CN102211203A - Method for preparing silver nanoparticles and method for preparing silver nanoparticle array - Google Patents
Method for preparing silver nanoparticles and method for preparing silver nanoparticle array Download PDFInfo
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- CN102211203A CN102211203A CN2010101410880A CN201010141088A CN102211203A CN 102211203 A CN102211203 A CN 102211203A CN 2010101410880 A CN2010101410880 A CN 2010101410880A CN 201010141088 A CN201010141088 A CN 201010141088A CN 102211203 A CN102211203 A CN 102211203A
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Abstract
The invention relates to a method for preparing silver nanoparticles and a method for preparing a silver nanoparticle array with uniform size distribution. The method for preparing the silver nanoparticles comprises the following steps of: mixing one of fatty acid sliver salt, aromatic silver carboxylate and triazole organic silver salt, a reduction accelerator and a stabilizer, namely hydrophobic macromolecular compound solution or aqueous solution of a hydrophilic macromolecular compound, uniformly stirring, performing ball milling by using a ball mill or performing ultrasonic dispersion by using an ultrasonic instrument, adding a reducing agent, controlling the reaction temperature to be between 30 and 60 DEG C with stirring, and performing reduction reaction to obtain dispersion containing the silver nanoparticles. The method for preparing the silver nanoparticle array comprises the following steps of: dispensing the dispersion containing the silver nanoparticles to a carbon-coated copper mesh, drying at room temperature, and self-assembling the silver nanoparticles into the silver nanoparticle array in which the silver nanoparticles are arranged in an ordered mode. By the methods, the silver nanoparticles with a small particle size and uniform size distribution can be prepared, and can be arranged on the carbon-coated copper mesh in a highly ordered mode.
Description
Technical field
The present invention relates to a kind of preparation method of Nano silver grain, and a kind of preparation method of nano grain of silver subarray of even size distribution.
Background technology
Nano silver grain demonstrates unique light, electricity, heat, magnetic property because of having higher specific surface area and surface-active, might obtain extensive use in fields such as nano electron device, effective catalyst, novel conductive and biomedical composite, high-performance conductive inks.
The pattern of nano particle, size, Size Distribution and preparation method are closely related.At present, Nano silver grain has multiple preparation method, and as microemulsion method, reverse micelle method, but these method preparation process are loaded down with trivial details, the control procedure complexity.Chemical reduction method is a kind of preparation method commonly used, and its advantage is that step is simple, and can prepare a large amount of nano particles in the short period of time, but still there are a lot of shortcomings in this method at present, and is big as prepared nano particle diameter, particle size distribution is unequal.
Summary of the invention
The objective of the invention is to overcome the shortcoming that exists among the above-mentioned existing preparation method, a kind of preparation method of the simple to operate and prepared Nano silver grain that the Nano silver grain size is little, particle diameter is evenly distributed is provided, and the method that described Nano silver grain is prepared into the nano grain of silver subarray of orderly arrangement.
The preparation method of Nano silver grain of the present invention is: with a kind of and reduction accelerator in fatty acid silver salt, aromatic carboxylic acid silver salt or the triazole organic silver salts and as the aqueous solution of the hydrophobic polymer compound solution of stabilizing agent or hydrophilic macromolecular compounds and stir, after ball mill ball milling or the ultrasonic dispersion of Ultrasound Instrument (general ball milling or ultrasonic time are 1~4 hour), adding reducing agent and control reaction temperature under stirring is 30 ℃~60 ℃, carry out reduction reaction, obtain containing the dispersion liquid of Nano silver grain.
It is 6 to 22 straight chain and/or branched carboxylic acids root that fatty acid radical in the described fatty acid silver salt is selected from carbon chain lengths.
Aliphatic acid silver in the described fatty acid silver salt is selected from silver stearate, mountain Yu acid silver, laurate is silver-colored, myristic acid is silver-colored, palmitic acid is silver-colored, oleic acid is silver-colored, adipic acid is silver-colored, a kind of in the decanedioic acid silver etc.
Described aromatic carboxylic acid silver salt is selected from a kind of in benzoic acid silver salt, phenylacetic acid silver salt, O-phthalic acid silver salt, tetrachlorophthalic acid silver salt, the salicylic acid silver salt etc.
Described triazole organic silver salts is selected from a kind of in BTA silver salt, the methyl benzotriazazole silver salt etc.
Described reduction accelerator is selected from a kind of in phthalazines, succinimide, phthalimide, the triphenyl phosphorus etc., and the addition of reduction accelerator is 5%~100% of fatty acid silver salt, aromatic carboxylic acid silver salt or a triazole organic silver salts molal quantity.
Described hydrophobic polymer compound solution is dissolved in the organic solvent by the hydrophobic polymer compound and obtains; Described organic solvent is selected from a kind of in ethanol, propyl alcohol, n-butanol, the n-amyl alcohol etc.; Described hydrophobic polymer compound is selected from a kind of in polyvinyl formal, the polyvinyl butyral resin etc.; The consumption of described hydrophobic polymer compound is preferably 0.5%~20% of fatty acid silver salt, aromatic carboxylic acid silver salt or triazole organic silver salts quality.
The described hydrophilic macromolecular compounds aqueous solution is dissolved in the deionized water by hydrophilic macromolecular compounds and obtains; Described hydrophilic macromolecular compounds is selected from a kind of in polyvinyl alcohol, polyacrylic acid, the polyethylene pyrrole network alkane ketone etc.; The consumption of described hydrophilic macromolecular compounds is preferably 5%~40% of fatty acid silver salt, aromatic carboxylic acid silver salt or triazole organic silver salts quality.
Described reducing agent is selected from a kind of in the phenolic compound shown in gallic acid, pyrogallic acid, hydroquinones, monoethanolamine, diethanol amine, triethanolamine, water and hydrazine, ascorbic acid, following formula 1 or the formula 2;
Formula 1
Formula 2
In the formula, R is that hydrogen atom or carbon atom quantity are 1~5 alkyl, and L is methylene or ethylidene,
Described reducing agent consumption is 1%~50% of fatty acid silver salt, aromatic carboxylic acid silver salt or a triazole organic silver salts molal quantity.
The present invention also provides a kind of preparation method of nano grain of silver subarray, and this method is that the dispersant liquid drop that contains Nano silver grain with above-mentioned preparation is coated in and covers on the carbon copper mesh, and after the drying at room temperature, Nano silver grain is self-assembled into the nano grain of silver subarray of orderly arrangement.
In the present invention, fatty acid silver salt, aromatic carboxylic acid silver salt or triazole organic silver salts are reduced into the method for Nano silver grain and the method for the nano grain of silver subarray that preparation is arranged in order, simple to operate, need not special test equipment, the reaction condition gentleness, by transmission electron microscope observing, gained Nano silver grain size is little and be evenly distributed, particle size is about 5nm, and the nano grain of silver subarray of the orderly arrangement of preparing has been realized the high-sequential arrangement.
Description of drawings
Fig. 1 is the transmission electron microscope photo of the Nano silver grain of the embodiment of the invention 1;
Fig. 2 is the transmission electron microscope photo of the nano grain of silver subarray of the embodiment of the invention 1.
The specific embodiment
The present invention is described in detail below in conjunction with embodiment and accompanying drawing.
Embodiment 1
Take by weighing silver stearate 10g, take by weighing triphenyl phosphorus by 5% of silver stearate molal quantity; Take by weighing 0.05g polyvinyl butyral resin (Xing Jin chemical plant, Beijing, butyraldehyde base content 40~50%, viscosity 80~100 seconds) and be dissolved in the 9.95g n-butanol by 0.5% of silver stearate quality, be mixed with the butanol solution of polyvinyl butyral resin; In the solution that the silver stearate that taken by weighing and triphenyl phosphorus are joined the polyvinyl butyral resin of being prepared and stir; Use then the planetary gear ball mill (Nanjing Univ. Instrument Factory, QM-ISP-2-CL) ball milling disperseed 1 hour; Add gallic acid and stir by 1% of silver stearate molal quantity; Under the mixing speed of 3500rpm, the control reaction temperature is 60 ℃, reacts 1 hour, can obtain containing the dispersion liquid of Nano silver grain; Filter, can obtain Nano silver grain.Get dispersant liquid drop that above-mentioned 1ml contains Nano silver grain be coated in cover the carbon copper mesh (the auspicious technology in Beijing emerging hundred Co., Ltd, G300-Cu) on, after the drying at room temperature, Nano silver grain just is self-assembled into the silver-colored nano-array of orderly arrangement.(the FDAC electronics, JEM2100) photo as shown in Figure 1 and Figure 2 for the prepared Nano silver grain and the transmission electron microscope of silver-colored nano-array.
Embodiment 2
Take by weighing silver stearate 10g, take by weighing triphenyl phosphorus by 100% of silver stearate molal quantity; Take by weighing 2g polyvinyl butyral resin (Xing Jin chemical plant, Beijing, butyraldehyde base content 40~50%, viscosity 80~100 seconds) and be dissolved in the 8g n-butanol by 20% of silver stearate quality, be mixed with the butanol solution of polyvinyl butyral resin; In the solution that the silver stearate that taken by weighing and triphenyl phosphorus are joined the polyvinyl butyral resin of being prepared and stir; Use planetary gear ball mill (the same) ball milling to disperse then 4 hours; Add catechol and stir by 50% of silver stearate molal quantity; Under the mixing speed of 3500rpm, the control reaction temperature is 30 ℃, reacts 3 hours, can obtain containing the dispersion liquid of Nano silver grain; Filter, can obtain Nano silver grain.Get dispersant liquid drop that above-mentioned 1ml contains Nano silver grain and be coated in and cover on the carbon copper mesh (the same), after the drying at room temperature, Nano silver grain just is self-assembled into the silver-colored nano-array of orderly arrangement.
Embodiment 3
Take by weighing silver stearate 10g, take by weighing triphenyl phosphorus by 50% of silver stearate molal quantity; Take by weighing 0.5g polyvinyl butyral resin (Xing Jin chemical plant, Beijing, butyraldehyde base content 40~50%, viscosity 80~100 seconds) and be dissolved in the 9.5g n-butanol by 5% of silver stearate quality, be mixed with the butanol solution of polyvinyl butyral resin; In the solution that the silver stearate that taken by weighing and triphenyl phosphorus are joined the polyvinyl butyral resin of being prepared and stir; Use the ultrasonic dispersion of Ultrasound Instrument 2 hours then; Add as shown in Equation 2 compound (production of Fluka company) and stir by 10% of silver stearate molal quantity; Under the mixing speed of 3500rpm, the control reaction temperature is 40 ℃, and simultaneously ultrasonic its reaction 1 hour that makes can obtain containing the dispersion liquid of Nano silver grain; Filter, can obtain Nano silver grain.Get dispersant liquid drop that above-mentioned 1ml contains Nano silver grain and be coated in and cover on the carbon copper mesh (the same), after the drying at room temperature, Nano silver grain just is self-assembled into the silver-colored nano-array of orderly arrangement.
Embodiment 4
Take by weighing the silver-colored 2g of mountain Yu acid, take by weighing phthalimide by 25% of the silver-colored molal quantity of mountain Yu acid; Take by weighing 0.5g polyacrylic acid (number-average molecular weight 2000) and be dissolved in the 9.5g deionized water by 25% of the silver amount of mountain Yu acid, be mixed with the polyacrylic aqueous solution; Join the mountain Yu that taken by weighing acid silver and phthalimide in the polyacrylic aqueous solution of being prepared and stir; Disperseed 3 hours with planetary gear ball mill ball milling then; Add pyrogallic acid and stir by 5% of the silver-colored molal quantity of mountain Yu acid; Under the mixing speed of 3500rpm, the control reaction temperature is 30 ℃, and simultaneously ultrasonic its reaction 2 hours that make can obtain containing the dispersion liquid of Nano silver grain; Filter, can obtain Nano silver grain.Get dispersant liquid drop that above-mentioned 1ml contains Nano silver grain and be coated in and cover on the carbon copper mesh (the same), after the drying at room temperature, Nano silver grain just is self-assembled into the silver-colored nano-array of orderly arrangement.
Embodiment 5
Take by weighing adipic acid silver 5g, take by weighing succinimide by 10% of the silver-colored molal quantity of mountain Yu acid, (average degree of polymerization is 1788+50, chemical pure to take by weighing the 2g polyvinyl alcohol by 40% of the silver amount of adipic acid, Xu Dong chemical plant, Beijing) and be dissolved in the 18g deionized water, be mixed with the aqueous solution of polyvinyl alcohol; Join the adipic acid silver that taken by weighing and succinimide in the polyvinyl alcohol water solution of being prepared and stir; Used the ball mill ball milling then 2 hours; Add triethanolamine and stir by 100% of adipic acid silver molal quantity; Under the mixing speed of 3500rpm, the control reaction temperature is 50 ℃, and simultaneously ultrasonic its reaction 2 hours that make can obtain containing the dispersion liquid of Nano silver grain; Filter, can obtain Nano silver grain.Get dispersant liquid drop that above-mentioned 1ml contains Nano silver grain and be coated in and cover on the carbon copper mesh (the same), after the drying at room temperature, Nano silver grain just is self-assembled into the silver-colored nano-array of orderly arrangement.
Embodiment 6
Take by weighing phthalic acid silver 5g, take by weighing triphenyl phosphorus by 50% of phthalic acid silver molal quantity; Take by weighing the 0.25g polyvinyl alcohol and be dissolved in the 4.75g deionized water by 5% of the silver amount of phthalic acid, be mixed with the aqueous solution of polyvinyl alcohol; In the aqueous solution that the phthalic acid silver that taken by weighing and triphenyl phosphorus are joined the polyvinyl alcohol of being prepared and stir; Used the ball mill ball milling then 3 hours; Add pyrogallic acid and stir by 10% of phthalic acid silver molal quantity; Under the mixing speed of 3500rpm, the control reaction temperature is 30 ℃, and simultaneously ultrasonic its reaction 3 hours that make can obtain containing the dispersion liquid of Nano silver grain; Filter, can obtain Nano silver grain.Get dispersant liquid drop that above-mentioned 1ml contains Nano silver grain and be coated in and cover on the carbon copper mesh (the same), after the drying at room temperature, Nano silver grain just is self-assembled into the silver-colored nano-array of orderly arrangement.
Embodiment 7
Take by weighing BTA silver 2g, take by weighing triphenyl phosphorus by 80% of BTA silver molal quantity; Take by weighing 0.1g polyvinyl alcohol (average degree of polymerization is 1788 ± 50, chemical pure, Xu Dong chemical plant, Beijing) and be dissolved in the deionized water of 9.9g by 5% of the silver amount of BTA, be mixed with the aqueous solution of polyvinyl alcohol; In the aqueous solution that the BTA silver that taken by weighing and triphenyl phosphorus are joined the polyvinyl alcohol of being prepared and stir; Used the ball mill ball milling then 3 hours; Add pyrogallic acid and stir by 15% of BTA silver molal quantity; Under the mixing speed of 4000rpm, the control reaction temperature is 60 ℃, and simultaneously ultrasonic its reaction 3 hours that make can obtain containing the dispersion liquid of Nano silver grain; Filter, can obtain Nano silver grain.Get dispersant liquid drop that above-mentioned 1ml contains Nano silver grain and be coated in and cover on the carbon copper mesh (the same), after the drying at room temperature, Nano silver grain just is self-assembled into the silver-colored nano-array of orderly arrangement.
Embodiment 8
Take by weighing methyl benzotriazazole silver 2g, take by weighing triphenyl phosphorus by 100% of methyl benzotriazazole silver molal quantity; Take by weighing 0.2g polyvinyl alcohol (average degree of polymerization is 1788 ± 50, chemical pure, Xu Dong chemical plant, Beijing) and be dissolved in the 9.8g deionized water by 10% of the silver amount of methyl benzotriazazole, be mixed with the aqueous solution of polyvinyl alcohol; In the aqueous solution that the methyl benzotriazazole silver that taken by weighing and triphenyl phosphorus are joined the polyvinyl alcohol of being prepared and stir; Used the ball mill ball milling then 4 hours; Add pyrogallic acid and stir by 20% of BTA silver molal quantity; Under the mixing speed of 3700rpm, the control reaction temperature is 60 ℃, and simultaneously ultrasonic its reaction 4 hours that make can obtain containing the dispersion liquid of Nano silver grain; Filter, can obtain Nano silver grain.Get dispersant liquid drop that above-mentioned 1ml contains Nano silver grain and be coated in and cover on the carbon copper mesh (the same), after the drying at room temperature, Nano silver grain just is self-assembled into the silver-colored nano-array of orderly arrangement.
Claims (9)
1. the preparation method of a Nano silver grain, it is characterized in that: with a kind of and reduction accelerator in fatty acid silver salt, aromatic carboxylic acid silver salt or the triazole organic silver salts and as the aqueous solution of the hydrophobic polymer compound solution of stabilizing agent or hydrophilic macromolecular compounds and stir, after ball mill ball milling or the ultrasonic dispersion of Ultrasound Instrument, adding reducing agent and control reaction temperature under stirring is 30 ℃~60 ℃, carry out reduction reaction, obtain containing the dispersion liquid of Nano silver grain.
2. the preparation method of Nano silver grain according to claim 1 is characterized in that: it is 6 to 22 straight chain and/or branched carboxylic acids root that the fatty acid radical in the described fatty acid silver salt is selected from carbon chain lengths;
Aliphatic acid silver in the described fatty acid silver salt is selected from silver stearate, mountain Yu acid silver, laurate is silver-colored, myristic acid is silver-colored, palmitic acid is silver-colored, oleic acid is silver-colored, adipic acid is silver-colored, a kind of in silver-colored of decanedioic acid.
3. the preparation method of Nano silver grain according to claim 1 is characterized in that: described aromatic carboxylic acid silver salt is selected from a kind of in benzoic acid silver salt, phenylacetic acid silver salt, O-phthalic acid silver salt, tetrachlorophthalic acid silver salt, the salicylic acid silver salt.
4. the preparation method of Nano silver grain according to claim 1 is characterized in that: described triazole organic silver salts is selected from a kind of in BTA silver salt, the methyl benzotriazazole silver salt.
5. the preparation method of Nano silver grain according to claim 1 is characterized in that: described reduction accelerator is selected from a kind of in phthalazines, succinimide, phthalimide, the triphenyl phosphorus; The addition of reduction accelerator is 5%~100% of fatty acid silver salt, aromatic carboxylic acid silver salt or a triazole organic silver salts molal quantity.
6. the preparation method of Nano silver grain according to claim 1, it is characterized in that: described hydrophobic polymer compound solution is dissolved in the organic solvent by the hydrophobic polymer compound and obtains, and described organic solvent is selected from a kind of in ethanol, propyl alcohol, n-butanol, the n-amyl alcohol; Described hydrophobic polymer compound is selected from a kind of in polyvinyl formal, the polyvinyl butyral resin; The consumption of described hydrophobic polymer compound is 0.5%~20% of fatty acid silver salt, aromatic carboxylic acid silver salt or a triazole organic silver salts quality.
7. the preparation method of Nano silver grain according to claim 1, it is characterized in that: the described hydrophilic macromolecular compounds aqueous solution is dissolved in the deionized water by hydrophilic macromolecular compounds and obtains; Described hydrophilic macromolecular compounds is selected from a kind of in polyvinyl alcohol, polyacrylic acid, the polyethylene pyrrole network alkane ketone; The consumption of described hydrophilic macromolecular compounds is 5%~40% of fatty acid silver salt, aromatic carboxylic acid silver salt or a triazole organic silver salts quality.
8. the preparation method of Nano silver grain according to claim 1 is characterized in that: described reducing agent is selected from a kind of in the phenolic compound shown in gallic acid, pyrogallic acid, hydroquinones, monoethanolamine, diethanol amine, triethanolamine, water and hydrazine, ascorbic acid, following formula 1 or the formula 2;
Formula 1
Formula 2
In the formula, R is that hydrogen atom or carbon atom quantity are 1~5 alkyl, and L is methylene or ethylidene,
Described reducing agent consumption is 1%~50% of fatty acid silver salt, aromatic carboxylic acid silver salt or a triazole organic silver salts molal quantity.
9. the preparation method of a nano grain of silver subarray, it is characterized in that: this method is the prepared dispersant liquid drop that contains Nano silver grain in any one of the claim 1~8 to be coated in cover on the carbon copper mesh, after the drying at room temperature, Nano silver grain is self-assembled into the nano grain of silver subarray of orderly arrangement.
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CN102886527A (en) * | 2012-10-12 | 2013-01-23 | 东华大学 | Method for preparing cubic crystal form nano-silver material by using oleic acid silver as raw material based on oil-water interface method |
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CN104136154A (en) * | 2012-01-11 | 2014-11-05 | 株式会社大赛璐 | Method for producing silver nanoparticles, silver nanoparticles, and silver coating composition |
CN104540622A (en) * | 2012-08-07 | 2015-04-22 | 株式会社大赛璐 | Method for producing silver nano-particles and silver nano-particles |
CN102886527A (en) * | 2012-10-12 | 2013-01-23 | 东华大学 | Method for preparing cubic crystal form nano-silver material by using oleic acid silver as raw material based on oil-water interface method |
CN102896326A (en) * | 2012-10-30 | 2013-01-30 | 东华大学 | Method for preparing cubic crystal type nano-silver material by utilizing oil-water interface method of oleic acid |
CN103302306A (en) * | 2013-06-19 | 2013-09-18 | 东南大学 | Method for reducing and preparing functionalized nano-silver based on polyphenol |
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CN107206490A (en) * | 2015-02-13 | 2017-09-26 | 三菱综合材料株式会社 | The manufacture method of silver powder and paste composition and silver powder |
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CN107084997A (en) * | 2017-04-10 | 2017-08-22 | 中国乐凯集团有限公司 | Silver behenate crystal morphology detection method in a kind of silver salt image forming material |
CN110181074A (en) * | 2019-06-26 | 2019-08-30 | 江苏汇诚医疗科技有限公司 | A kind of method that compound soft template method green prepares high length-diameter ratio silver nanowires |
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