IPC분류정보
국가/구분 |
United States(US) Patent
등록
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국제특허분류(IPC7판) |
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출원번호 |
US-0118519
(2002-04-06)
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발명자
/ 주소 |
- Matyjaszewski,Krzysztof
- Kowalewski,Tomasz
- Lambeth,David N.
- Spanswick,James
- Tsarevsky,Nicolay V.
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출원인 / 주소 |
- Carnegie Mellon University
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대리인 / 주소 |
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인용정보 |
피인용 횟수 :
146 인용 특허 :
37 |
초록
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The present invention comprises a novel process for the preparation of carbon based structured materials with controlled topology, morphology and functionality. The nanostructured materials are prepared by controlled carbonization, or pyrolysis, of precursors comprising phase separated copolymers. T
The present invention comprises a novel process for the preparation of carbon based structured materials with controlled topology, morphology and functionality. The nanostructured materials are prepared by controlled carbonization, or pyrolysis, of precursors comprising phase separated copolymers. The precursor materials are selected to phase separate and self organize in bulk, in solution, in the presence of phase selective solvents, at surfaces, interfaces or during fabrication, into articles, fibers or films exhibiting well-defined, self-organized morphology or precursors of well-defined, self-organized, bi-or tri-phasic morphology. Compositional control over the (co)polymers provides control over the structure of the phase separated precursor whose organization therein dictates the nanostructure of the material obtained after carbonization or pyrolysis, wherein each dimension of the formed structure can be predetermined. When the precursor morphology is selected to comprise cylindrical domains this procedure additionally allows for the direct formation of two dimensional nanowire grids or arrays of oriented nanostructures on surfaces. When these nanowire grids or arrays are perpendicularly oriented to the surface applications include field emitters, high surface area electrodes, electronic devices such as diodes and transistors, tools for AMF tips and elements of molecular electronics. When the first nanostructured morphology is selected to form cylinders parallel to the surface then nanowire arrays are formed after pyrolysis. When the composition of the first nanostructured morphology is selected to comprise a continuous precursor matrix then a continuous carbon based nanostructured material is formed. The internal structure of the carbon based material can be selected to comprise perpendicular pores or an interconnected array of pores. The carbon based structures can additionally find application in photovoltaics, supercapacitors, batteries, fuel cells, computer memory, carbon electrodes, carbon foams, actuators and hydrogen storage.
대표청구항
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We claim: 1. A process for the preparation of nanostructured materials, comprising: pyrolyzing a precursor, wherein the precursor comprises a self assembled phase-separated block copolymer to form a plurality of carbon nanostructures, wherein the carbon nanostructures are at least one of discrete c
We claim: 1. A process for the preparation of nanostructured materials, comprising: pyrolyzing a precursor, wherein the precursor comprises a self assembled phase-separated block copolymer to form a plurality of carbon nanostructures, wherein the carbon nanostructures are at least one of discrete carbon nanofibers, carbon nanotubes, and carbon nanocylinders, and wherein the block copolymer comprises: at least one carbon precursor block; and at least one sacrificial block, wherein the phase-separated copolymer separates on a molecular scale into at least one precursor phase and at least one sacrificial phase due to the immiscibility of the precursor and sacrificial blocks. 2. The process for the preparation of nanostructured materials of claim 1, wherein pyrolyzing the precursor comprises carbonizing the precursor material and pyrolyzing the sacrificial material. 3. The process for preparation of nanostructured materials of claim 1, wherein the precursor block comprises monomeric units derived from acrylonitrile based monomers. 4. The process for the preparation of nanostructured materials of claim 3, wherein the precursor comprises at least one phase of primarily precursor material and at least on phase of primarily sacrificial material. 5. The process for the preparation of nanostructured materials of claim 4, wherein pyrolyzing the precursor comprises heating the precursor to a temperature between 1000째 F. and 1400째 F. 6. The process for the preparation of nanostructured materials of claim 5, wherein heating the precursor is conducted in the absence of oxygen. 7. The process for preparation of nanostructured materials of claims 3, wherein the sacrificial material comprises monomeric units derived from butyl acrylate monomers. 8. The process for the preparation of nanostructured materials of claim 1, further comprising: preparing a film comprising the precursor; and heating the film. 9. The process for the preparation of nanostructured materials of claim 1, further comprising: providing conditions for phase separating a copolymer. 10. The process for the preparation of nanostructured materials of claim 9, wherein the conditions for phase separating a polymer comprise at least one of phase separating the polymer in bulk, in solution, in the presence of a phase selective solvent, at an interface, on a surface, in the polymerization medium, under vacuum, at pressures above atmospheric pressure, in the absence of oxygen and by annealing. 11. The process for the preparation of nanostructured materials of claim 1, wherein the copolymer forms a phase separated morphology. 12. The process for the preparation of nanostructured materials of claim 11, wherein the phase separated morphology is well defined. 13. The process for the preparation on nanostructured material of claim 12, wherein one phase of the phase separated morphology comprises nanostructured domains. 14. The process for the preparation of nanostructured materials of claim 11, wherein the phase separate morphology comprises at least two phases. 15. The process for the preparation of nanostructured materials of claim 14, wherein at least one of the phases comprises cylindrical domains. 16. The process for the preparation of nanostructured materials of claim 14, further comprising: annealing the precursor in the absence of oxygen. 17. The process for the preparation of nanostructured materials of claim 16, wherein the annealing the precursor reduces the surface energy of the phase separated morphology. 18. The process for the preparation of nanostructured materials of claim 14, further comprising: doping at least one phase of the phase separated morphology. 19. The process for the preparation of nanostructured materials of claim 18, wherein the precursor comprises a stabilized mixture of copolymers and homopolymers. 20. The process for the preparation of nanostructured materials of claim 18, wherein the doping at least one phase of the phase separated morphology comprises doping with at least one material comprising at least one of Si, S, P, B, and a transition metal. 21. The process for the preparation of nanostructured material of claim 14, wherein at least one phase comprises a precursor for a catalyst. 22. The process for the preparation of nanostructured material of claim 21, wherein the precursor for a catalyst is different than the precursor for the nanostructured material. 23. The process for the preparation of nanostructured materials of claim 14, wherein one phase comprises at least one N atom and another phase comprises at least one B atom. 24. The process for the preparation of nanostructured materials of claim 11, wherein the phase separate morphology comprises at least one continuous phase. 25. The process for the preparation of nanostructured materials of claim 11, wherein the phase separate morphology comprises at least two continuous phases. 26. The process for the preparation of nanostructured materials of claim 11, wherein the phase separate morphology comprises three phases. 27. The process for the preparation of nanostructured materials of claim 26, wherein the phase separate morphology comprises at least one continuous phase. 28. The process for the preparation of nanostructured materials of claim 27, wherein the phase separate morphology comprises at least two continuous phases. 29. The process for the preparation of nanostructured materials of claim 11, further comprising stabilizing the phase separated morphology by heating in the presence of oxygen. 30. The process for the preparation of nanostructured materials of claim 1, wherein the phase separated copolymer comprises at least one copolymer selected from the group comprising an AB block copolymers, an ABA block copolymer, an ABC block copolymer, multiblock copolymers, a graft copolymer, symmetrical and asymetrical star copolymers, a multiarm block copolymer, (hyper)branched copolymers, brush copolymers, and a blend of polymers. 31. The process for the preparation of nanostructured materials of claim 30, wherein the phase separated copolymer comprises acrylonitrile monomer units in at least one polymer segments. 32. The process for the preparation of nanostructured materials of claim 30, wherein the phase separated copolymer comprises a gradient acrylonitrile copolymer segment. 33. The process for the preparation of nanostructured materials of claim 1, further comprising: annealing the phase separated copolymer material; and stabilizing the phase separated copolymer material. 34. The process for the preparation of nanostructured materials of claim 33, wherein the stabilizing the phase separated copolymer is performed by heating the phase separated copolymer in the presence of oxygen. 35. The process for the preparation of nanostructured materials of claim 1, wherein the phase separated copolymer comprises free radically (co)polymerizable monomers. 36. The process for the preparation of nanostructured materials of claim 35, wherein the free radically copolymerizable monomers comprise a functional group. 37. The process for the preparation of nanostructured materials of claim 36, wherein the functional group comprises a transition metal. 38. The process for the preparation of nanostructured materials of claim 35, wherein the free radically (co)polymerizable monomers comprise at least one of styrenes, (meth)acrylates and (meth) acrylonitrile. 39. The process for the preparation of nanostructured materials of claim 1, wherein the properties of the nanostructured material are affected by the molecular weight of the blocks of the phase separated copolymer material and the conditions of the carbonizing. 40. The process for the preparation of nanostructured materials of claim 1, wherein the nanostructured material comprises a two-dimensional array of carbon nanostructures. 41. The process for the preparation of nanostructured materials of claim 1, further comprising: coating a surface with a film of a precursor comprising a phase separable copolymer. 42. The process for the preparation on nanostructured material of claim 41, wherein the nanostructured material is formed on the surface; and further comprising: removing the nanostructured material from the surface. 43. The process for the preparation of nanostructured materials of claim 41, further comprising: forming a two dimensional array of carbon nanostructures on the surface. 44. The process for the preparation of nanostructured material of claim 43, further comprising: forming atomic force microscopy tips from the two dimensional array of carbon nanostructures on the surface. 45. The process for the preparation of nanostructured material of claim 43, further comprising: functionalizing the tips of the carbon nanostructures. 46. The process for the preparation of nanostructured material of claim 45, wherein the tips are functionalized by coupling basic or hydrophobic functionalities to carboxyl groups attached to the carbon nanostructures. 47. The process for the preparation on nanostructured material of claim 43, wherein the two dimensional array is used to organize at least one of salts, dyes and responsive organic materials on the surface. 48. The process for the preparation of nanostructured materials of claim 43, wherein the carbon nanostructures are oriented perpendicular to the surface. 49. The process for the preparation of nanostructured materials of claim 48, wherein an aspect ratio of the carbon nanostructures is influenced by the thickness of the coating of the surface. 50. The process for the preparation of nanostructured materials of claim 43, wherein the carbon nanostructures are oriented substantially parallel to the surface. 51. The process for the preparation of nanostructured material of claim 43, wherein the surface is on a substrate and the two dimensional array of carbon nanostructures increases the thermal stability of the substrate. 52. The process for the preparation of nanostructured material of claim 43, further comprising: infusing the two dimensional array of carbon nanostructures with a reactive species. 53. The process for the preparation of nanostructured material of claim 52, wherein the infused reactive species form an electrolyte. 54. The process for the preparation of nanostructured material of claim 52, further comprising: adding an ionic species to form an electrolyte. 55. The process for the preparation of nanostructured material of claim 52, wherein the reactive species is comprises at least one of organic monomers and inorganic monomers. 56. The process for the preparation of nanostructured material of claim 55, wherein the reactive species comprises organic monomers. 57. The process for the preparation of nanostructured material of claim 55, wherein the reactive species comprises inorganic monomers. 58. The process for the preparation of nanostructured material of claim 52, wherein the reactive species are polymerizable. 59. The process for the preparation of nanostructured material of claim 58, further comprising: polymerizing the reactive species. 60. The process for the preparation of nanostructured material of claim 58, wherein the surface is on a substrate and wherein polymerizing the reactive species forms a nanocomposite coating on the substrate. 61. The process for the preparation of nanostructured material of claim 60, further comprising: removing the nanocomposite coating from the surface forming free standing structure. 62. The process for the preparation of nanostructured material of claim 52, the reactive species comprise an insulator. 63. The process for the preparation of nanostructured materials of claim 41, wherein the surface is on a substrate, and the surface is covered by the film. 64. The process for the preparation of nanostructured materials of claim 41, wherein the surface is on a substrate, and the surface is partially covered by the film. 65. The process for the preparation of nanostructured materials of claim 41, wherein the morphology of the precursor is influenced by the surface of the substrate. 66. The process for the preparation of nanostructured materials of claim 65, wherein the surface is on a substrate comprising a crystalline material. 67. The process for the preparation of nanostructured materials of claim 66, wherein the orientation of crystalline material influences the morphology of the precursor. 68. The process for the preparation of nanostructured materials of claim 41, wherein the surface is coated with one of an ultra thin film, a thin film, or a thick film of the phase separable material. 69. The process for the preparation of nanostructured materials of claim 68, further comprising: annealing the phase separable material to form a phase separated material. 70. The process for the preparation of nanostructured materials of claim 69, wherein annealing the phase separable material is conducted in the absence of oxygen. 71. The process for the preparation of nanostructured materials of claim 70, wherein anneal the phase separated polymer material is conducted in a controlled environment or under reduced pressure. 72. The process for the preparation of nanostructured materials of claim 69, further comprising: heating the phase separable material to stabilize the phase separation. 73. The process for the preparation of nanostructured materials of claim 72, wherein heating the phase separable material is conducted in the presence of oxygen. 74. The process for the preparation of nanostructured materials of claim 1, wherein the nanostructured materials comprise carbon nanostructures having adsorptive capacity. 75. The process for the preparation of nanostructured material of claim 74, wherein the carbon nanostructures function as an electronic tongue. 76. The process for the preparation of nanostructured materials of claim 1, wherein the phase separated copolymer material comprises a block copolymer having a block derived from at least two different monomer units. 77. The process for the preparation of nanostructured materials of claim 76, wherein at least one of the two different monomer units form a core in the phase separated polymer material. 78. The process for the preparation of nanostructured materials of claim 76, wherein the block derived from at least two different monomer units is a gradient copolymer block. 79. The process for the preparation of nanostructured materials of claim 1, wherein the phase separated copolymer material comprises a transition metal. 80. A high surface area carbon nanostructured material produced from the process of claim 79. 81. The process for the preparation of nanostructured materials of claim 79, wherein the transition metal is a complexed transition metal. 82. The process for the preparation of nanostructured materials of claim 81, wherein the nanostructured material comprises a catalyst. 83. The process for the preparation of nanostructured material of claim 1, wherein the nano structured material are for the manufacture of photovoltaic cells, supercapacitors, batteries, fuel cells, computer memory, carbon electrodes, carbon foams, actuators and materials for hydrogen storage. 84. The process for the preparation of nanostructured material of claim 1, further comprising: contacting the nanostructured material with a transition metal; and pyrolyzing the nanostructured material with the transition metal to form a carbide. 85. The process for the preparation of nanostructured material of claim 84, wherein the transition metal is a transition metal salt. 86. The process for the preparation of nanostructured materials of claim 1, wherein the nanostructured material comprises two dimensional array of carbon nanotubes. 87. The process for the preparation of nanostructured materials of claim 86, wherein at least a portion of the nanostructured material is incorporated in flat panel display. 88. The process of claim 1, wherein the nanostructured material is used for supercapacitor electrodes. 89. A high surface area carbon nanostructured material produced from the process of claim 1. 90. The process for the preparation of nanostructured materials of claim 1, wherein an array of carbon nanostructures is formed on a substrate; and, further comprising: infusing the array with a transition metal; and pyrolyzing the array. 91. The process of claim 90, wherein the transition metal forms a semiconductor on the substrate. 92. The process of claim 90, wherein the transition metal forms a conductor on the substrate.
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