WO2007096117A1

WO2007096117A1 - Method and device for the automated performance of high-throughput investigations

Info

Publication number: WO2007096117A1
Application number: PCT/EP2007/001418
Authority: WO
Inventors: Wolfgang Schrof; Eva Wagner; Thomas Meier; T. Brinz; Sebastian Koltzenburg; T. Burk; T. Geiger; Tiefenbacher
Original assignee: Basf Se; Robert Bosch Gmbh
Priority date: 2006-02-21
Filing date: 2007-02-19
Publication date: 2007-08-30
Also published as: DE102006008869A1; EP1988991A1

Abstract

The present invention relates to a method for the automated performance of high-throughput investigations of a plurality of materials for surface coatings, in which (a) the materials are provided from the plurality of materials within a given time interval; (b) at least one surface of at least one substrate is coated with the respective materials provided, to produce a respective coating, (c) the respectively produced coatings are cured, and (d) at least one property of each of the respective coatings produced is determined, wherein the respective coatings produced each have a two-dimensional, contiguous extent parallel to the surface of the substrate of at least 25 cm2. Furthermore, the present invention relates to a corresponding device for the automated performance of high-throughput investigations of a plurality of materials for surface coatings.

Description

Method and device for the automated performance of high-throughput investigations

The present invention relates to a method and a device for the automated performance of high-throughput investigations of a plurality of materials for Oberflächenbeschichtungen.

In the development of liquid formulations, such as dispersions, emulsions or solutions, these liquid formulations are subjected to so-called screening tests in order to test and optimize them with regard to various properties.

In particular, in the development of new coatings, such as paint formulations and their components, the technology of so-called high-throughput screening (HTS) is used. High-throughput screening or high-throughput screening is a technology in which the highest possible number of materials to be investigated are manufactured and tested for application properties in as short a time as possible, through the use of automation, miniaturization and possibly parallelization can be.

The use of HTS in the research and development of coatings, such as, for example, paints, varnishes and / or precursors thereof, makes it possible to react very quickly to changing needs or structure-effect relationships in formulations with in some cases complicated compositions. recognizing tongues. New needs or requirements are constantly arising, for example due to new specifications by the legislation, price requirements and new technical requirements of the customers. Such requirements can be, for example: reduction of volatile organic solvent constituents, improved scratch resistance or resistance to chemicals or new fashionable or technical properties.

Typical classes of paint formulations are e.g. One-component (IK) systems, such as e.g. Melamine resin based, two component (2K) systems, e.g. Isocyanate / hydroxy-based, radiation-curable formulations, etc. These can be used as clearcoat systems or as pigmented systems. In addition, the amount and type of additives, e.g. Flow control agents, UV absorbers, photoinitiators, fillers, catalysts, stabilizers, matting agents an important role.

It is important to test the properties of liquid formulations or their raw materials used for coating precisely, quickly, reproducibly and in terms of application or realism.

It has hitherto been known, for example, from WO 01/032320 A1, WO 02/34381 A1, US 2003/0077399 A1 and US 2003/0038941 A1, to remove liquid formulations usable for coating onto a titer plate, such a titer plate generally being used a multiplicity of so-called cavities or, in general, regions, in each of which a certain amount of the liquid formulation to be investigated can be introduced. However, the quantities of the liquid formulations to be investigated which are introduced into the regions are very small and therefore only partially reflect the practical properties of as coating or as film applied liquid formulations again. In small areas, edge effects play an important role and hardly any relevant film properties are achieved. Furthermore, only a part of characterization methods can be applied to such introduced amounts or drops of a liquid formulation, which have a partially destructive character, and this partly even with a reservation of due to the drop shape to be considered edge effects. Thus, even on the cured film an immediate realistic or application-oriented characterization is difficult. To carry out several characterization methods on the liquid formulation to be examined further drops must be applied.

On the basis of the prior art mentioned here, it would now be desirable to provide a method and a device with the aid of which it is possible to investigate as precisely as possible, fast and realistic properties of materials to be investigated, in particular of formulations, with respect to their use as a coating to be able to. In the context of the present invention, a coating is to be understood as meaning a film or a layer applied in the form of a film.

The present invention proposes now a method for the automated performance of high-throughput investigations of a plurality of materials in terms of formulation, surface coating, curing and performance characterization with the features of claim 1 before.

Furthermore, the present invention provides a corresponding device for the automated implementation of such high-throughput investigations with the features of patent claim 23 ready. Further advantageous embodiments are listed in the corresponding subclaims.

According to claim 1 there is provided a method of automated high throughput inspection of a plurality of surface coating materials, wherein in a step (a) the materials of the plurality of materials are provided within a predetermined time interval, in a step (b) at least coating a surface of at least one substrate with the respective materials so provided to form a respective coating, drying or optionally curing in a step (c), and (d) determining at least one property of each of the respective coatings produced respective coatings each have an axis extending parallel to the surface of the substrate surface, contiguous stretch of at least 25 cm ^2. At least one of the steps (a), (b), (c) or (d) is carried out automatically. However, two, three or all four of steps (a), (b), (c) and (d) may be automated.

The areal and contiguous extent of the coatings produced in each case is chosen so that the coating produced has a sufficiently large area, the properties of a large-area coating, as is usually the case in the application, such as in coatings of a motor vehicle with a designated paint film, reflects. The choice of the areal extent is based, on the one hand, on characterization methods to be carried out for determining the at least one property, which require different areas in order to be able to make an adequate statement, and, on the other hand, on carrying out the high-throughput investigations still easily manageable size of the at least one substrate, on whose at least one surface the respective coating is applied. When determining the at least one property of each of the respective coatings produced, marginal effects should as far as possible be excluded in the area intended to determine the property. In the area provided for determining the at least one property, the coating produced should have so-called "minimum film quality".

In one possible embodiment of the method according to the invention, the areal extent is in a range from 25 cm ² to 2000 cm ² , preferably 25 cm ² to 200 cm ² . The areal extent is advantageously 36 cm ² and more preferably 6 cm × 6 cm. Furthermore, the areal extent may preferably also be 123.25 cm ² and in particular 8.5 cm × 14.5 cm.

An areal expansion of the respective coatings in the stated range makes it possible to carry out certain DIN characterization methods on the respective coatings. A DIN method that can be carried out on the respective coatings may, for example, be one of the following methods: DIN-EN ISO 1520 and / or DIN 67530 and / or DIN 53151. Compared to previous investigations of liquid formulations using titer plates For example, the dimensions of the at least one surface of the substrate, which is coated with a coating to be examined, are large and accordingly also allow comparatively large-area coatings.

The areal extent of a respective coating can be selected in the said range in such a way that a sufficient size is provided for carrying out a specific characterization method and / or several, preferably non-destructive characterization methods can be carried out on one and the same coating. If several characterization methods are applied to one and the same areal extent of a coating to be examined, then a direct comparison of the various examined properties of the coating is made possible, whereupon optimizations can be carried out very quickly, without having to take effects into account, which are due to the fact that Certain characterization methods have been carried out on different coatings.

In one possible embodiment of the method according to the invention, the at least one surface of the at least one substrate is coated with less than six coatings of respectively different materials. It is possible to apply the up to five coatings mosaic on the at least one surface of the at least one substrate. However, the up to five coatings can also be realized one above the other.

Furthermore, it is conceivable to coat the at least one surface of the at least one substrate with exactly one coating of a material of the plurality of materials. This simplifies the determination of the at least one property of a given coating, since only substrates with a single corresponding coating applied thereto are to be examined, and no edge effects possibly caused by adjacent coatings have to be taken into account. The handling of each provided with only one coating substrates simplifies and thus speeds up the process.

In a further embodiment of the method according to the invention, the majority of the materials in which it is preferably are different materials, greater than or equal to 25, preferably greater than or equal to 50, and particularly preferably greater than or equal to 100 selected. Furthermore, it is conceivable to produce the majority of the materials within a time interval of 24 hours from up to 100 starting materials. For the purpose of a ripening process, which usually equals a completion of a curing reaction, the coated substrate (s) can be taken out of the leveling process or the corresponding device together for a predeterminable time prior to a characterization of the respective coatings and then returned to the process. In the meantime, other processes can run.

It is possible to provide the materials of the plurality of materials sequentially or in parallel. As already mentioned, the materials may be liquid formulations, such as dispersions, emulsions or solutions or combinations thereof. However, in addition to pigment-containing dispersions, which are often used in the form of colored pigments or inorganic fillers in paints to form a coating, all other types of liquid formulations used for coating may also be provided.

The liquid formulations can be prepared by homogenizing mixing or dispersing from various solid or liquid feedstocks or components. When producing such liquid formulations, such as, for example, pigment-containing dispersions, it is possible, for example, to use a so-called speed mixer. For better homogenization balls, for example. From metal, ceramic or glass can be used. These balls can be filled manually or offline or automatically and automati- Mogenisierten material to be separated. The produced liquid formulations can also be filled in a respective container and provided in this respective container.

The liquid formulations and also the pigment-containing dispersions can be formulated automatically. Automated production can be carried out by automated weighing or volumetric metering of at least two components of the formulation into at least one vessel and subsequent automated homogenization of the resulting mixture by automated mixing to form a coating formulation, for example a pigment-containing formulation.

Thus, step (a) of providing the materials for each of the materials to be provided may comprise a series of automated steps, namely, a step of automated production of a mixture by automated dosing, e.g., gravimetric or volumetric dosing, of appropriate components into a suitable vessel optionally, a step of automatically closing the vessel, a step of automatically homogenizing the prepared mixture by automated mixing, and optionally a step of automatically opening the vessel, for example, to remove a defined amount of the material provided to coat the at least one In this case, for example, by means of a suitable removal or pipetting method, a defined amount of the liquid formulation, such as, for example, a pigment ha For example, in order to apply a coating to the at least one surface of the at least one substrate. For removal can be used, for example, a syringe. In order to prevent the grinding medium from clogging the syringe inlet during aspiration of the liquid formulation, a disposable syringe may be used which is only immersed in the milling insert at a distance of 2 to 4 mm or the grinding media can be retained by means of filters of suitable mesh size. The immersion depth can be ensured by a distance measurement by ultrasound. A suitable syringe may also simultaneously serve as a vessel in which the corresponding liquid formulation is prepared as described. As a result, vessels and possibly cleaning steps can be avoided.

An automated dosing can be carried out, for example, while stirring or until a predetermined pH or a specific viscosity is set.

The plurality of materials may be so-called liquid formulations made from a plurality of components. In this case, 2 to 100, preferably 3 to 50, particularly preferably 3 to 25 components may be included, but it may also be more or less. The components may, for example, be a liquid, a solid or liquid substance that is insoluble or soluble in the liquid formulation, and, for example, a surfactant. In this case, the insoluble substance in the liquid formulation means that the substance does not dissolve at all or at most up to 10% by weight in the liquid formulation. Such a multicomponent system is generally present as dispersion, emulsion, liquid multicomponent system or solution. The starting materials or components may also be already mixed, preferably rolled, and tempered feedstock templates. The liquid may be a solvent or a solvent mixture, consisting in particular of water and / or an organic solvent which is typical for paint formulations and which may be polar or non-polar, such as, for example, As alcohols such as butanol, ethanol, methanol, polyhydric alcohols such as glycerol or polyols, organic solvents such. As xylenes, toluene, butyl acetate, ethyl acetate, DBE, ethyl acetate, methoxypropyl acetate, tetrahydrofuran, rapeseed oil, paraffins and / or hydrocarbon mixtures. The substance which is soluble or insoluble in the liquid formulation is, for example, dyes and / or pigments or various additives, initiators, other fillers; in the liquid formulation, soluble or insoluble organic solvents, for example as defined above; synthetic or natural waxes, e.g. B. beeswax, wool wax; synthetic, vegetable or animal oils, e.g. Paraffin oil, rapeseed oil, soybean oil, pine needle oil, rosemary oil, peanut oil, jojoba oil, coconut oil, almond oil, olive oil, palm oil, castor oil, wheat germ oil, isopropyl myristate, or essential oils, e.g. B. Mountain pine oil, lavender oil, rosemary oil, pine oil, eucalyptus oil, peppermint oil, sage oil, bergamot oil, turpentine oil, lemon balm oil, juniper oil, lemon oil, aniseed oil, cardamom, camphor oil, in the liquid formulation soluble or insoluble polymers, eg. B. specialty and process chemicals such. Antifoams, hydrophobizing agents for textiles and / or leather, paper sizing agents, corrosion inhibitors, fuel additives, complexing agents, antioxidants, bleaching agents, enzymes, stabilizers, eg. As UV stabilizers, biocides, block and random copolymers. The surface-active substances are, for example, solubilizers, surfactants, cosurfactants, hydrotropes, protective colloids, such as polyvinylpyrrolidone, generally neutral, cationic, anionic and metallic dispersants, such as polyacrylates, polyacrylic acid and their salts, maleic acid / acrylic acid copolymers, naphthalene-formaldehyde condensates, naphthalenesulfonic acid condensates, phenolsulfonic acid condensates, neutral and cationized starch, polyvinyl alcohol, polyethyleneimine and polyvinylamine and modified products thereof, emulsifiers and / or thickeners, in particular anionic ones , nonionic, cationic or amphoteric surfactants, e.g. Alkyl polyglycosides, fatty alcohol sulfates, fatty alcohol ethers, alkanesulfonates, fatty alcohol ethoxylates, fatty alcohol alcohols, fatty alcohol ethers, fatty alcohols, alkylbetaines, sorbitan esters, alkoxylated sorbitan esters, sugar fatty acid esters, fatty acid polyglycerol esters, fatty acid partial glycerides, fatty acid carboxylates, fatty alcohol sulfosuccinates, fatty acid arcosinates, fatty acid isethionates, fatty acid taurinates, citric acid esters, silicone Polymers, silicone copolymers and / or fatty acid polyglycol esters. The exact composition of the liquid formulation depends on the field of application. Suitable applications are mentioned below.

In a further possible embodiment of the method according to the invention, the materials are applied to the at least one surface of the at least one substrate, for example by knife coating and / or spraying and / or dipping and / or brushing and / or spin coating and / or ESTA coating. Process or applied by other suitable methods known in the art or applied. Coating can be automated.

It is conceivable, using liquid and solid starting materials, in particular of pigments, aerosils, so-called fillers and additives to provide at least one homogeneous material, in particular a molecular or particulate disperse material. In a further possible embodiment of the process according to the invention, step (c), namely the drying step, is carried out only at room temperature or at temperatures <80 ° C. This can be realized, for example, as a kind of venting step.

Furthermore, it is conceivable to cure or to dry the respective coating produced thermally, by UV light, under air or inert, and / or by NIR light and / or by a stoving process. A thermal curing can be carried out in a suitable oven at a temperature in the range of 50 ⁰ C to 350 ⁰ C. A curing at a temperature of 250 ⁰ C to 300 ⁰ C may be particularly suitable, for example, for so-called coil coating applications. In this case, an optional so-called quenching process may be carried out by immersing the coating in, for example, a water bath and associated cooling.

Furthermore, it is possible to subject a coating produced in each case to several curing steps. The several identical or different curing steps to be carried out may also be different curing steps. This means that, for example, a first curing step can be carried out with UV light, which is then followed by another, for example, a thermal curing step.

In addition, the duration of the curing steps or operations performed can be suitably set or selected. By carrying out the curing, that is to say the type, the duration of time and possibly the sequence of different curing steps, the at least one property to be determined of the coatings produced can be controlled be influenced, from which later conclusions can be drawn on a to be carried out in the application coating with a particular material. Curing can also be automated. In this case, the type of curing, if necessary, the sequence of different curing and / or different curing steps and the respective duration of a curing step and, if necessary, the radiation dose to be applied during irradiation processes can be preset.

In a further embodiment of the method according to the invention, it is also conceivable to carry out the steps of provisioning and coating and optionally hardening for different materials at least partially in parallel. Such a parallel execution of the proposed process steps for different materials increases the efficiency and speed of the process. This results in less, ideally no so-called idle times.

Furthermore, it is conceivable that the at least one surface of the at least one substrate is coated with a plurality of coatings of the materials of the plurality of materials to produce at least one multi-layer coating. It is conceivable that the plurality of coatings are successively applied to each other, wherein between the application of two successive coatings, the first applied coating is optionally subjected to a curing process. The curing process can, as described above, be designed differently. However, it is also conceivable that successive coatings are applied directly without successive intermediate curing and only the complete multi-layer coating is suitably cured. All other possible variations when applying the coatings and optional hardening Processing steps between the application of the individual coatings are conceivable and known to the person skilled in the art.

In one possible embodiment of the method according to the invention, the respective coatings are produced with a respective layer thickness which is in the range from 2 μm to 500 μm. In addition, it can be determined which layer thickness is optimal for a particular application. Depending on the characteristic to be determined, different layer thicknesses may be suitable. A comparison of different properties of a coating of a material of a certain layer thickness allows conclusions about the optimum layer thickness of the corresponding material.

It is also conceivable to produce the respective coatings in each case with a layer thickness having a definable gradient in a further embodiment of the method according to the invention. This makes it possible to determine, for example, on one and the same coating, from which layer thickness the coating, for example, a coating with a pigment-containing dispersion is covering. By means of such a gradient formation, it is no longer necessary to investigate from which layer thickness a coating is covering to carry out a plurality of coatings having different layer thicknesses, which are to be carried out successively, thereby always having different starting situations.

It can be envisaged to automatically use parts used, in particular vessels, doctor blades, measuring probes, or to use them as disposable parts.

The at least one property which is to be determined for each coating produced may be mechanical, physical, electrical or other measurable For example, with regard to stability, for example against temperature load, UV or optical radiation exposure, weathering, rockfall or earthquake, viscosity, homogeneity, scratch resistance, flexibility, hardness, chemical resistance, weathering resistance, elasticity, creep behavior, ductility, gloss, crack resistance, Determining layer thickness, adhesion or colorimetry of the coating to be examined. Even visually perceptible defects such as bubbles can be determined here. Different, even conventional characterization methods can be used to determine the respective property. Due to the areal and contiguous extent of the coating to be examined, it is also possible to carry out further visual and manual characterizations. A coating can also be subjected to a weathering test, wherein here too a planar expansion of the coating to be examined is advantageous. As a conventional mechanical characterization methods, for example, an Erichsentiefung and a study with the Fischerscope (micro penetration measurement, among other things, to determine hardness and elasticity) can be mentioned here.

The step (d) of determining the at least one property can also be carried out automatically.

For example, automated viscosity measurements, for example at one or more shear rates, transmission and remission measurements, particle size measurements and spectroscopic methods such as Raman, NIR and / or IR spectrometry and / or image analysis can be carried out for a homogeneity test. One or more examinations can be carried out one after the other on one and the same coating. In some cases, measuring systems used can be automatically cleaned, at least when needed. A viscosity measurement can be done with any viscometer be performed, for example. A rotational viscometer. The homogeneity can be determined via an image analysis with different lighting situations, for example different brightnesses and illumination angles.

It is conceivable that the at least one substrate having at least one coating to be examined for determining the at least one property in step (d) is brought to a corresponding measuring location by means of an axis-mounted, preferably multi-axis manipulation system, for example a robot.

Expediently, in particular, the measuring station or apparatus provided for determining the at least one property has a modular structure, which allows the exchange of different characterization methods as a function of the property to be determined.

The substrate on which the respective coatings are to be applied can be made of a material selected from a group comprising at least wood, metal, glass, ceramics, paper, fiberboard and plastic. However, any other suitable material on which a material of the plurality of materials may be applied to form a coating may also be employed.

It is conceivable to provide the at least one surface of the at least one substrate in a size of 14.5 cm × 8.5 cm and a thickness of up to 1 cm. This is a suitable surface size in order to be able to provide a sufficiently large areal and contiguous extent of a respective coating on the one hand and on the other hand to enable a substrate that is easy to handle for a fast, efficient and optimized implementation of the method. Moreover, the present invention relates to an apparatus for automated performance of high-throughput trials of a plurality of materials for surface coating. The device according to the invention has at least the following stations:

(A) a formulation station in which the materials of the plurality of materials can be provided within a predetermined time interval,

(B) a coating station, in which at least one surface of at least one substrate can be coated with the respective provided materials to produce a respective coating, wherein at least one surface of the at least one substrate is applied to a maximum of five, in particular only one coating,

(C) a curing station,

(D) a characterization station in which at least one property of each of the generated coatings can be determined, and

(E) an evaluation unit and / or an interface to a data management for the controlled variation of the composition of the formulation, the process parameters and / or the characterization on material properties.

The stations are, at least in part, modular. Such a modular structure means that the stations or parts of the stations can be exchanged, supplemented or modifiable. This modular construction makes the device according to the invention very flexible and adaptable to different boundary conditions. Any repairs or pending modifications can be carried out quickly and efficiently.

The formulation station can comprise a dosing station, a closing station and a homogenization station, at which individual steps of providing a material of the plurality of materials can be carried out. Preferably, syringe-like vessels serve as containers for starting materials, as dosing containers, as mixing containers, for coating and for formulated materials. These disposable containers reduce the cleaning effort drastically. The individual stations of the formulation station can be operated automatically. Intermediate products obtained at the individual stations or mixtures produced in the meantime to produce a material to be provided can be passed from station to station in an appropriate sequence by means of an axis-mounted, preferably multiaxial manipulation system, for example a robot.

Furthermore, it is conceivable that the individual stations are operated in parallel, d. H. that, for example, a mixture for a second material is already produced at the dosing station, while a mixture for a first material is homogenized in the homogenization station.

The dosing station may further comprise a pipetting station or a syringe dosing station. As dosing station Dosimaten, peristaltic pumps and / or dosing for liquids with a temperature up to 300 ⁰ C are suitable. A metered quantity can be controlled by a balance. to be controlled. Further, it is possible to provide metering with stirring.

The homogenization station may be an ultrafasturrax, an ultrasonic disperser, a vibrator / shaker or a mixer. A combination of two or more of these devices is possible. The homogenization station may comprise a tempering and / or cooling station, optionally with a mixing and / or shaking device. However, the formulator station may also perform steps to provide a material in a single station.

In one possible embodiment of the device according to the invention, the formulation station comprises a so-called speed mixer. By means of such a speed mixer, it is, for example, possible to homogenize a pigment-containing dispersion or viscous mixtures quickly and precisely.

It is also possible that, in a weighing station as part of the formulation station, mixtures of grinding media and pulverulent starting materials, such as, for example, pigments, are preferably produced for pulverulent feedstocks, such as pigments, and a downstream metering station for grinding bodies. With a downstream dosing station for solid or liquid additives desired additives can be added. The additives may be surface-active substances, including surfactants, polymers and pigment derivatives. These additives can act as defoamers, deaerators, wetting agents, dispersants and / or leveling additives and / or Reologiever- improvers. In a subsequent subsequent dosing preferably for non-pigmented coating raw materials then one or more coating raw materials are added. In a subsequent closing, preferably screw Preferably, by means of a suitable axle-mounted, preferably multi-axis manipulation system, for example a robot, the vessel containing the mixture is closed and preferably fed by means of a robot to a dispersing unit, for example a speed mixer such as that offered by Haunschild. In the dispersing unit, a homogeneous liquid formulation is produced by multi-axis, centrifuge-like motion. After an adjustable and variable dispersing time, the liquid formulation and vessels containing the grinding media may preferably be removed from the dispersing aggregate by means of a robot and conveniently passed to the characterization station in a suitable vessel. There, by means of a suitable removal or pipetting method, a defined amount of the liquid formulation, such as a pigment-containing dispersion, can be removed for application to form a coating on the at least one surface of the at least one substrate. For example, a syringe may be used for removal. In order to prevent the grinding media from clogging the syringe inlet when aspirating the pigment-containing dispersion, a disposable syringe may be used which is only immersed in the milling insert at a distance of 2 to 4 mm or a filter insert is used. The immersion depth and tracking during the aspiration of the sample is, for example, guaranteed by a distance measurement or calculated by a control unit. The homogenized liquid formulations may be suitably applied by means of a robot to the at least one surface of the at least one substrate to produce a given coating. In the case of a pigment-containing dispersion, it is conceivable that the pigment-containing dispersion before application to the at least one surface of the at least one substrate with a defined amount of white and black paste is mixed. By mixing with white and Black paste can be changed, for example, the coloristics of the pigment-containing dispersion. The measurement is carried out by means of a suitable colorimetry device, which is arranged in the characterization station and can measure the coating colorimetrically. In this case, light is irradiated with a suitable wavelength in the form of light flashes at a suitable angle in each case at a certain distance.

In a further possible embodiment of the device according to the invention, at least one container is provided which is suitable both for providing therein at least one material of the plurality of materials and from it for the at least one material provided from the plurality of materials on the at least one surface of the at least one substrate for producing a coating. The container provided for this purpose can be, for example, a syringe which, on the one hand, serves to store a manufactured material and, moreover, is suitable for directly applying or applying the material for producing a corresponding coating on the surface of the substrate , It is conceivable to bring this container by means of at least one axis-mounted, preferably multi-axis manipulation system, for example a robot, from the formulation station to the coating station. It is conceivable that the characterization station comprises various suitable measuring devices, such as, for example, measuring devices for determining the transmission and / or remission, for image analysis, Raman spectrometers, gloss measuring devices, NIR spectrometers, IR spectrometers and / or particle size measuring devices. It is also conceivable that a colorimetric device is also provided.

It is conceivable to configure the device such that for the material to be provided for a coating a pH and / or a specific viscosity are set automatically.

Furthermore, it is conceivable that the device according to the invention additionally has as further unit:

(F) an axle-mounted, preferably multi-axis manipulation system, in particular a robot.

Furthermore, it can be provided that the evaluation unit provided according to the invention of the device according to the invention has at least one computing unit, such as a computer, for data acquisition and evaluation. In this case, the evaluation unit can have suitable software on a computer-readable medium, with the help of which the data determined and passed on by the characterization station are available. certain properties of the respective coatings documented, further processed, evaluated, compared against each other and possibly can be correlated with performance properties. It is conceivable to provide an optimization algorithm in order to be able to determine optimally suitable starting materials or components for producing a corresponding coating material and its layer thickness to be optimally produced with respect to properties investigated for a coating.

This means that documentation of formulation compositions, the manufacturing or provisioning process, and the measurement results relating to particular properties can be made automated. Furthermore, the evaluation unit can be designed to take over flowcharts and compositions of materials electronically from other computers, for example via external data management or as files. In the case of pigment dispersions, for example, various measurements of various properties, such as colloidal stability, particle size of the particles in the dispersion and dispersibility, can be carried out by so-called colorimetric measurement, preferably by taking up a reflectance spectrum. The evaluation of the recorded remission spectrum then takes place by means of a suitable colorimetric software, where, for example, at least one of the following colorimetric parameters is determined, inter alia:

Δa *, Δb *, ΔC *, DH (δ-hue angle), dL (δ-brightness), dC (δ-chroma), ddE (δ-glaze), FAE (chroma / color equivalent).

It can be provided to remove samples after curing in a further step from the device and after a maturation time of, for example, 24 hours again fed to the device for further treatment.

Furthermore, the invention provides for the use of the method according to the invention or the device according to the invention for the automated performance of high-throughput investigations of a plurality of materials for a surface coating.

With the aid of the method according to the invention and / or the device according to the invention, it is possible to test coatings of materials on corresponding substrates precisely, quickly and in particular in a practical or application-oriented manner. It is conceivable to determine various properties simultaneously on the basis of a suitably selected areal and contiguous extent of a respective coating. The provision of a planar expansion makes it possible in part to apply certain characterization methods for determining certain properties of a coating. For example, certain characterization methods require a certain area on a coating in order to be performed, so that useful property or characterization statements can be made. By a suitably selected areal and contiguous extent, it is also possible to determine several properties on the same coating. As a result of the planar expansion of a coating to be examined, it is possible to exclude as far as possible edge effects in a region to be subjected to a corresponding characterization method. An areal extent of a coating to be examined makes it possible in addition to be able to recognize original defects of a coating which only occur or become clearly recognizable with a certain size of the coating.

Materials which can be subjected to a process according to the invention can, for example, be, as already mentioned, paint formulations consisting of paint precursors, in particular pigment dispersions, polymeric binders which, for example, find broad applications as paints in the automotive sector. In order to be able to carry out application-oriented characterizations of such a lacquer, it is also advantageous here to produce a coating with a flat and coherent extension which comes very close to a lacquer layer to be applied to a motor vehicle. On such a coating now almost all tests can be performed in terms of properties that are also required for a paint film, for example. On a motor vehicle. These include, for example, mechanical, physical, electrical or other measurable properties, for example stability, for example against temperature load, UV or optical radiation exposure, weathering, stone impact or earthquake, viscosity, homogeneity, scratch resistance, hardness, chemical resistance, weathering resistance, elasticity, creep behavior, ductility, gloss, crack resistance, adhesion, coloristics and rheology. A weathering test can also be carried out here. In order to obtain a reproducibility, it is advantageous, as already mentioned, to provide exactly one coating per substrate, so that the coated substrates are readily comparable with one another, since the coatings applied thereto have a similar "history".

The properties of respective coatings determined in the method according to the invention can be stored in a database and processed by automated evaluation algorithms and, if appropriate, can be used automatically in order to design a formulation proposal optimized for a specific field of application.

Furthermore, it can be provided that the method according to the invention is logged by a suitable data management and possibly planned.

With the aid of the method according to the invention it is possible to use a material, i. usually a liquid formulation, such as to optimize a pigmented dispersion with respect to several relevant parameters. In this case, for example, properties relevant for a coating, such as mechanical, color, adhesion and chemical resistance properties, can be weighed against one another and from this an optimized formulation for a specific application can be derived.

By providing an at least partially modular construction of the device according to the invention, it is also possible to use individual parts of the device in the form of modules exchange and / or supplement. The modular design makes the device according to the invention very user-friendly and largely flexible in its application.

Furthermore, it can be provided to integrate algorithms for error treatment as a further step in the method according to the invention. It can be provided in the device according to the invention, sensors that can indicate a defect occurred, provide that can trigger an adjustable error treatment. Depending on the defect occurring, it may be, for example, a stopping of the entire device or else a gradual termination at the time of currently performed process steps in order to initiate further process steps for troubleshooting or discarding the currently processed sample.

By means of the method according to the invention and / or the use of the device according to the invention, characterization methods can be used which are adapted very closely to corresponding industrial processes.

The process can be carried out automatically in all its steps, which will be explained again in summary below.

The provision of the materials from the plurality of materials within a predetermined time interval then includes an automated production of the respective materials. In the case of a pigment-containing dispersion, such an automated production comprises, for example, automated weighing of at least one pigment and at least one lacquer into at least one vessel and automated homogenization by means of automated shaking or another suitable process, such that a pigment-containing dispersion is formed. It is, for example, conceivable that an automated production of a liquid formulation consists in bringing together various components forming the liquid formulation in a vessel, wherein at least one of the components is automatically metered into the vessel. The vessel may conveniently be a glass or vial with screw cap or snap closure, preferably at a volume of 1 to 100 ml. The nature of the combination is subject to no restriction insofar as it can be carried out automatically. The bringing together of the corresponding liquid formulation characterizing components can be done by presenting one or more components, in particular a component, automatic dosing of one or more components and / or automatic removal, in particular pipetting one or more components from one or more storage containers. It is conceivable that the vessel is initially empty and at least one component in a defined amount is automatically pipetted from a reservoir into the empty vessel or dosed. In one possible embodiment of the method according to the invention, the components corresponding to a corresponding liquid formulation are brought together in the vessel by means of at least one suitable robot. It is also possible that metering, pipetting and / or dilution steps are carried out in parallel for several samples at the same time.

For the preparation of pigment dispersions, the automated production of the mixture can be effected by an automated weighing of at least one pigment and of at least one further use component in at least one vessel. It is also possible for the preparation of paint formulations to weigh the at least one pigment formulation in different dosages with the at least one paint in a vessel. Again, a suitable robot can be used again. After weighing, a homogenization step may be automated to obtain a desired liquid formulation. The implementation of the homogenization is subject to no restriction, as far as an automated implementation is possible. Homogenization is preferably carried out by ultrathurrax, stirring, ultrasonic dispersion and / or shaking. If shaking is carried out, the vessel is auto- matically closed before shaking, whereas in the case of ultrasonic dispersion, stirring or ultrathurrax, the vessel is subsequently auto- matically sealed. The closure preferably takes place by means of a suitable robot. Advantageously, the homogenization time can be automatically changed and adjusted in a controllable manner. Several liquid formulations can be homogenized in parallel.

It can be provided that parts used, such as, for example, vessels, doctor blades, measuring probes, are automatically cleaned or used as disposable parts without the need for cleaning.

Furthermore, it can be provided that a liquid formulation is automatically tempered and / or cooled, it being possible at the same time mixed, for example, shaken, can be. Appropriately, in this case the tempering or cooling time is automatically controlled and adjustable. It is also possible to temper and / or cool several liquid formulations in parallel. In the case of the production of certain liquid formulations, such as, for example, a dispersion containing pigment, automated homogenization can be achieved by an automatic be done by shaking, so that a liquid formulation is formed. Before the automated shaking, an automated closing of the at least one vessel takes place, in which the various components forming the liquid formulation were weighed. The at least one vessel can be closed by means of a robot. Furthermore, the closed vessel can be given by the robot for automated shaking into a dispersing device, preferably a dispersing unit, particularly preferably a Skandex dispersing unit or a speed mixer. The dispersion time can be changed and adjusted automatically. Depending on the dispersion time, dispersions having different particle size distributions and thus also having different properties, in particular different coloristic properties, are obtained. It is conceivable as containers for feedstocks, as a metering container, as a mixing container, as a reservoir for formulated materials and as containers from which an appropriate formulation is applied to the surface of a substrate to be coated to provide syringe-like vessels. Several functions can also be taken over by a syringe-like vessel. As a result, the cleaning effort is drastically reduced. The syringe-like vessels are often disposable containers.

Furthermore, it is conceivable to carry out the determination of the at least one property of a respective coating in an automated manner when carrying out the method according to the invention. The properties may be, for example, mechanical, physical, electrical or other measurable properties, for example the stability, for example against thermal stress, UV or optical radiation exposure, weathering, stone chipping or earthquakes, viscosity, homogeneity, scratch resistance, hardness, chemical resistance, Weathering resistance, elasticity, creep behavior, ductility, gloss, crack resistance, adhesion act. A measurement of the viscosity can take place, for example, by automated viscosity measurements. For a homogeneity test, an automated spectroscopic method such as Raman, NIR and / or IR spectrometry and / or image analysis can be used. It is conceivable to carry out one or more investigations in parallel or in succession. The measurement systems used to determine the respective properties, for example a rotation body of a re-meter, can be automatically cleaned if necessary. A viscosity measurement can be carried out with any viscometer, for example a rotation viscometer. The homogeneity can be determined by an image analysis with different brightness levels. To determine a respective property, the substrate provided with a corresponding coating can be brought to a corresponding measuring location by means of an axis-mounted, preferably multiaxial manipulation system, for example a robot.

For applying a material of the plurality of materials to the at least one surface of the at least one substrate and the production of a coating, a suitable robot can be used, which by means of a removal unit, preferably a syringe, a desired amount of material, such as, for example, paint formulation , takes off. In order to prevent the syringe inlet during suction, for example, a pigment-containing dispersion to block the syringe input, a disposable syringe can be immersed only 2 to 4 mm, the immersion depth is preferably ensured by a distance measurement or calculated by a control unit. An evaluation of the specific properties of the respective coatings is carried out by means of a suitable software, it being possible to stop the determination of a specific property of a coating to be examined as soon as the coating to be examined proves to be unsuitable. The evaluation may also include a documentation of the examined coatings of the respective materials, the production process and the measurement results.

The method according to the invention and / or the device according to the invention are particularly suitable for use in the area of paint coatings, for example in the automotive industry. However, the invention can also be used for coatings in other industrial sectors, in the deco sector, in the field of woodworking or processing, in the field of construction or architectural industries and other areas in which to provide coatings of the type mentioned in the invention are to be used.

Claims

claims

A method of automated high-throughput inspection of a plurality of surface coating materials, wherein

(a) the materials of the plurality of materials are provided within a predetermined time interval;

(b) coating at least one surface of at least one substrate with the respective provided materials to form a respective coating,

(c) the respective coatings produced are cured or physically dried, and

(D) at least one property of each of the generated respective coatings is determined, wherein the respective coatings produced each have a parallel to the surface of the substrate extending areal and contiguous extent of at least 25cm ² .

2. The method of claim 1, wherein the areal extent is in a range of 25 cm ² to 2000 cm ² , in particular in a range of 25 cm ² to 200 cm ² , in particular 36cm ² and in particular 6cm x 6cm or 123 , 25cm ² and is especially 8.5cm x 14.5cm.

3. The method of claim 1 or 2, wherein the at least one surface of the at least one substrate is coated with less than six coatings each of different materials.

4. The method of claim 3, wherein the at least one surface of the at least one substrate is coated with precisely one coating of a material of the plurality of materials.

5. The method according to any one of the preceding claims, wherein the plurality of materials greater than or equal to 25, in particular greater than or equal to 50, in particular greater than or equal to 100, in particular comprises different materials and in particular within a time interval of 24 hours up to 100 feedstocks is produced.

A method according to any one of the preceding claims, wherein the materials are provided sequentially or in parallel.

7. The method according to any one of the preceding claims, wherein using liquid and solid starting materials, in particular of pigments, aerosils, so-called fillers and additives at least one homogeneous material, in particular a molecular or particulate disperse material is provided.

8. The method according to any one of the preceding claims, wherein the respective coatings produced are cured or physically dried in one or more further steps.

A method according to any one of the preceding claims, wherein the steps of providing and coating, and optionally curing, are carried out, at least in part, in parallel for different materials of the plurality of materials.

10. The method according to any one of the preceding claims, wherein the generated respective coating is cured by UV light, both under an oxygen-containing atmosphere and inert, and / or NIR light and / or by the action of temperature.

11. The method of claim 10, wherein the generated respective coating is successively subjected to a plurality of curing steps in selectable orders for a definable period of time.

12. The method of claim 1, wherein the at least one surface of the at least one substrate is coated with a plurality of coatings of the materials of the plurality of materials to form at least one multi-layer coating.

13. The method of claim 12, wherein the plurality of coatings are applied sequentially, wherein between the application of two successive coatings, the first applied coating can be cured if necessary.

14. The method according to any one of the preceding claims, wherein the respective coatings are prepared by doctoring and / or spraying and / or dipping.

15. The method according to any one of the preceding claims, in which used parts, in particular vessels, doctor blades, probes, automatically cleaned or used as disposable parts.

16. The method according to any one of the preceding claims, wherein the respective coatings with a respective Layer thickness, which is in the range of 2 .mu.m to 500 .mu.m, are produced.

17. The method according to any one of the preceding claims, wherein the respective coatings are each prepared with a definable gradient having layer thickness.

18. The method according to claim 1, wherein the at least one property that is determined is a mechanical, electrical or other measurable property, which is in particular selected from the group consisting of: stability - for example against temperature load, UV or optical radiation exposure, weathering, rockfall or earthquake - viscosity, homogeneity, scratch resistance, hardness, chemical resistance, weathering resistance, elasticity, creep behavior, ductility, gloss, crack resistance, adhesion, colorimetry, visually perceptible defects, such as, for example, blisters.

19. The method according to any one of the preceding claims, wherein the at least one property is determined by a conventional characterization method.

20. The method of claim 1, wherein the at least one substrate is made of a substance selected from a group comprising at least wood, metal, glass, ceramics, paper and plastic.

21. The method of claim 1, wherein the at least one surface of the at least one substrate has a size of 14.5 cm x 8.5 cm and a thickness up to learning.

22. The method according to any one of the preceding claims, wherein at least a portion of the materials from the plurality of materials is provided in the form of a respective liquid formulation with metered addition and / or dispersion of suitable liquids and / or solids.

23. An apparatus for the automated performance of high-throughput investigations of a plurality of materials for surface coatings, the device comprising at least the following stations:

(A) a metering or formulation station wherein the materials of the plurality of materials can be provided within a predetermined time interval;

(C) a curing station and / or drying station,

(D) a characterization station in which at least one property of each of the generated respective coatings can be determined, and

wherein the stations are at least partially modular.

24. The device according to claim 23, wherein the formulation station comprises a so-called speed mixer.

25. Apparatus according to claim 23 or 24, wherein the pH and / or viscosity of the materials to be provided are automatically adjustable.

26. The apparatus of claim 23, 24 or 25, wherein at least one container is provided which is adapted to both provide therein at least one material of the plurality of materials and from thereon the at least one provided material of the plurality of materials on the to apply at least one surface of the at least one substrate to produce a coating.

27. Device according to one of claims 23 to 26, wherein the device additionally has as an additional element:

28. Device according to one of claims 23 to 27, wherein the evaluation unit has at least one arithmetic unit for data acquisition and / or data evaluation and electronically from other computers, eg. About an external data management, or as files accepts schedules and compositions of materials.

29. Device according to one of claims 23 to 28, taken in the sample after curing from the device and can be re-introduced after a predetermined maturation time.

30. Use of the method according to one of claims 1 to 22 or the device according to one of claims 23 to 29 for carrying out high-throughput investigations of a plurality of materials for surface coatings.