IPC분류정보
국가/구분 |
United States(US) Patent
등록
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국제특허분류(IPC7판) |
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출원번호 |
UP-0331230
(2006-01-13)
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등록번호 |
US-7749299
(2010-07-26)
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발명자
/ 주소 |
- Vanheusden, Karel
- Kunze, Klaus
- Kiim, Hyungrak
- Stump, Aaron D.
- Schult, Allen B.
- Hampden-Smith, Mark J.
- Edwards, Chuck
- James, Anthony R.
- Caruso, James
- Kodas, Toivo T.
- Haubrich, Scott Thomas
- Kowalski, Mark H.
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출원인 / 주소 |
|
인용정보 |
피인용 횟수 :
22 인용 특허 :
214 |
초록
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A process for the production of metal nanoparticles. The process comprises a rapid mixing of a solution of at least about 0.1 mole of a metal compound that is capable of being reduced to a metal by a polyol with a heated solution of a polyol and a substance that is capable of being adsorbed on the n
A process for the production of metal nanoparticles. The process comprises a rapid mixing of a solution of at least about 0.1 mole of a metal compound that is capable of being reduced to a metal by a polyol with a heated solution of a polyol and a substance that is capable of being adsorbed on the nanoparticles.
대표청구항
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What is claimed is: 1. A process for the production of metal nanoparticles, wherein the process comprises a rapid mixing of a solution of at least about 0.1 mole of a metal compound that is capable of being reduced to a metal by a polyol with a heated solution that comprises a polyol and a substanc
What is claimed is: 1. A process for the production of metal nanoparticles, wherein the process comprises a rapid mixing of a solution of at least about 0.1 mole of a metal compound that is capable of being reduced to a metal by a polyol with a heated solution that comprises a polyol and a substance that is capable of being adsorbed on the nanoparticles, wherein the rapid mixing comprises combining the solutions within not more than about 1 minute. 2. The process of claim 1, further comprising (a) isolating the metal nanoparticles; (b) suspending the metal nanoparticles in a liquid that is capable of dissolving the substance that is adsorbed on the nanoparticles; and (c) filtering the suspending metal nanoparticles. 3. The process of claim 2, wherein the liquid comprises ethanol. 4. The process of claim 1, wherein the metal comprises a transition metal. 5. The process of claim 4, wherein the transition metal comprises at least one of gold, silver, copper, nickel, cobalt, palladium, platinum, iridium, osmium, rhodium, ruthenium, rhenium, vanadium, chromium, manganese, niobium, molybdenum, tungsten, tantalum, iron and cadmium. 6. The process of claim 4, wherein the metal comprises at least one of gold, silver, copper and nickel. 7. The process of claim 1, wherein the metal comprises silver. 8. The process of claim 1, wherein the metal compound comprises a salt of an inorganic acid. 9. The process of claim 8, wherein the metal compound comprises a nitrate. 10. The process of claim 1, wherein the metal compound comprises a salt of an organic acid. 11. The process of claim 10, wherein the metal compound comprises an acetate or trifluoroacetate. 12. The process of claim 1, wherein the metal compound comprises at least one of silver nitrate, silver acetate, silver trifluoroacetate, silver oxide, copper oxide, copper hydroxide, copper sulfate, nickel oxide, nickel hydroxide, nickel chloride, nickel sulfate, nickel acetate, cobalt oxide, cobalt hydroxide, cobalt chloride and cobalt sulfate. 13. The process of claim 1, wherein the polyol comprises a polyol having from 2 to 6 hydroxy groups. 14. The process of claim 1, wherein the polyol comprises at least one glycol. 15. The process of claim 14, wherein the at least one glycol comprises from 2 to 4 carbon atoms. 16. The process of claim 14, wherein the polyol comprises at least one of ethylene glycol and propylene glycol. 17. The process of claim 1, wherein the polyol comprises ethylene glycol. 18. The process of claim 1, wherein the polyol comprises one or more of ethylene glycol, diethylene glycol, triethylene glycol, tetraethylene glycol, propylene glycol, dipropylene glycol, 1,3-propanediol, 1,2-butanediol, 1,3-butanediol, 1,4-butanediol, 2,3-butanediol, glycerol, trimethylolpropane, triethanolamine and trihydroxymethylaminomethane. 19. The process of claim 1, wherein the substance that is capable of being adsorbed on the nanoparticles comprises a substance that is capable of substantially preventing an agglomeration of the nanoparticles. 20. The process of claim 19, wherein the substance that is capable of being adsorbed on the nanoparticles is present in a sufficient amount to substantially prevent an agglomeration of the nanoparticles. 21. The process of claim 1, wherein the substance that is capable of being adsorbed on the nanoparticles comprises at least two heteroatoms selected from O and N. 22. The process of claim 1, wherein the substance that is capable of being adsorbed on the nanoparticles comprises one or more of a hydroxy group, a carbonyl group, an ether group and an amino group. 23. The process of claim 1, wherein the substance that is capable of being adsorbed on the nanoparticles comprises a substance that is capable of reducing the metal compound. 24. The process of claim 1, wherein the substance that is capable of being adsorbed on the nanoparticles comprises a polymer. 25. The process of claim 24, wherein the polymer comprises units of a monomer which comprises at least one heteroatom selected from O and N. 26. The process of claim 24, wherein the polymer comprises units of a monomer which comprises at least two heteroatoms selected from O and N. 27. The process of claim 24, wherein the polymer comprises units of a monomer which comprises one or more of a hydroxyl group, a carbonyl group, an ether group and an amino group. 28. The process of claim 24, wherein the polymer comprises at least one structural element selected from —COO—, —O—CO—O—, —CO—O—CO—, —C—O—C—, —CONR—, —NR—CO—O—, —NR1—CO—NR2—, —CO—NR—CO—, —SO2—NR—and —SO2—O—, wherein R, R1 and R2 each independently represent hydrogen or an organic radical. 29. The process of claim 24, wherein the polymer comprises a polymer of vinyl pyrrolidone. 30. The process of claim 29, wherein the polymer of vinyl pyrrolidone comprises a vinyl pyrrolidone homopolymer. 31. The process of claim 24, wherein the polymer has a weight average molecular weight of up to about 100,000. 32. The process of claim 24, wherein the polymer has a weight average molecular weight of not less than about 1,000. 33. The process of claim 24, wherein the polymer has a weight average molecular weight of not less than about 58,000. 34. The process of claim 24, wherein the polymer comprises water in an amount of about 1-10% by weight. 35. The process of claim 24, wherein the polymer comprises 2-pyrrolidone in an amount of about 1-10% by weight. 36. The process of claim 24, wherein the polymer comprises formic acid in an amount of about 0-2% by weight. 37. The process of claim 24, wherein the polyol comprises water in an amount of about 0.01-0.10% by weight. 38. The process of claim 1, wherein the solution of the metal compound comprises a polyol. 39. The process of claim 38, wherein the polyol comprises water in an amount of about 0.01-0.10% by weight. 40. The process of claim 38, wherein a polyol of the solution of the metal compound and a polyol of the heated solution are the same. 41. The process of claim 1, wherein the heated solution has a temperature of at least about 80° C. 42. The process of claim 1, wherein the heated solution has a temperature of at least about 120° C. 43. The process of claim 1, wherein the heated solution has a temperature of not higher than about 180° C. 44. The process of claim 1, wherein the heated solution has a temperature of not higher than about 140° C. 45. The process of claim 1, wherein a temperature of the solution of the metal compound is not higher than about 40° C. 46. The process of claim 1, wherein a temperature of the solution of the metal compound is not higher than about 40° C. and the heated solution has a temperature of at least about 80° C. 47. The process of claim 1, wherein the rapid mixing comprises combining the solutions within a period of not more than about 30 seconds. 48. The process of claim 1, wherein the solutions are mixed by a one-shot addition of one of the solutions to another one of the solutions. 49. The process of claim 1, wherein the rapid mixing is accompanied by at least one of stirring, shaking and sonication. 50. The process of claim 1, wherein the solution of the metal compound comprises at least about 0.5 mole of the metal compound. 51. The process of claim 1, wherein the solution of the metal compound comprises at least about 0.75 mole of the metal compound. 52. The process of claim 1, wherein a total volume of the solution of the metal compound and the heated solution per mole of the metal compound is not larger than about 6 liters. 53. The process of claim 52, wherein the total volume is not larger than about 4 liters. 54. The process of claim 1, wherein a volume ratio of the heated solution and the solution of the metal compound is not higher than about 10:1. 55. The process of claim 1, wherein a volume ratio of the heated solution and the solution of the metal compound is not lower than about 1:1. 56. The process of claim 1, wherein the substance that is capable of being adsorbed on the nanoparticles comprises a polymer comprising monomer units and a molar ratio of the monomer units and the metal compound is at least about 3:1. 57. The process of claim 56, wherein the molar ratio is at least about 6:1. 58. The process of claim 56, wherein the molar ratio is not higher than about 100:1. 59. The process of claim 1, wherein the process further comprises a heating of the mixed solutions at a temperature of at least about 80° C. for a sufficient period to reduce at least a substantial portion of the metal compound to the metal. 60. The process of claim 59, wherein at least about 90% of the metal compound is reduced. 61. The process of claim 59, wherein the mixed solutions are heated at a temperature of at least about 100° C. 62. The process of claim 59, wherein the mixed solutions are heated at a temperature of at least about 120° C. 63. The process of claim 1, wherein the process further comprises a precipitation of formed nanoparticles. 64. The process of claim 63, wherein the precipitation comprises an addition of a sufficient amount of a nanoparticle-precipitating substance to precipitate at least a substantial portion of the nanoparticles. 65. The process of claim 64, wherein the nanoparticle-precipitating substance comprises an aprotic solvent. 66. The process of claim 65, wherein the aprotic solvent comprises a polar aprotic solvent. 67. The process of claim 65, wherein the aprotic solvent comprises a ketone. 68. The process of claim 67, wherein the ketone comprises acetone. 69. The process of claim 64, wherein at least one of before, during and after the addition of the nanoparticle-precipitating substance a protic solvent is added. 70. The process of claim 69, wherein the protic solvent comprises at least one of an alcohol and a polyol. 71. The process of claim 1, wherein the process further comprises an isolation of formed nanoparticles. 72. The process of claim 71, wherein the isolation comprises at least one of an ultrafiltration and a diafiltration. 73. The process of claim 1, wherein the process further comprises a washing of formed nanoparticles with a liquid that is capable of dissolving the substance that is capable of being adsorbed on the nanoparticles. 74. The process of claim 73, wherein the liquid comprises a protic organic solvent. 75. The process of claim 73, wherein the liquid comprises at least one of an alcohol, a polyol and water. 76. The process of claim 73, wherein the liquid comprises ethanol. 77. The process of claim 1, wherein the process is carried out continuously. 78. A process for the production of metal nanoparticles, wherein the process comprises a rapid mixing of a solution of at least about 0.25 mole of a compound of at least one metal selected from gold, silver, palladium, platinum, rhodium, copper, nickel and cobalt with a heated solution that comprises a polyol and a polymer that is capable of substantially preventing an agglomeration of the nanoparticles, wherein the rapid mixing comprises combining the solutions within not more than about 1 minute. 79. The process of claim 78, wherein the metal is selected from at least one of silver, copper and nickel. 80. The process of claim 78, wherein the metal comprises silver. 81. The process of claim 79, wherein the metal compound comprises silver nitrate. 82. The process of claim 78, wherein the polyol comprises at least one of ethylene glycol and propylene glycol. 83. The process of claim 78, wherein the polymer comprises units of a monomer which comprises at least one heteroatom selected from O and N. 84. The process of claim 78, wherein the polymer comprises at least one structural element selected from —COO—, —O—CO—O—, —CO—O—CO—, —C—O—C— —CONR—, —NR—CO—O—, —NR1—CO—NR2—, —CO—NR—CO—, —SO2—NR— and —SO2—O—, wherein R, R1 and R2 each independently represent hydrogen or an organic radical. 85. The process of claim 78, wherein the polymer comprises polyvinylpyrrolidone. 86. The process of claim 85, wherein the polyvinylpyrrolidone has a weight average molecular weight of from about 3,000 to about 60,000. 87. The process of claim 78, wherein the heated solution has a temperature of at least about 90° C. 88. The process of claim 87, wherein a temperature of the solution of the metal compound is not higher than about 30° C. 89. The process of claim 78, wherein the heated solution has a temperature of at least about 110° C. 90. The process of claim 78, wherein the heated solution has a temperature of not higher than about 160° C. 91. The process of claim 78, wherein the rapid mixing comprises combining the solutions within not more than about 15 seconds. 92. The process of claim 78, wherein the solution of the metal compound comprises at least about 0.5 mole of the metal compound. 93. The process of claim 92, wherein a total volume of the solution of the metal compound and the heated solution is not higher than about 5 liters per one mole of the metal compound. 94. The process of claim 93, wherein a volume ratio of the heated solution and the solution of the metal compound is from about 10:1 to about 3:1. 95. The process of claim 78, wherein the polymer comprises monomer units and a molar ratio of said monomer units and the metal compound is from about 3:1 to about 50:1. 96. The process of claim 78, wherein the nanoparticles are of a substantially uniform shape and size. 97. The process of claim 78, wherein at least about 90% of the nanoparticles are of a substantially spherical shape. 98. The process of claim 97, wherein at least about 90% of the nanoparticles have a diameter of not more than about 80 nm. 99. The process of claim 78, wherein the process further comprises keeping the mixed solutions at an elevated temperature to convert a substantial portion of the metal compound to nanoparticles. 100. The process of claim 99, wherein the mixed solutions are heated at a temperature of at least about 100° C. 101. The process of claim 78, wherein the process further comprises a precipitation of formed nanoparticles. 102. The process of claim 101, wherein the precipitation comprises an addition of a nanoparticle-precipitating liquid in a sufficient amount to precipitate at least a substantial portion of the nanoparticles. 103. The process of claim 102, wherein the nanoparticle-precipitating liquid comprises a polar aprotic solvent. 104. The process of claim 102, wherein the nanoparticle-precipitating liquid comprises a ketone. 105. The process of claim 78, wherein the process further comprises a separation of formed nanoparticles from a liquid phase. 106. The process of claim 105, wherein the separation comprises at least one of a diafiltration and an ultrafiltration. 107. The process of claim 78, wherein the process further comprises a washing of isolated nanoparticles with a liquid that is capable of dissolving the polymer. 108. The process of claim 107, wherein the liquid comprises ethanol. 109. The process of claim 107, wherein the washing comprises at least one of a diafiltration and an ultrafiltration. 110. The process of claim 78, wherein the process affords a nanoparticle containing reaction mixture and the process further comprises subjecting the reaction mixture to at least one of a diafiltration and an ultrafiltration. 111. A process for the production of silver nanoparticles, wherein the process comprises a rapid mixing of a solution of at least about 0.5 mole of a silver compound with a heated solution which comprises a polyol and a vinyl pyrrolidone polymer, wherein the rapid mixing comprises combining the solutions within not more than about 1 minute. 112. The process of claim 111, wherein the silver compound comprises at least one of silver nitrate, silver acetate, silver trifluoroacetate and silver oxide. 113. The process of claim 111, wherein the polyol comprises from 2 to 4 hydroxy groups. 114. The process of claim 111, wherein the polyol comprises at least one glycol. 115. The process of claim 114, wherein the vinyl pyrrolidone polymer comprises a vinyl pyrrolidone homopolymer. 116. The process of claim 115, wherein the vinyl pyrrolidone homopolymer has a weight average molecular weight of up to about 60,000. 117. The process of claim 115, wherein the vinyl pyrrolidone homopolymer has a weight average molecular weight of about 10,000. 118. The process of claim 111, wherein the solution of the silver compound comprises a polyol. 119. The process of claim 118, wherein the polyol comprises ethylene glycol. 120. The process of claim 111, wherein the heated solution has a temperature of from about 100° C. to about 140° C. 121. The process of claim 120, wherein a temperature of the solution of the silver compound is not higher than about 30° C. 122. The process of claim 121, wherein the solutions are combined by a one-shot addition of the solution of the silver compound to the heated solution. 123. The process of claim 122, wherein the solution of the silver compound comprises at least about 0.75 mole of the silver compound. 124. The process of claim 111, wherein the heated solution has a temperature of about 120° C. 125. The process of claim 111, wherein a combined volume of the solution of the silver compound and the heated solution is not larger than about 4 liters per mole of the silver compound. 126. The process of claim 125, wherein a volume ratio of the heated solution and the solution of the silver compound is from about 8:1 to about 4:1. 127. The process of claim 126, wherein the volume ratio is at least about 5:1. 128. The process of claim 111, wherein the vinyl pyrrolidone polymer is present in a sufficient amount to prevent a substantial agglomeration of the silver nanoparticles. 129. The process of claim 111, wherein a molar ratio of vinyl pyrrolidone units in the vinyl pyrrolidone polymer and the silver compound is from about 3:1 to about 50:1. 130. The process of claim 129, wherein the molar ratio is at least about 6:1. 131. The process of claim 129, wherein the molar ratio is about 12:1. 132. The process of claim 111, wherein the process further comprises keeping the mixed solutions at a temperature of at least about 100° C. for a sufficient period to convert at lease about 90% of the silver compound to elemental silver. 133. The process of claim 132, wherein the mixed solutions are heated at a temperature of about 120° C. until substantially all of silver compound is converted to elemental silver. 134. The process of claim 111, wherein the process further comprises a precipitation of formed nanoparticles. 135. The process of claim 134, wherein the precipitation comprises adding a sufficient amount of a nanoparticle-precipitating liquid that is miscible with a polyol to precipitate at least a substantial portion of the nanoparticles. 136. The process of claim 135, wherein the nanoparticle-precipitating liquid comprises a polar aprotic solvent. 137. The process of claim 136, wherein the solvent comprises acetone. 138. The process of claim 111, wherein the process further comprises a separation of nanoparticles from a liquid phase. 139. The process of claim 138, wherein the separation comprises at least one of an ultrafiltration and a diafiltration. 140. The process of claim 111, wherein the process further comprises a washing of isolated nanoparticles with a liquid that is capable of dissolving the vinyl pyrrolidone polymer. 141. The process of claim 140, wherein the liquid comprises ethanol. 142. A process for the production of silver nanoparticles, wherein the process comprises a one-shot addition of a solution of at least about 0.75 mole of a silver compound in at least one of ethylene glycol and propylene glycol to a heated solution of polyvinylpyrrolidone in at least one of ethylene glycol and propylene glycol, wherein the solution of the silver compound is at a temperature of not higher than about 30° C., the polyvinylpyrrolidone solution is at a temperature of at least about 110° C., a total volume of the solution of the silver compound and the polyvinylpyrrolidone solution is from about 3 to about 4 liters per one mole of the silver compound, a volume ratio of the polyvinylpyrrolidone solution and the solution of the silver compound is from about 4:1 to about 6:1 and a molar ratio of vinyl pyrrolidone units in the polyvinylpyrrolidone and the silver compound is from about 5:1 to about 15:1. 143. The process of claim 142, wherein the silver compound comprises silver nitrate. 144. The process of claim 142, wherein the process further comprises a heating of the combined solutions at a temperature of at least about 120° C. until substantially all of silver nitrate has reacted. 145. The process of claim 142, wherein the process further comprises a precipitation of the nanoparticles, which precipitation comprises an addition of acetone. 146. The process of claim 144, wherein the process further comprises a separation of precipitated nanoparticles from a liquid phase by at least one of a centrifugation, an ultrafiltration and a diafiltration. 147. The process of claim 142, wherein the process further comprises a washing of isolated nanoparticles with ethanol. 148. The process of claim 142, wherein the process further comprises a work-up of an obtained nanoparticle containing reaction mixture for isolating the nanoparticles, the work-up comprising at least one of a diafiltration and an ultrafiltration.
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