Combinatorial synthesis and screening of non-biological polymers

• US 7,034,091 B2
• Filed: 02/11/2002
• Issued: 04/25/2006
• Est. Priority Date: 10/18/1994
• Status: Expired due to Fees

• Current Assignee: Intermolecular Incorporated
• Original Assignee: Symyx Technologies Incorporated (Dassault Systemes SA), Regents of the University of California (University of California)
• Inventors: Schultz, Peter G., Xiang, Xiao-Dong, Sun, Xiao-Dong, Briceno, Gabriel, Goldwasser, Isy, Wang, Kai-An
• Primary Examiner(s): Ponnaluri, Padmashri
• Assistant Examiner(s): SHIBUYA, MARK LANCE
• Application Number:
  US10/074,745
• Publication Number:
  US 20020119243A1
• Time in Patent Office: 1,534 Days
• Field of Search: 435/DIG.46, 435/DIG.49, 435/DIG.9, 435/DIG.10, 435/DIG.14, 435/19, 435/7.1, 435/7.2, 436/85, 436/149, 436/157, 436/170, 436/174, 436/501, 436/578, 427/8, 427/265, 427/266, 427/333, 427/488, 427/504, 427/510, 427/2.11, 430/5, 526/65, 526/66
• US Class Current: 526/65
• 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
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• CPC Class Codes: C04B 2235/3284 : Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
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• CPC Class Codes: C04B 2235/3296 : Lead oxides, plumbates or oxide forming salts thereof, e.g. silver plumbate
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• 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
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• 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: Y10T 428/24479 : including variation in thickness
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• CPC Class Codes: Y10T 436/25 : including sample preparation
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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 preparing an array of polymeric materials, the method comprising

preparing an array comprising first and second non-biological organic polymers on a substrate, the first and second non-biological organic polymers being copolymers or higher-ordered polymers, the first non-biological organic polymer being different from the second non-biological organic polymer, the array being prepared by a method that includes

delivering a first component and a second component of the first non-biological organic polymer to a first region of a substrate,

delivering a first component and a second component of the second non-biological organic polymer to a second region on the substrate,

polymerizing the delivered first and second components of the first non-biological organic polymer to form the first non-biological organic polymer at the first region of the substrate, and simultaneously

polymerizing the delivered first and second components of the second non-biological organic polymer to form the second non-biological organic polymer at the second region of the substrate.

2. The method of claim 1 wherein said non-biological organic polymers are selected from the group consisting of natural polymers, synthetic polymers, cross-linked polymers and non-cross-linked polymers.

3. The method of claim 1 wherein said non-biological organic polymers are selected from the group consisting of polyurethanes, polyesters, polycarbonates, polyethyleneimines, polyacetates, polystyrenes, polyamides, polyanilines, polyacetylenes and polypyrroles.

4. The method of claim 1 wherein said first component of said first material and said second component of said first material are simultaneously delivered to said first region on the substrate.

5. The method of claim 1 wherein said first component of said first material and said first component of said second material are simultaneously delivered to said first region and said second region on the substrate, respectively.

6. The method of claim 1 wherein said first component of said first material and said first component of said second material are the same, but are offered in different concentrations.

7. The method of claim 1 wherein said second component of said first material and said second component of said second material are the same, but are offered in different concentrations.

8. The method of claim 1 wherein the components of said materials are delivered to said first and second regions on said substrate from a dispenser.

9. The method of claim 8 wherein said dispenser is a pipette.

10. The method of claim 8 wherein said dispenser is selected from the group consisting of a pulse pressure ink-jet dispenser, a bubble jet ink-jet dispenser and a slit jet ink-jet dispenser.

11. The method of claim 1 wherein said steps of delivering said components each comprises the following steps:

(i) identifying a reference point on said substrate;

(ii) moving a dispenser of said component a fixed distance and direction from said reference point such that said dispenser is positioned approximately above said first region of said substrate;

(iii) delivering said component to said first region; and

(iv) repeating steps (ii) and (iii) for each remaining component for each remaining region.

12. The method of claim 1 wherein there is a sufficient amount of space between each of said regions on said single substrate such that said components cannot interdiffuse between said regions.

13. The method of claims 1 wherein at least 10 different materials are synthesized on said substrate.

14. The method of claims 1 wherein at least 100 different materials are synthesized on said substrate.

15. The method of claims 1 wherein at least 1000 different materials are synthesized on said substrate.

16. The method of claims 1 wherein at least 10⁶ different materials are synthesized on said substrate.

17. The method of claims 1 wherein at least 100 different materials are synthesized on said substrate, and each different material is contained within an area of about 1 cm² or less.

18. The method of claim 1, further comprising screening the first and second non-biological organic polymers for a property of interest selected from the group consisting of a thermal property, a mechanical property, a morphological property, a chemical property, an optical property, a magnetic property and an electrical property.

19. The method of claim 18 wherein said property of interest is an optical property.

20. The method of claim 19 wherein said optical property is measured using light scattering techniques.

21. The method of claim 18 wherein said property of interest is a chemical property.

22. The method of claim 18 wherein said array of materials is screened in parallel.

23. The method of claim 18 wherein said array of materials is screened sequentially.

24. The method of claim 18 wherein the array of non-biological organic polymers is screened for a thermal property.

25. The method of claim 18 wherein the array of non-biological organic polymers is screened for a mechanical property.

26. The method of claim 18 wherein the array of non-biological organic polymers is screened for a morphological property.

60. The method of claim 1, 27, 28, 29 or 37 wherein the substrate is a plate-type substrate.

61. The method of claim 1, 27, 28, 29 or 37 further comprising pressurizing with a gas during polymerization.

68. The method of claims 1, 29 or 37 further comprising mixing the delivered components at the first and second regions of the substrate during the polymerization reaction.

69. The method of claims 1, 29 or 37 further comprising heating the delivered components at the first and second regions of the substrate during the polymerization reaction.

70. The method of claims 1, 29 or 37 further comprising

mixing the delivered components at the first and second regions of the substrate simultaneously during the polymerization reaction, and

heating the delivered components at the first and second regions of the substrate simultaneously during the polymerization reaction.

71. The method of claims 1, 29 or 37 further comprising

pressurizing with a gas during polymerization, and

mixing the delivered components at the first and second regions of the substrate simultaneously during the polymerization reaction.

72. The method of claims 1, 29 or 37 further comprising

pressurizing with a gas during polymerization,

mixing the delivered components at the first and second regions of the substrate simultaneously during the polymerization reaction, and

heating the delivered components at the first and second regions of the substrate simultaneously during the polymerization reaction.

27. A method for evaluating polymeric materials, the method comprising

delivering monomers of non-biological organic polymers to ten or more regions of a substrate,

simultaneously polymerizing the delivered monomers to form ten or more different non-biological organic polymers on the substrate, the ten or more non-biological organic polymers being copolymers or higher-ordered polymers, and

screening the ten or more non-biological organic polymers for a property of interest selected from the group consisting of a thermal property, a mechanical property, a morphological property, a chemical property, an optical property, a magnetic property and an electrical property.

48. The method of claim 27, 28, 29, 37, 40, 42 or 44 wherein at least 100 different materials are synthesized on said substrate.

49. The method of claim 27, 28 or 40 wherein at least 1000 different materials are synthesized on said substrate.

50. The method of claim 27, 28 or 40 wherein at least 10⁶ different materials are synthesized on said substrate.

51. The method of claim 27, 28 or 40 wherein at least 100 different materials are synthesized on said substrate, and each different material is contained within an area of about 1 mm² or less.

52. The method of claim 27, 40, 42 or 44 wherein said property of interest is an optical property.

53. The method of claim 27, 40, 42 or 44 wherein said property of interest is a chemical property.

54. The method of claim 27, 40, 42 or 44 wherein said array of materials is screened in parallel.

55. The method of claim 27, 40, 42 or 44 wherein said array of materials is screened sequentially.

56. The method of claims 27, 40, 42 or 44 wherein the array of non-biological organic polymers is screened for a thermal property.

57. The method of claims 27, 40, 42 or 44 wherein the array of non-biological organic polymers is screened for a mechanical property.

58. The method of claims 27, 40, 42 or 44 wherein the array of non-biological organic polymers is screened for a morphological property.

59. The method of claim 27, 28, 29 or 37 wherein at least 100 different materials are synthesized on said substrate, and each different material is contained within an area of about 1 cm² or less.

28. A method for preparing an array of polymeric materials, the method comprising

delivering monomers of a first non-biological organic polymer to a first region on the substrate,

delivering monomers of a second non-biological organic polymer to a second region on the substrate,

polymerizing the delivered monomers of the first non-biological organic polymer, such that the monomers react, without linear, stepwise coupling thereof, to form the first non-biological organic polymer, and simultaneously,

polymerizing the delivered monomers of the second non-biological organic polymer, such that the monomers react, without linear, stepwise coupling thereof, to form the second non-biological organic polymer,

the first and second non-biological organic polymers being copolymers or higher-ordered polymers, the second non-biological organic polymer being different from the first non-biological organic polymer.

40. The method of claim 28, further comprising

screening the first and second non-biological organic polymers for a property of interest selected from the group consisting of a thermal property, a mechanical property, a morphological property, a chemical property, an optical property, a magnetic property and an electrical property.

41. The method of claim 40 wherein the first and second regions of the substrate are defined by dimples, wells or vessels, and the first and second non-biological organic polymers are screened in parallel for a property selected from the group consisting of a thermal property, a mechanical property, and a chemical property.

47. The method of claim 28, 29, 40 or 42 wherein at least 10 different materials are synthesized on said substrate.

29. A method for preparing an array of polymeric materials, the method comprising

delivering one or more monomers of a first non-biological organic polymer to a first region on the substrate,

delivering one or more monomers of a second non-biological organic polymer to a second region on the substrate,

polymerizing the delivered monomers of the first non-biological organic polymer, to form the first non-biological organic polymer,

polymerizing the delivered monomers of the second non-biological organic polymer to form the second non-biological organic polymer, and

independently controlling the polymerization reaction conditions at the first region and the second region of the substrate.

30. The method of claim 29 wherein the first and second non-biological organic polymers are homopolymers.

31. The method of claim 29 wherein the first and second non-biological organic polymers are copolymers or higher-ordered polymers.

32. The method of claim 29 wherein the delivered monomers of each of the first and second non-biological organic polymers are simultaneously polymerized.

33. The method of claim 29 wherein the temperatures at the first region and the second region of the substrate are independently controlled.

34. The method of claim 29 wherein the reaction times at the first region and the second region of the substrate are independently controlled.

35. The method of claim 29 wherein the reaction solvents at the first region and the second region of the substrate are independently controlled.

36. The method of claim 29 wherein the reaction conditions are controllably varied between the first region and the second region of the substrate.

42. The method of claim 29, further comprising:

screening the first and second non-biological organic polymers for a property of interest selected from the group consisting of a thermal property, a mechanical property, a morphological property, a chemical property, an optical property, a magnetic property and an electrical property.

43. The method of claim 42 wherein the first and second regions of the substrate are defined by dimples, wells or vessels, and the first and second non-biological organic polymers are screened in parallel for a property selected from the group consisting of a thermal property, a mechanical property, and a chemical property.

37. A method for preparing an array of polymeric materials, the method comprising

forming ten or more different non-biological organic polymers on a substrate, each of the ten or more non-biological organic polymers being copolymers or higher-ordered polymers comprising a first component and a second component, the first component being the same between the ten or more non-biological organic polymers, the polymers being formed by a method that includes

delivering the first component of the ten or more non-biological organic polymers in a gradient of stoichiometries to ten or more regions of the substrate,

delivering the second component of the ten or more non-biological organic polymers to the ten or more regions of the substrate, and

polymerizing the delivered first and second components of the ten or more non-biological organic polymers to form the ten or more non-biological organic polymers.

38. The method of claim 37 wherein the second component is the same between the ten or more non-biological organic polymers.

39. The method of claim 37 wherein the second component is the same between the ten or more non-biological organic polymers, and the second component is delivered in a gradient of stoichiometries to the ten or more regions of the substrate.

44. The method of claim 37, further comprising:

screening the ten or more non-biological organic polymers for a property of interest selected from the group consisting of a thermal property, a mechanical property, a morphological property, a chemical property, an optical property, a magnetic property and an electrical property.

45. The method of claim 44 wherein the ten or more regions of the substrate are defined by dimples, wells or vessels, and the ten or more non-biological organic polymers are screened in parallel for a property selected from the group consisting of a thermal property, a mechanical property and a chemical property.

46. The method of claim 37 or 44 wherein said delivered components are simultaneously polymerized.

62. A method for evaluating polymeric materials, the method comprising

delivering one or more monomers of non-biological organic polymers to two or more regions of a substrate, the two or more regions of the substrate being defined by dimples, wells or vessels,

simultaneously polymerizing the delivered monomers such that the monomers react, without linear, stepwise coupling thereof, to form two or more different non-biological organic polymers on the substrate,

controllably varying the reaction conditions between the two or more regions of the substrate during polymerization,

pressurizing with a gas during polymerization, and

screening the two or more non-biological organic polymers for a property of interest selected from the group consisting of a thermal property, a mechanical property and a chemical property.

63. The method of claim 62 wherein the substrate is a plate-type substrate having ten or more regions, each region having an area of about 1 cm², and at least ten different non-biological polymers are formed on the substrate.

64. The method of claim 62 wherein the reactant components are pressurized under an inert atmosphere during polymerization.

65. A method of evaluating an array of polycarbonate polymer materials, the method comprising

preparing an array comprising ten or more polycarbonate polymers on a substrate, the ten or more polycarbonate polymers being different from each other, the array being prepared by a method that includes

simultaneously delivering a first component and a second component of a first polycarbonate polymer to a first region of the substrate, simultaneously delivering a first component and a second component of a second polycarbonate polymer to a second region of the substrate, simultaneously delivering a first component and a second component of a third polycarbonate polymer to a third region of the substrate, simultaneously delivering a first component and a second component of a fourth polycarbonate polymer to a fourth region of the substrate, simultaneously delivering a first component and a second component of a fifth polycarbonate polymer to a fifth region of the substrate, simultaneously delivering a first component and a second component of a sixth polycarbonate polymer to a sixth region of the substrate, simultaneously delivering a first component and a second component of a seventh polycarbonate polymer to a seventh region of the substrate, simultaneously delivering a first component and a second component of an eight polycarbonate polymer to an eighth region of the substrate, simultaneously delivering a first component and a second component of a ninth polycarbonate polymer to a ninth region of the substrate, simultaneously delivering a first component and a second component of a tenth polycarbonate polymer to a tenth region of the substrate,

simultaneously polymerizing the delivered first and second components of each of the ten or more polycarbonate polymers to form the ten or more polycarbonate polymers at the ten or more regions of the substrate, respectively,

controlling the polymerization reaction conditions independently for each of the ten or more regions, and

screening the polymers in parallel for a chemical property.

66. The method of claim 65 wherein the first and second polycarbonate polymers are screened for one or more of the properties selected from the group consisting of a thermal property, a mechanical property, a morphological property, an optical property and a chemical property.

67. The method of claim 65 wherein the first and second polycarbonate polymers are screened for one or more of the properties selected from the group consisting of a thermal property, a mechanical property and a chemical property.