CN100391664C - Method for preparing single dispersion metal nanometer particles - Google Patents
Method for preparing single dispersion metal nanometer particles Download PDFInfo
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- CN100391664C CN100391664C CNB2005101092196A CN200510109219A CN100391664C CN 100391664 C CN100391664 C CN 100391664C CN B2005101092196 A CNB2005101092196 A CN B2005101092196A CN 200510109219 A CN200510109219 A CN 200510109219A CN 100391664 C CN100391664 C CN 100391664C
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Abstract
The present invention discloses a method for preparing single dispersion metal nanometer particles, which comprises the following step: reacting a metallic ion solution in a mixed system of alkali metal hydroxide, fatty acid and an organic polar solvent to obtain the single dispersion metal nanometer particles. The present invention forms a mixed solvent system by the fatty acid and the organic polar solvent and uses soluble metal salt and the alkali metal hydroxide as raw materials to prepare the single dispersion metal nanometer particles. The method of the present invention has the advantages of convenience, safety, low cost and wide applicability; simultaneously, the method for preparing single dispersion metal nanometer particles is suitable for synthesizing nanometer particles of various kinds of noble metal oxide; the present invention overcomes the problems of high cost and environmental pollution because large numbers of organic solvents are used in the existing synthetic route; noble metal nanometer particles obtained by the present invention can be applied to the fields of biology, medicine, catalytic action, analysis, etc.
Description
Technical field
The present invention relates to a kind of method for preparing single dispersion metal nanometer particles.
Background technology
Noble metal nano particles has in fields such as catalysis, medicine, analysis and biologies widely to be used.Developed at present the method for multiple synthetic single metal nanoparticle, ElSayed MA reported the synthetic of metal platinum nano-particle in 1996 on the Science magazine, this method is dispersant with the polymer, has obtained monodispersed nano platinum particle colloidal solution (science with hydrogen reducing metal platinum ion under inert gas shielding, 1996,272:1924); Based on similar method, people such as the domestic Xu Bai of Tsing-Hua University celebrating are that protective agent has prepared cubic metal platinum colloidal solution with the Sodium Polyacrylate, but these class methods can only be applicable to the preparation of liquid phase colloidal solution, synthesizing the very big difficulty (Science Bulletin of existence in batches, 2003,48,1919-1924); People such as Peng XG report synthetic (J.Am.Chem golden, nano platinum particle in 2003 on American Chemical Society's meeting will, Soc, 2003,125:14280), this method is raw material with the soluble metallic salt, has synthesized nano particles such as gold, copper in toluene solvant, and this method has related to the use of a large amount of toluene solvants.In sum, the synthetic method of the domestic and international noble metal nano particles of reporting all is only limited to the synthetic of single kind nano particle at present, and has generally used a large amount of organic solvents to be liquid-phase system, has problems such as environmental pollution.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing single dispersion metal nanometer particles.
The method for preparing single dispersion metal nanometer particles provided by the present invention is that metal ion solution is reacted in the mixed system of alkali metal hydroxide, aliphatic acid and organic polar solvent, obtains single dispersion metal nanometer particles.
Wherein, the step of above-mentioned preparation feedback is: earlier solid alkali metal hydroxide is joined in the mixed solvent of aliphatic acid and organic polar solvent, mix the back and add metal ion solution 20-300 ℃ of reaction down, obtain single dispersion metal nanometer particles.
In the preparation process, the volume ratio of aliphatic acid and organic polar solvent is 1: 0.5-10; The concentration of metal ion solution is 0.01-0.5mol/L, and the volume ratio of metal ion solution and mixed solvent is 1: 0.5-5; The mol ratio of alkali metal hydroxide and metal ion is 1-10: 1.Used metal ion can be gold, silver, palladium, platinum, ruthenium, rhodium or iridium ion etc., can pass through these metal soluble salt, as nitrate, hydrochloride waits provides.Aliphatic acid is oleic acid, stearic acid or capric acid etc.Organic polar solvent is ethanol, acetone, ethylene glycol or glycerine etc.
The present invention constitutes mixed dicyandiamide solution with aliphatic acid and polar solvent, is raw material with soluble metallic salt and alkali metal hydroxide, prepares single dispersion metal nanometer particles.The inventive method is easy, safety, cost is low, applicability is wide, be applicable to the synthetic of multiple noble metal nano particles simultaneously, overcome and adopted cost and the problem of environmental pollution that a large amount of organic solvent brought in the existing synthetic route, the noble metal nano particles that is obtained can be applied to fields such as biology, medicine, catalysis and analysis.
Description of drawings
Fig. 1 is the prepared silver-colored X-ray powder diffraction figure of embodiment 1.
Fig. 2 is that embodiment 1 prepared silver-colored TEM Electronic Speculum detects figure.
Fig. 3 is the prepared golden X-ray powder diffraction figure of embodiment 2.
Fig. 4 is that embodiment 2 prepared golden TEM Electronic Speculum detect figure.
Fig. 5 is the prepared palladium X-ray powder diffraction figure of embodiment 3.
Fig. 6 is that embodiment 3 prepared palladium TEM Electronic Speculum detect figure.
Fig. 7 is the prepared platinum X-ray powder diffraction figure of embodiment 4.
Fig. 8 is that embodiment 4 prepared platinum TEM Electronic Speculum detect figure.
Fig. 9 is the prepared ruthenium X-ray powder diffraction figure of embodiment 5.
Figure 10 is that embodiment 5 prepared ruthenium TEM Electronic Speculum detect figure.
Figure 11 is the prepared rhodium X-ray powder diffraction figure of embodiment 6.
Figure 12 is that embodiment 6 prepared rhodium TEM Electronic Speculum detect figure.
Figure 13 is the prepared iridium X-ray powder diffraction figure of embodiment 7.
Figure 14 is that embodiment 7 prepared iridium TEM Electronic Speculum detect figure.
The specific embodiment
Embodiment 1, single preparation that disperses Nano silver grain
Taking by weighing 0.5g KOH adding 20ml is dissolved with in the stearic ethylene glycol solvent of 5g, fully behind the about 30mins of reaction, taking by weighing 1g again analyzes pure silver nitrate and is dissolved in the 15mL water, and with in the silver ion solution adding mixed solvent that is made into, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 140 ℃ of reaction 24h, the gained precipitation obtains having the avy blue powder of metallic luster after centrifugation, washing, drying.Product is accredited as argent through X-ray powder diffraction as shown in Figure 1; (TEM) carries out morphology analysis to argent with transmission electron microscope, and as can be seen from Figure 2 its pattern is the dispersed nano particle, and particle diameter is between 5-6nm.
The preparation of embodiment 2, monodisperse gold nanometer particle
Taking by weighing 0.5g NaOH adds in the mixed solvent of 10ml oleic acid, 20ml acetone, fully behind the about 30mins of reaction, taking by weighing 0.4g again analyzes pure chlorauride and is dissolved in the 10mL water, and with in the gold ion solution adding mixed solvent that is made into, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 60 ℃ of reaction 24h, the gained precipitation obtains having the dark-brown powder of metallic luster after centrifugation, washing, drying.Product is accredited as metallic gold through X-ray powder diffraction as shown in Figure 3; (TEM) carries out morphology analysis to metallic gold with transmission electron microscope, and as can be seen from Figure 4 its pattern is the dispersed nano particle, and particle diameter is between 5-6nm.
Embodiment 3, single preparation that disperses Pd nano particle
Take by weighing 1gNaOH and add in 5ml capric acid, the 20ml ethanol mixed solvent, fully behind the about 30mins of reaction, take by weighing 0.6g again and analyze pure palladium bichloride and be dissolved in 20ml 0.4molL
-1In the HCl solution, and, stir in the palladium ion solution adding mixed solvent that is made into, place the withstand voltage reactor of stainless steel of 40ml, behind 80 ℃ of reaction 24h, gained precipitates after centrifugation, washing, drying, obtains having the black powder of metallic luster.Product is accredited as Metal Palladium through X-ray powder diffraction as shown in Figure 5; (TEM) carries out morphology analysis to Metal Palladium with transmission electron microscope, and as can be seen from Figure 6 its pattern is the dispersed nano particle, and particle diameter is between 3-4nm.
Embodiment 4, single preparation that disperses nano platinum particle
Taking by weighing 0.5gNaOH adds in 8ml oleic acid, the 15ml ethanol mixed solvent, fully behind the about 30mins of reaction, take by weighing again 0.3g analyze pure potassium chloroplatinate in the 10mL heated in water solution make it the dissolving, and with in the platinum ion solution adding mixed solvent that is made into, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 20 ℃ of reaction 24h, the gained precipitation obtains having the black powder of metallic luster after centrifugation, washing, drying.Product is accredited as metal platinum through X-ray powder diffraction as shown in Figure 7; (TEM) carries out morphology analysis to metal platinum with transmission electron microscope, and as can be seen from Figure 8 its pattern is the dispersed nano particle, and particle diameter is between 3-4nm.
Embodiment 5, single preparation that disperses ruthenium nano particle
Taking by weighing 0.4gNaOH adds in the mixed solvent of 6ml oleic acid, 20ml glycerine, fully behind the about 30mins of reaction, taking by weighing 0.5g again analyzes pure ruthenium trichloride and is dissolved in the 12mL aqueous solution, and with in the ruthenium ion solution adding mixed solvent that is made into, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 180 ℃ of reaction 24h, the gained precipitation obtains having the black powder of metallic luster after centrifugation, washing, drying.Product is accredited as metal Ru through X-ray powder diffraction as shown in Figure 9; (TEM) carries out morphology analysis to metal Ru with transmission electron microscope, and as can be seen from Figure 10 its pattern is the dispersed nano particle, and particle diameter is between 3-4nm.
Embodiment 6, single preparation that disperses the rhodium nano particle
Taking by weighing 0.7gKOH adds in 16ml oleic acid, the 10ml ethanol mixed solvent, fully behind the about 30mins of reaction, taking by weighing 0.4g again analyzes pure rhodium chloride and is dissolved in the 12mL aqueous solution, and with in the rhodium ion solution adding mixed solvent that is made into, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 120 ℃ of reaction 24h, the gained precipitation obtains having the black powder of metallic luster after centrifugation, washing, drying.Product is accredited as metal rhodium through X-ray powder diffraction as shown in Figure 9; (TEM) carries out morphology analysis to metal rhodium with transmission electron microscope, and as can be seen from Figure 10 its pattern is the dispersed nano particle, and particle diameter is between 2-3nm.
Embodiment 7, single preparation that disperses the iridium nano particle
Taking by weighing 0.8gKOH adds in 18ml oleic acid, the 10ml ethanol mixed solvent, fully behind the about 30mins of reaction, taking by weighing 0.9g again analyzes pure iridous chloride and is dissolved in the 10mL aqueous solution, and with in the iridium ion solution adding mixed solvent that is made into, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 160 ℃ of reaction 24h, the gained precipitation obtains having the black powder of metallic luster after centrifugation, washing, drying.Product is accredited as metal iridium through X-ray powder diffraction as shown in Figure 9; (TEM) carries out morphology analysis to metal iridium with transmission electron microscope, and as can be seen from Figure 10 its pattern is the dispersed nano particle, and particle diameter is between 2-3nm.
Claims (5)
1. a method for preparing single dispersion metal nanometer particles is that metal ion solution is reacted in the mixed system of alkali metal hydroxide, aliphatic acid and organic polar solvent, obtains described single dispersion metal nanometer particles; Concrete steps are that elder generation joins solid alkali metal hydroxide in the mixed solvent of aliphatic acid and organic polar solvent, adds metal ion solution after the mixing again, reacts under 20-300 ℃ of condition.
2. method according to claim 1 is characterized in that: the volume ratio of described aliphatic acid and organic polar solvent is 1: 0.5-10; The concentration of described metal ion solution is 0.01-0.5mol/L, and the volume ratio of metal ion solution and mixed solvent is 1: 0.5-5; The mol ratio of described alkali metal hydroxide and described metal ion is 1-10: 1.
3. method according to claim 1 and 2 is characterized in that: described metal ion is gold, silver, palladium, platinum, ruthenium, rhodium or iridium ion.
4. method according to claim 1 and 2 is characterized in that: described aliphatic acid is oleic acid, stearic acid or capric acid.
5. method according to claim 1 and 2 is characterized in that: described organic polar solvent is ethanol, acetone, ethylene glycol or glycerine.
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| KR100790457B1 (en) * | 2006-07-10 | 2008-01-02 | 삼성전기주식회사 | Method for producing metal nanoparticles |
| CN102205421A (en) * | 2010-03-31 | 2011-10-05 | 中国科学院福建物质结构研究所 | Method for preparing gold and silver nanoparticles with hydro-thermal method |
| CN102941350B (en) * | 2012-11-06 | 2015-04-22 | 南京工业大学 | Preparation method of copper nanoparticles |
| CN104439257A (en) * | 2014-12-22 | 2015-03-25 | 江苏博迁新材料有限公司 | Method for fully dispersing 150nm spherical nickel powder in organic solution |
| CN107626294B (en) * | 2017-10-23 | 2020-04-17 | 清华大学 | Preparation method of metal single-atom site catalyst |
Citations (6)
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| EP1175948A2 (en) * | 2000-07-29 | 2002-01-30 | OMG AG & Co. KG | Noble metal nanoparticles, a process for preparing these and their use |
| US6572673B2 (en) * | 2001-06-08 | 2003-06-03 | Chang Chun Petrochemical Co., Ltd. | Process for preparing noble metal nanoparticles |
| CN1442260A (en) * | 2002-03-01 | 2003-09-17 | 中国科学院理化技术研究所 | Preparation method of metallic nano powder |
| CN1463813A (en) * | 2002-06-24 | 2003-12-31 | 中国科学院大连化学物理研究所 | A nano precious metal, method for preparing the same and use thereof |
| US20040180785A1 (en) * | 2003-03-13 | 2004-09-16 | Long Jiang | Method for making monodispersed noble metal nanoparticles supported on oxide substrates |
| WO2005089986A1 (en) * | 2004-03-09 | 2005-09-29 | Osaka Municipal Government | Noble-metal nanoparticles and method for production thereof |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1175948A2 (en) * | 2000-07-29 | 2002-01-30 | OMG AG & Co. KG | Noble metal nanoparticles, a process for preparing these and their use |
| US6572673B2 (en) * | 2001-06-08 | 2003-06-03 | Chang Chun Petrochemical Co., Ltd. | Process for preparing noble metal nanoparticles |
| CN1442260A (en) * | 2002-03-01 | 2003-09-17 | 中国科学院理化技术研究所 | Preparation method of metallic nano powder |
| CN1463813A (en) * | 2002-06-24 | 2003-12-31 | 中国科学院大连化学物理研究所 | A nano precious metal, method for preparing the same and use thereof |
| US20040180785A1 (en) * | 2003-03-13 | 2004-09-16 | Long Jiang | Method for making monodispersed noble metal nanoparticles supported on oxide substrates |
| WO2005089986A1 (en) * | 2004-03-09 | 2005-09-29 | Osaka Municipal Government | Noble-metal nanoparticles and method for production thereof |
Non-Patent Citations (2)
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| A genetal strategy for nanocrystal synthesis. Xun Wang,Jing Zhuang,Qing Peng,Yadong Li.nature,Vol.437 . 2005 |
| A genetal strategy for nanocrystal synthesis. Xun Wang,Jing Zhuang,Qing Peng,Yadong Li.nature,Vol.437 . 2005 * |
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