Method for continuously preparing ultrafine sliver powder on basis of microchannel mixed reaction system

A reaction system and micro-channel technology, applied in the field of preparation of metal ultra-fine powder materials, can solve the problems of large volume production equipment, difficult product precision control, poor batch stability, etc., to improve production efficiency and product batch stability. performance, reduce equipment investment costs, and improve productivity

Active Publication Date: 2014-12-17
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the stirring and mixing chemical reduction method can prepare silver powders of various shapes and sizes, this method has many disadvantages in large-scale production, such as low production efficiency, large-scale production equipment, difficult product precision control, poor batch stability and high production costs. Aspects

Method used

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  • Method for continuously preparing ultrafine sliver powder on basis of microchannel mixed reaction system
  • Method for continuously preparing ultrafine sliver powder on basis of microchannel mixed reaction system
  • Method for continuously preparing ultrafine sliver powder on basis of microchannel mixed reaction system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Build a microchannel mixed reaction system, such as figure 1 shown. The internal diameter of two as transmission microchannel 4 is 3 millimeters, and one end of the latex tube that length is 0.5 meter is connected with an end of two peristaltic pumps 3 respectively, and the other end of described two latex tubes is respectively connected with a loader. The container 1 (material is glass) of oxidizing solution and the container 2 (material is glass) of a loading reducing solution; The other end of described two peristaltic pumps is 3 millimeters respectively as the internal diameter of transmission microchannel 4 respectively, A latex tube with a length of 1 meter is connected with two symmetrical ports of a Y-shaped tee 5 made of glass as a mixing unit of the reactant (the internal diameter of the symmetrical port is 3 millimeters), and the rest of the Y-shaped tee is One interface (inner diameter is 4 millimeters) connects one as the inner diameter of reaction microch...

Embodiment 2

[0045] The microchannel mixed reaction system built is basically the same as the microchannel mixed reaction system in Example 1, except that the inner diameter of the transmission microchannel is 4 millimeters, the inner diameter of the symmetrical interface of the Y-shaped tee is 5 millimeters, and the remaining one interface The inner diameter is 6 mm and the inner diameter of the reaction microchannel is 6 mm.

[0046] Utilize the above-mentioned microchannel mixing reaction system to continuously prepare ultrafine silver particle powder:

[0047] (1) Dissolve 22.5g of silver nitrate in 115ml of deionized water to prepare a silver nitrate solution, add 1.5ml of nitric acid (65-68% mass concentration) into the silver nitrate solution under stirring, and then add 35ml of absolute ethanol , the obtained mixed solution is used as the oxidation solution; 15g of ascorbic acid is dissolved in 150ml of deionized water as the reduction solution; in the container;

[0048] (2) Con...

Embodiment 3

[0051] The microchannel mixed reaction system built is basically the same as the microchannel mixed reaction system in Example 1, except that the internal diameter of the transmission microchannel is 2.5 mm, the length is 2 mm, and the Y-shaped tee is made of stainless steel and three interfaces. With an inner diameter of 2.5 mm, the reaction microchannel has an inner diameter of 3 mm and a length of 1.5 meters.

[0052] Utilize the above-mentioned microchannel mixed reaction system to continuously prepare ultra-fine silver powder:

[0053] (1) Dissolve 7.5g of silver nitrate in 120ml of deionized water to prepare a silver nitrate solution, add 1.5ml of nitric acid (65-68% mass concentration) into the silver nitrate solution under stirring, and then add 30ml of absolute ethanol , the obtained mixed solution is used as the oxidation solution; 15g of ascorbic acid is dissolved in 150ml of deionized water as the reduction solution; in the container;

[0054] (2) Control the tem...

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Abstract

The invention belongs to the field of preparation of metal ultrafine powder materials and particularly relates to a method for continuously preparing ultrafine sliver powder on the basis of a microchannel mixed reaction system. According to the method, an oxidation solution containing soluble silver salt and nitric acid and a reduction solution containing ascorbic acid or sodium ascorbate are continuously conveyed to the microchannel mixed reaction system respectively through driving devices, mixing is carried out in a Y-type tee joint or a tee joint in the microchannel mixed reaction system, wherein the Y-type tee joint or the tee joint serves as a mixing unit of reactive materials, the mixed solutions flow out of reaction microchannels after being subjected to a reaction in the reaction microchannels in the microchannel mixed reaction system, standing is carried out on obtained reaction products, washing and sediment are carried out on the products, and ultrafine sliver powder of different morphologies and sizes can be obtained after suction filtration and drying. According to the method, control over the crystallization morphologies and the sizes of ultrafine sliver powder particle products can be achieved by adjusting the components of the oxidation solution, the components of the reduction solution, the molar concentration, the temperature and other parameters.

Description

technical field [0001] The invention belongs to the field of preparation of metal ultrafine powder materials, and in particular relates to a method for continuously preparing ultrafine silver powder based on a microchannel mixed reaction system. Background technique [0002] Due to its excellent electrical properties, metal ultrafine silver powder materials are widely used as electrode materials for solar cells, membrane switches, semiconductor chips, etc., as well as conductive fillers in conductive adhesives, conductive inks, and electromagnetic shielding coatings. The traditional preparation methods of metal ultrafine silver powder include thermal decomposition method, atomization method, electrochemical method and chemical reduction method. At present, stirring and mixing chemical reduction preparation methods are mostly used, mainly using glass containers such as beakers or reaction kettles as reaction vessels, and using electromagnetic or mechanical stirring to quickly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/24
Inventor 刘春艳聂士东张志颖
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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