Such increased efficacy may alternatively, or additionally, allow to reduce the amount of the active ingredients in the end-product, while maintaining a similar efficacy as compared to an analogous article comprising the same active ingredients in a different (e.g., conventional) shape.

Example 8: Effects of Various Parameters on Process and Flakes

As readily appreciated and previously detailed, a number of operational parameters can be modified in the method according to the present teachings. These variables predominantly relate to the materials being fed to a nip (e.g., volume of application, number of points of application along a rotating cylinder, frequency of application, concentration of material in each dose, nature of the dissolving/dispersing liquid, etc.) and to the working conditions of a suitable apparatus (e.g., area of the rotating cylinders (axial length and diameter), speed and temperature of the cylinders, length of the nip, pressure at the nip, etc.). In this example the effect of the foregoing exemplary parameters has been studied.

Unless otherwise stated in the following tables, each experiment was performed by repeatedly applying every few seconds (e.g., less than every minute), a single dose of 1 ml of a liquid stock comprising 25 wt.% of table salt having grains with an initial diameter of about 500 pm dissolved in water. The doses were each time applied to a central position along a nip according to Fig. 4, once the previously applied liquid dose was transformed into flakes which could detach from the rotating cylinders, such that their surfaces could again be available for the formation of new flakes by application of a fresh dose. The periods of time between application of subsequent doses were recorded for each experiment, since depending on the operating conditions (e.g., the temperature of the cylinders, their dimensions and speed, the volume of each dose and the concentration of material in each dose, on ambient humidity, and like factors). These observed periods of time were then used to calculate the frequency of application in number doses per hour. For illustration, if in a particular experiment 10 seconds elapsed between two applications, the frequency of application can be said to be 360 doses/h.

The nip was formed between two identical cylinders of stainless steel on which a sleeve made of zirconia was mounted, each cylinder with the sleeve mounted thereon having a diameter of 11 cm and an axial length of 20 cm. The parameters tested included the temperature of the cylinders (25°C, 45°C, 60°C, 75°C and 90°C), their rotational speed (100 rpm, 200 rpm, 250 rpm, 300 rpm and 400 rpm), the calculated Hertz contact pressure at which they were urged into contact (110 MPa, 182 MPa, 258 MPa, 365 MPa, and 447 MPa) using a pneumatic piston, the volume applied (0.6 ml, 1 ml, 1.8 ml, 3 ml, 6 ml, 9 ml and 10 ml), the number of application points along the nip (1 and 3) and the final concentration of the salt in the water (25 wt.% and 59 wt.%). Experiments were terminated after 10 minutes from application of the first dose and the flakes collected under the different setups were weighted to assess the production rates and/or analyzed to determine their average dimensions or any other feature of interest (e.g., their water contents, if any) by any suitable method.

Details on each experiment, including modifications from the main setup and the frequency at which doses were applied, as well as exemplary results are summarized in the following Tables 8A to 8D. Table 8A - Impact of Temperature

As can be seen from the above table, gathered from a run of experiments in which a single dose of 1 ml was applied, raising the temperature of the rotating cylinders (both being heated, when relevant, to the temperature indicated in the table by internal electric heating elements) improved the rate of production of the flakes as expected from the acceleration of evaporation of the water out of the applied liquid stock, which in turn increased the frequency at which doses could be applied to the rotating cylinders’ nip.

Under the present study conditions, the temperature in the elevated range did not seem to have a significant effect on the dimensions of the obtained flakes. All flakes obtained at elevated temperatures had a relatively similar average thickness t of about 25 pm, average longest planar dimension L of about 1,200 pm and an aspect ratio ASP of about 48, the flakes obtained at room temperature being thinner and smaller (t ~10 pm, L -500 pm) than those obtained at higher temperatures, the aspect ratio being similar at all temperatures. A similar behavior of the production rate and frequency of dose application increasing with the temperature at the nip was observed at additional rotational speeds of 100 rpm, 300 rpm and 400 rpm.

Similar experiments were performed while pre-heating the stock solution prior to its application to the nip to a temperature similar to the temperature of the rotating cylinders, when heated to be above ambient temperature. Under the present study conditions, pre-heating the liquid to a temperature matching the surface temperature of the cylinders did not seem to significantly affect the resulting production rate, nor the flakes’ sizes.

Table 8B - Impact of Speed

As can be seen from the above table, gathered from a run of experiments in which a single dose of 1 ml was applied, raising the rotational speed of the cylinders increased the rate of production of the flakes as expected from the resulting augmentation of the number of passages of the applied liquid stock through the nip within a same time period. This, together with the speed itself favoring evaporation, accelerated the removal of the liquid from the applied dose, so that a subsequent dose could be applied at an increased frequency. The production rate tended to reach a plateau at higher speeds. Under the present study conditions, the rotational speed did not seem to have a significant effect on the dimensions of the flakes when increased from 100 rpm to 400 rpm. All resulting flakes had a relatively similar average thickness t of about 25 pm, average longest planar dimension L of about 1,200 pm and an aspect ratio ASP of about 48. A similar behavior of the production rate increasing with the rotational speed of the cylinders was observed at additional temperatures of 45°C, 75°C and 90°C.

For comparison, an experiment termed LF-LS was performed in a similar nip at the low speed of 3 rpm, the cylinders being heated to 90°C, the applied pressure being the same 365 MPa. While the rate of production of 60 g/h was comparable to what could be achieved at about 150 rpm and 60°C, this dramatic slowdown of the rotational speed affected the size of the flakes obtained thereby. LF-LS flakes were about 5-fold larger (£ -6,400 pm) and 8-fold thicker (t -195 pm) than their counterparts manufactured at high speed (100-400 rpm), their aspect ratio being accordingly reduced from 48 at higher speeds to 33 at lower speed. Without wishing to be bound to any particular theory, it is believed that as the lower speed reduces the number of passages through the nip during a predetermined period of time (e.g., 10 minutes in the present experiment), this in turns reduces the exposure of the liquid stocks and the films and coats forming therefrom to the compacting environment of the nip. It is additionally assumed that higher speeds provide for a greater relative velocity between the outer surfaces of the cylinders and the surrounding air, facilitating the removal of vapors of the liquid as they form.

Table 8C - Impact of Contact Pressure

As can be seen from the above table, increasing the calculated Hertz contact pressure perceived at the nip increased the frequency at which doses were repeatedly applied and raised the rate of production of the flakes in a non-linear manner, each tending to reach a plateau at higher pressures. Noticeably, in the phase preceding the plateau, the pressure at the nip also affected the thickness of the flakes and their longest planar dimensions, their aspect ratio however remaining relatively stable.

While not shown in the above tables, it has also been verified that increasing the surface of the cylinders, as achieved by using rolls having a larger diameter, can comparatively increase the production rate and the frequency of application, all other parameters being the same, but for the dimensions of the flakes that can be obtained.

Table 8D - Impact of Dose Size

As can be seen from the above table, increasing the volume of stock liquid dispensed to the nip at each application decreased the frequency at which new doses were required and raised the rate of production of the flakes in a non-linear manner, the production rate tending to reach a plateau at higher dose sizes. The optimum volume of an individual dose is expected to depend inter alia on the dimensions of the cylinders (setting the length of the nip and the surface that may be coated by the liquid film), their temperature, the speed at which they are rotated, and the force applied to reach any predetermined contact pressure at the nip. Interestingly, the volume of the applied dose may also affect the thickness of the flakes, but less so their longest planar dimensions, thus also impacting the aspect ratio of the flakes.

In a similar experiment conducted at 90°C, 250 rpm, and 365 MPa with doses of 1 ml, the impact of the concentration of the material (in the present case, sodium chloride) was assessed. When the concentration of salt was raised from 25 wt.% to 59 wt.%, the rate of production of the salt flakes concurrently increased from 244 g/h to 566 g/h, when the frequency of application was 976 and 959 doses/h respectively. As the liquid stock comprising 59 wt.% of salt is not a solution, but an overloaded dispersion, in this experiment the sample solutions regardless of final concentration of solids were prepared using extra fine sodium chloride in- house ground to have a grain size of less than 5 gm, instead of previous 500 pm. Under the present study conditions, the initial concentration of salt in the liquid stock did not seem to have a significant effect on the dimensions of the flakes. All had a relatively similar average thickness t of about 18 pm, average longest planar dimension L of about 1,400 pm and an aspect ratio ASP of about 78. A similar behavior of the production rate increasing with the concentration of salt in the liquid stock was observed at additional temperatures of 45°C and 75°C.

In a similar experiment conducted at 65°C, 250 rpm, and 365 MPa, the impact of the number of sites of application along the nip was tested, the total volume each time applied remaining the same. When the liquid stock was applied at a single (central) site along the nip (as done so far) and at a dose of 1.8 ml, the rate of production of the salt flakes was found to be 132 g/h. When the same liquid stock was instead applied to three equally spaced sites along the nip, each site receiving a dose of 0.6 ml (hence, 1.8 ml in total), the rate of production of the salt flakes increased to 175 g/h. Under the present study conditions, the number of sites employed along the nip to apply the liquid stock did not seem to have a significant effect on the dimensions of the flakes. All had a relatively similar average thickness t of about 20 pm, average longest planar dimension L of about 1,200 pm and an aspect ratio ASP of about 60.

It has been found by the Inventors that the torque of the motor rotating the cylinders may assist predicting suitable periods of time between application of subsequent doses, hence frequency of application. It is believed that upon application of a first dose, the liquid spreading along and throughout the nip generates a force resisting the rotation of the cylinders, which gradually decreases with the elimination of the liquid. When the flakes formed by the application of the first dose are ready (e.g., relatively dry), the motor(s) rotating the cylinders displays the lowest values of torque required to maintain an essentially constant speed. At such a point in the cycle, the flakes can be removed (or spontaneously detach), and a new dose applied upstream of the nip to start a further cycle of preparation. Hence, over time and repeated application of fresh doses of material to be flaked, the torque values of the motor follow a sinusoidal curve. This can be harnessed for a feedback mechanism in which the torque of motors rotating the cylinders is monitored, a signal being sent to a dispenser of the liquid stock to release a new dose each time the monitored torque reaches its smallest value under the operating conditions.

In all afore-said experiments, the production rate provided in grams per hour was assessed by weighing all the flakes produced within runs of 10 minutes and calculating accordingly the weight to be expected over a period of 60 minutes. The flakes were also sampled to determine their moisture content. For this purpose, about 1 g of each of the flakes produced under the above-detailed conditions were placed in an aluminum crucible and their exact weight measured, the crucibles were then placed for 2 hours in oven set to 120°C to eliminate residual water. The weight of the dried samples was determined, and their moisture content was calculated. All flakes produced in the present example were found to have less than 1 wt.% water content.

Example 9: Comparing Present Flakes to Commercial Samples

Flakes prepared according to the present teachings and afore-said exemplary experiments were compared to commercially available samples of the same material, some deemed granular and others “platelet-like”. In the present example, all tested items were made of sodium chloride. Four types of flakes prepared as herein described using a liquid stock of 25 wt.% of salt having initial grains’ diameter of 500 pm were named LF-24 to LF-27. Conditions of their preparation and average of their measured dimensions are provided in Table 9.

Table 9

Nine commercially available samples of sodium chloride, named CS-1 to CS-9, were independently tested for their dimensions by the same microscopy method as applied to the afore-said flakes. Average of their measured dimensions are provided in Table 10, one of the two dimensions being ignored and marked with a negative sign for substantially granular samples displaying an aspect ratio of about 1.

Table 10

As can be seen from the above tables, none of the comparative salt samples tested, despite some being commercialized as “flakes”, displayed an aspect ratio of more than 10, the highest calculated aspect ratios being 7.2 for CS-1 flakes and 6.9 for CS-3 Diamond Crystal® having a distinct, hollow-pyramid crystal shape, claimed to provide superior sensory benefits, rapid solubility, strong adherence, and lower bulk density. For reference, the flake samples listed in Table 9 and prepared according to the present method have all an aspect ratio of 35 or more.

LF-24 to LF-27 and CS-1 to CS-9 were tested head-to-head a) for their rate of dissolution DT, determined in seconds as previously detailed in Example 4 safe for the stirring of the sample being now set at 970 rpm instead of 400 rpm; and b) for their bulk pa and tapped pr density, determined in grams per cubic centimeter as previously detailed in Example 5.

The results of these comparative studies and factors calculated therefrom, as detailed in the following, are summarized in Table 11.

Table 11

As can be seen from the above table, and confirmed in a different series of experiments, flakes according to the present disclosure displayed a rapid dissolution essentially all taking place in less than about 2 seconds, most even dissolving in less than 1 second. For comparison, CS-5 which served to prepare the present flakes provided dissolution within 8.95 seconds in the same series of experiment (in agreement with previously found 8.7 s). Furthermore, the commercially available materials closest to flakes in the present series, namely CS-1 and CS- 3, displayed a dissolution time of at least 3 seconds. This suggests that the present flakes may favorably achieve dissolution rapidly and faster than existing products deemed similar.

Noticeably, when calculating a ratio Fl between the aspect ratio of the sample ASP and its rate of dissolution I)T. which can be mathematically expressed by F1=ASP/ DT (having units of seconds'¹), the difference between flakes according to the invention and commercially available comparative samples was found remarkable. While on average the comparative samples displayed a factor Fl of about 0.76, the highest values observed for CS-1 and CS-3 being respectively 1.59 and 2.32, the average value displayed by the flakes prepared as herein taught was about 60-fold higher, the lowest Fl factor in this set being above 15.

Regarding the bulk and the tap density of the samples, it is seen that generally flakes according to the invention have smaller densities than the commercially available comparative samples. The difference between the two groups can be enhanced by calculating a unit-less ratio F2 between the tap density pr and the bulk density pp> of each sample, which can be mathematically expressed by F2= pr/ps. While on average the tap density of the comparative samples is about 20% higher than their bulk density (z.e., F2 -1.19), the difference between these types of densities rises to 96% (z.e., F2 -1.96) when considering the flakes prepared as herein taught. This suggests that the present flakes may favorably have a better packing ability than existing products, which may facilitate their packaging, storage and transport, and therefore be commercially advantageous.

Noticeably, when calculating a ratio F3 between the aspect ratio of the sample ASP and its bulk density pp>, which can be mathematically expressed by F3=ASP/ PB (having units of cubic centimeters per gram), the difference between flakes according to the invention and commercially available comparative samples was found remarkable. While on average the comparative samples displayed a factor F3 of about 4.61, the highest values observed for CS-1 and CS-3 being respectively 16.7 and 11.8, the average value of F3 displayed by the flakes prepared as herein taught was more than 40-fold higher, the lowest F3 factor in this set being above 90.

A similar outcome was observed when calculating a ratio F4 between the aspect ratio of the sample ASP and its tap density pr, which can be mathematically expressed by F4=ASP/ pr (having units of cubic centimeters per gram). While the comparative samples displayed on average a factor F4 of about 3.96, the highest values observed for CS-1 and CS-3 being respectively 14.18 and 10.58, the average value of F4 displayed by the flakes prepared as herein taught was about 25-fold higher, the lowest F4 factor in this set being above 60.

In summary of the comparisons performed in the present example, flakes according to the invention are believed to be distinct from available products deemed equivalent. The features distinguishing the present flakes can be in values directly measurable, e.g., the flakes being relatively thinner and/or having a relatively larger longest dimension, and/or in values derived from such measurements, e.g., the calculated aspect ratio between their characterizing sizes being relatively higher than standard flakes. Such distinguishing features and the values each measured parameter may assume have been previously discussed and shall not be repeated here.

Among the parameters that can be calculated to emphasize the peculiarities of the present flakes are factors Fl to F4. While the limitations set out below that may, in some cases, characterize these factors have predominantly been established with flakes made of salt, it is believed that the following lower thresholds, upper limits and/or ranges therebetween are not restricted to this specific material, as demonstrated with the detergents described in Example 7.

In some cases, the ratio Fl between the aspect ratio ASP of flakes of the invention and their rate of dissolution I)T. mathematically expressed by F1=ASP/ DT, is 5 or more, 10 or more, 15 or more, 25 or more, 50 or more, 75 or more, or 100 or more. In some embodiments, Fl is equal to or less than 500, less than 400, less than 300, less than 200, or less than 150. In particular cases, Fl is between 5 and 500, between 10 and 300, or between 10 and 150.

In some cases, the ratio F2 between the tap density pr and the bulk density pp> of flakes of the invention, mathematically expressed by F2= pr /pB, is 1.25 or more, 1.50 or more, 1.75 or more, 2.00 or more, 2.25 or more, 2.50 or more, or 2.75 or more. In some embodiments, F2 is equal to or less than 5.0, less than 4.5, less than 4.0, or less than 3.5. In particular cases, F2 is between 1.25 and 5.0, between 1.35 and 4.0, between 1.45 and 3.5, or between 1.55 and 3.0. In some cases, the ratio F3 between the aspect ratio ASP of flakes of the invention and their bulk density pp>, mathematically expressed by F3=ASP/ pa, is 25 or more, 50 or more, 75 or more, 100 or more, 150 or more, 200 or more, 250 or more, 300 or more, or 350 or more. In some embodiments, F3 is equal to or less than 1,000, less than 750, less than 500, or less than 400. In particular cases, F3 is between 25 and 1,000, between 50 and 750, between 75 and 500, or between 100 and 400.

In some cases, the ratio F4 between the aspect ratio ASP of flakes of the invention and their tap density pr, mathematically expressed by F4=ASP/ pi, is 20 or more, 40 or more, 60 or more, 80 or more, 100 or more, 120 or more, 140 or more, 160 or more, or 180 or more. In some embodiments, F4 is equal to or less than 500, less than 400, less than 300, or less than 200. In particular cases, F4 is between 20 and 500, between 40 and 400, between 60 and 300, or between 80 and 200.

Figures 16A to 16E are pictures at a magnification of X100 of commercially available table salts prepared according to the art and having an aspect ratio of at least 2, the pictures being captured by SEM-FIB microscopy as previously described for the present flakes. Fig. 16A shows flakes of CS-1 (Asp ~7.2), Fig. 16B shows Diamond Crystal® hollow particles of CS-3 (Asp ~6.9), Fig. 16C shows topping flakes of CS-4 (Asp ~2.4), Fig. 16D shows coarse flakes of CS-6 (Asp ~2.7), and Fig. 16E shows fine flakes of CS-7 (Asp ~2.4). Figure 16F, presented nearby for convenience of comparison, shows present flakes LF-26 (Asp ~53). As can be seen, though most of the particles of the comparative samples are commercialized as flakes by their suppliers, their shapes as actually observed are closer to flattened chunks than to thin flakes, as confirmed by their relatively low aspect ratio (comprised between 2.4 and 7.2). As can be seen, the higher aspect ratio of the present flakes provides them with a distinctive shape, their planar faces also appearing relatively smoother than the corresponding edges of the samples they were compared to at this magnification.

Example 10: Compressibility of Flakes

When comparing flakes prepared according to the present teachings to commercially available samples of the same material, as done in Example 9, it was found that generally present flakes have smaller densities (pr and/or pp) than the commercially available comparative samples and/or a higher unit-less ratio F2 between their tap density / and their bulk density pp. This suggested that the present flakes may favorably have a better packing ability than existing products. The purpose of this example was to confirm these findings by assessing the compressibility of the flakes and their ability to revert to their original bulk densities following compression.

Flakes named LF-28 were prepared as herein taught by periodically feeding 1.5 ml of a liquid stock of 25 wt.% of sodium chloride to a nip formed between two cylinders having a diameter of 11 cm, an axial length of 20 cm and a sleeve outer surface made of zirconia, the cylinders being heated to 65°C, rotated at 250 rpm and urged into contact under a pressure of 365 MPa yielded by a pneumatic piston. The flakes so obtained had an average thickness t of about 16 pm, an average longest planar dimension L of about 1,100 pm and an aspect ratio ASP of about 69. They were tested and compared to some of the commercially available samples previously described.

First, syringes having an injectable volume of 50 ml were weighted and gently filled with the materials being tested up to a bulk volume of 50 ml. The filled syringes were weighted so as to determine the initial density of the samples and calculate their bulk density PB in grams per cubic centimeters. The piston was then pressed until the tested material could no longer be compressed. The volume of compressed material was measured and used to calculate the compressed density pc of the samples. The samples were left compressed for approximately 18 hours, following which the piston was removed and the samples taken out of the syringe cylinders and allowed to regain uncompressed density. The unconstrained samples were again gently loaded into their respective syringes to check whether they have regained their original volume of 50 ml or have suffered modifications leading to a different decompressed volume. The decompressed density pi>c was calculated based on the volume regained by the sample following its overnight compression.

A unit-less ratio F5 between the compressed density c and the initial bulk density ps of each sample, which can be mathematically expressed by F5= pc /pa, was calculated to assess the degree of compressibility each sample may display. Results and factors calculated therefrom are summarized in Table 12.

Table 12

As can be seen from the above table, while the comparative samples displayed on average a compressed density about 30% higher than their bulk density (i.e., F5 -1.29), this difference between the two types of densities dramatically raised to a 3-fold increase (z.e., F5 -3.33) when considering the flakes prepared as herein taught. All commercially available samples recovered following decompression, their decompressed density pi>c being identical or similar to their initial bulk density pp>. Present flakes displayed a decompressed density slightly higher than their original bulk density.

Without wishing to be bound to any particular theory, it is believed that since the aspect ratio of the present flakes (ASP -68) is greater by at least about an order of magnitude than the average aspect ratio of the materials to which they were compared (ASP-3A, with peaks of -7 for CS-1 and CS-3), the flakes of the invention could partly be broken in the experimental compressing process. Yet, even the broken flakes retained a relatively low decompressed density pnc of about 0.4 g/cm³ as compared to an average of about 0.8 g/cm³ for the comparative samples. As the fragility of a material, or the likelihood it would be modified by compression, depends in part on its initial aspect ratio, an additional unit-less factor F6 was calculated in order to find a relationship between the initial aspect ratio of a material ASP and its ability to be compressed, as can be estimated by F5. F6, which can be mathematically expressed by F6= ASP /F5, was found to emphasize the distinction between the present flakes and their comparative samples.

This example confirms that the present flakes having superior values for F2, F5 and F6 have a better packing ability than existing products, which is expected to facilitate their packaging, storage and transport.

Furthermore, the present example provides parameters that can be used to calculate additional factors F5 and F6 emphasizing the peculiarities of the present flakes. While the limitations set out below that may, in some cases, characterize these factors have been established with flakes made of salt, it is believed that the following lower thresholds, upper limits and ranges therebetween are not limited to this specific material. In some cases, the ratio F5 between the compressed density c and the initial bulk density s of the present flakes, mathematically expressed by F5= pc /pa, is 1.6 or more, 1.8 or more, 2.0 or more, 2.2 or more, 2.4 or more, 2.6 or more, 2.8 or more, 3.0 or more, or 3.2 or more. In some embodiments, F5 is equal to or less than 10.0, less than 7.5, less than 5.0, or less than 4.0. In particular cases, F5 is between 1.6 and 10.0, between 1.8 and 7.5, between 2.0 and 5.0, between 2.2 and 4.5, or between 2.4 and 4.0.

In some cases, the ratio F6 between the aspect ratio ASP of flakes of the invention and their compressibility as estimated by 5, mathematically expressed by F6=ASP/F5. is 6 or more, 10 or more, 15 or more, 20 or more, 25 or more, 30 or more, 35 or more, or 40 or more. In some embodiments, F6 is equal to or less than 200, less than 150, less than 100, less than 75, or less than 50. In particular cases, F6 is between 6 and 200, between 10 and 150, between 20 and 100, between 20 and 75, or between 20 and 50.

Example 11 : Organoleptic Test of Tastant Flakes

The effect of the morphology of the tastants on the taste that can be accordingly perceived can be tested with human volunteers. The tastant, before and after flaking as herein disclosed, can be tested “as is”, or once applied on or mixed with a food product otherwise deprived of the tastant. For illustration, the tastant can be applied on a popped popcorn or mixed in a relatively tasteless edible gel. The same proportion of reference tastant or flaked tastant can be applied on or mixed with the food, to establish how much stronger is the taste provided by the tastant flakes. Conversely, once a contents of reference tastant is set to provide a satisfactory taste, food samples can be prepared with decreasing amounts of the tastant flakes, until a similar satisfactory taste is obtained. By this methodology, one can establish by how much the quantity of tastant can be reduced when using the flaked tastants instead of the standard reference tastant.

In the present study, the ability of flakes of sodium chloride prepared as detailed for LF- 26 to provide a satisfactory salty taste was assessed on bare fried potato slices lacking any added tastant. The effect of tastant flakes of the invention on the salty taste achieved by potato chips coated thereby was compared to commercially available flakes of CS-8. 1 gram of tested flakes were mixed with 100 g of bare fried potato slices in a seasoning tumbler drum to ensure an even coating and subjected to evaluation by at least five trained panelists.

The trained panelists after rinsing their mouth with spring water in-between each evaluation, ingested a similar amount of food samples and assigned to each a taste strength value ranging from zero (no taste change, as compared to a food control coated with flakes CS- 8) to ten for the highest strength intensity above this baseline. Each panelist repeated the organoleptic test four times at 5 minutes interval, the food samples with the reference CS-8 or the currently flaked LF-26 tastant being randomly assigned at each round of evaluation.

The taste scores obtained for each food sample were summed for all panelists and repeat tests, and divided by the total number of tests, to obtain a calculated mean taste score for each food sample. In a first round of experiments, it was observed that at equivalent weights of salt flakes per chips, the flakes of LF-26 provided a significantly stronger salty taste than the commercial CS-8 flakes used as reference. In a second round of experiments, the relative amount of flakes of LF-26 applied to the bare potato slices was gradually decreased (e.g., -30%, -50%, -75%) until a taste similar to the one achieved by spreading 1 g of CS-8 flakes onto 100 g of potato slices was achieved. It was found that the weight of LF-26 could be reduced by about 30-40% (z.e., down to 0.6-0.7 g salt/100 g potato crisps), while providing a taste similar to the reference.

This experiment was repeated with flakes of sodium chloride prepared as detailed for LF- 13, also compared to commercially available CS-8. It was again unanimously found by all trained panelists, eight in this study, that the relative amount of flakes of LF-13 applied to bare potato slices could be reduced by at least about 30-35% (z.e., down to 0.65-0.70 g salt/100 g potato crisps), while providing a taste similar to the CS-8 reference (applied at 1 g salt/100 g potato crisps). This estimation is based on the observations that when the amount of flakes according to the invention was reduced to correspond to 75% of the weight of the reference flakes, none of the panelists was able to differentiate between the tested sample and the reference. When the amount of LF-13 was reduced to 50% of the CS-8 reference, a quarter of the panelists identified the crisps with the tested flakes as “less salty”, and when the amount of tested flakes was further reduced to only 25% of the reference, then half of the panelists perceived the difference in taste.

It should be noted that the salt used as reference in the present organoleptic tests is itself reported as providing for sodium reduction as compared to conventional table salt. Cargill reported that consumer sensory testing demonstrated that Alberger® Fine Flake Salt (i.e. CS-8) delivers the same flavor as table salt using less product, leading to a reduction of 30% in sodium. In other words, 1 g of CS-8 provides for a salty taste equivalent to about 1.4 g of table salt. As the present experiments showed that less than about 0.65-0.7 g of flakes according to the present teachings would be equivalent in taste to 1 g of CS-8 (as each applied to 100 g of potato crisps), it can be deduced that 0.65-0.7 g of LF-13 or LF-26 flakes, or less, are equivalent in taste to about 1.4 g of table salt. Hence, the present flakes of sodium chloride may provide a sodium reduction of at least 50% as compared to conventional table salt.

12: Pre-treatment of Raw Materials

As already reported in previous examples, the material to be flaked and/or the liquid stock prepared therefrom can be pre-treated before being used in the present method or apparatus. For illustration, in Example 3 raw material having an average diameter of about 500 pm was ground to an average diameter of about 50 pm to facilitate the preparation of a stock solution; in Example 8 raw material having an average diameter of about 500 pm was ground to an average diameter of about 5 pm to facilitate the preparation of a stock solution and a stock dispersion, and in the same example stock solutions were pre-heated to match the surface temperature of the rotating cylinder. These pre-treatments were performed as separate steps preceding the application of the liquid stocks to the outer surface of the rotating cylinders. In the present example, the pre-treatment was performed in-line with the following steps of the flaking process.

The pre-treating device was similar in construction to previously described flaking devices. It was constituted of two cylinders having an outer surface made of zirconia, each cylinder with the sleeve of zirconia mounted thereon having a diameter of 11 cm and an axial length of 20 cm, which were heated to 65°C, rotated at 250 rpm and urged into contact at a calculated Hertzian contact pressure of 365 MPa using a pneumatic piston. The axes of rotation of the cylinders of the pre-treating device were slightly tilted with respect to a horizontal surface, so that the nip was higher at one end than at the opposite one. In further contrast with the previously described flaking experiments, the liquid stock (25 wt.% NaCl in water) was continuously fed at the higher end of the nip at a flow rate sufficiently high (~33 ml/min) to generate a reservoir of liquid along the entire nip, an overflow taking place at the lower end of the nip. This feeding pace, which would have been excessive for the preparation of flakes under similar conditions, caused the shearing of the materials found upstream of the nip as it was displaced along the nip till it spilled over at its lower extremity. While the matter fed at the upper end of the nip was a transparent solution, the matter discharged at the lower end was a whitish sludge, supporting at least a first effect of concentrating the material. This was confirmed by weight loss analysis, the sludge having a salt concentration of at least 50 wt.%, the calculated flow rate at point of discharge being therefore at most about 16 ml/min. The dynamic viscosity of the concentrated liquid stock was found to be of about 1,500 mPa.s as measured at room temperature and at a shear rate of 100 s'¹. Without wishing to be bound to any particular theory, it is believed that part of the water present in the liquid stock was eliminated by passage through the nip, and any non-volatile material passing therethrough was recycled back to the upstream pool, gradually increasing the concentration of solid material in the pool despite the ongoing feeding of liquid stock at its upper end. As the solution turned into a dispersion, as supported by the increasing turbidity of the liquid, the particles having solidified could then be subjected to the shear forces generated by the rotating cylinders. This provided for a second effect, namely the size reduction of the material. In the present experiment, salt having an initial diameter of 500 pm (dissolved in the liquid applied at the upper end of the nip) was sheared down to form in the resulting sludge cubic particles having an average edge size of about 2.5 pm. It should be stressed that this dramatic size reduction was obtained in a few seconds (less than 10 sec in the present setup), when for comparison a standard ball milling method would have required 1.5 hours to achieve a similar size reduction. As this pre-treatment of the liquid stock achieves both a concentration of the material and a size reduction of the particles dispersed therein, it can serve to feed in-line the nip of a flaking apparatus, as for instance previously described in Example 8 considering the stock consisting of 59 wt.% of salt. Surface Area of Flakes

Flakes of materials prepared by the present method according to previous examples can be tested for their specific surface area SSA, which can be compared to the specific surface area of the respective material before flaking serving as reference, as follows. The surface area of the samples is measured by gas adsorption techniques using an ASAP 2020 Accelerated Surface Area and Porosimetry System of Micromeritics Instrument Corporation according to standard methods. Briefly, samples are weighed and placed in a measurement glass tube with a known free space in which a filler rod is inserted, the tube being sealed with a frit seal adapted to allow entry and exit of gas during the analysis. The samples are allowed to dry overnight under vacuum. The dry samples are then subjected to an evacuation phase under heating, the target temperature of 30°C being reached at a ramp up rate of 1 °C/min. The evacuation is performed at a rate of 5 mmHg/s, till a vacuum of 10 pmHg is obtained. The measurement glass tubes are then transferred to liquid nitrogen for the phase of nitrogen gas insertion which lasts 10 minutes to enable physical sorption of the molecule to the surface of the dry samples. The excess nitrogen gas is then evacuated under a vacuum of 100 mmHg and measurements are collected for 120 minutes of analysis with an equilibrium interval of 5 seconds. Each measurement is repeated at least three times, and the specific area of each sample is calculated by the BET method.

Example 14: Flowability of Flakes

The effect of the morphology of materials on their flowability can be determined by any suitable method. For illustration, a weighed mass of sample can be timed as it flows through the calibrated orifice of a flowmeter funnel, as described in ASTM B213 for a Hall flowmeter or in ASTM B964 for a Carney flowmeter, if the flakes or reference grains of water-soluble material fail to freely flow in a regular and constant way in the former instrument.

The experiment is preferably conducted in a laboratory with controlled temperature and humidity to ensure a relatively low relative humidity and stable temperature conditions. A dry and clean flowmeter funnel is held by a stand placed on a stable workbench, as the flow is to be measured unaided. As the discharge orifice of the funnel is blocked, a predetermined weight of the sample previously dried for 2 hours at 120°C is carefully placed in the funnel, without tapping, vibrations or movement that would artificially stack the sample. As the discharge orifice is open, a timing device is simultaneously started to monitor the time elapsing till the last of the sample exits the orifice. More than one flow test may be run, each time with a fresh quantity of dry sample, and the flow times corresponding to the same sample can be averaged. Flow times of different samples, or averages of repeats run on different samples, can be compared. The flow rates may be calculated and normalized according to a funnel dependent factor.

Summary of Working Examples

As can be seen from the above tables and results reported therein, the present methods and exemplary apparatus implementing them are suitable to rapidly manufacture micro flakes, some experiments providing sub-micro flakes in sufficient enough proportion to enable their separation. All flakes, regardless of the size range of their average thickness (demonstrated between about 0.5 and 200 pm), displayed a dimensionless aspect ratio of at least about 5 (see LF-6), most being above at least 30. It is believed that present flakes are all made up of solid particles being at least compacted, and in most cases also agglomerated as a result of said pressure caused compaction of the clusters of particles progressively separating from the liquid stock as liquid is eliminated.

While the feasibility of the present flaking method and apparatus was mainly demonstrated with tastants (alone or blended), this is not limited to such type of compounds and a variety of water-soluble and water-insoluble materials having additional purposes in industries other than the food industry have also been successfully flaked. Considering flakes of water-soluble materials manufactured by the application of a relatively non-viscous liquid to a movable surface forming with a countersurface a nip of compaction, flakes could be prepared when fed either as solutions (see e.g., LF-1 to LF-6, and LF-8 to LF-13) or dispersions (see LF- 7). The same was true for water-insoluble materials which have been flaked either from dispersions (see LF-14 to LF-17) or from solutions (see LF-18).

Advantageously, the flakes prepared by the present methods displayed an improved rate of dissolution as compared to the respective reference material (e.g., tastant) before flaking. The improvement was an about 10-fold acceleration of the dissolution when quantitatively measured for salt or a detergent mix (see LF-1 and LF-22), similar increases in speed of dissolution being reported for sodium phosphate dibasic and sodium phosphate monobasic monohydrate (see LF-9 and LF-10). Interestingly, the bulk and tapped densities of the actively detached flakes of salt that displayed the accelerated dissolution were also about 10% of the bulk or tapped density of the reference salt, respectively. Remarkably, when the material was a tastant having a crystalline structure, the flaked version of the tastant displayed a structure having at least about 3-times more microstrains than the crystal of the reference tastant originally dissolved to form the flakes. The size of the crystallites was also found to be at least about 36-times smaller for the flakes than for the reference granular tastant, further supporting that (e.g., tastant) flakes prepared as herein disclosed have been subjected to constrains (e.g., compressive forces as perceived during compaction in the nip(s)) normally absent from naturally growing crystals. The present flakes also demonstrated a compressibility favorable to standard commercial procedures.

Considering the particular case of flakes of sodium chloride, as exemplary tastant, they were shown in organoleptic studies to provide the same flavor as reference salt while being present in relatively reduced amounts, the current experiments suggesting a possible reduction in sodium of at least 50% as compared to regular table salt.

The methods have been found applicable to different materials which provide a wide range of activities to the flakes, not being limited to taste or the food industry. Importantly, flakes prepared by the present method or apparatus seem to have distinctive characteristics with respect to both measurable properties and values that can be calculated therefrom, as illustrated with ratios including ASP and Fl to F6. as herein defined. In some cases, the present flakes are distinguishable by more than one of the afore-said characteristics. In addition to the features of the above disclosure that are claimed in the appended claims, features believed to be inventive in their own right are set out in the clauses below, to provide fair basis for eventual filing of one or more divisional patent applications.

1. A method of manufacturing flakes, the method comprising: a) providing a stock comprising at least one material; b) applying the stock to a first movable surface, so as to form thereon an even layer of the stock of the material(s); and c) cyclically passing the material(s) through at least one nip formed by urging the first movable surface towards a counter surface; so as to progressively form solid particles of the material(s), said particles being compacted and agglomerated in step c), thereby forming flakes made from said material(s).

2. The method of clause 1, wherein the stock is applied in dry form.

3. The method of clause 1 , wherein the stock is applied as a paste, the paste stock having a dynamic viscosity of 5,000 milliPascal-seconds (mPa.s) or more, the method further comprising progressively eliminating any liquid present in the paste stock.

4. The method of clause 1, wherein the stock is applied as a liquid stock, optionally having a viscosity of at most 5,000 mPa.s, the method further comprising progressively eliminating any liquid present in the liquid stock.

5. The method of clause 3 or clause 4, wherein the liquid present in the paste stock or the liquid stock is selected to react with one or more materials of the at least one material of said stock, so that the flakes have a chemical composition different from the chemical composition of the one or more materials present in the stock.

6. The method of any one of clause 3 to clause 5, wherein the liquid is eliminated from the paste stock or the liquid stock in one or more cycles by evaporation of the liquid.

7. The method of any one of clause 1 to clause 6, wherein the flakes have an average thickness t not exceeding 200 pm.

8. The method of any one of clause 1 to clause 7, wherein the flakes have an average aspect ratio /t$7^> between the longest planar dimension L of the flakes and their largest thickness t being on average of not less than 10: 1.

9. The method of any one of clause 1 to clause 8, wherein the flakes comprising the compacted and agglomerated particles of the solid material(s) contain less than 5 wt.% of liquid.

10. The method of any one of clause 1 to clause 9, wherein the separation of opposed nip-forming surfaces at the or each nip is dynamically variable, the separation reducing to 1 pm or less in absence of the stock or flakes derived therefrom and being optionally at most 400 pm in presence of the stock.

11. An apparatus for making flakes from a stock comprising at least one material, the apparatus comprising: a) a support frame, b) two cylinders mounted in the frame with at least one of the cylinders movable relative to the support frame, c) a force mechanism for applying a force to urge the cylinders into contact with one another so as to form a nip, and d) a drive motor for rotating at least one of the two cylinders, characterized by e) a dosage device for applying the stock onto at least one cylinder to form a film including solid particles of the material(s) on the surfaces of both cylinders, the number or concentration of solid particles increasing, during use, with repeated passage of the film through the nip, and f) a controller serving to regulate the rate of application of the stock by the dosage device in dependence upon empirically prepared tables predicting such rate in dependence upon at least one of a rotational speed of the motor driven cylinder, a force applied at the nip, a temperature of the surfaces of the cylinders, and a composition of the stock.

12. The apparatus of clause 11, wherein the dosage device is adapted to apply the stock in paste or liquid the number or concentration of solid particles increasing, during use, with repeated passage of the film through the nip.

13. The apparatus of clause 12, further comprising a heating device to facilitate removal of the liquid comprised in the paste or liquid stock.

15. An apparatus for making flakes from a stock comprising at least one material, the apparatus comprising: a) a support frame, b) two cylinders mounted in the frame with at least one of the cylinders movable relative to the support frame, c) a force mechanism for applying a force to urge the cylinders into contact with one another so as to form a nip, and d) a drive motor for rotating at least one of the two cylinders, characterized by e) a dosage device for applying the stock onto at least one cylinder to form a film including solid particles of the material(s) on the surfaces of both cylinders, the number or concentration of solid particles increasing, during use, with repeated passage of the film through the nip, f) a torque measuring device to determine the torque being applied by the drive motor, the torque varying with the proportion of solid particles in the film, and g) a controller serving to regulate the rate of application of the stock by the dosage device in dependence upon the measured torque.

16. An apparatus for making flakes from a liquid stock comprising a material dissolved or dispersed in a liquid, the apparatus comprising: a) a support frame, b) two cylinders mounted in the frame with at least one of the cylinders movable relative to the support frame, c) a force mechanism for applying a force to urge the cylinders into contact with one another so as to form a nip, and d) a drive motor for rotating at least one of the two cylinders, characterized by e) a dosage device for applying the liquid stock onto at least one cylinder so as only to apply thin films to the surfaces of the cylinders, the concentration of solid material in the films increasing with repeated passage of the films through the nip resulting in the formation of flakes of the material, and f) a controller for regulating the rate at which liquid stock is applied onto the cylinders to match the rate at which liquid is lost from the films during continued passage of the films through the nip.

17. An apparatus for making flakes from liquid stock comprising a material dissolved or dispersed in a liquid, the apparatus comprising: a) a support frame, b) two cylinders mounted in the frame with at least one of the cylinders movable relative to the support frame, c) a force mechanism for applying a force to urge the cylinders into contact with one another so as to form a nip, d) a drive motor for rotating at least one of the two cylinders, and e) a device for applying a film of the liquid stock to the cylinders during their rotation, characterized in that at least one of the cylinders is internally heated such that the concentration of solid material in the films increases with repeated passage of the films through the nip resulting in the formation of flakes of the material on the cylinders.

18. Flakes consisting of sodium chloride, said material having at least one of the following crystallographic features:

A- the crystallite size of the sodium chloride in the flakes is at least 20%, at least 30%, at least 40%, or at least 50% smaller than a crystallite size of a reference unflaked sodium chloride, the crystallite size in the flakes being optionally at least 2-fold, at least 3-fold, or at least 4-fold smaller than said reference crystallite size; and

B- the percent microstrain value of the sodium chloride in the flakes is at least 20%, at least 30%, at least 40%, or at least 50% larger than a percent microstrain value of a reference unflaked sodium chloride, the percent microstrain value in the flakes being optionally at least 2-fold, at least 3 -fold, or at least 4-fold larger than said reference percent microstrain value.

19. Flakes made from at least one material, the flakes having thin planar dimensions wherein each flake has a longest dimension and a plurality of flakes has an average longest dimension (Z) in the plane, wherein each flake has a largest thickness and a plurality of flakes has an average largest thickness (f) from one side of the plane to the other side, and wherein a flake has a dimensionless aspect ratio between a longest dimension and a largest thickness so that the plurality of flakes has an average aspect ratio (Asp=L/f) of at least 10: 1; the flakes being characterized by at least three of the structural features recited in any one of following a) to j) and furthermore by at least one, at least two or at least three of the features recited in any one of following k) to w): a) t is at most 200 pm, 150 pm, 100 pm, 80 pm, 60 pm, or 40 pm; b) t is at most 20 pm, 18 pm, 16 pm, 14 pm, 12 pm, or 10 pm; c) t is at most 9 pm, 8 pm, 7 pm, 6 pm, 5 pm, 4 pm, 3 pm, or 2 pm; d) t is at most 1 pm, 0.9 pm, 0.8 pm, 0.7 pm, 0.6 pm, 0.5 pm, 0.4 pm, or 0.3 pm; e) t is at least 50 nm, at least 100 nm, at least 150 nm, or at least 200 nm; f) Z is at most 10,000 pm, at most 7,500 pm, at most 5,000 pm, at most 4,000 pm, at most 3,000 pm, at most 2,000 pm, at most 1,500 pm, or at most 1,000 pm; g) L is at most 500 pm, at most 400 pm, at most 300 pm, at most 200 pm, at most 100 pm, or at most 50 pm; h) L is at least 5 pm, at least 7.5 pm, at least 10 pm, at least 12.5 pm, or at least 15 pm; i) Asp is at least 20: 1, at least 30: 1, at least 40: 1, or at least 50: 1; j) Asp is at most 150: 1, at most 125: 1, at most 100:1, or at most 75: 1; k) the flakes have a specific surface area 5 4 of at least 0.001 m²/g, at least 0.005 m²/g, at least 0.01 m²/g, at least 0.05 m²/g, at least 0.1 m²/g, at least 0.2 m²/g, at least 0.3 m²/g, at least 0.4 m²/g, or at least 0.5 m²/g; l) the flakes have a specific surface area 5 4 of at most 10 m²/g, at most 8 m²/g, at most 6 m²/g, at most 4 m²/g, or at most 2 m²/g; m) the flakes have a rate of dissolution DT, as can be measured in water at 23°C, and a ratio F1=ASP/ DT of at least 5, at least 10, at least 15, at least 25, at least 50, at least 75, or at least 100; n) the flakes have a rate of dissolution DT, as can be measured in water at 23°C, and a ratio F1=ASP/ DT of at most 500, at most 400, at most 300, at most 200, or at most 150; o) the flakes have a tap density pr and a bulk density ps, and a ratio between the two F2=pr/pB of at least 1.25, at least 1.5, at least 1.75, at least 2, at least 2.25, at least 2.5, or at least 2.75; p) the flakes have a tap density pi and a bulk density pa, and a ratio between the two F2=pr/pB of at most 5, at most 4.5, at most 4, or at most 3.5; o) the flakes have a bulk density pp> and a ratio F3=ASP/ PB of at least 25, at least 50, at least 75, at least 100, at least 150, at least 200, at least 250, at least 300, or at least 350; p) the flakes have a bulk density pp> and a ratio F3=ASP/ PB of at most 1,000, at most 750, at most 500, or at most 400; q) the flakes have a tap density pr and a ratio F4=ASP/ pr of at least 20, at least 40, at least 60, at least 80, at least 100, at least 120, at least 140, at least 160, or at least 180; r) the flakes have a tap density pr and a ratio F4=ASP/ pr of at most 500, at most 400, at most 300, or at most 200; s) the flakes have a compressed density pc and a bulk density pp>, and a ratio between the two F5=pc/pB of at least 1.6, at least 1.8, at least 2.0, at least 2.2, at least 2.4, at least 2.6, at least 2.8, at least 3.0, or at least 3.2; t) the flakes have a compressed density pc and a bulk density pp>, and a ratio between the two F5=pc/pB of at most 10, at most 7.5, at most 5, or at most 4; u) the flakes have a compressed density pc and a bulk density pp>, and a ratio F6=(ASP x PB) /pc of at least 6, at least 10, at least 15, at least 20, at least 25, at least 30, at least 35, or at least 40; v) the flakes have a compressed density pc and a bulk density pp>, and a ratio F6=(ASP PB) /pc of at most 200, at most 150, at most 100, at most 75, or at most 50; and w) the, or each, material of the flakes is a crystalline material.

20. Flakes as in clause 18 or clause 19, prepared by any method and/or any apparatus herein described and claimed.

21. Flakes as in clause 19 or clause 20, wherein at least one material of the one or more materials making the flakes is a tastant adapted to provide a taste to a product containing or consisting of the same.

22. Flakes as in any one of clause 19 to clause 21, wherein the material is sodium chloride, said crystalline material having at least one of the following crystallographic features:

23. Flakes as in clause 19 or clause 20, wherein at least one material of the one or more materials making the flakes is an active or inactive ingredient adapted to provide an efficacy and/or a manufacturing advantage to a manufactured article containing or consisting of the same.

24. A food comprising flakes as claimed in any one of clause 18 to clause 21, the flakes being disposed on and/or within said food and being optionally insoluble therein.

25. A manufactured article comprising flakes as in any one of claim 19, clause 20 and clause 23.

26. A method for improving a food, the method comprising incorporating into the food flakes as in any one of clause 21 to clause 23.

27. A method for improving an efficacy of a manufactured article, the method comprising incorporating into the manufactured article flakes as in any one of clause 20, clause 23 and clause 25.

28. A method for reducing the amount of a tastant adapted to provide a desired taste to a food, the method comprising replacing at least a part of the tastant in the food, and optionally all of said tastant, by flakes as in clause 21 or clause 22.

29. A method for reducing the amount of an active or inactive ingredient adapted to provide a desired efficacy to a manufactured article, the method comprising: replacing at least a part of the ingredient in the manufactured article, and optionally all of said ingredient, by flakes as in clause 23.

It is appreciated that certain features of the disclosure, which are, for clarity, described in the context of separate embodiments, may also be provided in combination in a single embodiment. Conversely, various features of the disclosure, which are, for brevity, described in the context of a single embodiment, may also be provided separately or in any suitable sub- combination or as suitable in any other described embodiment of the disclosure. Certain features described in the context of various embodiments are not to be considered essential features of those embodiments, unless the embodiment is inoperative without those elements.

Although the present disclosure has been described with respect to various specific embodiments presented thereof for the sake of illustration only, such specifically disclosed embodiments should not be considered limiting. Many other alternatives, modifications and variations of such embodiments will occur to those skilled in the art based upon Applicant’s disclosure herein. Accordingly, it is intended to embrace all such alternatives, modifications and variations and to be bound only by the spirit and scope of the disclosure and any change which comes within their meaning and range of equivalency.

In the description and claims of the present disclosure, each of the verbs “comprise”, “include” and “have”, and conjugates thereof, are used to indicate that the object or objects of the verb are not necessarily a complete listing of features, members, steps, components, elements or parts of the subject or subjects of the verb. Nevertheless, it is contemplated that the compositions of the present teachings also consist essentially of, or consist of, the recited components, that the methods of the present teachings also consist essentially of, or consist of, the recited process steps, and that the apparatus of the present teachings also consist essentially of, or consist of, the recited devices.

Positional or motional terms such as “upper”, “lower”, “right”, “left”, “bottom”, “below”, “lowered”, “low”, “top”, “above”, “elevated”, “high”, “vertical”, “horizontal”, “front”, “back”, “backward”, “forward”, “upstream” and “downstream”, as well as grammatical variations thereof, may be used herein for exemplary purposes only, to illustrate the relative positioning, placement or displacement of certain components, to indicate a first and a second component in present illustrations or to do both. Such terms do not necessarily indicate that, for example, a “bottom” component is below a “top” component, as such directions, components or both may be flipped, rotated, moved in space, placed in a diagonal orientation or position, placed horizontally or vertically, or similarly modified.

As used herein, the singular form “a”, “an” and “the” include plural references and mean “at least one” or “one or more” unless the context clearly dictates otherwise. As used herein, the term at least one of A and B is intended to mean either A or B, and may mean, in some embodiments, A and B. Unless otherwise stated, the use of the expression “and/or” between the last two members of a list of options for selection indicates that a selection of one or more of the listed options is appropriate and may be made.

The word “exemplary” is used herein to mean “serving as an example, instance or illustration”. Any embodiment described as “exemplary” is not necessarily to be construed as preferred or advantageous over other embodiments and/or to exclude the incorporation of features from other embodiments.

As used herein, unless otherwise stated, adjectives such as “substantially”, “approximately” and “about” that modify a condition or relationship characteristic of a feature or features of an embodiment of the presently disclosed subject matter, are to be understood to mean that the condition or characteristic is defined to within tolerances that are acceptable for operation of the embodiment for an application for which it is intended, or within variations expected from the measurement being performed and/or from the measuring instrument being used. For example, when the term “about” or “approximately” precedes a numerical value, it may indicate +/-15%, or +/-10%, or even only +/-5%, or any other suitable +/- variation within such ranges, and in some instances may indicate the precise value. Furthermore, unless otherwise stated, the terms (e.g., numbers) used in an embodiment of the presently disclosed subject matter, even without such adjectives, should be construed as having tolerances which may depart from the precise meaning of the relevant term but would enable the embodiment or a relevant portion thereof to operate and function as described, and/or as understood by a person skilled in the art.

Claims

1. A method of manufacturing flakes, which method comprises: a) providing a liquid stock comprising at least one solid material dissolved or dispersed in a liquid; b) applying the liquid stock to a first movable surface, so as to form thereon a thin film of liquid stock; c) cyclically i) evaporating at least a part of the liquid from the thin film of liquid stock, so as to increase the concentration of solid particles in the film, and ii) applying pressure to the film by passing the film through at least one nip formed by urging opposed nip-forming surfaces towards one another, so as to progressively form a layer comprised of flakes consisting of agglomerated and compacted solid particles, until the flakes contain less than 5 wt.% of the liquid.

2. A method as claimed in claim 1, wherein the flakes have an average largest thickness t of at most 200 pm.

3. A method as claimed in claim 1 or claim 2, wherein the flakes have an average aspect ratio ASP between the longest planar dimension L of the flakes and their largest thickness t of at least 10: 1.

4. A method as claimed in any one of claim 1 to claim 3, wherein the liquid stock is applied by an applicator, the first movable surface and the applicator being in relative motion during the application step, and at least one of the formation of the thin film of liquid stock, the concentration of the solid particles in the film, and the obtention of the flakes is caused by passage through the nip(s).

5. A method as claimed in any one of claim 1 to claim 4, further comprising forming the thin film of liquid stock prior to passage through the at least one nip.

6. A method as claimed in any one of claim 1 to claim 5, wherein the first movable surface is the outer surface of a first rotating cylinder that forms one of the opposed nip-forming surfaces, the other nip-forming surface of said nip being optionally formed by the outer surface of a second rotating cylinder.

7. A method as claimed in any one of claim 1 to claim 6, wherein the liquid stock is applied on the first movable surface at a temperature higher than ambient temperature and lower by at least 5°C than a boiling temperature of the liquid.

8. A method as claimed in any one of claim 1 to claim 7, wherein at least one of the nip-forming surfaces is heated to a temperature higher than ambient temperature.

9. A method as claimed in any one of claim 1 to claim 8, wherein the pressure exerted at the or each nip is independently between 10 MPa and 1,500 MPa, between 50 MPa and 1,250 MPa, or between 100 MPa and 1,000 MPa.

10. A method as claimed in any one of claim 1 to claim 9, further comprising collecting the flakes downstream of at least one nip-forming surface.

11. A method as claimed in any one of claim 1 to claim 10, wherein the liquid stock is continuously applied, and the obtained flakes are continuously collected.

12. A method as claimed in any one of claim 1 to claim 11, wherein the opposed nip- forming surfaces at the or each nip each have a dynamically variable separation, the separation reducing to 1 pm or less in absence of any of the liquid stock, the film, the layer and the flakes derived therefrom, said separation being optionally at most 400 pm in presence of the liquid stock.

13. A method as claimed in any one of claim 1 to claim 12, wherein the material(s) are crystalline.

14. A method as claimed in any one of claim 1 to claim 13, wherein at least one material of the one or more materials is a tastant.

15. An apparatus for making flakes from a liquid stock comprising at least one material dissolved or dispersed in a liquid, the apparatus comprising: a support frame, two cylinders mounted in the frame with at least one of the cylinders movable relative to the support frame, a force mechanism for applying a force to urge the cylinders into contact with one another so as to form a nip, and a drive motor for rotating at least one of the two cylinders, characterized by a dosage device for applying the liquid stock onto at least one cylinder to form a film on the surfaces of both cylinders, the concentration of solid particles of the material(s) increasing, during use, with repeated passage of the film through the nip, a torque measuring device to determine the torque being applied by the drive motor, the torque varying with the proportion of liquid in the film, and a controller serving to regulate the rate of application of the liquid stock by the dosage device in dependence upon the measured torque.

16. An apparatus as claimed in claim 15, wherein the dosage device is adapted to apply discrete quantities of the liquid stock, the controller regulating the dose and/or the repetition rate of the discrete applications.

17. An apparatus as claimed in claim 15, wherein the dosage device is adapted to apply a continuous stream of the liquid stock, the controller regulating the flow rate of the continuous stream.

18. An apparatus as claimed in any one of claim 15 to claim 17, wherein at least one cylinder is heated, during use, the at least one device heating the or each cylinder being positioned internally and/or externally to the heated cylinder.

19. An apparatus as claimed in any one of claim 15 to claim 18, wherein the force mechanism includes a pneumatic piston or a hydraulic piston including an accumulator.

20. An apparatus as claimed in any one of claim 15 to claim 19, further comprising a collector for the flakes.

21. An apparatus as claimed in claim 20, further comprising a detaching device to separate the flakes from the surfaces of the cylinders, said separation being dependent upon a low proportion of liquid in the film.

22. An apparatus as claimed in claim 21, wherein the detaching device retractably contacts the surface of at least one of the cylinders and is positioned so that the separated flakes are collected in the collector, said detaching device being selected from a group comprising a doctor blade and a scraper.

23. An apparatus as claimed in any one of claim 15 to claim 22, further comprising a levelling device adapted to level the liquid stock applied by the dosage device prior to passage through the nip.

24. An apparatus as claimed in any one of claim 15 to claim 23, further comprising at least one of: a) a pre-treating station adapted to (i) heat the liquid stock, (ii) reduce the size of material(s) dispersed therein, and/or (iii) increase the concentration of material(s) dissolved or dispersed therein, said pre-treating station being upstream of the dosage device and in fluid communication therewith; and b) a post-flaking station adapted to (i) dry and/or (ii) sort the collected flakes, and/or adapted to (iii) recycle to the dosage device flakes not conforming to desired dimensions.

25. An apparatus as claimed in any one of claim 15 to claim 24, wherein the axis of rotation of the cylinders is not horizontal, the dosage device being positioned to apply the liquid stock at an upper end of the cylinders and the flakes being collected at a lower end of the same.

26. An apparatus as claimed in any one of claim 15 to claim 25, further comprising at least one more cylinder urged into contact with one of the two cylinders so as to form at least one additional nip, the three or more cylinders being arranged linearly or radially one with respect to another.

27. An apparatus as claimed in any one of claim 15 to claim 26, wherein, during use, opposed nip-forming surfaces at the or each nip each have a dynamically variable separation, the separation reducing to 1 pm or less in absence of any of the liquid stock, the film, and the flakes derived therefrom, said separation being optionally at most 400 pm in presence of the liquid stock.