WO2007096117A1 - Procede et dispositif de realisation automatisee de recherches a haut rendement - Google Patents

Procede et dispositif de realisation automatisee de recherches a haut rendement Download PDF

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Publication number
WO2007096117A1
WO2007096117A1 PCT/EP2007/001418 EP2007001418W WO2007096117A1 WO 2007096117 A1 WO2007096117 A1 WO 2007096117A1 EP 2007001418 W EP2007001418 W EP 2007001418W WO 2007096117 A1 WO2007096117 A1 WO 2007096117A1
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WO
WIPO (PCT)
Prior art keywords
materials
coating
coatings
substrate
station
Prior art date
Application number
PCT/EP2007/001418
Other languages
German (de)
English (en)
Inventor
Wolfgang Schrof
Eva Wagner
Thomas Meier
T. Brinz
Sebastian Koltzenburg
T. Burk
T. Geiger
Tiefenbacher
Original Assignee
Basf Se
Robert Bosch Gmbh
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Basf Se, Robert Bosch Gmbh filed Critical Basf Se
Priority to EP07722854A priority Critical patent/EP1988991A1/fr
Publication of WO2007096117A1 publication Critical patent/WO2007096117A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0046—Sequential or parallel reactions, e.g. for the synthesis of polypeptides or polynucleotides; Apparatus and devices for combinatorial chemistry or for making molecular arrays
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84—Systems specially adapted for particular applications
    • G01N21/8422—Investigating thin films, e.g. matrix isolation method
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277—Apparatus
    • B01J2219/00351—Means for dispensing and evacuation of reagents
    • B01J2219/00436—Maskless processes
    • B01J2219/00443—Thin film deposition
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277—Apparatus
    • B01J2219/00497—Features relating to the solid phase supports
    • B01J2219/00527—Sheets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00583—Features relative to the processes being carried out
    • B01J2219/00585—Parallel processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00583—Features relative to the processes being carried out
    • B01J2219/00596—Solid-phase processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00718—Type of compounds synthesised
    • B01J2219/00756—Compositions, e.g. coatings, crystals, formulations
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D1/00—Processes for applying liquids or other fluent materials
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/251—Colorimeters; Construction thereof
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3577—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/55—Specular reflectivity
    • G01N21/57—Measuring gloss
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/59—Transmissivity
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/65—Raman scattering
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84—Systems specially adapted for particular applications
    • G01N21/88—Investigating the presence of flaws or contamination

Definitions

  • the present invention relates to a method and a device for the automated performance of high-throughput investigations of a plurality of materials for heatnbe harshungen.
  • liquid formulations such as dispersions, emulsions or solutions
  • screening tests in order to test and optimize them with regard to various properties.
  • 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.
  • HTS 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.
  • IK One-component
  • 2K two component
  • additives e.g. Flow control agents, UV absorbers, photoinitiators, fillers, catalysts, stabilizers, matting agents an important role.
  • 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.
  • 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.
  • 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.
  • marginal effects should as far as possible be excluded in the area intended to determine the property.
  • the coating produced should have so-called "minimum film quality".
  • 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.
  • the areal extent may preferably also be 123.25 cm 2 and in particular 8.5 cm ⁇ 14.5 cm.
  • 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.
  • DIN-EN ISO 1520 and / or DIN 67530 and / or DIN 53151 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.
  • 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.
  • 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.
  • 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.
  • the materials of the plurality of materials may be liquid formulations, such as dispersions, emulsions or solutions or combinations thereof.
  • the materials may be liquid formulations, such as dispersions, emulsions or solutions or combinations thereof.
  • 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.
  • liquid formulations such as, for example, pigment-containing dispersions
  • speed mixer it is possible, for example, to use a so-called speed mixer.
  • homogenization balls for example. From metal, ceramic or glass can be used. These balls can be filled manually or offline or automatically and automati- Mogenrawen 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.
  • 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
  • a defined amount of the liquid formulation such as, for example, a pigment ha
  • a coating to the at least one surface of the at least one substrate.
  • a syringe For removal can be used, for example, a syringe.
  • a disposable 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.
  • 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.
  • 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.
  • As alcohols such as butanol, ethanol, methanol, polyhydric alcohols such as glycerol or polyols, organic solvents such.
  • 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.
  • 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, iso
  • 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.
  • 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.
  • 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.
  • 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.
  • an optional so-called quenching process may be carried out by immersing the coating in, for example, a water bath and associated cooling.
  • a coating produced in each case may be subject 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.
  • the duration of the curing steps or operations performed can be suitably set or selected.
  • 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.
  • 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.
  • 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.
  • 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.
  • 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.
  • the respective coatings are produced with a respective layer thickness which is in the range from 2 ⁇ m to 500 ⁇ m.
  • a respective layer thickness which is in the range from 2 ⁇ m to 500 ⁇ m.
  • the at least one property which is to be determined for each coating produced may be mechanical, physical, electrical or other measurable
  • 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.
  • 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.
  • 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.
  • 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.
  • 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.
  • 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.
  • 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.
  • 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:
  • 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.
  • 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.
  • 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.
  • a pipetting station or a syringe dosing station.
  • 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.
  • the formulator station may also perform steps to provide a material in a single station.
  • the formulation station comprises a so-called speed mixer.
  • a 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.
  • mixtures of grinding media and pulverulent starting materials are preferably produced for pulverulent feedstocks, such as pigments, and a downstream metering station for grinding bodies.
  • pulverulent feedstocks such as pigments
  • a downstream metering station for grinding bodies.
  • 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.
  • a subsequent subsequent dosing preferably for non-pigmented coating raw materials then one or more coating raw materials are added.
  • a subsequent closing preferably screw
  • 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.
  • a dispersing unit for example a speed mixer such as that offered by Haunschild.
  • a homogeneous liquid formulation is produced by multi-axis, centrifuge-like motion.
  • 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.
  • a defined amount of the liquid formulation such as a pigment-containing dispersion
  • a syringe may be used for removal.
  • 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.
  • 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.
  • white and Black paste 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.
  • 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.
  • 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.
  • the device according to the invention additionally has as further unit:
  • 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.
  • 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.
  • 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.
  • 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:
  • ⁇ a *, ⁇ b *, ⁇ C *, DH ⁇ -hue angle
  • dL ⁇ -brightness
  • dC ⁇ -chroma
  • ddE ⁇ -glaze
  • FAE chroma / color equivalent
  • 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.
  • 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.
  • paint formulations consisting of paint precursors, in particular pigment dispersions, polymeric binders which, for example, find broad applications as paints in the automotive sector.
  • compositions 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.
  • the method according to the invention is logged by a suitable data management and possibly planned.
  • a material i. usually a liquid formulation, such as to optimize a pigmented dispersion with respect to several relevant parameters.
  • 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.
  • the device according to the invention 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.
  • sensors that can indicate a defect occurred provide that can trigger an adjustable error treatment.
  • an adjustable error treatment 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.
  • characterization methods can be used which are adapted very closely to corresponding industrial processes.
  • the provision of the materials from the plurality of materials within a predetermined time interval then includes an automated production of the respective materials.
  • 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.
  • 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.
  • 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.
  • 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.
  • 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.
  • the homogenization time can be automatically changed and adjusted in a controllable manner. Several liquid formulations can be homogenized in parallel.
  • parts used such as, for example, vessels, doctor blades, measuring probes, are automatically cleaned or used as disposable parts without the need for cleaning.
  • a liquid formulation is automatically tempered and / or cooled, it being possible at the same time mixed, for example, shaken, can be.
  • the tempering or cooling time is automatically controlled and adjustable. It is also possible to temper and / or cool several liquid formulations in parallel.
  • automated homogenization can be achieved by an automatic be done by shaking, so that a liquid formulation is formed.
  • 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.
  • 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.
  • 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.
  • 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.
  • an automated spectroscopic method such as Raman, NIR and / or IR spectrometry and / or image analysis can be used.
  • the measurement systems used to determine the respective properties 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.
  • 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.
  • a suitable 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.
  • a removal unit preferably a syringe
  • a desired amount of material such as, for example, paint formulation
  • 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.
  • 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.

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  • Life Sciences & Earth Sciences (AREA)
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  • Health & Medical Sciences (AREA)
  • Organic Chemistry (AREA)
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  • General Physics & Mathematics (AREA)
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  • Application Of Or Painting With Fluid Materials (AREA)

Abstract

La présente invention concerne un procédé de réalisation automatisée de recherches à haut rendement parmi une pluralité de matériaux de revêtements de surface, selon lequel (a) les matériaux de la pluralité de matériaux sont disponibles dans un intervalle de temps donné ; (b) au moins une surface d'au moins un substrat est enduite avec les matériaux respectifs pour produire les revêtements respectifs, (c) les revêtements respectifs obtenus sont durcis et (d) au moins une propriété de chacun des revêtements respectifs obtenus est évaluée, lesdits revêtements respectifs obtenus présentant une étendue plane parallèle à la surface des substrats et cohérente supérieure ou égale à 25 cm2. La présente invention concerne également un dispositif associé pour réalisation automatisée de recherches à haut rendement parmi une pluralité de matériaux de revêtements de surface.
PCT/EP2007/001418 2006-02-21 2007-02-19 Procede et dispositif de realisation automatisee de recherches a haut rendement WO2007096117A1 (fr)

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DE102006008869.7 2006-02-21
DE200610008869 DE102006008869A1 (de) 2006-02-21 2006-02-21 Verfahren und Vorrichtung zur automatisierten Durchführung von Hochdurchsatz-Untersuchungen

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008135290A1 (fr) * 2007-05-08 2008-11-13 Hte Aktiengesellschaft Plateforme d'enduction et procédé pour la préparation de revêtements minces
EP2872262B1 (fr) 2012-07-13 2018-12-12 PPG Industries Ohio, Inc. Système et procédé de production automatisée, application et évaluation de compositions de revêtement

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Publication number Priority date Publication date Assignee Title
DE19834184A1 (de) * 1998-07-29 2000-02-03 Basf Ag Verfahren und Vorrichtung zur Optimierung von Lacken
US6151123A (en) * 1997-07-14 2000-11-21 Symyx Technologies, Inc. Systems and methods for employing optical probes to characterize material properties
WO2002034381A1 (fr) * 2000-10-26 2002-05-02 General Electric Company Systemes et procedes permettant de fabriquer des banques d'enrobages
US6460417B1 (en) * 2001-08-24 2002-10-08 General Electric Company Formability testing of small-size coatings and materials
US20030077390A1 (en) * 2001-10-23 2003-04-24 Potyrailo Radislav Alexandrovich Systems and methods for the deposition and curing of coating compositions

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Publication number Priority date Publication date Assignee Title
US6151123A (en) * 1997-07-14 2000-11-21 Symyx Technologies, Inc. Systems and methods for employing optical probes to characterize material properties
DE19834184A1 (de) * 1998-07-29 2000-02-03 Basf Ag Verfahren und Vorrichtung zur Optimierung von Lacken
WO2002034381A1 (fr) * 2000-10-26 2002-05-02 General Electric Company Systemes et procedes permettant de fabriquer des banques d'enrobages
US6460417B1 (en) * 2001-08-24 2002-10-08 General Electric Company Formability testing of small-size coatings and materials
US20030077390A1 (en) * 2001-10-23 2003-04-24 Potyrailo Radislav Alexandrovich Systems and methods for the deposition and curing of coating compositions

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008135290A1 (fr) * 2007-05-08 2008-11-13 Hte Aktiengesellschaft Plateforme d'enduction et procédé pour la préparation de revêtements minces
EP2002886A1 (fr) * 2007-05-08 2008-12-17 HTE Aktiengesellschaft The High Throughput Experimentation Company Plateforme de revêtement et procédé pour la préparation de revêtements minces
EP2872262B1 (fr) 2012-07-13 2018-12-12 PPG Industries Ohio, Inc. Système et procédé de production automatisée, application et évaluation de compositions de revêtement
EP2872262B2 (fr) † 2012-07-13 2021-12-22 PPG Industries Ohio, Inc. Système et procédé de production automatisée, application et évaluation de compositions de revêtement
US11395997B2 (en) 2012-07-13 2022-07-26 Ppg Industries Ohio, Inc. Systems for automated production, application and evaluation of coating compositions

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EP1988991A1 (fr) 2008-11-12

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