Preparation method of high performance conductive gold balls with monodispersity

A conductive gold ball, monodisperse technology, applied in metal material coating process, liquid chemical plating, coating and other directions, can solve the problems of plating solution collapse, hydrolysis failure, microsphere agglomeration, etc., and achieve smooth surface gold layer. , the preparation method is simple, the reaction conditions are mild

Inactive Publication Date: 2012-02-15
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are certain defects in this traditional electroless plating pretreatment process. This process requires a large amount of hydrochloric acid for sensitization and activation, and many times of washing with water can remove free chloride ions. The operation is inconvenient, and the sensitization solution is easy to oxidize and dissolve. Hydrolysis fails, and the surface of pre-treated polymer microspheres is sensitized to adsorb some tin ions, which will affect the uniformity and bonding force of the coating (CN100451166C)
After electroless nickel plating, electroless metal plating is a displacement type gold plating, and the replaced metal ions (such as ferrous ions, cobalt ions, nickel ions) in the plating solution will easily cause the aggregation of microspheres; the ion concentration is as high as 10 -3 mol / L will even decompose the plating solution, resulting in the collapse of the plating solution
In addition, most of the gold salts used in the gold plating process are cyanides, which are highly toxic

Method used

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  • Preparation method of high performance conductive gold balls with monodispersity
  • Preparation method of high performance conductive gold balls with monodispersity
  • Preparation method of high performance conductive gold balls with monodispersity

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Add 6.3g of styrene, 1g of polyvinylpyrrolidone, 0.075g of azobisisobutyronitrile, 15g of ethanol, and 1.667g of water into a four-neck flask, stir evenly, and under nitrogen protection, polymerize at 65°C for 24 hours, centrifuge , alcohol washing, vacuum drying;

[0030] (2) Disperse the polymer microspheres in concentrated sulfuric acid at 80°C, treat them with stirring for 30 minutes, wash with water until neutral, add them to an aqueous solution of 0.02M polyethyleneimine (MW=20000) for surface modification, wash;

[0031] (3) Disperse the polymer microspheres in the negatively charged gold sol (dissolve 0.05mmol chloroauric acid, 0.1g polyvinylpyrrolidone, 0.1mmol sodium borohydride in 100mL water) and activate the reaction temperature at 20°C. After ultrasonic reaction for 20 minutes, wash with water, wash with alcohol, and dry in vacuum;

[0032] (4) polymer microspheres after the activation are finally dispersed in the chemical gold plating solution (the ...

Embodiment 2

[0035] (1) Add 6.3g of methyl methacrylate, 0.4g of polyvinylpyrrolidone, 0.25g of azobisisobutyronitrile, and 16g of ethanol into a four-neck flask, stir well, and under nitrogen protection, polymerize at 60°C for 24 hours, centrifuge , alcohol washing, vacuum drying;

[0036] (2) Disperse the polymer microspheres in chlorosulfonic acid at 20°C, treat them under stirring for 10 minutes, wash with water until neutral, and add them to an aqueous solution of 0.01M polyallyl ammonium chloride (MW=70000) to carry out Surface modification, water washing;

[0037] (3) Disperse the polymer microspheres in negatively charged gold sol (dissolve 0.05mmol chloroauric acid, 0.1g polyvinylpyrrolidone, 0.1mmol ascorbic acid in 100mL water) After 40 minutes, wash with water, wash with alcohol, and dry in vacuum;

[0038] (4) polymer microspheres after activation are finally dispersed in chemical gold plating solution (the composition of chemical plating solution: 1.5g / L chloroauric acid, 2...

Embodiment 3

[0040] (1) Add 5g of methyl methacrylate, 0.75g of polyacrylic acid, 0.075g of azobisisobutyronitrile, and 16g of methanol into a four-neck flask, stir evenly, and under nitrogen protection, polymerize at 70°C for 20h, centrifuge, ethanol washing, vacuum drying;

[0041] (2) Disperse the polymer microspheres in chlorosulfonic acid at 60°C, treat them with stirring for 90 minutes, wash with water until neutral, and add them to an aqueous solution of 0.02M polyethyleneimine (MW=20000) for surface modification , washed with water;

[0042] (3) Disperse the polymer microspheres in negatively charged gold sol (dissolve 0.05mmol chloroplatinic acid, 0.1g polyvinylpyrrolidone, 0.08mmol sodium borohydride in 100mL water) and activate the reaction temperature at 50°C. After ultrasonic reaction for 20 minutes, wash with water, wash with alcohol, and dry in vacuum;

[0043](4) polymer microspheres after activation are finally dispersed in chemical gold plating solution (the composition...

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Abstract

The invention relates to a preparation method of high performance conductive gold balls with monodispersity. The method comprises the steps of: (1) adding a monomer, a dispersant, an initiator and a solvent into a reaction container for a reaction of 12-24h so as to obtain polymer microspheres; (2) dispersing the polymer microspheres into a strong acid for treatment, then adding them into a polyelectrolyte aqueous solution with positive electricity; (3) dispersing the microspheres treated in step (2) into a precious metal sol, the surface of which has negative electricity; (4) conducting ultrasonic dispersing to the microspheres treated in step (3) to disperse the microspheres in an electroless gold plating bath, after the reaction, carrying out centrifugation, washing and drying, thus obtaining the high performance conductive gold balls. The method of the invention provides a solution to the problems of tin ion interference, activation under an acidic condition, complex operations and toxicity of electroless gold plating bath etc. in traditional electroless plating activation technologies. With simple preparation process, the method provided in the invention can be used for batchproduction and has good application prospects.

Description

technical field [0001] The invention belongs to the field of preparation of conductive particles, in particular to a method for preparing monodisperse high-performance conductive gold balls. Background technique [0002] Anisotropic conductive film ACF material mainly includes resin adhesive and conductive particles. The conductive particles are the core part of the ACF material. For some interconnections that require high reliability and stability, conductive particles generally use gold as the conductive shell. Patent CN 100441613C and patent US 2008 / 0078977A1 ​​propose a method for preparing conductive gold balls for ACF, both of which are formed by electroless nickel plating on the surface of polymer microspheres and then electroless gold plating. However, there are certain defects in this traditional electroless plating pretreatment process. This process requires a large amount of hydrochloric acid for sensitization and activation, and many times of washing with water...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C18/44C23C18/28C08F112/08C08F120/14
Inventor 张清华马跃辉任煜栋陈大俊
Owner DONGHUA UNIV
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