Method for separating single-wall carbon nanotubes and compositions thereof
원문보기
IPC분류정보
국가/구분
United States(US) Patent
등록
국제특허분류(IPC7판)
G01N-027/447
B03C-005/00
B01D-015/08
출원번호
US-0379273
(2003-03-04)
발명자
/ 주소
Smalley,Richard E.
Hauge,Robert H.
Kittrell,W. Carter
Sivarajan,Ramesh
Strano,Michael S.
Bachilo,Sergei M.
Weisman,R. Bruce
출원인 / 주소
William Marsh Rice University
대리인 / 주소
Winstead Sechrest &
인용정보
피인용 횟수 :
67인용 특허 :
2
초록▼
The invention relates to a process for sorting and separating a mixture of (n, m) type single-wall carbon nanotubes according to (n, m) type. A mixture of (n, m) type single-wall carbon nanotubes is suspended such that the single-wall carbon nanotubes are individually dispersed. The nanotube suspens
The invention relates to a process for sorting and separating a mixture of (n, m) type single-wall carbon nanotubes according to (n, m) type. A mixture of (n, m) type single-wall carbon nanotubes is suspended such that the single-wall carbon nanotubes are individually dispersed. The nanotube suspension can be done in a surfactant-water solution and the surfactant surrounding the nanotubes keeps the nanotube isolated and from aggregating with other nanotubes. The nanotube suspension is acidified to protonate a fraction of the nanotubes. An electric field is applied and the protonated nanotubes migrate in the electric fields at different rates dependent on their (n, m) type. Fractions of nanotubes are collected at different fractionation times. The process of protonation, applying an electric field, and fractionation is repeated at increasingly higher pH to separated the (n, m) nanotube mixture into individual (n, m) nanotube fractions. The separation enables new electronic devices requiring selected (n, m) nanotube types.
대표청구항▼
What is claimed is: 1. A method for separating a mixture of (n, m) single-wall carbon nanotubes into fractions based on the (n, m) types comprising: a) suspending a mixture of (n, m) single-wall carbon nanotubes in a liquid to form a suspension of individually-suspended nanotubes; b) adjusting the
What is claimed is: 1. A method for separating a mixture of (n, m) single-wall carbon nanotubes into fractions based on the (n, m) types comprising: a) suspending a mixture of (n, m) single-wall carbon nanotubes in a liquid to form a suspension of individually-suspended nanotubes; b) adjusting the pH of the suspended nanotube mixture to cause protonation of a first fraction of x fractions of nanotubes, wherein x is an arbitrary whole number of at least 1; c) separating the suspended nanotube mixture by applying an electric field to the suspended nanotubes wherein the (n, m) single-wall carbon nanotube types migrate at different rates within the electric field, and wherein the different migration rates cause the protonated (n, m) single-wall carbon nanotubes to be separated by type; d) collecting by type the separated (n, m) single-wall carbon nanotubes. 2. The method of claim 1 further comprising: a) adjusting the pH of the suspended nanotube mixture to cause protonation of additional fractions of the remaining x-1 fractions of nanotubes; b) separating the suspended nanotube mixture for the remaining x-1 fractions of nanotubes; and c) collecting by type the separated (n, m) single-wall carbon nanotubes for the remaining x-1 fractions of nanotubes. 3. The method of claim 1 further comprising removing bundles of single-wall carbon nanotubes and non-nanotube material from the suspension of individually-suspended nanotubes. 4. The method of claim 3 wherein the removing is done by centrifuging the single-wall carbon nanotube mixture, wherein the bundles of single-wall carbon nanotubes and the non-nanotube material are concentrated in the sediment and removed, and wherein the individually-suspended nanotubes remain in suspension. 5. The method of claim 1 wherein the pH is adjusted with an acid. 6. The method of claim 5 wherein the acid is selected from the group consisting of hydrochloric acid, hydrofluoric acid, carbonic acid, sulfuric acid, nitric acid, chlorosulfonic acid, fluorosulfuric acid, methane sulfonic acid, trifluoromethane sulfonic acid, oleum and combinations thereof. 7. The method of claim 1 wherein the liquid comprises a surfactant and water. 8. The method of claim 7 wherein the surfactant is selected from the group consisting of anionic surfactant, cationic surfactant and nonionic surfactant. 9. The method of claim 7 wherein the surfactant is sodium dodecylsulfate. 10. The method of claim 7 wherein the surfactant forms a micellular structure around the individually-suspended nanotube. 11. The method of claim 1 wherein the liquid comprises a polymer and water. 12. The method of claim 11 wherein the polymer coats the individually-suspended nanotubes. 13. The method of claim 11 wherein the polymer is selected from the group consisting of: polyvinyl pyrrolidone (PVP), polystyrene sulfonate (PSS), poly(1-vinyl pyrrolidone-co-vinyl acetate) (PVP/VA), poly(1-vinyl pyrrolidone-co-acrylic acid), poly(1-vinyl pyrrolidone-co-dimethylaminoethyl methacrylate), polyvinyl sulfate, poly(sodium styrene sulfonic acid-co-maleic acid), polyethylene oxide (PEO), polypropylene oxide (PPO), dextran, dextran sulfate, bovine serum albumin (BSA), poly(methyl methacrylate-co-ethyl acrylate), polyvinyl alcohol, polyethylene glycol, polyallyl amine, copolymers thereof and mixtures thereof. 14. The method of claim 1 wherein the separating step is done by electrophoresis. 15. The method of claim 14 where in the electrophoresis method is selected from the group consisting of capillary electrophoresis, gel electrophoresis, paper electrophoresis and a combination thereof. 16. The method of claim 1 wherein the separating step is done by capillary electrophoresis. 17. The method of claim 1 wherein the (n, m) nanotube mixture is separated into at least two types of single-wall carbon nanotubes, wherein the first type comprises metallic (n, m) nanotubes and the second type comprises semiconducting (n, m) nanotubes. 18. The method of claim 1 wherein the adjusting step causes the pH to be lower. 19. The method of claim 1 further comprising deprotonating the separated protonated nanotubes. 20. The method of claim 19 wherein the deprotonation is done by increasing the pH to greater than the pH wherein the separated nanotubes were protonated. 21. A method for separating a mixture of (n, m) single-wall carbon nanotubes into fractions based on the (n, m) types comprising: a) suspending a mixture of (n, m) single-wall carbon nanotubes in a liquid to form a suspension of individually-suspended nanotubes; b) adjusting the ionic strength of the suspended nanotube mixture to cause a first fraction of x fractions of nanotubes to carry a charge, wherein x is an arbitrary whole number of at least 1; c) separating the suspended nanotube mixture wherein the charged-carrying (n, m) single-wall carbon nanotube types migrate at different rates, and wherein the different migration rates cause the charged (n, m) single-wall carbon nanotubes to be separated from each other; and d) collecting the separated (n, m) single-wall carbon nanotube types and the fraction of nanotubes that were uncharged. 22. The method of claim 21 further comprising repeating steps b), c) and d) with the uncharged fraction of the nanotube mixture x-1 times, wherein the x fractions of (n, m) nanotubes are charged and collected. 23. The method of claim 21 further comprising removing bundles of single-wall carbon nanotubes and non-nanotube material from the suspension of individually-suspended nanotubes. 24. The method of claim 23 wherein the removing is done by centrifuging the single-wall carbon nanotube mixture, wherein the bundles of single-wall carbon nanotubes and the non-nanotube material are concentrated in the sediment and removed, and wherein the individually-suspended nanotubes remain in suspension. 25. The method of claim 21 wherein the charge is imparted by a species selected from the group consisting of proton (H+), hydronium ion (H3O+), and combinations thereof. 26. The method of claim 21 wherein the charge is imparted by an acid capable of protonating the individually-suspended nanotubes. 27. The method of claim 26 wherein the acid is selected from the group consisting of hydrochloric acid, hydrofluoric acid, chlorosulfonic, carbonic acid, sulfuric acid, nitric acid, fluorosulfuric acid, chlorosulfonic acid, methane sulfonic acid, trifluoromethane sulfonic acid, oleum and combinations thereof. 28. The method of claim 26 wherein the acid is selected from the group consisting of hydrochloric acid, sulfuric acid, nitric acid, oleum and combinations thereof. 29. The method of claim 21 wherein the liquid comprises a surfactant and water. 30. The method of claim 29 wherein the surfactant is selected from the group consisting of anionic surfactant, cationic surfactant and nonionic surfactant. 31. The method of claim 30 wherein the anionic surfactant is selected from the group consisting of N-lauroylsarcosine sodium salt, N-dodecanoyl-N-methylglycine sodium salt and sodium N-dodecanoyl-N-methylglycinate, polystyrene sulfonate, sodium dodecyl sulfate, sodium dodecyl sulfonate, sodium alkyl allyl sulfosuccinate and combinations thereof. 32. The method of claim 30 wherein the cationic surfactant is selected from the group consisting of dodecyltrimethylammonium bromide, cetyltrimethylammonium bromide, cetyltrimethylammonium chloride and combinations thereof. 33. The method of claim 30 wherein the nonionic surfactant is selected from the group consisting of N-lauroylsarcosine, N-dodecanoyl-N-methylglycine, polyethylene glycol dodecyl ether, polyethylene glycol lauryl ether, polyethylene glycol hexadecyl ether, polyethylene glycol stearyl ether, polyethylene glycol oleyl ether, block copolymers of polyethylene and polypropylene glycol, alkylaryl polyethether alcohols, ethoxylated propoxylated C8-C10 alcohols, t-octylphenoxypolyethoxyethanol, polyethylene glycol tert-octylphenyl ether, polyoxyethylene isooctylcyclohexyl ether, polyethylene glycol sorbitan monolaurate, polyoxyethylene monostearate, polyoxyethylenesorbitan tristearate, polyoxyethylenesorbitan monooleate, polyoxyethylenesorbitan trioleate, and polyoxyethylenesorbitan monopalmitate, polyvinylpyrrolidone, and combinations thereof. 34. The method of claim 29 wherein the surfactant is sodium dodecyl sulfate. 35. The method of claim 29 wherein the surfactant is dodecyltrimethylammonium bromide. 36. The method of claim 29 wherein the surfactant is a selected from the group consisting of alkylaryl polyethether alcohols, ethoxylated propoxylated C8-C10 alcohols, t-octylphenoxypolyethoxyethanol, polyethylene glycol tert-octylphenyl ether, polyoxyethylene isooctylcyclohexyl ether, and combinations thereof. 37. The method of claim 29 wherein the surfactant forms a micellular structure around the individually-suspended nanotube. 38. The method of claim 29 wherein the liquid comprises a polymer and water. 39. The method of claim 38 wherein the polymer coats the individually-suspended nanotubes. 40. The method of claim 38 wherein the polymer is selected from the group consisting of: polyvinylpyrrolidone (PVP), polystyrene sulfonate (PSS), poly(1-vinyl pyrrolidone-co-vinyl acetate) (PVP/VA), poly(1-vinyl pyrrolidone-co-acrylic acid), poly(1-vinyl pyrrolidone-co-dimethylaminoethyl methacrylate), polyvinyl sulfate, poly(sodium styrene sulfonic acid-co-maleic acid), polyethylene oxide (PEO), polypropylene oxide (PPO), dextran, dextran sulfate, bovine serum albumin (BSA), poly(methyl methacrylate-co-ethyl acrylate), polyvinyl alcohol, polyethylene glycol, polyallyl amine, copolymers thereof and mixtures thereof. 41. The method of claim 21 further comprising removing aggregates or impurities from the suspension of individually-suspended nanotubes by a means based on differences in density. 42. The method of claim 41 wherein the aggregates and impurities are removed from the suspension of individually-suspended nanotubes by centrifugation. 43. The method of claim 21 wherein the separating step is done by chromatographic means in the presence of an electric field. 44. The method of claim 21 wherein the separating step is done by electrophoresis. 45. The method of claim 44 where in the electrophoresis method is selected from the group consisting of capillary electrophoresis, gel electrophoresis, paper electrophoresis and a combination thereof. 46. The method of claim 21 wherein the separating step is done by capillary electrophoresis. 47. The method of claim 21 wherein the (n, m) nanotube mixture is separated into at least two types of single-wall carbon nanotubes, wherein the first type comprises metallic (n, m) nanotubes and the second type comprises semiconducting (n, m) nanotubes. 48. The method of claim 21 wherein the adjusting step causes the ionic strength to be higher. 49. The method of claim 21 further comprising neutralizing the charged separated nanotubes. 50. A method of separating single-wall carbon nanotubes according to (n, m) type, comprising the steps of: a) dispersing a mixture of (n, m) type single-wall carbon nanotubes in a surfactant-containing suspending medium to form a suspension comprising individual single-wall carbon nanotubes encapsulated in surfactant micelles; b) acidifying the suspension to protonate metallic and small band gap nanotubes; and c) separating single-wall carbon nanotubes of individual (n, m) type based on the degree of their protonation. 51. The method of claim 50 wherein the surfactant is selected from the group consisting of cationic surfactants, anionic surfactants, neutral surfactants, and combinations thereof. 52. The method of claim 50, wherein the surfactant is sodium dodecyl sulfate. 53. The method of claim 50, wherein ultrasonication is used to facilitate the dispersing step. 54. The method of claim 50, wherein the acidifying step comprises a stepwise addition involving separation of protonated nanotubes after each stepwise acid addition. 55. The method of claim 50, wherein the acidifying step comprises by adding a non-oxidizing acid. 56. The method of claim 50, wherein the separation step comprises processing through a chromatographic column. 57. The method of claim 50, wherein the separation step comprises processing over a chromatographic plate. 58. The method of claim 50, wherein the separation step comprises separation in an electric field. 59. The method of claim 50, wherein the separation step comprises capillary electrophoresis. 60. The method of claim 50, wherein the separation step comprises gel electrophoresis. 61. The method of claim 50, further comprising identifying the individual (n, m) type of single-wall carbon nanotube using Raman spectroscopy. 62. The method of claim 50, further comprising identifying the individual (n, m) type of single-wall carbon nanotube using luminescence spectroscopy.
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