Screening combinatorial arrays of inorganic materials with spectroscopy or microscopy

• US 6,686,205 B1
• Filed: 11/28/2000
• Issued: 02/03/2004
• Est. Priority Date: 10/18/1994
• Status: Expired due to Term

• Current Assignee: Intermolecular Incorporated
• Original Assignee: Symyx Technologies Incorporated (Dassault Systemes SA), Lawrence Berkeley National Laboratory (University of California)
• Inventors: Schultz, Peter G., Xiang, Xiaodong, Goldwasser, Isy
• Primary Examiner(s): Soderquist, Arlen
• Application Number:
  US09/728,202
• Time in Patent Office: 1,162 Days
• Field of Search: 436/37, 436/73, 436/164, 436/172, 436/183
• US Class Current: 506/12
• CPC Class Codes: B01J 19/0046 Sequential or parallel reactions, e.g. for the synthesis of polypeptides or polynucleotides; Apparatus and devices for combinatorial chemistry or for making molecular arrays synthesis methods per se C40B50/00
• CPC Class Codes: B01J 2219/00313 the reactor vessels being formed by arrays of wells in blocks
• CPC Class Codes: B01J 2219/00317 Microwell devices, i.e. having large numbers of wells
• CPC Class Codes: B01J 2219/00378 Piezoelectric or ink jet dispensers
• CPC Class Codes: B01J 2219/0043 for direct application of reagents, e.g. through openings in a shutter
• CPC Class Codes: B01J 2219/00432 Photolithographic masks
• CPC Class Codes: B01J 2219/00436 Maskless processes
• CPC Class Codes: B01J 2219/00441 using lasers
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• CPC Class Codes: B01J 2219/0054 Means for coding or tagging the apparatus or the reagents
• CPC Class Codes: B01J 2219/00585 Parallel processes
• CPC Class Codes: B01J 2219/0059 : Sequential processes
• CPC Class Codes: B01J 2219/00592 : Split-and-pool, mix-and-divide processes
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• CPC Class Codes: B01J 2219/00605 : the compounds being directly bound or immobilised to solid supports
• CPC Class Codes: B01J 2219/0061 : The surface being organic
• CPC Class Codes: B01J 2219/00612 : the surface being inorganic
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• CPC Class Codes: B01J 2219/00621 : by physical means, e.g. trenches, raised areas
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• CPC Class Codes: B01J 2219/00648 : by the use of solid beads
• CPC Class Codes: B01J 2219/00659 : Two-dimensional arrays
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• CPC Class Codes: B82Y 30/00 : Nanotechnology for materials or surface science, e.g. nanocomposites
• CPC Class Codes: C01G 51/006 : Compounds containing, besides cobalt, two or more other elements, with the exception of oxygen or hydrogen cobaltates C01G51/40
• CPC Class Codes: C01G 51/68 : containing rare earth, e.g. La0.3Sr0.7CoO3
• CPC Class Codes: C01P 2002/34 : perovskite-type (ABO3)
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• CPC Class Codes: C04B 2235/327 : Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
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• CPC Class Codes: C04B 2235/3284 : Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
• CPC Class Codes: C04B 2235/3286 : Gallium oxides, gallates, indium oxides, indates, thallium oxides, thallates or oxide forming salts thereof, e.g. zinc gallate
• CPC Class Codes: C04B 2235/3296 : Lead oxides, plumbates or oxide forming salts thereof, e.g. silver plumbate
• CPC Class Codes: C04B 2235/3298 : Bismuth oxides, bismuthates or oxide forming salts thereof, e.g. zinc bismuthate
• CPC Class Codes: C04B 2235/3418 : Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint glass constituents C04B2235/36
• CPC Class Codes: C04B 2235/3463 : Alumino-silicates other than clay, e.g. mullite
• CPC Class Codes: C04B 2235/656 : characterised by specific heating conditions during heat treatment
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• CPC Class Codes: C04B 2235/762 : Cubic symmetry, e.g. beta-SiC
• CPC Class Codes: C04B 2235/768 : Perovskite structure ABO3
• CPC Class Codes: C04B 2235/96 : Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
• CPC Class Codes: C04B 35/01 : based on oxide ceramics
• CPC Class Codes: C04B 35/16 : based on silicates other than clay zircon C04B35/48
• CPC Class Codes: C04B 35/4508 : Type 1-2-3
• CPC Class Codes: C04B 35/4521 : containing bismuth oxide
• CPC Class Codes: C04B 35/4525 : also containing lead oxide
• CPC Class Codes: C04B 35/62218 : obtaining ceramic films, e.g. by using temporary supports
• CPC Class Codes: C23C 14/042 : using masks
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• CPC Class Codes: C23C 16/042 : using masks
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• CPC Class Codes: C40B 40/14 : Libraries containing macromolecular compounds and not covered by groups C40B40/06 - C40B40/12
• CPC Class Codes: C40B 40/18 : Libraries containing only inorganic compounds or inorganic materials
• CPC Class Codes: C40B 60/08 : Integrated apparatus specially adapted for both creating and screening libraries
• CPC Class Codes: C40B 60/14 : for creating libraries
• CPC Class Codes: C40B 70/00 : Tags or labels specially adapted for combinatorial chemistry or libraries, e.g. fluorescent tags or bar codes
• CPC Class Codes: C40B 80/00 : Linkers or spacers specially adapted for combinatorial chemistry or libraries, e.g. traceless linkers or safety-catch linkers
• CPC Class Codes: G01R 33/16 : Measuring susceptibility G01R33/1238 takes precedence
• CPC Class Codes: H01F 1/401 : diluted
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• CPC Class Codes: H01F 10/007 : ultrathin or granular films H01F10/005 and H01F10/3227 take precedence; applying ultrathin or granular layers to substrates H01F41/301
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• CPC Class Codes: H01F 41/18 : by cathode sputtering
• CPC Class Codes: H01F 41/34 : in patterns, e.g. by lithography
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• CPC Class Codes: Y10T 428/24479 : including variation in thickness
• CPC Class Codes: Y10T 428/24612 : Composite web or sheet
• CPC Class Codes: Y10T 428/2462 : with partial filling of valleys on outer surface
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• CPC Class Codes: Y10T 436/25 : including sample preparation
• CPC Class Codes: Y10T 436/2525 : Stabilizing or preserving
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• CPC Class Codes: Y10T 436/25875 : Gaseous sample or with change of physical state

Abstract

Methods and apparatus for the preparation and use of a substrate having an array of diverse materials in predefined regions thereon. A substrate having an array of diverse materials thereon is generally prepared by delivering components of materials to predefined regions on a substrate, and simultaneously reacting the components to form at least two materials. Materials which can be prepared using the methods and apparatus of the present invention include, for example, covalent network solids, ionic solids and molecular solids. More particularly, materials which can be prepared using the methods and apparatus of the present invention include, for example, inorganic materials, intermetallic materials, metal alloys, ceramic materials, organic materials, organometallic materials, non-biological organic polymers, composite materials (e.g., inorganic composites, organic composites, or combinations thereof), etc. Once prepared, these materials can be screened for useful properties including, for example, electrical, thermal, mechanical, morphological, optical, magnetic, chemical, or other properties. Thus, the present invention provides methods for the parallel synthesis and analysis of novel materials having useful properties.

Claims

1. A method for evaluating an array of materials, the method comprising

providing an array of materials comprising at least ten different inorganic materials at discrete regions of a substrate, the array consisting essentially of the substrate and the materials, each of the at least ten materials comprising first and second components, with a gradient of stoichiometries as compared between the at least ten material-containing regions of the substrate, the regions being isolated, such that the materials or components thereof cannot interdiffuse between adjacent regions after being formed or deposited on the substrate;

and

screening the array of materials for a useful property of interest by using spectroscopy or microscopy to generate data, and analyzing the generated data to evaluate the materials.

2. The method of claim 1 further comprising determining the relative performance of the at least ten different inorganic materials with respect to the screened property.

3. The method of claim 1, wherein the materials are screened using infrared spectroscopy.

5. The method of claim 1 or 4 wherein the entire array is screened in parallel.

7. The method of claim 1 or 4 wherein the array of materials is screened in parallel.

8. The method of claim 1 or 4 wherein the array of materials is screened sequentially.

9. The method of claim 1 or 4 wherein the array of materials comprises at least one hundred different inorganic materials.

10. The method of claim 1 or 4 wherein the array of materials comprises at least one thousand different inorganic materials.

11. The method of claim 1 or 4 wherein the array of materials comprises at least ten thousand different inorganic materials.

12. The method of claim 1 or 4 wherein a section of the array is screened in parallel.

13. The method of claim 1 or 4 wherein the material-containing regions have an area of less than about 10 cm².

14. The method of claim 1 or 4, wherein the inorganic materials are selected from the group consisting of intermetallics, metal alloys, magnetic alloys, and ceramics.

15. The method of claim 1 or 4, wherein the inorganic materials are selected from the group consisting of oxides and sulphides of carbon and metallic carbides.

22. The method of claims 1 or 21, wherein the data is analyzed using a computer.

27. The method of claims 1, 4, 17, 18, 21, 23 or 25 wherein each of the at least ten inorganic materials comprise three or more components.

28. The method of claim 27, wherein the at least ten different inorganic materials are provided in a gradient of stoichiometries of three of the components.

4. A method for evaluating an array of materials, the method comprising

providing an array of materials comprising at least ten different inorganic materials at discrete regions of a substrate, the array consisting essentially of the substrate and the materials, the regions being isolated such that the materials or components thereof cannot interdiffuse between adjacent regions after being formed or deposited on the substrate;

and

screening the array of materials using infrared spectroscopy.

6. The method of claim 4, wherein the method comprises screening the array of materials using infrared spectroscopy to generate data, and analyzing the generated data, and wherein the data is analyzed using a computer.

16. A method for evaluating an array of materials, the method comprising

providing an array of materials comprising at least ten different inorganic materials at discrete regions of a substrate, each of the at least ten materials comprising first and second components, with a gradient of stoichiometries as compared between the at least ten material-containing regions of the substrate, the regions being isolated, such that the materials or components thereof cannot interdiffuse between adjacent regions after being formed or deposited on the substrate;

and

screening the array of materials for a useful property of interest by using spectroscopy or microscopy to generate data, and analyzing the generated data to evaluate the materials, wherein the materials are screened using Raman spectroscopy.

17. A method for evaluating an array of materials, the method comprising

providing an array of materials comprising at least ten different inorganic materials at discrete regions of a substrate, the regions being isolated such that the materials or components thereof cannot interdiffuse between adjacent regions after being formed or deposited on the substrate,

screening the array of materials for a useful property using infrared spectroscopy, and

correlating the screened property with the stoichiometry of the material,

wherein the array of materials is formed in a first synthesis cycle on the substrate, and wherein analytical results are fed back to a delivery system to permit selection of the stoichiometry of one or more materials in a next synthesis cycle on a second substrate to form a second array of materials.

20. The method of claim 19 or 17, wherein a computer is used to correlate the screened property with the stoichiometry of the material.

18. A method for evaluating an array of materials, the method comprising

providing an ray of materials comprising at least ten different inorganic materials at discrete regions of a substrate, each of the at least ten materials comprising first and second components, with a gradient of stoichiometries as compared between the at least ten material-containing regions of the substrate, the regions being isolated, such that the materials or components thereof cannot interdiffuse between adjacent regions after being formed or deposited on the substrate, and

screening the array of materials for a useful property of interest by using spectroscopy or microscopy to generate data, and analyzing the generated data to evaluate the materials,

wherein the array of materials is formed in a first synthesis cycle on the substrate, and wherein analytical results are fed back to a delivery system to permit selection of the stoichiometry of one or more materials in a next synthesis cycle on a second substrate to form a second array of materials.

19. The method of claim 18, further comprising correlating the screened property with the stoichiometry of the material.

21. A method for evaluating an array of materials, the method comprising:

providing an array of materials comprising at least ten different inorganic materials at discrete regions of a substrate, the array consisting essentially of the substrate and the materials, the regions being isolated such that the materials or components thereof cannot interdiffuse between adjacent regions after being formed or deposited on the substrate; and

screening the array of materials in parallel for a useful property of interest by using spectroscopy or microscopy to generate data, and analyzing the generated data.

23. A method for evaluating an array of materials, the method comprising:

providing an array of materials comprising at least ten different inorganic materials at discrete regions of a substrate, the regions being isolated such that the materials or components thereof cannot interdiffuse between adjacent regions after being formed or deposited on the substrate; and

screening the array of materials in parallel for a useful property of interest by using spectroscopy or microscopy to generate data, and analyzing the generated data,

wherein the array of materials is formed in a first synthesis cycle on the substrate, and the analytical results generated in the screening step are fed back to a delivery system to form a second array of materials comprising one or more materials determined from screening the first array.

24. The method of claim 23, wherein the data is analyzed using a computer.

25. A method for evaluating an array of materials, the method comprising

providing array of materials comprising at least ten different inorganic materials at discrete regions of a substrate, the regions being isolated such that the materials or components thereof cannot interdiffuse between adjacent regions after being formed or deposited on the substrate, and

screening the array of materials using infrared spectroscopy to generate data, and analyzing the generated data,

wherein the array of materials is formed in a fit synthesis cycle on the substrate, and the analytical results generated in the screening step are fed back to a delivery system to form a second array of materials comprising one or more materials determined from screening the first array.

26. The method of claim 25, wherein the data is analyzed using a computer.