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Method for manufacturing metal nanometer particle

A technology of metal nanoparticles and manufacturing methods, applied in the direction of nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problems of easy precipitation, large particle size, poor dispersion, etc., and achieve simplified procedures and particle size evenly distributed effect

Inactive Publication Date: 2010-01-06
DONGJIN SEMICHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] However, the copper particles obtained by the manufacturing method proposed by the Japanese patent are 90-650nm, the particle size is relatively large, the dispersion is poor and easy to precipitate, and the lower sintering temperature required for FPCB manufacturing cannot be realized.
In particular, in the case of using an organic amine, a larger amount of a sugar reducing agent has to be added in order to generate cuprous oxide, so after a complicated reaction process, in the case of a sugar reducing agent, in the case of a high alkalinity Vigorous reactions occur in the solution and it is difficult to control the particle size

Method used

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  • Method for manufacturing metal nanometer particle
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Examples

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Effect test

experiment example 1

[0036] In a solvent mixture consisting of 10ml of ultrapure water, 90ml of ethylene glycol, 5ml of 2-pyrrolidone as a polar solvent, and 4g of polyvinylpyrrolidone (PVP) with a molecular weight of 20,000 or more, dissolve 0.1 mole of Precursor CuSO 4 Finally, 0.2 mol of triethylamine was added and forced stirring was performed until the green mixed solution became a gel-like green substance. Thereafter, 0.1 mol of hydrazine was slowly added over 10 minutes, and forced stirring was performed until the solution turned reddish black or deep red. The reaction temperature at this time was maintained at 25°C.

[0037] Reclaim red and black powder by centrifugation, wash and reclaim several times with acetone and water, and finally mix into metal nano powder 30% by weight and then stored.

[0038] As a result of observing the particle size of the metal nanopowder by SEM, it was confirmed that it had a particle size distribution of 50 to 80 nm.

experiment example 2

[0040] In a solvent mixture consisting of 10 ml of ultrapure water, 90 ml of diethylene glycol, 5 ml of N-methylpyrrolidone as a polar solvent, and 4 g of PVP with a molecular weight of 20,000 or more, dissolve 0.1 mole of CuSO as a metal precursor by forced stirring 4 Finally, 0.1 mol of triethanolamine was added, and forced stirring was performed until the green mixed solution became a gel-like green substance. Thereafter, after raising the temperature of the solution to 50° C., wait for the temperature to stabilize, slowly add 0.1 mol of hydroxylamine in 10 minutes, and perform forced stirring until the solution turns deep red. The crimson powder is recovered by centrifugation, washed and recovered several times with acetone and water, and finally mixed into a metal nano-powder. 30% by weight and then stored.

[0041] As a result of observing the particle size of the metal nanopowder by SEM, it was confirmed that figure 1 Shown has a uniform particle size distribution of ...

experiment example 3

[0043] In a solvent mixture composed of 10 ml of ultrapure water, 90 ml of ethylene glycol, 5 ml of N-methylformamide as a polar solvent, and 4 g of PVP with a molecular weight of 20,000 or more, 0.1 mole of PVP as a metal precursor was dissolved by forced stirring. CuSO 4 Finally, 0.1 mol of diethylamine was added and forced stirring was performed until the green mixed solution became a gel-like green substance. Thereafter, 0.1 mol of 30% hydrazine in an ultrapure aqueous solution was slowly added over 10 minutes, and forced stirring was performed until the solution turned deep red. The crimson powder is recovered by centrifugation, washed and recovered several times with acetone and water, and finally mixed into a metal nano-powder. 30% by weight and then stored.

[0044] As a result of observing the particle size of the metal nanopowder by SEM, it was confirmed that it had a particle size distribution of 50 to 90 nm.

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Abstract

A method for manufacturing metal nanometer replaces two stages (firstly producing cuprous oxide, then producing copper particles by a reducing agent) of a metal particle producing process by one stage, such that it is capable of simplifying the working process obviously, obtaining metal copper particles easily by a short-time reaction at a low temperature (15-60 DEG C), omitting a complicated rinshing process of removing metal salts by secondary rinshing, and particle size dispersion is uniform and there is non requirement of a hierarchical process, thus the method is suitable for lot production. The method includes a first stage of dissolving metal precursor in a dissolvent containing a glycols dissolvent; a second stage of adding organic amine to the prepared solution, stirring until the color of the solution does not change; and a third stage of slowly adding more than one compounds selected from hydrazine derivatives, sodium hypophosphate, hydroxyl amine and sodium borohydride to the solution containing the organic amine of the second stage, so as to deoxidize and precipitate the metal(s).

Description

technical field [0001] The present invention relates to the manufacture method of metal nanoparticle, relate in particular to the manufacture method of such a kind of metal nanoparticle, this method will existing two-stage metal particle generation process (after first generating cuprous oxide, then generate copper particle by reducing agent ) is reduced to one stage, so that the process can be significantly simplified; metal copper particles can be easily obtained through a short-term reaction at low temperature (15-60°C); no complicated water washing process to remove metal salts through secondary water washing; particle size The distribution is uniform and does not require a grading process, so it is suitable for mass production. Background technique [0002] Recently, due to the miniaturization of electronic components and the tendency to use a variety of substrates, it is increasingly required to form thin-film fine wiring by various printing methods. metal particles. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/24
CPCB22F9/24B22F2301/10B22F2304/054B82Y30/00B82Y40/00
Inventor 金柄郁金圣培李圣贤刘炫硕
Owner DONGJIN SEMICHEM CO LTD
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