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Method for preparing nano-silver wire with high length-diameter ratio

A technology of nano-silver wire and high aspect ratio, which is applied in the field of preparation of high-aspect-ratio nano-silver wire, can solve the problems of complex reaction conditions, long dropping time, poor conductivity, etc., and achieve simple preparation process and uniform length Good, easy-to-reproduce effects

Active Publication Date: 2012-10-24
JIANGSU NANOWELL ADVANCED MATERIALS SCI&TECH
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AI Technical Summary

Problems solved by technology

However, the polyol method has the following problems: 1) adopting a peristaltic pump to add silver nitrate and PVP solution simultaneously, the cost is high, and the adding time is long; 2) the preparation of nano-silver with different shapes requires adjustment of the dropping rate; 3 ) The process is complicated, which is not conducive to expanding production
All of the above methods can prepare silver nanowire materials, but the reaction conditions are very complicated, the reaction time is very long, generally takes 2 to 3 hours, the aspect ratio of the prepared silver nanowires is relatively small, and the yield is relatively low. ; or other particles need to be introduced, such as adding platinum nanoparticles as a catalyst during the reaction, resulting in impure products
The microwave method makes it possible to quickly prepare silver nanowire materials. Chinese patents: (1) A method for preparing silver nanowires in large quantities (application number: 200810019828.6), (2) a method for preparing noble metal nanowires in batches (application number For: 200810163102.X) (3) A microwave-assisted method for preparing silver nanostructure materials with different shapes (application number: 200910006131.X) (4) A method for preparing silver nanowires with controllable diameter by cation-controlled microwave method , (Application No.: 201010559335.9) respectively reported the preparation of nano-silver wire materials by microwave-assisted wet chemical method. Although the reported silver nano-wire materials can be prepared, the diameters of the prepared nano-silver wire materials are relatively short , generally no more than 30 microns, and the aspect ratio is relatively small. In this way, when preparing electrode materials, under the same filling rate, the silver nanowires with low aspect ratio will be larger than the silver nanowires with high aspect ratio due to the number of nodes. The number of lines is greatly increased, and its conductivity is an order of magnitude worse

Method used

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  • Method for preparing nano-silver wire with high length-diameter ratio
  • Method for preparing nano-silver wire with high length-diameter ratio
  • Method for preparing nano-silver wire with high length-diameter ratio

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preparation example Construction

[0075] The present invention provides two preparation methods of high aspect ratio nano-silver wires, the first method is: the following substances

[0076] 1) At least one polyhydroxy liquid organic compound;

[0077] 2) Silver nitrate;

[0078] 3) Polyvinylpyrrolidone (PVP) with a K value of 30 or above;

[0079] 4) At least one chloride compound that is soluble in polyhydroxy liquid organic matter and can produce chloride ions after dissolution;

[0080] 5) At least one hydrogen-containing compound, which is soluble in polyhydric liquid organic matter and can generate hydrogen ions after dissolution;

[0081] To form a reaction solution, the amount of the above substances needs to meet the following conditions: the molar concentration of silver nitrate is not higher than 0.1mol / L, the molar concentration of polyvinylpyrrolidone is not higher than 1.0mol / L, and the molar ratio of chloride ions to silver ions is at 1:10000~1:100, the molar ratio of hydrogen ion to silver i...

Embodiment 1

[0130] 1. Prepare the polyhydroxy liquid organic matter solution as follows:

[0131] A: Concentration is the ethylene glycol solution of the silver nitrate of 0.2mol / L;

[0132] B: Ethylene glycol solution with a concentration of 0.4mol / L polyvinylpyrrolidone (PVP, K30);

[0133] 2. Take 1000ml of ethylene glycol solution of silver nitrate prepared above and 1000ml of ethylene glycol solution of polyvinylpyrrolidone (PVP, K30), mix them well, stir them well, and add 37.5% of them under the condition of 60℃ 0.05g of concentrated hydrochloric acid and 0.1g of concentrated nitric acid with a concentration of 65%, continue to stir evenly to form a reaction precursor, and heat the precursor solution by microwave to make it react at a temperature of 155°C for a reaction time of more than 10 minutes, so that The chemical reaction in the solution is completed or partially completed, and the nano-silver wire or the dispersion liquid of the nano-silver wire is obtained after solid-liq...

Embodiment 2

[0135] 1. First, prepare the ethylene glycol solution with the following concentration:

[0136] A: concentration is the silver nitrate ethylene glycol solution of 0.2mol / L;

[0137] B: Ethylene glycol solution of polyvinylpyrrolidone (PVP) with a concentration of 0.4mol / L;

[0138] 2. Take 1000ml of the above-mentioned ethylene glycol solution of polyvinylpyrrolidone (PVP), and add 0.1g of diphenylphosphine chloride and 0.05g of concentrated hydrochloric acid with a concentration of 37.5% to it, mix and stir well to form a mixed solution ;

[0139] 3. Use an oil bath to heat the mixed solution so that the temperature of the solution reaches 120°C, add the standby silver nitrate solution to it, and after the dropwise addition, make the whole solution continue to react at 140°C for more than 60 minutes to make the solution The chemical reaction that takes place is completed to form a solution of silver nanowires, and the silver nanowires or dispersion liquid of silver nanowir...

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Abstract

The invention provides a method for preparing a nano-silver wire with high length-diameter ratio. At least one polyhydroxy liquid organic (1), silver nitrate (2), polyvinylpyrrolidone (PVP) with a K value equal to or larger than 30 (3), at least one hydrogen nitrate compound or one hydrogen-containing compound (4) and at least one chloride for a reaction solution, wherein the chloride can be dissolved in the polyhydroxy liquid organic and can produce chloride ions after dissolved. Reaction is perform for more than 10 minutes under the condition that the reaction temperature is lower than the boiling temperature of the polyhydroxy liquid organic or a part of ingredients is subjected to chemical reaction to form a nano-silver wire solution containing length-diameter ratio exceeding 200, and solid-liquid separation is performed to obtain the nano-silver wire or nano-silver wire dispersing liquid. The nano-silver wire prepared by means of the method is high in length-diameter ratio and yield, few in impurities and good in thickness and length uniformity, and the shortcomings including complicated preparing technology process by means of a traditional polyol method, many impurities and non-uniformity by means of a microwave method and the like are overcome.

Description

technical field [0001] The invention relates to the field of preparation of silver nanomaterials, in particular to a preparation method of nano silver wires with high aspect ratio. Background technique [0002] As an important branch of nanomaterial research, metal nanomaterials are represented by precious metals such as gold, silver, and copper, among which nanosilver has received the most attention because of its broad application prospects. Because nano silver has very stable physical and chemical properties, it has excellent performance in electronics, optics, antibacterial and catalysis, and can be widely used in catalyst materials, battery electrode materials, optical materials, antibacterial materials, coatings, etc. For example, nano-silver has high electrical conductivity and thermal conductivity, so that it can be used as a conductive filler for conductive adhesives. On the basis of obtaining better electrical conductivity, it can greatly reduce the amount of condu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/24C30B29/02C30B29/62C30B7/10
Inventor 姜清奎常振宇丁渐宝
Owner JIANGSU NANOWELL ADVANCED MATERIALS SCI&TECH
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