EP1242192A1 - Procede et dispositif de test combinatoire ameliore pour formulations de matieres de revetement et procedes associes - Google Patents

Procede et dispositif de test combinatoire ameliore pour formulations de matieres de revetement et procedes associes

Info

Publication number
EP1242192A1
EP1242192A1 EP00976736A EP00976736A EP1242192A1 EP 1242192 A1 EP1242192 A1 EP 1242192A1 EP 00976736 A EP00976736 A EP 00976736A EP 00976736 A EP00976736 A EP 00976736A EP 1242192 A1 EP1242192 A1 EP 1242192A1
Authority
EP
European Patent Office
Prior art keywords
samples
coating
centrifuge
well
array
Prior art date
Legal status (The legal status 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 status listed.)
Withdrawn
Application number
EP00976736A
Other languages
German (de)
English (en)
Inventor
Jay R. Akhave
Dennis L. Saunders
Radislav Alexanrovich Potyrailo
Daniel Robert Olson
William Patrick Flanagan
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Avery Dennison Corp
General Electric Co
Original Assignee
Avery Dennison Corp
General Electric Co
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 Avery Dennison Corp, General Electric Co filed Critical Avery Dennison Corp
Publication of EP1242192A1 publication Critical patent/EP1242192A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
    • B01L3/508—Containers for the purpose of retaining a material to be analysed, e.g. test tubes rigid containers not provided for above
    • B01L3/5085—Containers for the purpose of retaining a material to be analysed, e.g. test tubes rigid containers not provided for above for multiple samples, e.g. microtitration plates
    • B01L3/50853—Containers for the purpose of retaining a material to be analysed, e.g. test tubes rigid containers not provided for above for multiple samples, e.g. microtitration plates with covers or lids
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
    • B01L3/505—Containers for the purpose of retaining a material to be analysed, e.g. test tubes flexible containers not provided for above
    • 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
    • B05D1/002—Processes for applying liquids or other fluent materials the substrate being rotated
    • 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
    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/06—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to radiation
    • B05D3/061—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to radiation using U.V.
    • B05D3/065—After-treatment
    • B05D3/067—Curing or cross-linking the coating
    • 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
    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/12—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by mechanical means
    • 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
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N19/00—Investigating materials by mechanical methods
    • G01N19/04—Measuring adhesive force between materials, e.g. of sealing tape, of coating
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/26—Oils; viscous liquids; paints; inks
    • G01N33/32—Paints; inks
    • 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
    • B01J2219/00279—Features relating to reactor vessels
    • B01J2219/00306—Reactor vessels in a multiple arrangement
    • B01J2219/00313—Reactor vessels in a multiple arrangement the reactor vessels being formed by arrays of wells in blocks
    • B01J2219/00315—Microtiter plates
    • 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
    • B01J2219/00364—Pipettes
    • 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
    • B01J2219/00479—Means for mixing reactants or products in the reaction vessels
    • B01J2219/00481—Means for mixing reactants or products in the reaction vessels by the use of moving stirrers within the reaction vessels
    • 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
    • B01J2219/00587—High throughput 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
    • B01J2219/00603—Making arrays on substantially continuous surfaces
    • B01J2219/00605—Making arrays on substantially continuous surfaces the compounds being directly bound or immobilised to solid supports
    • 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
    • B01J2219/00603—Making arrays on substantially continuous surfaces
    • B01J2219/00605—Making arrays on substantially continuous surfaces the compounds being directly bound or immobilised to solid supports
    • B01J2219/00614—Delimitation of the attachment areas
    • B01J2219/00621—Delimitation of the attachment areas by physical means, e.g. trenches, raised areas
    • 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
    • B01J2219/00603—Making arrays on substantially continuous surfaces
    • B01J2219/00605—Making arrays on substantially continuous surfaces the compounds being directly bound or immobilised to solid supports
    • B01J2219/00632—Introduction of reactive groups to the surface
    • B01J2219/00637—Introduction of reactive groups to the surface by coating it with another layer
    • 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
    • B01J2219/0068—Means for controlling the apparatus of the process
    • B01J2219/00686—Automatic
    • B01J2219/00691—Automatic using robots
    • 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
    • B01J2219/0072—Organic compounds
    • B01J2219/00722—Nucleotides
    • 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
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/08—Geometry, shape and general structure
    • B01L2300/0887—Laminated structure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2400/00—Moving or stopping fluids
    • B01L2400/04—Moving fluids with specific forces or mechanical means
    • B01L2400/0403—Moving fluids with specific forces or mechanical means specific forces
    • B01L2400/0409—Moving fluids with specific forces or mechanical means specific forces centrifugal forces
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
    • C07B2200/00—Indexing scheme relating to specific properties of organic compounds
    • C07B2200/11—Compounds covalently bound to a solid support
    • C—CHEMISTRY; METALLURGY
    • C40—COMBINATORIAL TECHNOLOGY
    • C40B—COMBINATORIAL CHEMISTRY; LIBRARIES, e.g. CHEMICAL LIBRARIES
    • C40B40/00—Libraries per se, e.g. arrays, mixtures
    • C40B40/04—Libraries containing only organic compounds
    • C40B40/14—Libraries containing macromolecular compounds and not covered by groups C40B40/06 - C40B40/12
    • C—CHEMISTRY; METALLURGY
    • C40—COMBINATORIAL TECHNOLOGY
    • C40B—COMBINATORIAL CHEMISTRY; LIBRARIES, e.g. CHEMICAL LIBRARIES
    • C40B60/00—Apparatus specially adapted for use in combinatorial chemistry or with libraries
    • C40B60/14—Apparatus specially adapted for use in combinatorial chemistry or with libraries for creating libraries
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N2035/00465—Separating and mixing arrangements
    • G01N2035/00534—Mixing by a special element, e.g. stirrer
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/02—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor using a plurality of sample containers moved by a conveyor system past one or more treatment or analysis stations
    • G01N35/04—Details of the conveyor system
    • G01N2035/0401—Sample carriers, cuvettes or reaction vessels
    • G01N2035/0418—Plate elements with several rows of samples
    • G01N2035/0422—Plate elements with several rows of samples carried on a linear conveyor
    • G01N2035/0424—Two or more linear conveyors
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/02—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor using a plurality of sample containers moved by a conveyor system past one or more treatment or analysis stations
    • G01N35/028—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor using a plurality of sample containers moved by a conveyor system past one or more treatment or analysis stations having reaction cells in the form of microtitration plates

Definitions

  • the invention relates generally to methods and apparatus for identification and optimization of coating materials and properties for desired applications. More specifically, the invention relates to an improved process of creating coatings, involving identifying candidate materials and screening and optimizing formulations and coating parameters for desired applications.
  • coating materials for example adhesive coatings, release coats, protective coatings, and the like as well as films and laminate constructions of layered materials, has conventionally been a time consuming and labor intensive process.
  • Candidate materials are identified primarily based on knowledge and experience with what compositions have worked before in related applications and investigating like materials and combinations of materials. This usually involves preparing a coating formulation, preparing a test coating for evaluation (often involving several tries to attain the desired parameters such as coat weight, cure. etc. for evaluation), drying or otherwise curing the coating, then evaluating the coating by testing the property of interest, such as permeability, tack, shear and bending strength, surface roughness, etc., and entering the results in a database for comparison with further coatings to be developed and tested.
  • the property of interest such as permeability, tack, shear and bending strength, surface roughness, etc.
  • Holdover effects result in the contamination of one candidate coating material due to residual coating material remaining in the coat dispensing apparatus and/or coat-receiving substrate from a prior test coating material. Contamination as a result of holdover effects are generally additive and provide a level of error in coat formulation that is difficult to control. It is therefore preferable, especially when the volume of coating material to be tested is small, to use a coating method that either eliminates or significantly reduces holdover effects. Use of a disposable method for dispensing as well as receiving the test coat material would eliminate problems associated with holdover effects.
  • a variety of methods for coating desired substrates or materials are available and include spin coating, die coating and non-contact jet coating methods.
  • Spin coating is a technique commonly used in the field of electronics where the coat material is dispensed onto a desired surface by centrifugal force (spinning).
  • the coatweights resulting from this method are limited to very thin coatings and there is a significant loss of material during the coating process.
  • die and jetting nozzle costs prohibit their modification to disposable units.
  • an inexpensive, efficient and disposable method for testing a large number of coating materials has not been known. While many significant advances in coating technology have been made in recent years. acceleration of the rate at which coating materials can be identified, screened, investigated and optimized will be recognized as a desirable goal by those skilled in the an.
  • An object of the invention is to provide a multi-well apparatus for making arrays of coating materials.
  • Such arrays are suitable for analysis and may comprise a disposable two-layer assembly where the first layer contains a plurality of wells and the second layer is a substrate layer. Both layers can be flexible, with the second or bottom layer being detachable from the overlying first layer.
  • Such an apparatus can be made of disposable material, thus providing a cost-effective, efficient and reliable means of testing numerous formulations of coating material.
  • the invention also provides a method of developing a new coating having a desired performance characteristic with regard to a property of a coating, comprising: a) providing an array of coating wells, b) placing a coating material having the known parameter in each coating well, varying the parameter so as to provide a plurality of coatings having different parameter values in a plurality of coating wells; c) correlating the value of the parameter for the coatings deposited in each of the plurality of coating wells with the position of the coating well in the array, whereby a parameter value is associated with each coating well position in the array; d) applying a leveling force to the array of wells to level the coating material in the coating wells; and e) testing the coatings in the array to analyze the relationship between the position in the array and performance with regard to the property of the coating material, whereby the value of the parameter can be correlated to the performance of the coating with regard to the property of the coating.
  • the coatings in the array can be dried while the leveling force is applied.
  • the above combinatorial, high-throughput method of screening candidate coat materials results in a significant increase in the discovery rate of new coating materials.
  • the leveling force may be provided by a centrifuge.
  • FIG. 1 is a generic schematic of the combinatorial discovery process
  • FIG. 2 is a perspective view of an example of a robotic dispenser usable in one embodiment of the invention
  • FIG. 3 is a top view of an example of a well plate usable in one embodiment of the invention.
  • FIG. 4 is a perspective view of an example of a well plate having a removable well bottom, comprising a substrate to which sample coatings are applied, usable in one embodiment of the invention
  • FIG. 5 is a perspective view of another example of a well plate having a removable well bottom comprising a substrate to which sample coatings are applied, usable in one embodiment of the invention
  • FIG. 6 is a side view of a well plate having a curved bottom usable in one embodiment of the invention
  • FIG. 7 is a side view of a flexible well plate having a removable top portion usable in one embodiment of the invention
  • FIG. 8 is a side view of a well plate having a laminate construction usable in one embodiment of the invention
  • FIG. 9 is a schematic diagram showing leveling of coating array materials by application of a leveling force and curing by hot air;
  • FIG. 10a is a is a perspective view of an example of a vertical centrifuge with a horizontal axis of rotation, usable in one embodiment of the invention.
  • FIG. 10b is a perspective view of an example of a centrifuge usable in another embodiment of the invention.
  • FIG. 1 1 is a perspective view of an example of a swing arm centrifuge rotor assembly usable in one embodiment of the invention, showing the assembly loaded with well plates;
  • FIG. 12 is a perspective view of an example of a 96- well plate usable in one embodiment of the invention
  • FIG 13 is a perspective view of a vertical centrifuge with an attached ultraviolet light source usable in one embodiment of the invention
  • FIG 14a is a schematic side view of the vertical centrifuge with an external ultraviolet light source and centrifuge mounted mirror.
  • FIG 14b is a schematic frontal view of a vertical centrifuge with mounted mirror.
  • the term "combinatorial” refers to the combined approach of high-throughput analysis of libraries consisting of arrays of coat material formulations. Included in the high- throughput analysis are automated or robotic processing of the sample arrays. Combinatorial methods have been used in the medical, pharmaceutical and biotechnology industries to develop chemical compositions, particularly pharmaceuticals and medicaments, for a number of years. However, these prior combinatorial methods have not been well suited to development of new coatings. Applicants herein provide techniques for generating arrays of coating formulations, well suited to the application of combinatorial chemistry methods. These techniques allow new coatings to be screened and evaluated on a high throughput basis, in order to produce new coatings economically.
  • a system 10 in accordance with principles of the invention comprises a method of developing new coatings by means of a combinatorial approach.
  • a first step 12 is to define what end result coating is desired, and what characteristics and qualities such a coating will have.
  • a new material, or a new construction of several materials, such as a laminate for example, comprising new and/or conventional materials combined in a novel way may be required.
  • the next step 13 is to select likely candidate materials. These can comprise formulations of generally dilute solutions of raw material ingredients 14 that are contemplated as likely elements or components that may provide a coating material with desired characteristics.
  • a material library of a few to a few hundred thousand, or more, chemical combinations are formed and dispensed into an array of coating wells 18 using a robot or other automated device 17 to make a library or array of coating materials .
  • the "libraries" may include the samples in a single array, or the samples may form a plurality of arrays, processed either concurrently or successively.
  • the chemical combinations forming at least part of the library are then processed in parallel as indicated at reference numeral 19.
  • Processing can include exposing the coating array to a variety of processing variables such as heat, pressure and time as well as applied leveling forces to shape the resultant library or array of coat samples, as can be accomplished, for example, by a vertical centrifuge 20.
  • high throughput analysis is performed whereby the library is screened by detectors that quickly scan various properties of the coating materials. After the high throughput analysis, materials with the desired properties are identified 22 with the results entered into a large database 23.
  • Each library is comprised of one or more arrays of variations of materials to be tested.
  • Each individual site in an array will correspond to a specific formulation of a coat material, wherein the parameter or coat descriptor(s) of the material located at that site is known.
  • Miniaturization of the sample size facilitates processing and greatly saves cost and time thereby increasing efficiency and the rate of discovery.
  • the end result is discovery and determination of the most successful new material(s) and the process or parameters used to produce the new materials. These materials are then selected for large scale production and commercialization 24.
  • the combinatorial approach to development and testing of novel coat materials greatly benefits from use of devices and apparatus that allow flat coating samples in the arrays or within wells in the arrays. Additional embodiments encompassing such devices and apparatus are included in the present invention and further described below.
  • holdover is defined as the volume of material that is residual in a cavity after it is emptied and could contaminate the next batch of material deposited into the cavity.
  • the potential for holdover increases. For example, tubes, pipette tips, material dispensers and such all have potential holdover volumes.
  • the contamination is also a function of the rheological nature or viscosity of the material that is deposited into the cavity. Holdover effects in traditional methods of developing coating materials greatly increases the level of error, compromising the identification of correct parameters of a new coat material.
  • a disposable dispensing device 25 (FIG. 2) and a disposable substrate assembly (formatted as a multi-well apparatus) 26. both of which are further described below.
  • substrate is defined as any coat-receiving surface or material, or a substance upon which a sample coat material resides which allows the testing of that sample.
  • a "substrate assembly” is a composite of materials formed into a unit or apparatus for holding a large number of different coating samples in an array format (FIG. 3).
  • An "array format” as used herein, is a matrix format where the samples of coating material are arranged as discrete coated areas 31 on a surface, such as a planar surface. For example, a 48- well coating array (FIG. 3) would have 48 discrete coated areas arranged as 6 rows 27 and 8 columns 28.
  • Multi-well Apparatus for Parallel Processing of a Material Library An initial step in the development of a coating is to create the various mixed formulations to be placed in the wells in the array.
  • sample formulations can be mixed or prepared in a multi-well plate format (FIG. 3) with each individual well containing a unique, pre-defined formulation to be tested.
  • FOG. 3 multi-well plate format
  • a variety of types of commercially available multi-well plates suitable for use in the present invention can be used (Millipore Corp.. Polyfiltronics. VWR Scientific).
  • Such multi-well plates can vary in size of plate dimension, size of well (outer circumference as well as well-depth), type of material used to construct the multi-well plate (for example, polystyrene or polypropylene, rigid plastic or flexible plastic).
  • the biotechnology and pharmaceutical industry utilizes multi-well plates (generally 48-, 96- or 256-well plates) whose outer dimensions are standardized for use with robotic dispensers.
  • standardized multi-well plates are rectangular, rigid, stackable plates with right edges of the top or lid portion being curved 29.
  • the outside dimensions of a complete multi-well unit are approximately 5 x 3.25 inches.
  • Such multi-well plates are suitable for use in the present invention.
  • the well size used should be of substantial volume so as to allow adequate robotic mixing of the required or needed amount of each formulation without drying up of the solutions contained in the wells.
  • Robotic, automated mixing of the formulations can be achieved by utilizing commercially available positioning equipment, such as Asymtek's x.y.z. coordinate motion equipment.
  • a mixing apparatus that drives a microblade attachment.
  • the microblade consists of mixing blades that when placed into the appropriate mixing well and spun by the mixing apparatus, mixes the components of the formulations.
  • This microblade may be disposable or washed and reused.
  • a well volume of .5 to 3 cubic centimeters in volume is contemplated for use in the present invention.
  • the minimum quantity or volume of sample to be mixed in a "mother" wellplate will vary depending upon the desired coating thickness, domain size and formulation of the coating solution.
  • a “mother” well plate is defined as a source well plate.
  • a 25 micron thick coating that is 1 cm " in domain size with a coating solution that is 50% solids will require (1 cm " x 25 microns / 0.5) volume units or 0.0050 cc of solution.
  • Domain size refers to the minimum area required for the coated sample as determined by downstream testing. The appropriate volume of individual formulations from this mother well plate can then be dispensed to a sample or "daughter" well plate to make a coating with the desired domain size for subsequent analysis and data collection. It should be understood, that alternative embodiments include use of a single well plate as both the mother and daughter well plate.
  • the well plate into which the sample formulations are mixed will also serve as the well plate from which the coating materials will be tested. Again, considerations of desired coating thickness, domain size and formulation of coating solutions will be included in determination of minimum volume of well size required. Additional embodiments of well plate apparatus design will be discussed further below. Automated Dispensing of Candidate Coat Materials for Testing
  • a disposable metering device can be used to dispense the formulations from a mother well plate to a daughter well plate.
  • a robotic dispenser available commercially for example, from Hamilton Zinser Packard ( FIG. 2) ( FIG. 2) is one such device. Robotic dispensers allow for rapid and automated dispensing of a specified quantity of a large number of samples.
  • the well plate format to be used for the daughter well plate will also depend on the domain size requirement of the coating. For example, a 6-, 12-, 24-, 48-, 96-. or 384- well plate format are commercially available formats which can be used in the present invention with the commercially available robotic dispensers.
  • the robotic dispenser will have a platform area upon which the substrate well plates reside (FIG. 2; "A").
  • a robotic device can also be used for mixing as well as dispensing component materials for the sample coating formulation to be tested.
  • a robotic device can also be used for mixing as well as dispensing component materials for the sample coating formulation to be tested.
  • Such a device could have multiple dispensing units 30 from which specific and precise amount of an individual component is dispensed into a single well.
  • the sample solution can be dispensed using disposable pipette tips 30b attached to the pipettors 30c.
  • a separate dispensing unit for each component can be used to dispense the appropriate amount of a respective component into a single sample well.
  • Such a dispensing unit can be disposable which will allow rapid and accurate automation of the combinatorial method for formulating or synthesizing a new coating with elimination of holdup or contamination problems.
  • disposable dispensing units include, polyethylene or other type of tubing and disposable pipette tips.
  • FIG. 5 shows an example of a multi-well plate depicting the array format useful in the invention. Coating material samples are placed within the apertured. multi-well template top 47.
  • Such multi-well plates will form an array 41 or library format of the different formulations as discrete coated areas 40 on a planar substrate sheet 42.
  • a multi-well plate with a removable top or cover can also be used as a well plate assembly.
  • An example of such a multi- well plate design is shown in FIG. 7.
  • the well plate design can also include modifications to the well plate to prevent distribution of coating material onto the inner walls of the wells. For example, a release coating can be applied to the inner walls 43 of the wells to prevent any sample material from moving up and onto the well walls during application of a leveling force.
  • An additional embodiment of the present invention includes multi-well plates designed to obtain flat coatings in all of the wells of assembly.
  • Current commercially available multi-well plates have a flat-bottom surface for the entire plate. This results in an uneven distribution of sample material in the wells located along the perimeter of the multi-well plate 68 when current swing arm type of centrifuge rotors 70 are used to apply a leveling force.
  • FIG. 6 shows an example of a modified multi-well plate designed to obtain flat coatings in all of the wells.
  • Such a well plate will have a curved base plate 44 where the curvature of this base is parallel to the circumference of the centrifuge rotor, or is curved so as to substantially match the curvature of the curvilinear path of the well plate during centrifugation.
  • sample material or coating solutions in all of the wells, including perimeter wells 45 will be at the same distance from the spin axis of the centrifuge.
  • coating material in all of the wells will have a flat distribution following centrifugation.
  • the top view of such a multi-well plate can be as depicted in FIG. 5.
  • a flexible substrate and apertured well plate may be employed to provide a multi-well plate of curved configuration when mounted in a curved rotor of a centrifuge.
  • This flexible, apertured well plate may be constructed of materials that provide a tight , non-slip seal when placed upon the flexible, lower substrate. When such material is utilized for the top, well- forming portion of the well plate apparatus, no adhesive is necessary to secure this top to bottom portions of the well plate assembly.
  • the wells in which the coating samples are placed are leak- proof.
  • Such an apertured well plate can be made of silicone rubber; and pressure sensitive adhesive is not required to sealingly attach the silicone well plate to the lower substrate surface.
  • FIG. 8 shows cross sectional views of a representative laminate multi-well plate assemblies.
  • the assembly is made up of at least 4 layers and is shown in FIG.8.
  • the top or first layer 46 corresponds to the multi-well or sample holding portion of the assembly.
  • This layer need only be thick enough to provide a sufficient barrier between adjacent wells so that the dispensed coating material 50 does not cross contaminate adjacent samples. Where a very small amount of coating material 50 is to be tested, this layer need not be very thick and could be made of. for example, thin plastic, foam or paper with each well formed of holes placed in linear, multiple rows to form an array pattern.
  • the top layer will be .01 to 1 mm.
  • This top layer 46 can be coated with a Pressure Sensitive Adhesive (PSA) (not shown) to attach it to the substrate layer 48. This will also help to seal the wells so that cross-contamination of sample coating material from one well does not mix with its neighbors.
  • PSA Pressure Sensitive Adhesive
  • the second layer is the substrate layer 48 and can be formed of a variety of materials, such as plastic, polymeric resin or paper, so long as it will hold the sample coating material 50 in a flattened manner. The second layer will preferably be 1 to 100 microns, or 1 to 10 mm, or 1 to 5 cm in thickness.
  • the third layer is a Pressure Sensitive Adhesive layer (PSA) 52.
  • the PSA layer 52 can be 5 to 30 ⁇ m , or .005 to .03 mm. or .0005 to .003 cm in thickness depending upon the type of adhesive and degree of adhesion desired.
  • the fourth layer is a liner 54 coated with a release layer such as silicone, which can be removed or peeled away from the PSA layer 52 leaving the adhesive on the bottom of the substrate layer as the new bottom layer.
  • This type of multi-well plate design is suitable for example, where the stickiness or tackiness of a coating material is to be tested. In such a case, it is desirable to have an array library which will remain stationary or adhere to a support surface by the PSA layer 52 while each individual coating sample is tested. Use of the PSA 52 on the layer 48 will allow the array library to remain stationary and not lift up during testing.
  • the of multi-well plates described above with coating samples placed within their wells can be covered.
  • This covering may be comprised of different materials in order to vary the coating sample ' s exposure to the conditions within the centrifuge during centrifugation and curing. Samples may also be covered so that drying times may be varied, according to user preference.
  • Such coverings can include paper or other materials. For example, Whatman filter paper of varying thickness can be utilized to vary the drying or curing time of coating samples in the multi-well plates.
  • a leveling force as used herein, is defined as any force sufficient to cause a sample or coat material to distribute evenly and flatly onto a substrate. A leveling force will also remove any residual air bubbles present within the sample coat formulation.
  • a variety of leveling forces are contemplated for use in the present invention including, for example, use of centrifugal force, use of a vacuum or negative pressure force, use of an electrostatic force, or use of a magnetic force. In the case where magnetic leveling force is used, the test coat formulation will contain magnetic particles, powder, or a compound such as ferrite.
  • a leveling force need not be limited to single-coat assessments. Where the processing of a multi-layer construction of coat material is desired, a leveling force can be repeatedly applied following dispensing of individual layers of a coat to be tested. The final array obtained will be a planar sheet containing discrete areas in a grid format of multi-layer coat formulations.
  • FIG. 10b shows an example of a centrifuge that can be used for applying a leveling force to a multi-well plate.
  • Such swing arm-type centrifuges with multi-well plate holders (FIG. 11) are available commercially (for example, VWR Scientific, "MicroPlus GH 3.8 rotor centrifuge).
  • the rotor for use in such a centrifuge is designed so as to hold an even number of multi-well plate assemblies.
  • the multi-well plate assemblies 68 are loaded into the rotor 70 in an upright or horizontal position. During centrifugation. the plates are directed into a vertical position which then levels or flattens the sample formulations onto the substrate layer.
  • the assembly is placed in a swing-arm centrifuge and the coatings are spun at controlled speeds so as to form a flat coating within each well 64.
  • a 10-min. spin at 2000 rpm will be sufficient to evenly distribute the coat materials within each well.
  • FIG. 10a shows an example of a vertical "rotating drum” type centrifuge that has a horizontal axis of rotation, that can be used to apply a leveling force to a multi-well plate.
  • a flexible multi-well plate is mounted in the bottom potion of the inner surface of the "drum “ centrifuge.
  • the inside surface of the "rotating drum” subjects all of the samples in the multi-well plate to the same forces during spinning, since in this configuration, the samples are equidistant to the force vectors generated by centrifugation. Utilizing this method, differences in the physical shape and profiles of the samples in the well-plate during centrifugation are minimized. Additionally, centrifugation eliminates any meniscus in each well. If samples are cured during centrifugation, this method locks the spinning sample's non- meniscus containing profile, resulting in cured samples lacking a meniscus.
  • the coating samples may be subjected to curing during their centrifugation.
  • a centrifuge which has been modified to hold circulating hot air or other gas which will aid in the evaporation of carrier solvents in the coating formulations is also contemplated for use in the present invention and is diagrammed schematically in FIG. 9.
  • the hot air 66 circulating over the formulations during centrifugation aids in the curing of the coating by heat or evaporation of volatiles or solvents.
  • Curing the coat samples during their centrifugation may also be achieved by exposing the samples to ultraviolet (UV) radiation, filament heaters as well as other methods.
  • UV radiation ultraviolet
  • filament heaters as well as other methods.
  • a UV "crawler" 80 is mounted inside the drum portion 81 of the vertical centrifuge.
  • This device emits a UV beam as wide as the sample array mounted on the inner rotating cylinder wall of the vertical centrifuge.
  • the samples are intermittently exposed to the UV beam on each rotation while the "crawler" 81 is mounted at a position along the circumference of the centrifuge.
  • One is able to vary the position of the UV emitting portion of the "crawler” so as to change the distance between the emission source positions and the coating samples thereby changing the intensity of the UV radiation that the sample experience during centrifugation. This variation may be used to alter curing parameters.
  • more than one crawler may be mounted along the circumference of the centrifuge and emission may be switched on and off depending on the desired protocol. It is also contemplated, as shown in FIG 14a.
  • a mirror may be placed inside the "drum " 81 of the vertical centrifuge and the UV source 90 located externally with a reflector 92. If the mirror 85 is stationary, the samples 94 will be exposed to the reflected UV beam 96 intermittently during rotation, as described previously.
  • the mirror may also be configured as to rotate with the drum, to direct UV beams at a stationary location on the "drum " wall where samples would be placed and receive continuous UV exposure.
  • these mounting configurations may be adapted to mount other sources of radiation, such as microwave, infrared , filament heaters as well as others, either within the centrifuge or externally. This setup, combined with the fact that shape differences are minimized during centrifugation. provides a more uniform sample array for testing new coating formulas.
  • Centrifuges can also be modified so as to vary other additional parameters during the centrifugation and curing of coat samples.
  • the centrifuges can be manufactured so as to have a tight, sealable. and enclosed atmosphere wherein samples undergoing centrifugation and curing are exposed to various atmospheres or gases such as nitrogen, for example.
  • atmospheres or gases such as nitrogen, for example.
  • ambient pressure inside such an apparatus may also be varied according to user preference. Applied vacuums, in addition to their effects on sample curing, will also result in more efficient spinning of the centrifuge rotors.
  • devices used to provide alternative methods of applying a leveling force can also be modified so as to simultaneously cure the coat formulations.
  • an apparatus utilizing a vacuum or electrostatic force as the leveling force can be modified to circulate hot air and include alternate arrangements for curing
  • the above methods provide an array 40 of coating materials with each site in the grid array containing a coat material having a known parameter which differs from parameter values of the materials contained on the other sites (FIG 1 ; step 16). With this array, the plurality of coating materials can each be tested for performance of each coating. Because the parameter value of the coating contained at each site is known, the value of a parameter associated with a desired performance of a coating can be determined. All information obtained by this high throughput analysis screening a coat material library are then entered into a database. From this database identification of the most successful new coat materials and the parameters and descriptors used to produce them is achieved (FIG. 1, step 23). Such a database will also serve as a storage library to aid in the formulation of future parameters to characterize the coatings.
  • Example I This example demonstrates the use of a multi-well plate combined with a centrifugal leveling force for estimation of coat weight of a sample coat material formulation. This example is intended to be representative of one embodiment of the invention, and not intended as limiting the scope of the invention.
  • the emulsion polymer formulation used was S-2000.
  • S-2000 is a nondispersable emulsion acrylic polymer manufactured by Avery Dennison Corporation. Pasadena CA in accordance with U.S. Patent No. 5.221,706.
  • a 96-well plate obtained from Polytronics was used as a daughter well plate. The well plate remained flat during centrifugation. Each well contained an equivalent sample material formulation for determination of coat weight.
  • This example demonstrates the utility of using a multi-well plate combined with a leveling force for high-throughput analysis of specific parameters or characteristics of coat material formulations in an individualized manner.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Clinical Laboratory Science (AREA)
  • Hematology (AREA)
  • Biochemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Wood Science & Technology (AREA)
  • Food Science & Technology (AREA)
  • Plasma & Fusion (AREA)
  • Mechanical Engineering (AREA)
  • Medicinal Chemistry (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Coating Apparatus (AREA)
  • Investigating Or Analysing Biological Materials (AREA)
  • Automatic Analysis And Handling Materials Therefor (AREA)

Abstract

L'invention concerne un procédé de formation d'un nouveau revêtement présentant des caractéristiques de rendement souhaitées (12). Ce procédé consiste (a) à former (13) un réseau de cavités de revêtement (14), chaque cavité étant conçue pour recevoir une matière de revêtement présentant un paramètre connu, (b) à placer (16), au moyen d'un dispositif automatisé (17), une matière de revêtement présentant un paramètre connu dans chaque cavité (18) en faisant varier les valeurs de paramètre dans une pluralité de cavités, (c) à établir une corrélation entre la valeur de paramètre pour les revêtements déposés dans chacune des cavités et la position de la cavité dans ce réseau, (d) à appliquer (19) une force de nivellement de revêtement audit réseau de façon à niveler la matière dans les cavités au moyen d'une centrifugeuse (20), et éventuellement à effectuer un séchage, puis (e) à tester les revêtements dans le réseau afin d'analyser (21), à l'aide de détecteurs (5), la relation entre la position dans le réseau et le rendement par rapport à une propriété donnée, la valeur de paramètre pouvant être mise en corrélation (22) avec le rendement de propriété, et les résultats pouvant être entrés dans une base de données (23), d'où une sélection destinée à la production (24). Ce procédé de criblage permet d'augmenter sensiblement la fréquence des découvertes de nouvelles matières de revêtement.
EP00976736A 1999-10-29 2000-10-30 Procede et dispositif de test combinatoire ameliore pour formulations de matieres de revetement et procedes associes Withdrawn EP1242192A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US16234999P 1999-10-29 1999-10-29
US162349P 1999-10-29
PCT/US2000/029990 WO2001032320A1 (fr) 1999-10-29 2000-10-30 Procede et dispositif de test combinatoire ameliore pour formulations de matieres de revetement et procedes associes

Publications (1)

Publication Number Publication Date
EP1242192A1 true EP1242192A1 (fr) 2002-09-25

Family

ID=22585251

Family Applications (2)

Application Number Title Priority Date Filing Date
EP00976736A Withdrawn EP1242192A1 (fr) 1999-10-29 2000-10-30 Procede et dispositif de test combinatoire ameliore pour formulations de matieres de revetement et procedes associes
EP00974017A Withdrawn EP1234173A4 (fr) 1999-10-29 2000-10-30 Appareil destine a la production a haut rendement de reseaux de materiaux de revetement, et procedes analytiques utilisant ces reseaux

Family Applications After (1)

Application Number Title Priority Date Filing Date
EP00974017A Withdrawn EP1234173A4 (fr) 1999-10-29 2000-10-30 Appareil destine a la production a haut rendement de reseaux de materiaux de revetement, et procedes analytiques utilisant ces reseaux

Country Status (4)

Country Link
EP (2) EP1242192A1 (fr)
JP (1) JP2003513257A (fr)
AU (2) AU1245401A (fr)
WO (2) WO2001032320A1 (fr)

Families Citing this family (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7448258B2 (en) * 1999-10-29 2008-11-11 Avery Dennison Corporation High throughput screening for moisture barrier characteristics of materials
US20030134033A1 (en) * 1999-10-29 2003-07-17 Avery Dennison Corporation Combinatorial screening/testing apparatus and method
EP1243409A3 (fr) * 2000-05-01 2003-05-14 Agfa-Gevaert Procédé de revêtement combinatoire pour le développement de nouveaux matériaux
WO2002077772A2 (fr) * 2001-03-23 2002-10-03 Transform Pharmaceuticals, Inc. Procede et systeme servant a planifier, executer et evaluer un criblage a haut rendement de compositions chimiques a constituants multiples et de formes solides de composes
WO2003028878A1 (fr) * 2001-09-28 2003-04-10 Dynametrix Limited Procedes et moyens permettant de creer des arrangements
US6881363B2 (en) 2001-12-07 2005-04-19 Symyx Technologies, Inc. High throughput preparation and analysis of materials
DE10201075A1 (de) * 2002-01-14 2003-07-24 Basf Ag Verfahren und Vorrichtung zur Untersuchung des Weissanlaufens
DE10206620B4 (de) * 2002-02-15 2005-08-18 Henkel Kgaa Vorrichtung und Verfahren zum gleichzeitigen Testen der Einwirkung von Flüssigkeiten auf Flächengebilde sowie Verwendung der Vorrichtung
AU2003303302A1 (en) * 2002-05-30 2004-09-06 Symyx Technologies, Inc. Apparatus and methods for forming films on substrates
ES2199080B1 (es) * 2002-07-16 2005-02-16 Universidad Politecnica De Valencia Soporte rotatorio y aparato para la caracterizacion multiple espectroscopica de muestras de materiales solidos.
AT411334B (de) * 2002-07-17 2003-12-29 Hexal Pharma Gmbh Aufnahmevorrichtung für proben
EP1464723B1 (fr) * 2003-04-04 2018-02-21 Siemens Energy, Inc. Revêtement barrière thermique avec caractéristiques nanométriques
JP3978500B2 (ja) * 2005-02-18 2007-09-19 国立大学法人埼玉大学 多種微量試料の注入、移行方法
JP4706389B2 (ja) * 2005-08-23 2011-06-22 東亞合成株式会社 活性エネルギー線硬化型組成物の調合方法及び評価方法
US9952237B2 (en) 2011-01-28 2018-04-24 Quanterix Corporation Systems, devices, and methods for ultra-sensitive detection of molecules or particles
EP2929939A1 (fr) * 2014-04-07 2015-10-14 Yantai AusBio Laboratories Co., Ltd. Microplaque
JP2020150229A (ja) * 2019-03-15 2020-09-17 日亜化学工業株式会社 発光装置およびその製造方法

Family Cites Families (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3198657A (en) * 1964-09-17 1965-08-03 Ibm Process for spin coating objects
DE2259360C2 (de) * 1972-12-04 1982-06-09 Basf Ag, 6700 Ludwigshafen Verfahren zur Herstellung von dünnen Schichten auf Basis von Polyurethan-Elastomeren
FR2382709A1 (fr) * 1977-03-04 1978-09-29 Thomson Csf Famille de composes comportant un cycle thiirane, reticulables par irradiation photonique
NL7714570A (nl) * 1977-12-30 1979-07-03 Akzo Nv Werkwijze voor de vervaardiging van voorwerpen uit een polyestercompositie.
DE2902026C3 (de) * 1979-01-19 1981-10-29 Peters, J. Hinrich, Dr., 5064 Rösrath Biologisches Gefäß
US4789601A (en) * 1987-05-04 1988-12-06 Banes Albert J Biocompatible polyorganosiloxane composition for cell culture apparatus
EP0363504A1 (fr) * 1988-10-10 1990-04-18 Dräger Nederland B.V. Procédé pour réaliser une couche comprenant un hydrogel à base de polyvinyle et une substance à activité biochimique sur un substrat
JPH05253535A (ja) * 1992-03-12 1993-10-05 Nkk Corp 回転塗布方法
US6004617A (en) * 1994-10-18 1999-12-21 The Regents Of The University Of California Combinatorial synthesis of novel materials
US5985356A (en) * 1994-10-18 1999-11-16 The Regents Of The University Of California Combinatorial synthesis of novel materials
CA2260807C (fr) * 1996-07-18 2006-03-28 Basf Aktiengesellschaft Supports solides pour processus de mesure analytiques, procede permettant de les obtenir et utilisation

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO0132320A1 *

Also Published As

Publication number Publication date
WO2001032320A1 (fr) 2001-05-10
WO2001032320A9 (fr) 2002-08-15
WO2001033211A1 (fr) 2001-05-10
EP1234173A1 (fr) 2002-08-28
EP1234173A4 (fr) 2005-08-17
AU1245401A (en) 2001-05-14
AU1447101A (en) 2001-05-14
JP2003513257A (ja) 2003-04-08

Similar Documents

Publication Publication Date Title
WO2001032320A1 (fr) Procede et dispositif de test combinatoire ameliore pour formulations de matieres de revetement et procedes associes
US7448258B2 (en) High throughput screening for moisture barrier characteristics of materials
AU2001239760B2 (en) Array of individual arrays as substrate for bead-based simultaneous processing of samples and manufacturing method therefor
US8741630B2 (en) Methods of detecting targets on an array
US6485690B1 (en) Multiple fluid sample processor and system
US8628952B2 (en) Array kits and processing systems
JP4678516B2 (ja) 材料の分離、反応、および顕微鏡分析のための基板
US20040141887A1 (en) Apparatus and methods to process substrate surface features
JP2004510148A (ja) 生体分子アレイを処理するための方法および装置
AU2001239760A1 (en) Array of individual arrays as substrate for bead-based simultaneous processing of samples and manufacturing method therefor
US20120108461A1 (en) High-throughput slide processing apparatus
US7094607B1 (en) Apparatus for high-throughput production of coat material arrays, and analytical methods using such arrays
CN111521591B (zh) 用于微滴式数字pcr仪的计数校准装置、制备及使用方法

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 20020426

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AT BE CH CY DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE

AX Request for extension of the european patent

Free format text: AL;LT;LV;MK;RO;SI

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: THE APPLICATION IS DEEMED TO BE WITHDRAWN

18D Application deemed to be withdrawn

Effective date: 20031103