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Palladium-free chemical copper-plating method on graphite nanosheet surface

A technology of nano-graphite microflakes and electroless copper plating, which is applied in liquid chemical plating, metal material coating process, coating, etc., can solve the problems of expensive palladium catalyst, low deposition rate of copper plating, low stability of plating solution, etc. problems, to achieve good mechanical properties, low equipment requirements, and excellent electrical conductivity

Active Publication Date: 2013-12-25
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the expensive palladium catalyst in the past with graphite electroless copper plating, residual SnCl 2 It is also not easy to remove. The complexing agent tartaric acid commonly used in the plating solution makes the deposition rate of copper plating low, the stability of the plating solution is low, and the coating toughness is poor. However, the single use of ethylenediaminetetraacetic acid is expensive as a complexing agent. No Palladium No SnCl 2 The copper plating process activates the surface of the nano-graphite microflakes, and uses a new chemical copper plating formula to plate copper on the surface of the nano-graphite microflakes, and obtains a copper-plated nano-graphite microchip whose volume of copper accounts for 60-80% of the total volume. piece

Method used

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  • Palladium-free chemical copper-plating method on graphite nanosheet surface
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  • Palladium-free chemical copper-plating method on graphite nanosheet surface

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Experimental program
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Effect test

Embodiment 1

[0035] Step 1: Dispersion treatment: Weigh 0.1g of nano-graphite microflakes and ultrasonically disperse them in 50ml of absolute ethanol for 15 minutes, then filter to obtain dispersed nano-graphite microflakes;

[0036] The second step: coarsening treatment: put the nano-graphite microflakes obtained in the first step into 100ml of 20g / L NaOH solution, sonicate at 35°C for 30 minutes, then filter, wash with deionized water until the filtrate is neutral sex;

[0037] The third step: surface hydroxylation treatment: putting the nano-graphite microflakes after the roughening treatment in the second step into 50ml concentration of hydrogen peroxide and 60g / L ammonia solution, and continuously stirring, the reaction temperature is 85°C, the reaction time is 50 minutes, then filter, wash with deionized water until the filtrate is neutral, and obtain nano-graphite microflakes with a large number of hydroxyl groups on the surface;

[0038] The fourth step: activation treatment: wei...

Embodiment 2

[0046] Step 1: Dispersion treatment: Weigh 0.1g of nano-graphite microflakes and ultrasonically disperse them in 50ml of absolute ethanol for 15 minutes, then filter to obtain dispersed nano-graphite microflakes;

[0047] The second step: coarsening treatment: put the nano-graphite microflakes obtained in the first step into 100ml of 20g / L NaOH solution, sonicate at 35°C for 30 minutes, then filter, wash with deionized water until the filtrate is neutral sex;

[0048] The third step: surface hydroxylation treatment: putting the nano-graphite flakes after the roughening treatment in the second step into 50ml concentration of hydrogen peroxide and 80g / L ammonia solution, and continuously stirring, the reaction temperature is 85°C, the reaction time is 50 minutes, then filter, wash with deionized water until the filtrate is neutral, and obtain nano-graphite microflakes with a large number of hydroxyl groups on the surface;

[0049] The fourth step: activation treatment: weigh 0....

Embodiment 3

[0057] Step 1: Dispersion treatment: Weigh 0.2g of nano-graphite microflakes and ultrasonically disperse them in 100ml of absolute ethanol for 20 minutes, then filter to obtain dispersed nano-graphite microflakes;

[0058] The second step: coarsening treatment: put the nano-graphite microflakes obtained in the first step into 200ml of 20g / L NaOH solution, ultrasonicate at 35°C for 35 minutes, then filter, wash with deionized water until the filtrate is neutral sex;

[0059] The third step: surface hydroxylation treatment: putting the nano-graphite flakes after the roughening treatment in the second step into 100ml concentration of hydrogen peroxide and 60g / L ammonia solution, and continuously stirring, the reaction temperature is 85°C, the reaction time is 50 minutes, then filter, wash with deionized water until the filtrate is neutral, and obtain nano-graphite microflakes with a large number of hydroxyl groups on the surface;

[0060] The fourth step: activation treatment: w...

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Abstract

The invention discloses a palladium-free chemical copper-plating method on a graphite nanosheet surface. The palladium-free chemical copper-plating method is characterized in that a graphite nanosheet which is coated with a complete and compact metal copper housing on the surface is finally obtained through dispersing, coarsening, surface hydroxylation, activating, copper plating and passivating in sequence. The graphite nanosheet has a plurality of hydroxyls after surface hydroxylation treatment, and is activated, so that active ions and the graphite nanosheet are combined by chemical bonds, and binding force between a coating and the graphite nanosheet is strong; moreover, a problem that stannous chloride and palladium chloride which are dear and not environment-friendly are used in conventional graphite surface treatment is overcome. Besides, a complexing agent used by copper plating liquid provided by the invention is a composite complexing agent of sodium ethylene diamine tetracetate and citrate, wherein addition of the citrate is 100-400 times the sodium ethylene diamine tetracetate, hardness of the coating is regulated by regulating a proportion of the citrate and the sodium ethylene diamine tetracetate, thereby avoiding only using dear sodium ethylene diamine tetracetate as the complexing agent. The palladium-free chemical copper-plating method disclosed by the invention has environment-friendly effect, is economical and practical, and has good application prospect.

Description

technical field [0001] The invention relates to an electroless copper plating treatment on the surface of nano-graphite microchips and a method for preparing copper-plated nano-graphite microchips, belonging to the technical field of electroless copper plating, and the prepared copper-plated nano-graphite microchips can be used as conductive fillers in composite conductive polymers . Background technique [0002] With the continuous development of science and technology, conductive polymers have become a research hotspot due to their unique electrical and magnetic properties. The conductive polymers widely used at present are filled type, common fillers include metal powder, carbon black, carbon nanotubes, graphite (including graphene), etc. Among many conductive fillers, nano-graphite microflakes are widely used in conductive materials due to their large diameter-thickness ratio, the ability to form a conductive network in the polymer matrix, low price, and abundant reserv...

Claims

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Application Information

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IPC IPC(8): C23C18/40C23C18/18
Inventor 齐暑华杨莎程博马莉娜邱华黄英
Owner NORTHWESTERN POLYTECHNICAL UNIV
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