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1. WO2020113171 - METHODS FOR PRODUCING N-DOPED GRAPHENE FILMS

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We Claim:

1. A method for producing n-doped graphene films on a substrate wherein the method comprises:

(i) preparing a doped polymer solution comprising an alkali metal salt, a polymer and a solvent;

(ii) coating a surface of a substrate with the doped polymer solution to form a coated substrate; and

(iii) contacting a graphene layer with the coated substrate.

2. The method of claim 1, further comprising a heating step.

3. The method of claim 2, further comprising a cooling step.

4. The method of claim 1, wherein coating comprises spin coating, drop casting, blade coating or dip coating.

5. The method of claim 1, wherein the graphene layer is on a growth substrate.

6. The method of claim 1, in which the method further comprises release of the growth substrate from the graphene layer.

7. The method of claim 6, wherein the release of the growth substrate from the graphene layer comprises chemical etching, electrochemical delamination, a heating step followed by a cooling step, or a heating step followed by a cooling step followed by mechanical peeling.

8. The method of claim 1, wherein the polymer is selected from the group consisting of polyamides, polyimides, polychloroethylenes, polyurethanes, polyvinylethers, polythioureas, polyacrylates, polycarbonates, polyesters, polyethylenes,

polypropylenes, polysytrenes, PTFE, polyethylacetates, polyvinylacetates and fluoropolymers.

9. The method of claim 8, wherein the polymer is selected from the group consisting of poly(methyl methacrylate), polyvinylbutyral, ethylene-vinyl acetate, thermoplastic polyurethane, polyethylene terephthalate, thermoset ethylene-vinyl acetate, polycarbonate and polyethylene.

10. The method of claim 1, wherein the alkali-metal salt is selected from the group

consisting of MCIO4 or MI, wherein M is selected from the group consisting of Li, Na and K.

11. The method of claim 10, wherein the concentration of M is in the range about 2% to about 45% by weight (w/w).

12. The method of claim 1, wherein the substrate is selected from the group consisting of polyamides, polyimides, polychloroethylenes, polyurethanes, polyvinylethers, polythioureas, polyacrylates, polycarbonates, polyesters, polyethylenes,

polypropylenes, polysytrenes, nylons, polyethylacetates, polyvinylacetates and fluoropolymers.

13. The method of claim 12, wherein the substrate is selected from the group consisting of poly(methyl methacrylate), polycarbonate, polyethylene, polypropylene, polyester, nylon, and polyvinyl chloride.

14. The method of claim 1, wherein the solvent is selected from the group consisting of water, chlorobenzene, acetone, methanol, N-Methyl-2-pyrrolidone, tetrahydrofuran, dimethylformamide, hexane, toluene, isopropyl alcohol, acetonitrile, chloroform, acetic acid, 2-methoxyethanol, or n-butylamine.

15. The method of claim 5, wherein the growth substrate is a metal substrate.

16. The method of claim 15, wherein the metal substrate is selected from the group

consisting of copper, nickel, platinum, and iridium.

17. The method of claim 1, wherein the substrate comprises an alkali metal salt

incorporated within the substrate.

18. The method of claim 1, wherein the doped polymer solution comprises about 10

weight percent to about 50 weight percent poly(methyl methacrylate) and about 10 weight percent to about 50 weight percent NaClCL in a solvent, wherein the solvent is selected from the group consisting of chlorobenzene, N-Methyl-2-pyrrolidone, tetrahydrofuran, and dimethylformamide.

19. The method of claim 1, wherein the heating step is performed in the range of about 100 °C to about 160 °C, and the temperature is held for a time ranging from about 5 minutes to about 4 hours.

20. The method of claim 1, wherein the cooling step is performed in the range of

about -10 °C to about 20 °C, and the temperature is held for a time ranging from about 5 minutes to about 4 hours.

21. The method of claim 1, wherein the graphene layer is doped prior to contacting the graphene layer with the coated substrate.

22. A method for producing n-doped graphene films on a substrate wherein the method comprises:

(i) preparing a doped polymer solution comprising an alkali metal salt, a polymer and a solvent;

(ii) coating a graphene layer with the doped polymer solution to form a coated graphene layer

(iii) coating a surface of a substrate with the doped polymer solution to form a coated substrate; and

(iv) contacting the coated graphene layer with the coated substrate.

23. The method of claim 22, further comprising a heating step.

24. The method of claim 22, further comprising a cooling step.

25. The method of claim 22, further comprising a mechanical peeling step.

26. The method of claim 22, wherein coating comprises spin coating, drop casting, blade coating or dip coating.

27. The method of claim 22, wherein the graphene layer is on a growth substrate.

28. The method of claim 22, in which the method further comprises release of the growth substrate from the graphene.

29. The method of claim 28, wherein the release of the growth substrate from the graphene comprises chemical etching, electrochemical delamination, a heating step followed by a cooling step, or a heating step followed by a cooling step followed by a mechanical peeling step.

30. The method of claim 22, wherein the polymer is selected from the group consisting of polyamides, polyimides, polychloroethylenes, polyurethanes, polyvinylethers, polythioureas, polyacrylates, polycarbonates, polyesters, polyethylenes,

polypropylenes, polysytrenes, PTFE, polyethylacetates, polyvinylacetates and fluoropolymers.

31. The method of claim 30, wherein the polymer is selected from the group consisting of poly(methyl methacrylate), polyvinylbutyral, ethylene-vinyl acetate, thermoplastic polyurethane, polyethylene terephthalate, thermoset ethylene-vinyl acetate, polycarbonate and polyethylene.

32. The method of claim 22, the alkali-metal salt is selected from the group consisting of MCIO4 or MI, wherein M is selected from the group consisting of Li, Na and K.

33. The method of claim 32, wherein the concentration of M is in the range about 2% to about 45% by weight (w/w).

34. The method of claim 22, wherein the solvent is selected from the group consisting of water, chlorobenzene, acetone, methanol, N-Methyl-2-pyrrolidone, tetrahydrofuran, dimethylformamide, hexane, toluene, isopropyl alcohol, acetonitrile, chloroform, acetic acid, 2-methoxyethanol, or n-butylamine.

35. The method of claim 27, wherein the growth substrate is a metal substrate.

36. The method of claim 35, wherein the metal substrate is selected from the group

consisting of copper, nickel, platinum, and iridium.

37. The method of claim 22, wherein the doped polymer solution comprises about 10 weight percent to about 50 weight percent poly(methyl methacrylate) and about 10 weight percent to about 50 weight percent NaClCri in a solvent, wherein the solvent is selected from the group consisting of chlorobenzene, N-Methyl-2-pyrrolidone, tetrahydrofuran, and dimethylformamide.

38. The method of claim 23, wherein the heating step is performed in the range of about 100 °C to about 160 °C, and the temperature is held for a time ranging from about 5 minutes to about 4 hours.

39. The method of claim 24, wherein the cooling step is performed in the range of

about -10 °C to about 20 °C, and the temperature is held for a time ranging from about 5 minutes to about 4 hours.

40. The method of claim 22, wherein the graphene layer is doped prior to coating the graphene layer with the doped polymer solution to form the coated graphene layer.

41. A method for producing n-doped graphene films on a substrate wherein the method comprises:

(i) preparing a doped polymer solution comprising an alkali metal salt, a polymer and a solvent;

(ii) coating a graphene layer with the doped polymer solution to form a coated graphene layer; and

(iii) curing the doped polymer.

42. The method of claim 41, wherein the graphene layer is on a growth substrate.

43. The method of claim 42, in which the method further comprises release of the growth substrate from the graphene layer.

44. The method of claim 43, wherein the release of the growth substrate from the

graphene layer comprises chemical etching, electrochemical delamination, a heating step followed by a cooling step, or a heating step followed by a cooling step followed by a mechanical peeling step.

45. The method of claim 42, wherein the growth substrate is a metal substrate.

46. The method of claim 45, wherein the metal substrate is selected from the group

consisting of copper, nickel, platinum, and iridium.

47. The method of claim 41, wherein the polymer is selected from the group consisting of polyamides, polyimides, polychloroethylenes, polyurethanes, polyvinylethers,

polythioureas, polyacrylates, polycarbonates, polyesters, polyethylenes, polypropylenes, polysytrenes, PTFE, polyethylacetates, and polyvinylacetates.

48. The method of claim 47, wherein the polymer is selected from the group consisting of poly(methyl methacrylate), polyvinylbutyral, ethylene-vinyl acetate, thermoplastic polyurethane, polyethylene terephthalate, thermoset ethylene-vinyl acetate, polycarbonate and polyethylene.

49. The method of claim 41, wherein the alkali-metal salt is selected from the group

consisting of MCIO4 or MI, wherein M is selected from the group consisting of Li, Na and K.

50. The method of claim 49, wherein the concentration of M is in the range of about 2% to about 45% by weight (w/w).

51. The method of claim 41, wherein the solvent is selected from the group consisting of water, chlorobenzene, acetone, methanol, N-Methyl-2-pyrrolidone, tetrahydrofuran, dimethylformamide, hexane, toluene, isopropyl alcohol, acetonitrile, chloroform, acetic acid, 2-methoxyethanol, or n-butylamine.

52. The method of claim 41, wherein the doped polymer solution comprises about 10 weight percent to about 50 weight percent poly(methyl methacrylate) and about 10 weight percent to about 50 weight percent NaClCri in a solvent selected from chlorobenzene, N-Methyl-2-pyrrolidone, tetrahydrofuran, and dimethylformamide.

53. The method of claim 44, wherein the heating step is performed in the range of about 100 °C to about 160 °C, and the temperature is held for a time ranging from about 5 minutes to about 4 hours.

54. The method of claim 44, wherein the cooling step is performed in the range of

about -10 °C to about 20 °C, and the temperature is held for a time ranging from about 5 minutes to about 4 hours.

55. The method of claim 41, wherein the graphene layer is doped prior to coating the graphene layer with the doped polymer solution to form the coated graphene layer.

56. A composition comprising: (i) a substrate, (ii) a doped polymer, and (iii) graphene.

57. The composition of claim 56, wherein the doped polymer comprises an alkali metal salt and a polymer.

58. The composition of claim 56, wherein the polymer is selected from the group

consisting of polyamides, polyimides, polychloroethylenes, polyurethanes, polyvinyl ethers, polythioureas, polyacrylates, polycarbonates, polyesters,

polyethylenes, polypropylenes, polysytrenes, PTFE, polyethylacetates, and polyvinylacetates.

59. The composition of claim 59, wherein the polymer is selected from the group

consisting of poly(m ethyl methacrylate), polyvinylbutyral, ethylene-vinyl acetate, thermoplastic polyurethane, polyethylene terephthalate, thermoset ethylene-vinyl acetate, polycarbonate and polyethylene.

60. The composition of claim 56, wherein the substrate is selected from the group

consisting of poly(methylmethacrylate), polycarbonate, polyethylene, polypropylene, polyester, nylon, polyvinyl chloride.

61. The composition of claim 57, wherein the alkali-metal salt is selected from the group consisting of MClCri or MI, wherein M is selected from the group consisting of Li, Na and K.

62. The composition of claim 56, wherein the graphene is a doped graphene.

63. The composition of claim 56, wherein the electron mobility of the graphene is greater than 2000 cm2/Vs.

64. The composition of claim 56, wherein the charge carrier concentration of the

graphene is greater than 5xl012 electrons per cm2.

65. An electronic and/or optical device comprising the composition of claim 56.

66. The electronic device of claim 65, wherein the electronic device is a flexible

electronic device.

67. The electronic device of claim 65, wherein the electronic device is an electrically conductive window material.