CN113059155B - Preparation method of nickel-coated graphite composite powder material for conductive silica gel - Google Patents
Preparation method of nickel-coated graphite composite powder material for conductive silica gel Download PDFInfo
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- CN113059155B CN113059155B CN202110301151.0A CN202110301151A CN113059155B CN 113059155 B CN113059155 B CN 113059155B CN 202110301151 A CN202110301151 A CN 202110301151A CN 113059155 B CN113059155 B CN 113059155B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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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
- C23C18/16—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 reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
- C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
- C23C18/1886—Multistep pretreatment
- C23C18/1893—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
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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
- C23C18/16—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 reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
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Abstract
The invention discloses a preparation method of a nickel-coated graphite composite powder material for conductive silica gel. The preparation process comprises the following steps: 1) removing oil on the surface of graphite powder, cleaning, filtering and drying; 2) activating the cleaned graphite powder, cleaning, filtering and drying; 3) and (3) putting the graphite powder treated in the step 2) into a chemical plating solution, performing chemical plating, performing suction filtration, washing and drying to obtain the nickel-coated graphite composite powder material for conductive silica gel. The preparation process is simple and convenient, and the prepared nickel-coated graphite composite powder has good coating effect and high production efficiency, and is suitable for large-scale industrial production.
Description
Technical Field
The invention belongs to the field of preparation of nickel-coated graphite composite powder materials, and particularly relates to a preparation method of a nickel-coated graphite composite powder material for conductive silica gel.
Background
The common conductive filler for the conductive silica gel comprises pure silver powder, silver-coated copper powder, silver-coated aluminum powder, silver-coated glass powder, nickel-coated copper powder, nickel-coated graphite powder and the like. The conductive compound using pure silver powder as a conductive filler has good conductivity and good oxidation resistance, but the range of use of silver particles is limited due to migration and high price. In order to overcome the defects of pure silver powder, conductive composite powder such as silver-coated copper powder, silver-coated aluminum powder, silver-coated glass powder and the like is developed in sequence. However, the price of the silver-containing conductive composite powder is still high, and the silver-containing conductive composite powder does not have magnetic permeability, so the magnetic shielding effect is poor. Since nickel is a metal material having both electrical and magnetic conductivity, nickel has been studied as an inexpensive conductive silica gel filler in recent years.
As a typical carbon material, the graphite has the advantages of high conductivity, light weight, low price, rich reserves and the like, and has an ultra-large diameter-thickness ratio (ratio of diameter to thickness), so that a conductive network can be formed in a polymer, the conductive percolation threshold of a conductive composite material is reduced, and the graphite has a wide application prospect in the aspects of conductive and electromagnetic shielding composite materials. The nickel-coated graphite composite powder material has various excellent performances of graphite and nickel, can improve the conductivity of graphite and endow composite particles with certain magnetism, thereby being expected to widen the electromagnetic shielding frequency range of the conductive composite material.
At present, most of methods for preparing nickel-coated graphite composite powder have the problems of complex process, poor coating effect, low production efficiency, unsuitability for large-scale industrial production and the like. For example: chenzhuchun (patent application No. 201510575644.8) adopts a hydrogen reduction method, but has low production efficiency and high cost, and is not suitable for industrial production, Yangfuhe (patent application No. 201410097071.8) adopts a chemical plating method, but uses toxic stannous chloride, palladium and other noble metal reagents in the sensitization and activation processes, and nickel ions are difficult to directionally deposit on the surface of graphite powder, and the coating is not ideal. The preparation process is simple and convenient, and the prepared nickel-coated graphite composite powder has good coating effect and high production efficiency, and is suitable for large-scale industrial production.
Disclosure of Invention
The invention aims to solve the problems of non-compact coating of a nickel shell layer, complex preparation process and the like of nickel-coated graphite composite particles prepared by the existing method, and provides a preparation method of a nickel-coated graphite composite powder material for conductive silica gel, which comprises the following steps:
step 1, placing graphite powder into a degreasing agent according to the proportion of 1g of graphite powder to 500ml of degreasing agent, and mechanically heating and stirring, wherein the heating temperature is controlled to be 50-70 ℃, and the stirring time is 20-60 min;
step 2, placing the graphite powder subjected to oil removal in the step one into an activation solution, and then pouring a sodium borohydride solution with the mass concentration of 18-20g/L into the activation solution for activation, wherein the activation treatment time is 28-30 min; wherein the activating solution is a nickel acetate methanol solution with the mass concentration of 80-90 g/L; wherein the proportion relationship of the graphite powder, the activating solution and the sodium borohydride solution after oil removal is that 1g of graphite corresponds to 100ml of activating solution and 50ml of sodium borohydride solution.
Step 3, placing the graphite treated in the step two in the prepared chemical plating solution according to the proportion of 1g of graphite powder to 500ml of plating solution, mechanically heating and stirring, controlling the heating temperature at 88-90 ℃, stirring for 80-90min, cleaning and drying; wherein the concentration range of each component in the chemical plating solution is 28-30g/L of nickel sulfate, 15-17ml/L of hydrazine hydrate, and 154-156g/L of potassium sodium tartrate.
Preferably, the particle size of the graphite is 180-200 μm.
Preferably, the degreasing agent is a sodium hydroxide solution with the mass concentration of 10-20 g/L.
Preferably, during the oil removing treatment, the graphite powder is continuously stirred, and the stirring time is 30 r/min.
Preferably, the activating solution is a methanol solution of nickel acetate with the mass concentration of 80-90 g/L.
Preferably, the pH value of the electroless plating solution is 10 to 12.
Compared with the prior art, the invention has the beneficial effects that:
1) the process is simple and convenient, and the prepared nickel-coated graphite composite powder has good coating effect.
2) High production efficiency and is suitable for large-scale industrial production.
Drawings
FIG. 1 is a flow chart of the preparation method of the nickel-coated graphite composite powder material in the method of the invention.
FIG. 2 is an SEM image of a nickel-coated graphite composite powder material in example 3 of the invention.
Fig. 3 is an XRD spectrum of the nickel-coated graphite composite powder material in example 3 of the present invention.
Fig. 4 is an SEM image of the nickel-coated graphite composite powder material in comparative example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the following detailed description of the operation of the present invention is provided with reference to the accompanying drawings and specific examples. It should be understood that the specific examples described herein are intended only to illustrate the present invention, and are not intended to limit the scope of the invention.
Example 1:
the preparation method of the nickel-coated graphite composite powder material for the conductive silica gel comprises the following specific preparation steps:
the particle size of the graphite powder is 180 mu m;
the method comprises the following steps: putting 1g of graphite powder into 500ml of sodium hydroxide solution with the mass concentration of 10g/L, cleaning for 20min at the temperature of 50 ℃, carrying out suction filtration, washing and drying for later use, and stirring the graphite powder continuously at the stirring speed of 30r/min during oil removal treatment;
step two: putting 1g of deoiled graphite powder into 100ml of methanol solution of nickel acetate with the mass concentration of 80g/L, then pouring 50ml of sodium borohydride solution with the mass concentration of 18g/L into the activation solution for activation, activating for 28min, and performing suction filtration, washing and vacuum drying for later use;
step three: preparing chemical plating solution, taking 14g of nickel sulfate, 7.5ml of hydrazine hydrate and 77g of potassium sodium tartrate to prepare 500ml of chemical plating solution, taking a proper amount of ammonia water by using a dropper to be dripped into the plating solution, changing the color from green to blue, and adjusting the pH value of the plating solution to 12 by using a pH meter.
Step four: and (3) placing 500ml of chemical plating solution into a three-neck flask, heating to 90 ℃, adding 1g of activated graphite particles, reacting for 90min under the condition of stirring, performing suction filtration, washing and drying for later use to obtain the nickel-coated graphite composite powder.
Example 2:
the preparation method of the nickel-coated graphite composite powder material for the conductive silica gel comprises the following specific preparation steps:
the particle size of the graphite powder is 190 mu m;
the method comprises the following steps: putting 1g of graphite powder into 500ml of sodium hydroxide solution with the mass concentration of 15g/L, cleaning for 40min at the temperature of 60 ℃, carrying out suction filtration, washing and drying for later use, and stirring the graphite powder continuously at the stirring speed of 30r/min during oil removal treatment;
step two: 1g of graphite powder after oil removal is placed in 100ml of methanol solution of nickel acetate with the mass concentration of 85g/L, 50ml of sodium borohydride solution with the mass concentration of 18g/L is poured into the activation solution for activation for 29min, and the activation solution is subjected to suction filtration, washing and vacuum drying for later use;
step three: preparing chemical plating solution, preparing 500ml chemical plating solution by taking 14.5g nickel sulfate, 8ml hydrazine hydrate and 77.5g potassium sodium tartrate, dropwise adding a proper amount of ammonia water into the plating solution by using a dropper, wherein the color is changed from green to blue, and adjusting the pH value of the plating solution to be about 12 by using a pH meter.
Step four: and (3) placing 500ml of chemical plating solution into a three-neck flask, heating to 90 ℃, adding 1g of activated graphite particles, reacting for 90min under the condition of stirring, performing suction filtration, washing and drying for later use to obtain the nickel-coated graphite composite powder.
Example 3:
the preparation method of the nickel-coated graphite composite powder material for the conductive silica gel comprises the following specific preparation steps:
the particle size of the graphite powder is 200 mu m;
the method comprises the following steps: putting 1g of graphite powder into 500ml of sodium hydroxide solution with the mass concentration of 20g/L, cleaning for 60min at the temperature of 70 ℃, carrying out suction filtration, washing and drying for later use, and stirring the graphite powder continuously at the stirring speed of 30r/min during oil removal treatment;
step two: putting 1g of graphite powder after oil removal into 100ml of methanol solution of nickel acetate with the mass concentration of 90g/L, then pouring 50ml of sodium borohydride solution with the mass concentration of 18g/L into the activation solution for activation for 30min, and performing suction filtration, washing and vacuum drying for later use;
step three: preparing chemical plating solution, taking 15g of nickel sulfate, 9ml of hydrazine hydrate and 78g of potassium sodium tartrate to prepare 500ml of chemical plating solution, taking a proper amount of ammonia water by using a dropper to be dripped into the plating solution, changing the color from green to blue, and adjusting the pH value of the plating solution to be 12 by using a pH meter.
Step four: and (3) putting 500ml of chemical plating solution into a three-neck flask, heating to 90 ℃, adding 1g of activated graphite particles, reacting for 90min under the condition of stirring, performing suction filtration, washing and drying for later use to obtain the nickel-coated graphite composite powder.
Comparative example 1:
the preparation method of the nickel-coated graphite composite powder material for the conductive silica gel comprises the following specific preparation steps:
the particle size of the graphite powder is 200 mu m;
the method comprises the following steps: putting 1g of graphite powder into 500ml of sodium hydroxide solution with the mass concentration of 20g/L, cleaning for 60min at the temperature of 70 ℃, carrying out suction filtration, washing and drying for later use, and stirring the graphite powder continuously at the stirring speed of 30r/min during oil removal treatment;
step two: preparing chemical plating solution, taking 15g of nickel sulfate, 9ml of hydrazine hydrate and 78g of potassium sodium tartrate to prepare 500ml of chemical plating solution, taking a proper amount of ammonia water by using a dropper to be dripped into the plating solution, changing the color from green to blue, and adjusting the pH value of the plating solution to be 12 by using a pH meter.
Step three: and (3) placing 500ml of chemical plating solution into a three-neck flask, heating to 90 ℃, adding 1g of activated graphite particles, reacting for 90min under the condition of stirring, performing suction filtration, washing and drying for later use to obtain the nickel-coated graphite composite powder.
The nickel-coated graphite powder directly subjected to chemical plating without activation has poor plating effect, only part of the graphite surface has granular nickel, and most of the graphite has no nickel deposition. The main reason is that the graphite surface is less active and nickel particles are difficult to deposit on its surface.
Claims (5)
1. A preparation method of a nickel-coated graphite composite powder material for conductive silica gel is characterized by comprising the following steps:
step 1, placing graphite powder into a degreasing agent according to the proportion of 1g of graphite powder to 500ml of degreasing agent, and mechanically heating and stirring, wherein the heating temperature is controlled to be 50-70 ℃, and the stirring time is 20-60 min;
step 2, placing the graphite powder subjected to oil removal in the step 1 into an activation solution, and then pouring a sodium borohydride solution with the mass concentration of 18-20g/L into the activation solution for activation, wherein the activation treatment time is 28-30 min; wherein the activating solution is a nickel acetate methanol solution with the mass concentration of 80-90 g/L; wherein the proportion relation of the graphite powder, the activating solution and the sodium borohydride solution after oil removal is that 1g of graphite corresponds to 100ml of activating solution and 50ml of sodium borohydride solution;
step 3, placing the graphite treated in the step 2 into the prepared chemical plating solution according to the proportion of 1g of graphite powder to 500ml of plating solution, mechanically heating and stirring, controlling the heating temperature at 88-90 ℃, stirring for 80-90min, cleaning and drying; wherein the concentration range of each component in the chemical plating solution is 28-30g/L of nickel sulfate, 15-17ml/L of hydrazine hydrate, and 154-156g/L of potassium sodium tartrate.
2. The method for preparing the nickel-coated graphite composite powder material for conductive silica gel according to claim 1, wherein the method comprises the following steps: the particle size of the graphite is 180-200 mu m.
3. The method for preparing the nickel-coated graphite composite powder material for conductive silica gel according to claim 1, wherein the method comprises the following steps: the degreasing agent in the step 1 is a sodium hydroxide solution with the mass concentration of 10-20 g/L.
4. The method for preparing the nickel-coated graphite composite powder material for conductive silica gel according to claim 1, wherein the method comprises the following steps: and (2) during oil removal treatment in the step 1, continuously stirring the graphite powder at the stirring speed of 30 r/min.
5. The method for preparing the nickel-coated graphite composite powder material for conductive silica gel according to claim 1, wherein the method comprises the following steps: and 2, the pH value of the chemical plating solution is 10-12.
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