CN115799937A - graphene/MoS 2 -copper graphite brush and preparation method - Google Patents
graphene/MoS 2 -copper graphite brush and preparation method Download PDFInfo
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Abstract
The invention relates to graphene/MoS 2 The copper-graphite brush material comprises the following components in percentage by mass: 10 to 60 percent of graphite powder; 0.5 to 10 percent of graphene powder; 1 to 5 percent of molybdenum disulfide powder; 2 to 20 percent of thermosetting resin; 0 to 8 percent of additive, and the balance being copper powder. The material provided by the invention can improve the mechanical property, reduce the wear rate and the resistivity, prolong the service life of the electric brush, meet the requirements of a large number of scenes on the electric brush, and has a wide application prospect. The method has the advantages of simple operation, capability of realizing automatic continuous stable large-scale production and low production cost.
Description
Technical Field
The invention relates to the field of electric brush materials, in particular to graphene/MoS 2 Copper graphite brush and method of manufacture.
Background
The electric brush is a key element between a rotating mechanism and a conductive mechanism which are connected with a commutator or a collecting ring, is used as a core component for conducting signals and transmitting energy, and has excellent conductive performance and lubricating performance.
Graphene is a periodic hexagonal lattice honeycomb two-dimensional crystal which is one of the discovered crystals and is formed by densely packing carbon atoms, and is the thinnest, highest strength, toughest, best heat transfer property and best conductive nanomaterial discovered to date. MoS 2 The composite material has a layered hexagonal lattice structure similar to graphite, has a stable structure, is often used as a lubricant, has a synergistic lubrication effect with graphite, can greatly reduce the wear of the material, and prolongs the service life. At present, the fine two-dimensional layered structure of graphene of the brush containing graphene can bridge the space between graphite particles without increasing the distance, and the fracture toughness and the electrical conductivity of the brush can be improved. There is also research on MoS 2 Added to the brush to find MoS 2 Can maintain extremely high lubricity in vacuum and dry harsh environments.
In conclusion, it is an urgent need in the market to develop a brush with excellent conductivity, good friction performance and good mechanical performance.
Disclosure of Invention
The invention aims to provide graphene/MoS 2 The copper graphite brush and the preparation method are used for solving the problems of high resistivity, large friction coefficient and poor mechanical energy of the existing brush.
In order to realize the purpose, the invention adopts the following technical scheme:
graphene/MoS 2 -a copper graphite brush material, the material comprising, in mass percent: 10 to 60 percent of graphite powder; 0.5 to 10 percent of graphene powder; 1 to5% of molybdenum disulfide powder; 2 to 20 percent of thermosetting resin; 0 to 8 percent of additive, and the balance being copper powder.
The additive is one or more of tin, zinc, lead, silicon dioxide, boron nitride and silicon carbide.
The material comprises the following components in percentage by mass: 30 to 55 percent of graphite powder; 0.5 to 5 percent of graphene powder; 1 to 5 percent of molybdenum disulfide powder; 5 to 10 percent of thermosetting resin; the additive is lead, the mass fraction of the additive is 1-5%, and the balance is copper powder.
The thermosetting resin is phenolic resin or furfural resin.
The graphene is a single layer or multiple layers of Graphene Oxide (GO), reduced graphene oxide (rGO) or Graphene Nanosheets (GNO), and the average particle size of the graphene is less than or equal to 2 mu m;
preferably, the graphite powder is natural flake graphite powder of 100 to 800 meshes;
preferably, the copper powder is electrolytic copper powder of 300 to 800 meshes.
graphene/MoS 2 -a method for preparing a copper graphite brush material, comprising the steps of:
taking the components according to the mixture ratio;
1) Adding thermosetting resin into an organic solvent, and stirring to obtain a resin solution;
2) Adding graphene powder into a resin solution, stirring and vibrating to obtain graphene resin slurry;
3)MoS 2 dispersing the powder into graphene resin slurry to obtain graphene/MoS 2 Compounding resin slurry;
4) Mixing graphene/MoS 2 Pouring the composite resin slurry into graphite powder, fully stirring, and kneading for 2-3h to obtain a graphite powder colloid with resin uniformly coated on the surface of graphite;
5) Drying and crushing the graphite powder colloid, and sieving the crushed graphite powder colloid by a 100-300-mesh sieve to obtain a resin layer containing graphene/MoS 2 The graphite powder of (3);
6) Mixing graphite powder, copper powder and an additive, pressing and sintering to obtain graphene/MoS 2 -copper graphite brush material.
The organic solvent in the step 1) is ethanol or acetone.
Step 3) the dispersion is that MoS is mixed 2 Stirring the powder and the graphene resin slurry at the rotating speed of 100-1000rpm for 0.5-1h, and carrying out ultrasonic oscillation at the frequency of 20-80kHz for 1-2h.
The step 6) is stirring and mixing, wherein the stirring time is 6 to 24h;
the pressing pressure is 100 to 500MPa.
And 6) sintering in a protective atmosphere, wherein the sintering temperature is 600-900 ℃, the sintering time is 1-4 h, and the protective atmosphere is hydrogen, argon or nitrogen.
The thermosetting resin as a binder can improve the strength of the brush, can be hardened during heat treatment, and can be pyrolyzed when treated at 500 ℃ or more.
When the average particle size of the graphene is less than or equal to 2 mu m, the brush body can obtain particularly high conductivity.
Graphene and MoS 2 The dispersion method can effectively solve the problems of large specific surface area, small density and easy agglomeration of the graphene, and can obtain particularly uniform graphene and MoS 2 And (4) slurry.
In the material, the copper powder mainly plays a role in conducting electricity and providing strength, and the graphite mainly plays a role in lubricating. If the content of the copper powder in the raw material of the electric brush is too high, the wear resistance of the electric brush is insufficient; if the copper powder content in the brush raw material is too low, the conductivity and strength of the brush are affected. The thermosetting resin can make up for the deficiency of strength caused by the small content of copper powder, but the introduction of the resin can cause the reduction of lubricity and conductivity, and the graphene can not only improve the conductivity of the resin layer but also improve the wear resistance.
MoS 2 The decrease of the abrasion property caused by the resin layer can be greatly improved, and the additional lubricating capability can be provided.
The metal elements such as tin, zinc, lead and the like can improve the sintering fluidity, improve the density of the material and improve the oxidation resistance and other performances of the material; the hexagonal boron nitride has excellent lubricity, and the wear resistance of the brush body can be further improved; silica and silicon carbide are used as grinding agents to prevent the lubricating film from being too thick, and the conductivity of the brush body is reduced.
In the production method of the present invention, the organic solvent can be removed after or during pressing by heat treatment in the production process.
graphene/MoS of the invention 2 Copper graphite brush materials have the following advantages:
due to the graphene/MoS 2 Due to the composite action, the material disclosed by the invention not only has good mechanical properties, but also can greatly reduce the friction coefficient and the resistivity of the electric brush, and compared with the traditional electric brush product, the use effect and the service life of the material are greatly improved.
Compared with the prior art, the graphene/MoS provided by the invention 2 The preparation method of the copper graphite brush has the following advantages: the method adopted by the invention is simple to operate, can realize automatic continuous stable large-scale production and has low production cost.
The experimental results of the applicant show that the volume density of the brush material obtained by the method of the invention is 2.78-3.52 (g/cm) 3 ) (ii) a Resistivity of 1.03 to 3.19 (μ Ω · m); the wear rate is 0.08-0.18 (less than or equal to mm) within 50 h; the breaking strength is 29-33 (MPa); hardness 13-18 (HBW).
The material can reduce the wear rate and the resistivity while improving the mechanical performance, prolong the service life of the electric brush, meet the performance requirements of the electric brush in various complex environments, and have wide application prospects.
Drawings
FIG. 1 shows that the resin layer prepared in example 1 of the present invention contains graphene/MoS 2 SEM picture of graphite powder;
FIG. 2 shows the graphene/MoS prepared in example 1 of the present invention 2 Cross-sectional SEM images of copper graphite brush products.
Detailed Description
The reagents used in this example were all commercially available analytical reagents; the used graphene is reduced graphene oxide (rGO) with a lamellar layer less than or equal to 5 layers and a particle size less than or equal to 2 um; the used phenolic resin adopts the carbon residue rate>55% free phenol<2.5% of a commercial thermosetting phenolic resin; moS used 2 Adopts 2500 meshes with purity>98% commercialPowder; all the metal powders have the purity>99% commercial powder.
Example 1
Step 1) taking 20g of phenolic resin powder, and pouring the phenolic resin powder into 100ml of acetone solution while stirring until the phenolic resin powder is completely dissolved to obtain the phenolic resin solution.
Step 2) pouring 5g of graphene into the phenolic resin solution in the step 1), adjusting the electromagnetic stirring speed to 500rpm, and stirring for 1h; and then oscillating for 1h in an ultrasonic oscillator at the frequency of 50kHz to obtain the graphene resin slurry.
Step 3) MoS 2 Pouring 3g of the powder into the graphene resin slurry obtained in the step 2), adjusting the electromagnetic stirring speed to 800rpm, and stirring for 0.5h; then oscillating for 1h in an ultrasonic oscillator at the frequency of 50kHz to obtain graphene/MoS 2 And (3) compounding resin slurry.
Step 4) preparing graphene/MoS 2 And pouring the composite resin slurry into 80g of 400-mesh graphite powder, fully stirring, and pouring into a kneader for kneading for 2h to obtain the resin-coated graphite powder colloid.
Step 5) baking the resin-coated graphite powder colloid in an oven at 80 ℃ for 12h to remove the acetone solvent, crushing in a crusher, and sieving with a 300-mesh sieve to obtain the resin containing graphene/MoS 2 Coated with graphite powder.
Step 6) taking 36g of graphite powder, 60g of 400-mesh copper powder and 4g of 400-mesh lead powder obtained in the step 5), pouring into a Y-shaped mixer, and mixing for 12 hours; then keeping the pressure of the mixed powder in a mold for 20s at 300MPa to obtain an electric brush blank; then heating the electric brush blank to 900 ℃ in a hydrogen reduction furnace at the speed of 10 ℃/min, and preserving the heat for 2h to obtain graphene/MoS 2 -copper graphite brushes.
FIG. 1 shows that the resin layer prepared in this example contains graphene/MoS 2 SEM image of graphite powder, from which fine graphene and MoS contained in the resin layer can be seen 2 Lamellar particles.
FIG. 2 shows the graphene/MoS prepared in this example 2 Cross-sectional SEM images of the copper graphite brush product, from which it can be seen that the brush components are uniformly distributed without significant defects.
In Table 1, the present embodiment is adoptedExamples graphene/MoS made from the materials described 2 And-the performance detection results of the copper graphite electric brush through mechanical property, frictional wear and resistivity test experiments.
TABLE 1
Example 2:
step 1) taking 20g of phenolic resin powder, and pouring the phenolic resin powder into 150ml of alcohol solution while stirring until the phenolic resin powder is completely dissolved to obtain the phenolic resin solution.
Step 2) pouring 6g of graphene into the phenolic resin solution in the step 1), adjusting the electromagnetic stirring speed to 400rpm, and stirring for 1h; and then oscillating for 1h in an ultrasonic oscillator at the frequency of 60kHz to obtain the graphene resin slurry.
Step 3) MoS 2 Pouring 4g of powder into the graphene resin slurry obtained in the step 2), adjusting the electromagnetic stirring speed to 800rpm, and stirring for 0.5h; then oscillating for 1h in an ultrasonic oscillator at the frequency of 50kHz to obtain graphene/MoS 2 And (3) compounding resin slurry.
Step 4) preparing graphene/MoS 2 And pouring the composite resin slurry into 80g of 400-mesh graphite powder, fully stirring, and pouring into a kneader for kneading for 2h to obtain the resin-coated graphite powder colloid.
Step 5) baking the powder obtained in the step 4) in an oven at 80 ℃ for 12h to remove the alcohol solvent, crushing the powder in a crusher, and sieving the crushed powder with a 300-mesh sieve to obtain the resin containing graphene/MoS 2 Coated with graphite powder.
Step 6), 47g of graphite powder, 50g of 400-mesh copper powder and 3g of 400-mesh tin powder obtained in the step 5) are poured into a Y-shaped mixer to be mixed for 12 hours; then keeping the pressure of the mixed powder in a mold for 20s at 300MPa to obtain an electric brush blank; then heating the electric brush blank to 900 ℃ in a hydrogen reduction furnace at the speed of 10 ℃/min, and preserving the heat for 2h to obtain graphene/MoS 2 -copper graphite brushes.
Table 2 shows the graphene/MoS prepared from the material of this example 2 The performance of the copper graphite electric brush after mechanical property, frictional wear and resistivity test experimentsAnd (6) detecting the result.
TABLE 2
Example 3:
step 1) taking 20g of phenolic resin powder, and pouring the phenolic resin powder into 100ml of acetone solution while stirring until the phenolic resin powder is completely dissolved to obtain the phenolic resin solution.
Step 2) pouring 7g of graphene into the resin solution obtained in the step 1), adjusting the electromagnetic stirring speed to 500rpm, and stirring for 1h; then the mixture is oscillated again for 1h in an ultrasonic oscillator at the frequency of 50 kHz.
Step 3) MoS 2 5g of powder is poured into the mixture solution obtained in the step 2), the electromagnetic stirring speed is adjusted to 800rpm, and the stirring is carried out for 0.5h; then the mixture is oscillated again for 1h in an ultrasonic oscillator at the frequency of 50 kHz.
And 4) pouring the mixture solution obtained in the step 3) into 75g of 400-mesh graphite powder, fully stirring, and pouring into a kneading machine for kneading for 2 hours to obtain the resin-coated graphite powder colloid.
Step 5) baking the powder obtained in the step 4) in an oven at 80 ℃ for 12h to remove the acetone solvent, crushing the powder in a crusher, and sieving the crushed powder with a 300-mesh sieve to obtain the resin containing graphene/MoS 2 Coated graphite powder.
Step 6), 55g of graphite powder, 42g of 400-mesh copper powder and 3g of 400-mesh lead powder obtained in the step 5) are poured into a Y-shaped mixer to be mixed for 12 hours; then keeping the pressure of the mixed powder in a mold for 20s at 300MPa to obtain an electric brush blank; then heating the electric brush blank to 900 ℃ in a hydrogen reduction furnace at the speed of 10 ℃/min, and preserving the heat for 2h to obtain graphene/MoS 2 -copper graphite brushes.
Table 3 shows the graphene/MoS prepared from the material of this example 2 And-the performance detection results of the copper graphite electric brush through mechanical property, frictional wear and resistivity test experiments.
TABLE 3
Claims (10)
1. graphene/MoS 2 -a copper graphite brush material, characterized in that the material comprises, in mass percent: 10 to 60 percent of graphite powder; 0.5 to 10 percent of graphene powder; 1 to 5 percent of molybdenum disulfide powder; 2 to 20 percent of thermosetting resin; 0 to 8 percent of additive, and the balance being copper powder.
2. The material of claim 1, wherein: the additive is one or more of tin, zinc, lead, silicon dioxide, boron nitride and silicon carbide.
3. The material of claim 1, wherein: the material comprises the following components in percentage by mass: 30 to 55 percent of graphite powder; 0.5 to 5 percent of graphene powder; 1 to 5 percent of molybdenum disulfide powder; 5 to 10 percent of thermosetting resin; the additive is lead, the mass fraction of the additive is 1-5%, and the balance is copper powder.
4. The material of claim 1, wherein: the thermosetting resin is phenolic resin or furfural resin.
5. The material of claim 1, wherein: the graphene is a single layer or multiple layers of Graphene Oxide (GO), reduced graphene oxide (rGO) or Graphene Nanosheets (GNO), and the average particle size of the graphene is less than or equal to 2 mu m;
preferably, the graphite powder is natural flake graphite powder of 100 to 800 meshes;
preferably, the copper powder is electrolytic copper powder of 300 to 800 meshes.
6. A method for the preparation of a material according to any of claims 1 to 5, characterized by the following steps:
taking the components according to the mixture ratio of any one of claims 1 to 5;
1) Adding thermosetting resin into an organic solvent, and stirring to obtain a resin solution;
2) Adding graphene powder into a resin solution, stirring and vibrating to obtain graphene resin slurry;
3)MoS 2 dispersing the powder into graphene resin slurry to obtain graphene/MoS 2 Compounding resin slurry;
4) Mixing graphene/MoS 2 Pouring the composite resin slurry into graphite powder, fully stirring, and kneading for 2-3 hours to obtain a graphite powder colloid with resin uniformly coated on the surface of graphite;
5) Drying and crushing the graphite powder colloid, and sieving the crushed graphite powder colloid by a 100-300-mesh sieve to obtain a resin layer containing graphene/MoS 2 The graphite powder of (3);
6) Mixing graphite powder, copper powder and an additive, pressing and sintering to obtain graphene/MoS 2 -copper graphite brush material.
7. The method of claim 6, wherein: the organic solvent in the step 1) is ethanol or acetone.
8. The method of claim 6, wherein: step 3) the dispersion is that MoS is mixed 2 Stirring the powder and the graphene resin slurry at the rotating speed of 100-1000rpm for 0.5-1h, and carrying out ultrasonic oscillation at the frequency of 20-80kHz for 1-2h.
9. The method of claim 6, wherein: the step 6) is stirring and mixing, wherein the stirring time is 6 to 24h;
the pressing pressure is 100 to 500MPa.
10. The method of claim 6, wherein: step 6), sintering in a protective atmosphere at the sintering temperature of 600-900 ℃ for 1-4 h;
preferably, the protective atmosphere is hydrogen, argon or nitrogen.
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