CN111074243A - Method for plating silver on surface of carbon material - Google Patents
Method for plating silver on surface of carbon material Download PDFInfo
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- CN111074243A CN111074243A CN202010001644.8A CN202010001644A CN111074243A CN 111074243 A CN111074243 A CN 111074243A CN 202010001644 A CN202010001644 A CN 202010001644A CN 111074243 A CN111074243 A CN 111074243A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/04—Pretreatment of the material to be coated
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/08—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of metallic material
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Abstract
The invention relates to a method for plating silver on the surface of a carbon material. Firstly, surface modification is carried out on a carbon material by adopting a surface wetting agent, then a silver salt solution is added, the solution is dried after being uniformly mixed, and the carbon material with silver plated on the surface is obtained by high-temperature thermal reduction in an inert atmosphere. The size range of silver particles in the silver-plated carbon material is 10-600 nm, and the silver content is 15-60 wt.%. The invention simplifies the preparation process, reduces the impurity residues, improves the bonding strength of the coating, enhances the conductivity of the carbon material, and has important application value in the fields of conductive composite materials, electromagnetic shielding materials and the like.
Description
Technical Field
The invention relates to a method for plating silver on the surface of a carbon material, in particular to a method for modifying the surface of the carbon material by adopting maleic anhydride grafted polypropylene, then adding silver salt solution and drying, depositing silver nano particles on the surface of the carbon material through thermal decomposition of silver salt, being used for preparing a high-conductivity carbon material and having important application value in the fields of conductive composite materials, electromagnetic shielding materials and the like.
Background
Carbon materials are widely found in nature and have a variety of allotropes, commonly zero-dimensional fullerenes, one-dimensional carbon nanotubes and carbon fibers, two-dimensional graphene and graphite flakes, and three-dimensional carbon nanocones and nanodiamonds. The carbon material is widely applied to the fields of aerospace, medical instruments, automobiles and the like by virtue of excellent mechanical properties, electrical properties and thermal properties.
With the development of science and technology, the market demand for highly conductive carbon materials is becoming stronger, especially for carbon nanotubes, carbon fibers, graphene, graphite sheets and the like, and silver is the metal with the best conductivity, so that the conductivity of the carbon material can be remarkably improved by plating silver on the surface of the carbon material. The existing methods for plating silver on the surface of a carbon material mainly comprise a chemical plating method, an electroplating method, a light radiation method, a thermal decomposition method and the like. The chemical plating method is mainly characterized in that a carbon material is pretreated through the processes of coarsening, sensitization, activation and the like, then the carbon material is soaked in a silver salt solution, substances such as a reducing agent, a stabilizing agent, a complexing agent and the like are added at the same time, and silver nanoparticles are plated on the surface of the carbon material. The electroplating method mainly uses a carbon material as a cathode, insoluble metal materials such as stainless steel and the like as an anode, silver salt solution as electrolyte, and applies voltage between the electrodes to plate silver on the surface of the carbon material, so that the electroplating method has the advantages of uniform and firm plating layer and the like, but the equipment is more complex and the operation is complicated. The light radiation method mainly comprises the steps of immersing a carbon material into a silver nitrate solution, and then continuously irradiating to decompose silver nitrate to generate silver nanoparticles. The thermal decomposition method is to dip the carbon material into silver salt solution and then to plate silver on the surface of the carbon material through the high-temperature decomposition of silver salt, and has the advantages of simple operation, high silver plating efficiency and the like.
Generally, the surface of the carbon material is smooth, and a chemical bond cannot be formed between the carbon element and the silver element, so that the surface of the carbon material needs to be modified to improve the adsorption of silver. The surface modification methods commonly used at present mainly include a surface oxidation method, a surface coating method, a surface deposition method and the like. The surface oxidation method is mainly characterized in that a gas phase medium or a liquid phase medium is added to enable the surface of the carbon material to generate oxygen-containing functional groups, so that the adsorption of silver ions is improved, and specific oxidation modes comprise gas phase oxidation, liquid phase oxidation, anodic oxidation and the like. The surface coating method is mainly characterized in that a layer of intermediate phase is formed between the surface of the carbon material and silver particles by adding chemical substances, so that the bonding strength between the carbon material and the silver particles is improved, and the specific coating mode comprises a polymer coating, a coupling agent coating and the like. The surface deposition method is to deposit a layer of substance capable of combining with silver particles on the surface of the carbon material by a physical or chemical method so as to improve the adsorption of the silver particles, and the specific deposition mode comprises chemical vapor deposition, surface whisker formation and the like.
Disclosure of Invention
The invention aims to provide a simple and efficient preparation method of silver-plated carbon material aiming at the defects of the prior art.
The solution of the invention is to modify the surface of the carbon material by maleic anhydride grafted polypropylene, adsorb silver ions on the surface of the carbon material by the maleic anhydride grafted polypropylene, and then deposit metal silver particles on the surface of the carbon material by high-temperature calcination and reduction.
In one aspect of the invention, a method for silver plating on the surface of a carbon material is provided, which comprises the following steps:
(1) modification of carbon material: preparing a surface impregnating agent solution, adding a carbon material, and uniformly mixing to obtain a modified carbon material solution;
(2) impregnation and drying of the carbon material: preparing a silver salt solution, then adding the silver salt solution into the modified carbon material solution prepared in the step (1), uniformly mixing, and drying to obtain a silver salt-attached carbon material;
(3) calcining and reducing: and (3) calcining the silver salt-attached carbon material obtained in the step (2) at high temperature in an inert atmosphere, and carrying out thermal reduction to obtain the silver-plated carbon material.
In the technical scheme of the invention, the surface sizing agent is one of maleic anhydride grafted polypropylene, polyvinyl alcohol, polyvinylpyrrolidone or polyvinyl acetate.
In the technical scheme of the invention, the carbon material is one of activated carbon, graphite flakes, natural graphite, expanded graphite, graphene oxide, carbon fibers or carbon nanotubes.
In the technical scheme of the invention, the mass ratio of the carbon material to the surface sizing agent is 0.1-2: 1.
In the technical scheme of the invention, the silver salt is one of silver nitrate, silver carbonate, silver acetate, silver trifluoroacetate or silver sulfate.
In the technical scheme, the mass ratio of the carbon material to the silver salt is 1: 1-16.
In the technical scheme of the invention, the heating rate of high-temperature calcination and thermal reduction in the step (3) is 2-20 ℃/min, the calcination temperature is 500-1000 ℃, and the temperature is kept for 0.5-5 h.
According to the technical scheme, silver nanoparticles are attached to the surface of the silver-plated carbon material, and the size range of the silver nanoparticles is 10-600 nm.
In the technical scheme of the invention, the silver content of the silver-plated carbon material is 15-60 wt.%.
In another aspect of the invention, silver-plated carbon material prepared by the method of the invention is provided.
The chemical reaction formula of the thermal decomposition of the silver nitrate is as follows:
2AgNO3→2Ag+2NO2↑+O2↑
the chemical reaction formula of the thermal decomposition of the silver carbonate is as follows:
2Ag2CO3→4Ag+2CO2↑+O2↑
the chemical reaction formula of the thermal decomposition of the silver acetate is as follows:
2CH3COOAg→2Ag+CH3COOH↑+CO2↑+H2↑+C
the chemical reaction formula of the thermal decomposition of silver trifluoroacetate is as follows:
2CF3COOAg+H2O→2Ag+2CF3COOH↑+O2↑
the chemical reaction formula of the thermal decomposition of the silver sulfate is as follows:
2Ag2SO4→4Ag+2SO3↑+O2↑
detecting the silver content in the silver-plated carbon material: weighing the mass of the carbon material powder before and after silver plating, and calculating by the following formula, namely
Silver content of silver-plated carbon material (mass of silver-plated carbon material-mass of carbon material before plating)/mass of silver-plated carbon material
Advantageous effects
The method is used for preparing the silver-plated carbon material powder, has the characteristics of solid plating layer and less impurity residues, is simple in process, high in efficiency and easy for large-scale preparation, and is expected to be used for industrial production. Compared with the conventional thermal decomposition process, the carbon material is subjected to surface modification in advance, so that the adsorption capacity of the carbon material on silver ions is improved, the combination between silver and the carbon material is improved, and the silver loading is improved. Compared with the chemical reduction method, a large amount of NO is generated at high temperature due to the silver salt and the surface sizing agent2、O2And CO2And the content of residues is low, so that the residues are removed without subsequent treatment, and the cost is reduced.
Drawings
The left image of fig. 1 is a scanning electron micrograph of the graphite sheet of example 1, and the right image of fig. 1 is a scanning electron micrograph of the silver-plated graphite sheet of example 1.
The left image of fig. 2 is a scanning electron micrograph of graphene oxide in example 2, and the right image of fig. 2 is a scanning electron micrograph of silver-plated graphene in example 2.
The left image of fig. 3 is a scanning electron micrograph of the carbon fiber in example 3, and the right image of fig. 3 is a scanning electron micrograph of the silver-plated carbon fiber in example 3.
The left image of fig. 4 is the scanning electron micrograph of the carbon nanotubes in example 4, and the right image of fig. 4 is the scanning electron micrograph of the silver-plated carbon nanotubes in example 4.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, specific embodiments accompanied with figures are described in detail below, but the present invention is not to be construed as limiting the implementable range thereof.
EXAMPLE 1 silver plating of graphite sheet
(1) Modification of graphite flakes: 1g of polyvinylpyrrolidone is added into 49g of deionized water, 5g of graphite flake powder is added after stirring for 10min, and stirring is carried out for 30min at the stirring speed of 400 rpm/min.
(2) Impregnation and drying of graphite flakes: dissolving 5g of silver nitrate in 45g of deionized water, then adding the solution into the mixed solution prepared in the step (1), stirring for 4 hours at the stirring speed of 400rpm/min, and then freeze-drying the solution in a dark environment to constant weight.
(3) Calcining and reducing: and placing the impregnated and dried graphite flake powder into a corundum crucible, placing the corundum crucible into a tube furnace, and heating, calcining and reducing in an argon atmosphere at the heating rate of 10 ℃/min and the calcining temperature of 500 ℃ for 30min to obtain the silver-plated graphite flake powder.
The silver content of the resulting silver-plated graphite sheet was 36 wt.%.
Example 2 graphene oxide silver plating method
(1) Modification of graphene oxide: adding 1g of maleic anhydride grafted polypropylene emulsion into 49g of deionized water, stirring for 10min, adding 100mL of graphene oxide solution, wherein the concentration of the graphene oxide solution is 5g/L, and stirring for 30min at the stirring speed of 400 rpm/min.
(2) Impregnating and drying graphene oxide: dissolving 3g of silver nitrate in 47g of deionized water, then adding the solution into the mixed solution prepared in the step (1), stirring for 4 hours at the stirring speed of 400rpm/min, then heating, stirring and drying the solution to constant weight in a dark environment, wherein the drying temperature is 60 ℃.
(3) Calcining and reducing: and (3) placing the carbon fiber powder after being soaked and dried into a corundum crucible, placing the corundum crucible into a tubular furnace, and heating, calcining and reducing in an argon atmosphere at the heating rate of 10 ℃/min and the calcining temperature of 1000 ℃ for 60min to obtain the silver-plated graphene powder.
The silver content of the obtained silver-plated graphene is 60 wt.%.
Example 3 carbon fiber silver plating method
(1) Modification of carbon fibers: adding 1g of polyvinyl alcohol solution into 49g of deionized water, stirring for 10min, adding 5g of carbon fiber powder, and stirring for 30min at the stirring speed of 400 rpm/min.
(2) Impregnation and drying of carbon fibers: dissolving 10g of silver nitrate into 40g of deionized water, then adding the dissolved silver nitrate into the mixed solution prepared in the step (1), stirring for 4 hours at the stirring speed of 400rpm/min, then heating, stirring and drying the mixed solution in a dark environment to constant weight, wherein the drying temperature is 60 ℃.
(3) Calcining and reducing: and (3) placing the carbon fiber powder after being soaked and dried into a corundum crucible, placing the corundum crucible into a tube furnace, and heating, calcining and reducing in an argon atmosphere at the heating rate of 10 ℃/min and the calcining temperature of 500 ℃ for 30min to obtain the silver-plated carbon fiber powder.
The silver content of the obtained silver-plated carbon fiber was 47 wt.%.
Example 4 carbon nanotube silver plating method
(1) Modification of carbon nanotubes: adding 2g of maleic anhydride grafted polypropylene emulsion into 48g of deionized water, stirring for 10min, adding 0.2g of carbon nanotube powder, and stirring for 30min at the stirring speed of 400 rpm/min.
(2, dipping and drying the carbon nano tube, namely dissolving 3g of silver nitrate in 47g of deionized water, then adding the solution into the mixed solution prepared in the step (1), stirring for 4 hours at the stirring speed of 400rpm/min, then heating, stirring and drying the solution to constant weight in a dark environment, wherein the drying temperature is 60 ℃.
(3) Calcining and reducing: and (3) placing the impregnated and dried carbon nanotube powder into a corundum crucible, placing the corundum crucible into a tube furnace, and heating, calcining and reducing in an argon atmosphere at the heating rate of 5 ℃/min and the calcining temperature of 500 ℃ for 60min to obtain the silver-plated carbon nanotube powder.
The silver content of the obtained silver-plated carbon nanotube was 56 wt.%.
Claims (10)
1. A method for plating silver on the surface of a carbon material comprises the following steps:
(1) modification of carbon material: preparing a surface impregnating agent solution, adding a carbon material, and uniformly mixing to obtain a modified carbon material solution;
(2) impregnation and drying of the carbon material: preparing a silver salt solution, then adding the silver salt solution into the modified carbon material solution prepared in the step (1), uniformly mixing, and drying to obtain a silver salt-attached carbon material;
(3) calcining and reducing: calcining the carbon material with the silver salt obtained in the step (2) at high temperature in an inert atmosphere, and carrying out thermal reduction to obtain a silver-plated carbon material;
the surface sizing agent is one of maleic anhydride grafted polypropylene, polyvinyl alcohol, polyvinylpyrrolidone or polyvinyl acetate.
2. The method for plating silver on a carbon material surface according to claim 1, wherein: the carbon material is one of activated carbon, graphite flakes, natural graphite, expanded graphite, graphene oxide, carbon fibers or carbon nanotubes.
3. The method for plating silver on a carbon material surface according to claim 1, wherein: the mass ratio of the carbon material to the surface wetting agent is 0.1-2: 1.
4. The method for plating silver on a carbon material surface according to claim 1, wherein: the silver salt is one of silver nitrate, silver carbonate, silver acetate, silver trifluoroacetate or silver sulfate.
5. The method for plating silver on a carbon material surface according to claim 1, wherein: the mass ratio of the carbon material to the silver salt is 1: 1-16.
6. The method for plating silver on a carbon material surface according to claim 1, wherein: and (3) heating rates of high-temperature calcination and thermal reduction in the step (3) are 2-20 ℃/min, the calcination temperature is 500-1000 ℃, and the temperature is kept for 0.5-5 h.
7. The method for plating silver on a carbon material surface according to claim 1, wherein: silver nanoparticles are attached to the surface of the silver-plated carbon material, and the size range of the silver nanoparticles is 10-600 nm.
8. A method for plating silver on a carbon material surface according to claim 1, wherein the drying is temperature-raising air-blowing drying, heating stirring drying or freeze drying.
9. The method for plating silver on a carbon material surface according to claim 1, wherein the silver content of the silver-plated carbon material is 15 to 60 wt.%.
10. Silver-plated carbon material obtained by the process according to any one of claims 1 to 9.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114497567A (en) * | 2022-03-07 | 2022-05-13 | 中船重工黄冈水中装备动力有限公司 | Silver/carbon nanotube composite material for aluminum-silver oxide battery and preparation method and application thereof |
| CN114808052A (en) * | 2022-04-02 | 2022-07-29 | 武汉材料保护研究所有限公司 | Cyanide-free conversion method of cyanide silver plating solution |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114497567A (en) * | 2022-03-07 | 2022-05-13 | 中船重工黄冈水中装备动力有限公司 | Silver/carbon nanotube composite material for aluminum-silver oxide battery and preparation method and application thereof |
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