CN118173402A - Silver-graphite-based contact material and preparation method thereof - Google Patents

Silver-graphite-based contact material and preparation method thereof Download PDF

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CN118173402A
CN118173402A CN202410315413.2A CN202410315413A CN118173402A CN 118173402 A CN118173402 A CN 118173402A CN 202410315413 A CN202410315413 A CN 202410315413A CN 118173402 A CN118173402 A CN 118173402A
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graphite
silver
contact material
based contact
powder
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朱振国
白朔
徐红军
成会明
罗川
王硕
钱锡懿
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Institute of Metal Research of CAS
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Institute of Metal Research of CAS
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Abstract

The invention provides a silver graphite-based contact material and a preparation method thereof, and belongs to the technical field of carbon graphite composite materials. Is prepared by the following preparation method: (1) Mixing flake graphite powder, asphalt rubber powder, carbon black and coal asphalt, and sequentially performing pressing, calcining and graphitizing treatment to obtain a graphite matrix; (2) silver-coated casting the graphite matrix to obtain an intermediate; (3) And soaking silver in the intermediate to obtain the silver graphite-based contact material. The invention prepares the silver-graphite-based contact material with the density of 4.8+/-0.3 g/cm 3, the chemical component Ag content of 70wt% +/-5 wt% and the balance C by soaking silver in a graphite matrix. The invention organically combines the good conductivity of the metallic silver with the performances of burning loss resistance, arc extinction and the like of the graphite, thereby preparing the silver-graphite-based contact material with the advantages of high strength, good conductivity, long service life, ablation resistance, good fusion welding resistance and the like.

Description

Silver-graphite-based contact material and preparation method thereof
Technical Field
The invention relates to the technical field of carbon graphite composite materials, in particular to a silver graphite-based contact material and a preparation method thereof.
Background
At present, most of electric contact materials used in the electric appliance industry are mainly silver-based materials, and the electric contact material with the largest domestic application and yield is AgCdO, but because metal cadmium is heavy metal, the electric contact material has toxicity, is easy to volatilize in the processes of material preparation and contact use, and causes environmental pollution.
In order to reduce pollution, the research of Ag-C series electrical contact materials is increasing, and at present, a silver graphite electrical contact is generally prepared by adopting a powder metallurgy method in China, such as: chinese patent (publication numbers CN105506342A and CN 105551859A) uses graphite powder and silver carbonate powder to mix, press and shape in a mould, then obtain silver graphite ingot through procedures of roasting, sintering, and the like, and further process to obtain silver graphite contact material. The graphite content of the silver-graphite contact material prepared by the method is only 1-6wt%, and graphite particles in the material are easy to fall off due to the fact that metallic silver and graphite are not wetted, and the electric contact material is easy to generate an electric arc in the use process and has the risk of fusion welding. Therefore, development of a novel silver-graphite contact material is urgently needed to remedy the defects of the material.
Disclosure of Invention
The invention aims to provide a silver-graphite-based contact material and a preparation method thereof, which are used for solving the problems that graphite particles are easy to fall off when metal silver and graphite are infiltrated, and an electric arc is easy to generate in the use process of the silver-based electrical contact material, so that fusion welding risk is caused.
In order to achieve the above object, the present invention provides the following technical solutions:
The invention provides a preparation method of a silver graphite-based contact material, which is prepared by the following preparation method:
(1) Mixing flake graphite powder, asphalt rubber powder, carbon black and coal asphalt, and sequentially performing pressing, calcining and graphitizing treatment to obtain a graphite matrix;
(2) Silver coating and casting are carried out on the graphite matrix to obtain an intermediate;
(3) And soaking silver in the intermediate to obtain the silver graphite-based contact material.
Preferably, the particle sizes of the flake graphite powder, the asphalt rubber powder and the carbon black in the step (1) are independently 30-50 microns.
Preferably, in the step (1), the mass ratio of the flake graphite powder to the asphalt rubber powder to the carbon black is 50-60:35-45:3-10.
Preferably, in the step (1), the coal tar pitch accounts for 30% -40% of the total mass of the flake graphite powder, the asphalt rubber powder and the carbon black.
Preferably, the calcination temperature in step (1) is 850 to 950 ℃.
Preferably, the graphitization treatment in step (1) is performed at a temperature of 2800 ℃ to 2900 ℃.
Preferably, the temperature of the silver leaching in the step (3) is 1100-1260 ℃, and the heat preservation time for reaching the silver leaching temperature is 0.5-2 h.
Preferably, the pressure of the immersion silver in the step (3) is 50 to 100MPa.
The invention also provides the silver-graphite-based contact material obtained by the preparation method of the silver-graphite-based contact material.
The invention has the following beneficial effects:
1. The invention provides a preparation method of a silver graphite-based contact material, which is prepared by the following preparation method: (1) Mixing flake graphite powder, asphalt rubber powder, carbon black and coal asphalt, and sequentially performing pressing, calcining and graphitizing treatment to obtain a graphite matrix; (2) silver-coated casting the graphite matrix to obtain an intermediate; (3) And soaking silver in the intermediate to obtain the silver graphite-based contact material. The invention firstly designs the components and granularity of the graphite matrix, and prepares the graphite matrix by using the traditional preparation process of the carbon graphite material. The silver metal melted at high temperature and high pressure can fill most of the pores in the graphite matrix by using an advanced hot isostatic pressing silver leaching process, thereby preparing the silver-graphite-based contact material.
2. The invention also provides the silver-graphite-based contact material obtained by the preparation method of the silver-graphite-based contact material. The invention prepares the silver-graphite-based contact material with the density of 4.8+/-0.3 g/cm 3, the chemical component Ag content of 70wt% +/-5 wt% and the balance C by soaking silver in a graphite matrix. The invention organically combines the good conductivity of the metallic silver with the performances of burning loss resistance, arc extinction and the like of the graphite, thereby preparing the silver-graphite-based contact material with the advantages of high strength, good conductivity, long service life, ablation resistance, good fusion welding resistance and the like.
Drawings
Fig. 1 is a microscopic characterization test chart of the silver graphite-based contact material obtained in example 1.
Detailed Description
The invention provides a preparation method of a silver graphite-based contact material, which is prepared by the following preparation method:
(1) Mixing flake graphite powder, asphalt rubber powder, carbon black and coal asphalt, and sequentially performing pressing, calcining and graphitizing treatment to obtain a graphite matrix;
(2) Silver coating and casting are carried out on the graphite matrix to obtain an intermediate;
(3) And soaking silver in the intermediate to obtain the silver graphite-based contact material.
In the invention, flake graphite powder, asphalt rubber powder and carbon black are used as raw materials, and coal pitch is used as a binder.
In the present invention, the particle sizes of the flake graphite powder, the asphalt powder and the carbon black in the step (1) are independently preferably 30 to 50 micrometers, more preferably 35 to 45 micrometers, and even more preferably 38 to 42 micrometers.
In the invention, asphalt rubber powder is prepared by calcining coal asphalt, forming, crushing, grinding and sieving.
In the present invention, the mass ratio of the flake graphite powder, the asphalt powder and the carbon black in the step (1) is preferably 50-60:35-45:3-10, and more preferably 52-58: 37 to 43:4 to 9, more preferably 54 to 56:39 to 41:5 to 8.
In the present invention, the coal pitch in the step (1) preferably accounts for 30 to 40% of the total mass of the flake graphite powder, the asphalt cement powder and the carbon black, more preferably 32 to 38%, and even more preferably 34 to 36%.
In the present invention, the mixing in the step (1) is preferably performed by uniformly kneading the flake graphite powder, the asphalt powder, the carbon black and the coal pitch.
In the present invention, the temperature of the calcination in the step (1) is preferably 850 to 950 ℃, more preferably 870 to 930 ℃, and still more preferably 890 to 910 ℃.
In the present invention, the graphitization treatment in step (1) is preferably performed at a temperature of 2800℃to 2900℃and more preferably 2820℃to 2880℃and still more preferably 2840℃to 2860 ℃.
In the invention, the specific process in the step (2) is as follows:
And (3) placing the graphite matrix into a graphite mold, and casting in an intermediate frequency induction furnace by adopting a corresponding positioning mechanism, so that the metal silver is uniformly coated around the graphite matrix.
In the invention, the specific steps of the silver leaching in the step (3) are as follows: putting the silver-coated graphite ingot prepared in the step (2) into a hot isostatic pressing machine, immersing silver at a set temperature and pressure, preserving heat and pressure, cooling to room temperature along with a furnace, and processing to obtain a silver-graphite-based contact material
In the present invention, the temperature of the immersion silver in the step (3) is preferably 1100 to 1260 ℃, more preferably 1130 to 1240 ℃, still more preferably 1150 to 1220 ℃, and the holding time to reach the immersion silver temperature is preferably 0.5 to 2 hours, more preferably 1 to 1.5 hours, still more preferably 1.2 to 1.3 hours.
In the present invention, the pressure of the immersion silver in the step (3) is preferably 50 to 100MPa, more preferably 60 to 90MPa, and still more preferably 70 to 80MPa.
The invention firstly designs the components and granularity of the graphite matrix, and prepares the graphite matrix by using the traditional preparation process of the carbon graphite material. The silver metal melted at high temperature and high pressure can fill most of the pores in the graphite matrix by using an advanced hot isostatic pressing silver leaching process, thereby preparing the silver-graphite-based contact material.
The invention also provides the silver-graphite-based contact material obtained by the preparation method of the silver-graphite-based contact material.
The invention organically combines the good conductivity of the metallic silver with the performances of burning loss resistance, arc extinction and the like of the graphite, thereby preparing the silver-graphite-based contact material with the advantages of high strength, good conductivity, long service life, ablation resistance, good fusion welding resistance and the like.
In the invention, the density of the silver graphite-based contact material provided by the invention is 4.8+/-0.3 g/cm 3, the content of chemical component Ag is 70wt% +/-5 wt%, and the balance is C.
In the present invention, the preparation materials are commercially available as known to those skilled in the art unless otherwise specified.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
In the embodiment, the flake graphite powder, the asphalt rubber powder and the carbon black are used as raw materials, the coal asphalt is used as a binder, and the particle sizes of the flake graphite powder, the asphalt rubber powder and the carbon black are 40 microns. The mass ratio of the flake graphite powder to the asphalt rubber powder to the carbon black is 50:45:5, the coal asphalt accounts for 35 percent of the total weight of the flake graphite powder, the asphalt rubber powder and the carbon black, the mixture is uniformly kneaded and pressed into a shape, the shape is calcined at 900 ℃, and then graphitized at 2800 ℃ to obtain the graphite matrix with the density of 1.31g/cm 3. And (3) placing the graphite matrix into a graphite mold, adopting a corresponding positioning mechanism, casting in a 100KW medium-frequency induction furnace, uniformly coating the metal silver around the graphite matrix, placing into a hot isostatic pressing machine, soaking silver at the temperature of 1110 ℃ and 60MPa for 2 hours, stopping gas when power is cut off, and cooling to room temperature along with the furnace. The performance indexes of the prepared silver graphite-based contact are shown in table 1.
Table 1 performance index of silver graphite based contact prepared in example 1
As shown in fig. 1, the silver-graphite-based contact obtained in example 1 is subjected to microscopic characterization test, and as can be seen from fig. 1, the metallographic structure (200×) of the silver-graphite-based contact material shows that after silver leaching by hot isostatic pressing, the metallic silver fills most of the pores of the graphite matrix to form a network-like communication structure, so that the strength of the graphite matrix is improved, the resistivity of the composite material is greatly reduced, and the advantages of high strength, good conductivity, long service life, ablation resistance and good fusion welding resistance are realized.
Example 2
In the embodiment, the flake graphite powder, the asphalt rubber powder and the carbon black are used as raw materials, the coal asphalt is used as a binder, and the particle sizes of the flake graphite powder, the asphalt rubber powder and the carbon black are 35 microns. The mass ratio of the flake graphite powder to the asphalt rubber powder to the carbon black is 60:36:4, the coal asphalt accounts for 40 percent of the total mass of the flake graphite powder, the asphalt rubber powder and the carbon black, the mixture is uniformly kneaded and pressed into a shape, the shape is calcined at the temperature of 850 ℃, and then graphitized at the temperature of 2850 ℃ to obtain the graphite matrix with the density of 1.28g/cm 3. And (3) placing the graphite matrix into a graphite mold, adopting a corresponding positioning mechanism, casting in a 100KW medium-frequency induction furnace, uniformly coating the metal silver around the graphite matrix, placing into a hot isostatic pressing machine, immersing silver at the temperature of 1260 ℃ and under the pressure of 90MPa for 0.5 hour, stopping gas when power is cut off, and cooling to room temperature along with the furnace. The performance indexes of the prepared silver graphite-based contact are shown in Table 2.
Example 3
In the embodiment, the flake graphite powder, the asphalt rubber powder and the carbon black are used as raw materials, the coal asphalt is used as a binder, and the particle sizes of the flake graphite powder, the asphalt rubber powder and the carbon black are 45 micrometers. The mass ratio of the flake graphite powder to the asphalt rubber powder to the carbon black is 55:36:9, the coal asphalt accounts for 32% of the total mass of the graphite powder, the asphalt rubber powder and the carbon black, the mixture is uniformly kneaded and pressed into a shape, the shape is calcined at 950 ℃, and then graphitized at 2800 ℃ to obtain the graphite matrix with the density of 1.30g/cm 3. And (3) placing the graphite matrix into a graphite mold, adopting a corresponding positioning mechanism, casting in a 100KW medium-frequency induction furnace, uniformly coating the metal silver around the graphite matrix, placing the graphite matrix into a hot isostatic pressing machine, soaking silver at 1200 ℃ and 80MPa for 1 hour, stopping the gas supply after power failure, and cooling to room temperature along with the furnace. The performance indexes of the prepared silver graphite-based contact are shown in Table 3.
Example 4
In the embodiment, flake graphite powder, asphalt rubber powder and carbon black are used as raw materials, coal asphalt is used as a binder, and the particle sizes of the flake graphite powder, the asphalt rubber powder and the carbon black are 38 microns. The mass ratio of the flake graphite powder to the asphalt rubber powder to the carbon black is 52:37:5, the coal asphalt accounts for 38 percent of the total mass of the graphite powder, the asphalt rubber powder and the carbon black, the mixture is uniformly kneaded and pressed into a shape, the shape is calcined at 870 ℃, and then graphitized at 2840 ℃ to obtain the graphite matrix with the density of 1.35g/cm 3. And (3) placing the graphite matrix into a graphite mold, adopting a corresponding positioning mechanism, casting in a 100KW medium-frequency induction furnace, uniformly coating the metal silver around the graphite matrix, placing into a hot isostatic pressing machine, immersing silver at 1150 ℃ and 60MPa for 1 hour, stopping gas supply after power failure, and cooling to room temperature along with the furnace.
Example 5
In the embodiment, flake graphite powder, asphalt rubber powder and carbon black are used as raw materials, coal asphalt is used as a binder, and the particle sizes of the flake graphite powder, the asphalt rubber powder and the carbon black are 38 microns. The mass ratio of the flake graphite powder to the asphalt rubber powder to the carbon black is 54:39:5, the coal asphalt accounts for 36 percent of the total mass of the graphite powder, the asphalt rubber powder and the carbon black, the mixture is uniformly kneaded and pressed into a shape, the shape is calcined at 950 ℃, and then graphitized at 2820 ℃ to obtain the graphite matrix with the density of 1.32g/cm 3. And (3) placing the graphite matrix into a graphite mold, adopting a corresponding positioning mechanism, casting in a 100KW medium-frequency induction furnace, uniformly coating the metal silver around the graphite matrix, placing into a hot isostatic pressing machine, immersing silver at 1050 ℃ and 80MPa for 1 hour, stopping gas supply after power failure, and cooling to room temperature along with the furnace.
Example 6
In the embodiment, the flake graphite powder, the asphalt rubber powder and the carbon black are used as raw materials, the coal asphalt is used as a binder, and the particle sizes of the flake graphite powder, the asphalt rubber powder and the carbon black are 42 microns. The mass ratio of the flake graphite powder to the asphalt rubber powder to the carbon black is 55:40:7, the coal asphalt accounts for 36 percent of the total mass of the graphite powder, the asphalt rubber powder and the carbon black, the mixture is uniformly kneaded and pressed into a shape, the shape is calcined at the temperature of 910 ℃, and then graphitized at the temperature of 2880 ℃ to obtain the graphite matrix with the density of 1.34g/cm 3. And (3) placing the graphite matrix into a graphite mold, adopting a corresponding positioning mechanism, casting in a 100KW medium-frequency induction furnace, uniformly coating the metal silver around the graphite matrix, placing into a hot isostatic pressing machine, soaking silver at the temperature of 1210 ℃ and 80MPa for 1.5 hours, stopping gas when power is cut off, and cooling to room temperature along with the furnace.
Example 7
In the embodiment, the flake graphite powder, the asphalt rubber powder and the carbon black are used as raw materials, the coal asphalt is used as a binder, and the particle sizes of the flake graphite powder, the asphalt rubber powder and the carbon black are 45 micrometers. The mass ratio of the flake graphite powder to the asphalt rubber powder to the carbon black is 50:36:6, coal asphalt accounts for 34 percent of the total mass of the graphite powder, the asphalt rubber powder and the carbon black, and the mixture is uniformly kneaded, pressed and molded, calcined at the temperature of 930 ℃, and graphitized at the temperature of 2820 ℃ to obtain the graphite matrix with the density of 1.32g/cm 3. And (3) placing the graphite matrix into a graphite mold, adopting a corresponding positioning mechanism, casting in a 100KW medium-frequency induction furnace, uniformly coating the metal silver around the graphite matrix, placing the graphite matrix into a hot isostatic pressing machine, soaking silver at the temperature of 1200 ℃ and the pressure of 78MPa for 1 hour, stopping the gas supply after power failure, and cooling to the room temperature along with the furnace.
Example 8
In the embodiment, the flake graphite powder, the asphalt rubber powder and the carbon black are used as raw materials, the coal asphalt is used as a binder, and the particle sizes of the flake graphite powder, the asphalt rubber powder and the carbon black are 43 microns. The mass ratio of the flake graphite powder to the asphalt rubber powder to the carbon black is 52:37:5, coal asphalt accounts for 35 percent of the total mass of the graphite powder, the asphalt rubber powder and the carbon black, and the mixture is uniformly kneaded, pressed and molded, calcined at the temperature of 910 ℃, and graphitized at the temperature of 2840 ℃ to obtain the graphite matrix with the density of 1.34g/cm 3. And (3) placing the graphite matrix into a graphite mold, adopting a corresponding positioning mechanism, casting in a 100KW medium-frequency induction furnace, uniformly coating the metal silver around the graphite matrix, placing into a hot isostatic pressing machine, soaking silver at 1250 ℃ and 75MPa for 1.2 hours, stopping power supply, and cooling to room temperature along with the furnace.
From the above examples, the present invention provides a method for preparing a silver graphite-based contact material, which comprises the following steps: (1) Mixing flake graphite powder, asphalt rubber powder, carbon black and coal asphalt, and sequentially performing pressing, calcining and graphitizing treatment to obtain a graphite matrix; (2) silver-coated casting the graphite matrix to obtain an intermediate; (3) And soaking silver in the intermediate to obtain the silver graphite-based contact material. The invention firstly designs the components and the granularity of the graphite matrix, and prepares the graphite matrix by using the traditional carbon graphite material preparation process, wherein the density of the graphite matrix is 1.20-1.40 g/cm 3. The silver metal melted at high temperature and high pressure can fill most of the pores in the graphite matrix by using an advanced hot isostatic pressing silver leaching process, thereby preparing the silver-graphite-based contact material. The invention prepares the silver-graphite-based contact material with the density of 4.8+/-0.3 g/cm 3, the chemical component Ag content of 70wt% +/-5 wt% and the balance C by soaking silver in a graphite matrix. The compressive strength is 100-120 MPa, and the resistivity is 1.2X10 -7~2.0×10-7 ohm-m.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.

Claims (9)

1. The preparation method of the silver-graphite-based contact material is characterized by comprising the following steps:
(1) Mixing flake graphite powder, asphalt rubber powder, carbon black and coal asphalt, and sequentially performing pressing, calcining and graphitizing treatment to obtain a graphite matrix;
(2) Silver coating and casting are carried out on the graphite matrix to obtain an intermediate;
(3) And soaking silver in the intermediate to obtain the silver graphite-based contact material.
2. The method for preparing a silver graphite based contact material according to claim 1, wherein the particle sizes of the flake graphite powder, the asphalt cement powder and the carbon black in the step (1) are independently 30 to 50 μm.
3. The method for preparing a silver graphite-based contact material according to claim 1 or 2, wherein the mass ratio of the flake graphite powder, the asphalt cement powder and the carbon black in the step (1) is 50-60:35-45:3-10.
4. The method for preparing a silver graphite-based contact material according to claim 3, wherein the coal pitch in the step (1) accounts for 30% -40% of the total mass of the flake graphite powder, the asphalt rubber powder and the carbon black.
5. The method of producing a silver graphite based contact material according to claim 4, wherein the calcining temperature in step (1) is 850 ℃ to 950 ℃.
6. The method of producing a silver graphite based contact material according to claim 4 or 5, wherein the graphitization treatment in step (1) is performed at a temperature of 2800 ℃ to 2900 ℃.
7. The method for preparing a silver graphite based contact material according to claim 6, wherein the temperature of the immersion silver in the step (3) is 1100 ℃ to 1260 ℃ and the holding time to reach the immersion silver temperature is 0.5 to 2 hours.
8. The method for producing a silver graphite based contact material according to claim 7, wherein the pressure of the immersion silver in step (3) is 50 to 100MPa.
9. A silver-graphite-based contact material obtained by the method for producing a silver-graphite-based contact material according to any one of claims 1 to 8.
CN202410315413.2A 2024-03-19 2024-03-19 Silver-graphite-based contact material and preparation method thereof Pending CN118173402A (en)

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CN202410315413.2A CN118173402A (en) 2024-03-19 2024-03-19 Silver-graphite-based contact material and preparation method thereof

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Application Number Priority Date Filing Date Title
CN202410315413.2A CN118173402A (en) 2024-03-19 2024-03-19 Silver-graphite-based contact material and preparation method thereof

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CN118173402A true CN118173402A (en) 2024-06-11

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