Nano-sized particles, processes of making, compositions and uses thereof
First Claim
1. A method of preparing metal oxide nanoparticles, comprising:
- (a) mixing a metal acetate precursor with a non-aqueous organic solvent comprising at least one organic stabilizing ligand to form a reaction mixture;
(b) subjecting the mixture of step (a) to a temperature greater than about 100°
C. for a time sufficient to allow formation of metal oxide nanoparticles and decomposition of the metal acetate; and
(c) extracting the metal oxide nanoparticles into a hydrocarbon solvent at a temperature lower than the temperature of step (b) by precipitation with a flocculating agent.
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Abstract
The present invention describes methods for preparing high quality nanoparticles, i.e., metal oxide based nanoparticles of uniform size and monodispersity. The nanoparticles advantageously comprise organic alkyl chain capping groups and are stable in air and in nonpolar solvents. The methods of the invention provide a simple and reproducible procedure for forming transition metal oxide nanocrystals, with yields over 80%. The highly crystalline and monodisperse nanocrystals are obtained directly without further size selection; particle size can be easily and fractionally increased by the methods. The resulting nanoparticles can exhibit magnetic and/or optical properties. These properties result from the methods used to prepare them. Also advantageously, the nanoparticles of this invention are well suited for use in a variety of industrial applications, including cosmetic and pharmaceutical formulations and compositions.
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Citations
75 Claims
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1. A method of preparing metal oxide nanoparticles, comprising:
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(a) mixing a metal acetate precursor with a non-aqueous organic solvent comprising at least one organic stabilizing ligand to form a reaction mixture;
(b) subjecting the mixture of step (a) to a temperature greater than about 100°
C. for a time sufficient to allow formation of metal oxide nanoparticles and decomposition of the metal acetate; and
(c) extracting the metal oxide nanoparticles into a hydrocarbon solvent at a temperature lower than the temperature of step (b) by precipitation with a flocculating agent. - View Dependent Claims (2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 75)
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30. A method of preparing iron oxide nanoparticles, comprising:
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(a) mixing an iron acetate precursor with an organic solvent comprising at least one organic stabilizing ligand to form a reaction mixture;
(b) subjecting the mixture of step (a) to a temperature of from about 200°
C. to about 260°
C. for a time sufficient to allow formation of iron oxide nanoparticles and decomposition of the iron acetate; and
(c) extracting the iron oxide nanoparticles of step (b) into a hydrocarbon solvent at a temperature lower than the temperature of step (b) by precipitation with a flocculating agent.
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31. A method of preparing manganese oxide nanoparticles, comprising:
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(a) mixing a manganese acetate precursor with an organic solvent comprising at least one organic stabilizing ligand to form a reaction mixture;
(b) subjecting the mixture of step (a) to a temperature of from about 300°
C. to about 350°
C. for a time sufficient to allow formation of monodisperse manganese oxide nanoparticles and decomposition of the manganese acetate; and
(c) extracting the manganese oxide nanoparticles of step (b) into a hydrocarbon solvent at a temperature lower than the temperature of step (b) by precipitation with a flocculating agent.
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32. A method of preparing zinc oxide nanoparticles, comprising:
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(a) mixing a zinc acetate precursor with an organic solvent comprising at least one organic stabilizing ligand to form a reaction mixture;
(b) subjecting the mixture of step (a) to a temperature of from about 300°
C. to about 400°
C. for a time sufficient to allow formation of zinc oxide nanoparticles and decomposition of the zinc acetate; and
(c) extracting the zinc oxide nanoparticles of step (b) into a hydrocarbon solvent at a temperature lower than the temperature of step (b) by precipitation with a flocculating agent. - View Dependent Claims (33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, 50, 51, 52, 53, 54, 55, 56, 71, 72, 73, 74)
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57. A method of preparing monodisperse, stable metal oxide nanoparticles, comprising:
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(a) mixing a metal acetate precursor with a non-aqueous organic solvent comprising at least one organic stabilizing ligand to form a reaction mixture;
(b) subjecting the mixture of step (a) to a temperature of from about 150°
C. to about 400°
C. for a time sufficient to allow formation of metal oxide nanoparticles and decomposition of the metal acetate; and
(c) extracting the metal oxide nanoparticles into a hydrocarbon solvent at a temperature of about 100°
C. or lower by precipitation with a polar organic solvent. - View Dependent Claims (60, 61, 62, 63, 64, 65, 66, 67, 68, 69, 70)
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58. A method of preparing monodisperse, stable metal oxide nanoparticles, comprising:
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(a) mixing a metal acetate precursor with a trialkylamine solvent comprising at least one organic stabilizing ligand comprising a long chain alkyl with one or more carboxylic acid functional groups to form a reaction mixture;
(b) subjecting the mixture of step (a) to a temperature of from about 150°
C. to about 400°
C. for a time sufficient to allow formation of metal oxide nanoparticles and decomposition of the metal acetate; and
(c) extracting the metal oxide nanoparticles into a hydrocarbon solvent at a temperature of about 100°
C. or lower by precipitation with a polar organic solvent.
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59. A method of preparing monodisperse, stable metal oxide nanoparticles, comprising:
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(a) mixing a metal acetate precursor with a trialkylamine solvent comprising at least one organic stabilizing ligand comprising a long chain alkyl with one or more carboxylic acid functional groups to form a reaction mixture;
(b) subjecting the mixture of step (a) to a temperature of from about 250°
C. to about 400°
C. for a time sufficient to allow formation of metal oxide nanoparticles and decomposition of the metal acetate; and
(c) extracting the metal oxide nanoparticles into a hydrocarbon solvent at a temperature of about 100°
C. or lower by precipitation with a polar organic solvent.
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Specification