Titanium-coated diamond-reinforced copper-based material and preparation method thereof
Through the cold spraying process of titanium-coated diamond powder and atomized spherical electrolytic copper powder, the problems of low density and thermal conductivity of diamond-reinforced copper-based materials have been solved, and the preparation of high-density and high-thermal conductivity materials has been achieved. It is suitable for large-scale integrated circuits, CPU packaging materials, and high-power traveling wave tube structural and functional integrated heat dissipation components.
Patent Information
- Application Number
- CN202510280173.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-11
- Publication Date
- 2025-09-12
- Estimated Expiration
- 2045-03-11
AI Technical Summary
Existing methods for preparing diamond-reinforced copper-based materials have problems with low density and low thermal conductivity. In particular, when using pressure-assisted infiltration, diamond crystals are prone to defects, while materials prepared by spark plasma sintering have low density.
Surface titanium-coated diamond powder is mixed with atomized spherical electrolytic copper powder, and a diamond-reinforced copper-based material layer is formed on a copper substrate by cold spraying. By controlling process parameters such as working gas temperature, pressure and spray gun distance, and combining with a cutting and separation process, a material with high density and high thermal conductivity is prepared.
The density and thermal conductivity of diamond-reinforced copper-based materials are improved, the porosity is reduced, and efficient deposition and shape controllability of the materials are achieved, making them suitable for rapid preparation of different shapes.
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Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of high thermal conductivity copper alloy materials, and in particular to a titanium-plated diamond-reinforced copper-based material, a preparation method thereof, and applications thereof. Background Art
[0002] Diamond-reinforced copper-based material is a type of high thermal conductivity copper alloy material. Due to its excellent thermophysical properties and suitable mechanical properties, it is an ideal electronic packaging material. It is widely used in packaging materials for large-scale integrated circuits and CPUs, high-power traveling wave tube structural and functional integrated heat dissipation components, and high-power antenna heat dissipation substrates.
[0003] Current methods for preparing diamond-reinforced copper-based materials include pressure-assisted infiltration and spark plasma sintering. Pressure-assisted infiltration is prone to creating defects in the diamond crystals, reducing the material's thermal conductivity. Copper-based materials prepared using spark plasma sintering have low density, leading to low thermal conductivity. Summary of the Invention
[0004] In view of the above problems, the purpose of the present invention is to provide a diamond-reinforced copper-based material and its preparation method and application. The diamond-reinforced copper-based material prepared by the present invention has high density and effectively improves the thermal conductivity of the material.
[0005] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:
[0006] The present invention provides a method for preparing a titanium-plated diamond-reinforced copper-based material, comprising the following steps:
[0007] Surface titanium-coated diamond powder is mixed with atomized spherical electrolytic copper powder, wherein the mass ratio of the atomized spherical electrolytic copper powder to the surface titanium-coated diamond powder is 80:20; the mixed powder is cold sprayed on a copper substrate to obtain a diamond-reinforced copper-based material layer on the surface of the copper substrate, and the temperature of the working gas used for cold spraying is 500-700°C; in the diamond-reinforced copper-based material layer, the mass of the surface titanium-coated diamond powder accounts for 20%.
[0008] In the preparation method provided by the present invention, the average thickness of the diamond-reinforced copper-based material layer is 2 to 10 mm.
[0009] In the preparation method provided by the present invention, the particle size of the titanium-coated diamond powder is 60-120 μm, and the titanium coating amount is 10 wt% of the titanium-coated diamond powder.
[0010] The preparation method provided by the present invention has the following characteristics: the particle size of the atomized spherical electrolytic copper powder is 5-60 μm, the purity is ≥99.9%, and the oxygen content is ≤600 ppm.
[0011] In the preparation method provided by the present invention, nitrogen is used as the working gas during the cold spraying process, the temperature of the working gas is 500-700° C., and the pressure of the working gas is 5 MPa.
[0012] In the preparation method provided by the present invention, the purity of the nitrogen is 99.9% to 99.99%.
[0013] In the preparation method provided by the present invention, the vertical distance between the muzzle of the cold spraying spray gun and the copper substrate is 20 mm, and the moving speed of the spray gun is 20 mm / s.
[0014] The preparation method provided by the present invention further comprises: cutting and separating the obtained diamond-reinforced copper-based material layer from the copper substrate.
[0015] The invention provides a diamond-reinforced copper-based material, which is prepared by adopting the provided preparation method.
[0016] 1. The present invention provides a method for preparing a titanium-plated diamond-reinforced copper-based material, comprising the following steps:
[0017] Surface titanium-coated diamond powder is mixed with atomized spherical electrolytic copper powder, wherein the mass ratio of the atomized spherical electrolytic copper powder to the surface titanium-coated diamond powder is 80:20; the mixed powder is cold sprayed on a copper substrate to obtain a diamond-reinforced copper-based material layer on the surface of the copper substrate, and the temperature of the working gas used for cold spraying is 500-700°C; in the diamond-reinforced copper-based material layer, the mass of the surface titanium-coated diamond powder accounts for 20%.
[0018] In the present invention, the surface titanium-coated diamond powder can significantly improve the deposition efficiency of pure diamond on the surface of a copper substrate; by adding atomized spherical electrolytic copper powder, the ratio of copper to diamond can be adjusted to obtain a suitable component ratio and increase the thermal conductivity of the material; at the same time, the surface titanium-coated diamond powder is not spherical and the deposition efficiency is not high, while the addition of atomized spherical electrolytic copper powder is conducive to improving the deposition rate of the surface titanium-coated diamond powder, thereby obtaining a diamond-reinforced copper-based material with high density and high thermal conductivity.
[0019] 2. The present invention provides a method for preparing a titanium-plated diamond-reinforced copper-based material. The sprayed powder is deposited in a solid state without oxidation, phase change, or other changes, thereby reducing the degree of graphitization of the diamond and increasing the diamond content in the coating.
[0020] By controlling process parameters such as the particle size of the raw materials, the pressure of the working gas, and the vertical distance between the spray gun muzzle and the copper substrate, the bonding strength between the diamond-reinforced copper-based material and the copper substrate can be controlled, and the copper substrate can ultimately be easily removed. This process can control the thickness and shape of the diamond-reinforced copper-based material, has high production efficiency, and can directly and quickly prepare diamond-reinforced copper-based materials of different shapes. BRIEF DESCRIPTION OF THE DRAWINGS
[0021] Figure 1 The morphology of the gas-atomized spherical electrolytic copper powder and the titanium-coated diamond powder used in the examples;
[0022] Figure 2 Surface scanning of the atomized spherical electrolytic copper powder and titanium-coated diamond powder used in the examples;
[0023] Figure 3 This is a morphology diagram of the cross section of the diamond-reinforced copper-based material prepared in Example 1;
[0024] Figure 4 This is a morphology diagram of the cross section of the diamond-reinforced copper-based material prepared in Example 2;
[0025] Figure 5 This is a morphology diagram of the cross section of the diamond-reinforced copper-based material prepared in Example 3;
[0026] Figure 6 This is a morphology diagram of the cross section of the diamond-reinforced copper-based material prepared in Example 3. DETAILED DESCRIPTION
[0027] Example 1
[0028] This embodiment provides a method for preparing a titanium-coated diamond-reinforced copper-based material, comprising the following steps:
[0029] Mixing titanium-coated diamond powder with atomized spherical electrolytic copper powder. There is no special requirement for the mixing method, as long as the mixture is uniform. The mass ratio of the atomized spherical electrolytic copper powder to the titanium-coated diamond powder is 80:20.
[0030] In this embodiment, the surface titanium-coated diamond powder is a material in which a layer of titanium metal or titanium compound is plated on the surface of the diamond powder through a specific process, and it has the excellent properties of both diamond and titanium. The preparation process of the surface titanium-coated diamond powder is not limited. In this embodiment, titanium is vaporized into atoms or ions under vacuum conditions and directly deposited on the diamond surface. Specific technical means include magnetron sputtering coating technology, vacuum evaporation coating technology, vacuum micro-evaporation coating technology, etc. Among them, magnetron sputtering is to vaporize titanium into ions, introduce inert gas under vacuum conditions, and accelerate the coating of titanium ions on the diamond surface to form a film through the action of electric and magnetic fields; vacuum evaporation coating is to place titanium in a material boat, apply electricity to increase the temperature to vaporize it, and then deposit the vapor on the diamond surface after cooling; vacuum micro-evaporation coating is to allow diamond to contact highly activated titanium metal under certain vacuum and temperature conditions, so that the titanium surface atoms react with the diamond surface to form a compound.
[0031] Further, aerosolized spherical electrolytic copper powder is a high-performance metal powder having the advantages of aerosolized copper powder and electrolytic copper powder. In the present embodiment, the preparation of the powder is achieved by electrolysis, with a refined copper plate as an anode, a red copper plate as a cathode, and copper sulfate and sulfuric acid solution as an electrolyte. After energization, copper dissolves into the electrolyte from the anode and is then deposited and precipitated on the cathode to form electrolytic copper powder. The copper powder obtained by electrolysis or the copper raw material is directly heated and melted, and then the molten copper liquid stream is broken into fine droplets with high-pressure gas (such as inert gases such as nitrogen). These droplets are rapidly condensed in a cold environment to form aerosolized spherical copper powder.
[0032] In this embodiment, the powder is further dried, and the drying is preferably performed in a vacuum drying oven; specifically, the mixture is dried in a vacuum drying oven at 90° C. for 1 hour to obtain a mixed powder.
[0033] Furthermore, the mixed powder is cold sprayed on a copper substrate to obtain a diamond-reinforced copper-based material layer on the surface of the copper substrate;
[0034] Specifically, the copper substrate preferably includes a copper alloy substrate, more preferably a copper substrate; the present invention has no special requirements for the size of the copper substrate, and a size commonly used by those skilled in the art can be selected; a copper substrate with a size (length, width, and height) of 200×50×5 mm is polished with 36 mesh, 240 mesh, 400 mesh, 800 mesh, 1200 mesh, 2000 mesh, 3000 mesh, and 5000 mesh sandpaper in sequence, and polished with a 0.5 μm diamond spray polishing agent until there are no obvious scratches on the surface, and the surface-treated copper substrate is cleaned with acetone and alcohol until there are no impurities on the surface;
[0035] The particle size of the titanium-coated diamond powder is 60 to 120 μm, and the titanium coating amount of the titanium-coated diamond powder is 10 wt% of the titanium-coated diamond powder. The particle size of the atomized spherical electrolytic copper powder is 5 to 60 μm, the purity is ≥99.9%, and the oxygen content is ≤600 ppm. Preferably, the particle size of the titanium-coated diamond powder is 90 μm, and the particle size of the atomized spherical electrolytic copper powder is 30 μm. The morphology of the atomized spherical electrolytic copper powder is as follows: Figure 1 As shown in the figure, it can be seen that the sphericity of the gas-atomized spherical electrolytic copper powder is very high, and it is approximately spherical. The titanium coating amount of the titanium-coated diamond powder used in the embodiment is 20wt%, and its morphology is as follows Figure 2 As shown, it can be seen that the shape of the titanium-coated diamond powder on the surface is similar to that of pebbles and has irregular morphology.
[0036] The mixed powder was cold sprayed on a surface-treated copper substrate to obtain a diamond-reinforced copper-based material layer on the copper substrate surface. The working gas pressure was 5 MPa, the powder feeding gas pressure was 3 MPa, the working gas temperature was 500°C, the vertical distance between the spray gun muzzle and the copper substrate was 20 mm, and the spray gun movement speed was 20 mm / s.
[0037] The cold spray gun used in this embodiment is of model PCS-1000L, the gas supply equipment is a POG series high-pressure volumetric powder feeder, model POG-2030, and both the working gas and the powder supply gas are nitrogen with a purity of 99.9%.
[0038] The copper substrate coated with the diamond-reinforced copper-based material layer was removed by wire cutting to obtain a diamond-reinforced copper-based layer. Impurities on the surface of the diamond-reinforced copper-based layer were first cleaned with an acetone solution and then cleaned with alcohol to obtain a diamond-reinforced copper-based material with an average thickness of 10 mm.
[0039] Example 2
[0040] This embodiment provides a method for preparing a diamond-reinforced copper-based material, comprising the following steps:
[0041] Mixing titanium-coated diamond powder with atomized spherical electrolytic copper powder. There is no special requirement for the mixing method, as long as the mixture is uniform. The mass ratio of the atomized spherical electrolytic copper powder to the titanium-coated diamond powder is 80:20.
[0042] In this embodiment, the surface titanium-coated diamond powder is a material in which a layer of titanium metal or titanium compound is plated on the surface of the diamond powder through a specific process, and it has the excellent properties of both diamond and titanium. The preparation process of the surface titanium-coated diamond powder is not limited. In this embodiment, titanium is vaporized into atoms or ions under vacuum conditions and directly deposited on the diamond surface. Specific technical means include magnetron sputtering coating technology, vacuum evaporation coating technology, vacuum micro-evaporation coating technology, etc. Among them, magnetron sputtering is to vaporize titanium into ions, introduce inert gas under vacuum conditions, and accelerate the coating of titanium ions on the diamond surface to form a film through the action of electric and magnetic fields; vacuum evaporation coating is to place titanium in a material boat, apply electricity to increase the temperature to vaporize it, and then deposit the vapor on the diamond surface after cooling; vacuum micro-evaporation coating is to allow diamond to contact highly activated titanium metal under certain vacuum and temperature conditions, so that the titanium surface atoms react with the diamond surface to form a compound.
[0043] Further, aerosolized spherical electrolytic copper powder is a high-performance metal powder having the advantages of aerosolized copper powder and electrolytic copper powder. In the present embodiment, the preparation of the powder is achieved by electrolysis, with a refined copper plate as an anode, a red copper plate as a cathode, and copper sulfate and sulfuric acid solution as an electrolyte. After energization, copper dissolves into the electrolyte from the anode and is then deposited and precipitated on the cathode to form electrolytic copper powder. The copper powder obtained by electrolysis or the copper raw material is directly heated and melted, and then the molten copper liquid stream is broken into fine droplets with high-pressure gas (such as inert gases such as nitrogen). These droplets are rapidly condensed in a cold environment to form aerosolized spherical copper powder.
[0044] In this embodiment, the powder is further dried, and the drying is preferably performed in a vacuum drying oven; specifically, the mixture is dried in a vacuum drying oven at 90° C. for 1 hour to obtain a mixed powder.
[0045] Furthermore, the mixed powder is cold sprayed on a copper substrate to obtain a diamond-reinforced copper-based material layer on the surface of the copper substrate;
[0046] Specifically, the copper substrate preferably includes a copper alloy substrate, more preferably a copper substrate; the present invention has no special requirements for the size of the copper substrate, and a size commonly used by those skilled in the art can be selected; a copper substrate with a size (length, width, and height) of 200×50×5 mm is polished with 36 mesh, 240 mesh, 400 mesh, 800 mesh, 1200 mesh, 2000 mesh, 3000 mesh, and 5000 mesh sandpaper in sequence, and polished with a 0.5 μm diamond spray polishing agent until there are no obvious scratches on the surface, and the surface-treated copper substrate is cleaned with acetone and alcohol until there are no impurities on the surface;
[0047] The particle size of the titanium-coated diamond powder is 60 to 120 μm, and the titanium coating amount of the titanium-coated diamond powder is 10 wt% of the titanium-coated diamond powder. The particle size of the atomized spherical electrolytic copper powder is 5 to 60 μm, the purity is ≥99.9%, and the oxygen content is ≤600 ppm. Preferably, the particle size of the titanium-coated diamond powder is 90 μm, and the particle size of the atomized spherical electrolytic copper powder is 30 μm. The morphology of the atomized spherical electrolytic copper powder is as follows: Figure 1 As shown in the figure, it can be seen that the sphericity of the gas-atomized spherical electrolytic copper powder is very high, and it is approximately spherical. The titanium coating amount of the titanium-coated diamond powder used in the embodiment is 20wt%, and its morphology is as follows Figure 2 As shown, it can be seen that the shape of the titanium-coated diamond powder on the surface is similar to that of pebbles and has irregular morphology.
[0048] The mixed powder was cold sprayed on a surface-treated copper substrate to obtain a diamond-reinforced copper-based material layer on the surface of the copper substrate. The working gas pressure was 5 MPa, the powder feeding gas pressure was 3 MPa, the working gas temperature was 550°C, the vertical distance between the spray gun muzzle and the copper substrate was 20 mm, and the spray gun movement speed was 20 mm / s.
[0049] The cold spray gun used in this embodiment is of model PCS-1000L, the gas supply equipment is a POG series high-pressure volumetric powder feeder, model POG-2030, and both the working gas and the powder supply gas are nitrogen with a purity of 99.9%.
[0050] The copper substrate coated with the diamond-reinforced copper-based material layer was removed by wire cutting to obtain a diamond-reinforced copper-based layer. Impurities on the surface of the diamond-reinforced copper-based layer were first cleaned with an acetone solution and then cleaned with alcohol to obtain a diamond-reinforced copper-based material with an average thickness of 10 mm.
[0051] Example 3
[0052] This embodiment provides a method for preparing a diamond-reinforced copper-based material, comprising the following steps:
[0053] Mixing titanium-coated diamond powder with atomized spherical electrolytic copper powder. There is no special requirement for the mixing method, as long as the mixture is uniform. The mass ratio of the atomized spherical electrolytic copper powder to the titanium-coated diamond powder is 80:20.
[0054] In this embodiment, the surface titanium-coated diamond powder is a material in which a layer of titanium metal or titanium compound is plated on the surface of the diamond powder through a specific process, and it has the excellent properties of both diamond and titanium. The preparation process of the surface titanium-coated diamond powder is not limited. In this embodiment, titanium is vaporized into atoms or ions under vacuum conditions and directly deposited on the diamond surface. Specific technical means include magnetron sputtering coating technology, vacuum evaporation coating technology, vacuum micro-evaporation coating technology, etc. Among them, magnetron sputtering is to vaporize titanium into ions, introduce inert gas under vacuum conditions, and accelerate the coating of titanium ions on the diamond surface to form a film through the action of electric and magnetic fields; vacuum evaporation coating is to place titanium in a material boat, apply electricity to increase the temperature to vaporize it, and then deposit the vapor on the diamond surface after cooling; vacuum micro-evaporation coating is to allow diamond to contact highly activated titanium metal under certain vacuum and temperature conditions, so that the titanium surface atoms react with the diamond surface to form a compound.
[0055] Further, aerosolized spherical electrolytic copper powder is a high-performance metal powder having the advantages of aerosolized copper powder and electrolytic copper powder. In the present embodiment, the preparation of the powder is achieved by electrolysis, with a refined copper plate as an anode, a red copper plate as a cathode, and copper sulfate and sulfuric acid solution as an electrolyte. After energization, copper dissolves into the electrolyte from the anode and is then deposited and precipitated on the cathode to form electrolytic copper powder. The copper powder obtained by electrolysis or the copper raw material is directly heated and melted, and then the molten copper liquid stream is broken into fine droplets with high-pressure gas (such as inert gases such as nitrogen). These droplets are rapidly condensed in a cold environment to form aerosolized spherical copper powder.
[0056] In this embodiment, the powder is further dried, and the drying is preferably performed in a vacuum drying oven; specifically, the mixture is dried in a vacuum drying oven at 90° C. for 1 hour to obtain a mixed powder.
[0057] Furthermore, the mixed powder is cold sprayed on a copper substrate to obtain a diamond-reinforced copper-based material layer on the surface of the copper substrate;
[0058] Specifically, the copper substrate preferably includes a copper alloy substrate, more preferably a copper substrate; the present invention has no special requirements for the size of the copper substrate, and a size commonly used by those skilled in the art can be selected; a copper substrate with a size (length, width, and height) of 200×50×5 mm is polished with 36 mesh, 240 mesh, 400 mesh, 800 mesh, 1200 mesh, 2000 mesh, 3000 mesh, and 5000 mesh sandpaper in sequence, and polished with a 0.5 μm diamond spray polishing agent until there are no obvious scratches on the surface, and the surface-treated copper substrate is cleaned with acetone and alcohol until there are no impurities on the surface;
[0059] The particle size of the titanium-coated diamond powder is 60 to 120 μm, and the titanium coating amount of the titanium-coated diamond powder is 10 wt% of the titanium-coated diamond powder. The particle size of the atomized spherical electrolytic copper powder is 5 to 60 μm, the purity is ≥99.9%, and the oxygen content is ≤600 ppm. Preferably, the particle size of the titanium-coated diamond powder is 90 μm, and the particle size of the atomized spherical electrolytic copper powder is 30 μm. The morphology of the atomized spherical electrolytic copper powder is as follows: Figure 1 As shown in the figure, it can be seen that the sphericity of the gas-atomized spherical electrolytic copper powder is very high, and it is approximately spherical. The titanium coating amount of the titanium-coated diamond powder used in the embodiment is 20wt%, and its morphology is as follows Figure 2 As shown, it can be seen that the shape of the titanium-coated diamond powder on the surface is similar to that of pebbles and has irregular morphology.
[0060] The mixed powder was cold sprayed on a surface-treated copper substrate to obtain a diamond-reinforced copper-based material layer on the copper substrate surface. The working gas pressure was 5 MPa, the powder feeding gas pressure was 3 MPa, the working gas temperature was 600°C, the vertical distance between the spray gun muzzle and the copper substrate was 20 mm, and the spray gun movement speed was 20 mm / s.
[0061] The cold spray gun used in this embodiment is of model PCS-1000L, the gas supply equipment is a POG series high-pressure volumetric powder feeder, model POG-2030, and both the working gas and the powder supply gas are nitrogen with a purity of 99.9%.
[0062] The copper substrate coated with the diamond-reinforced copper-based material layer was removed by wire cutting to obtain a diamond-reinforced copper-based layer. Impurities on the surface of the diamond-reinforced copper-based layer were first cleaned with an acetone solution and then cleaned with alcohol to obtain a diamond-reinforced copper-based material with an average thickness of 10 mm.
[0063] Example 4
[0064] This embodiment provides a method for preparing a diamond-reinforced copper-based material, comprising the following steps:
[0065] Mixing titanium-coated diamond powder with atomized spherical electrolytic copper powder. There is no special requirement for the mixing method, as long as the mixture is uniform. The mass ratio of the atomized spherical electrolytic copper powder to the titanium-coated diamond powder is 80:20.
[0066] In this embodiment, the surface titanium-coated diamond powder is a material in which a layer of titanium metal or titanium compound is plated on the surface of the diamond powder through a specific process, and it has the excellent properties of both diamond and titanium. The preparation process of the surface titanium-coated diamond powder is not limited. In this embodiment, titanium is vaporized into atoms or ions under vacuum conditions and directly deposited on the diamond surface. Specific technical means include magnetron sputtering coating technology, vacuum evaporation coating technology, vacuum micro-evaporation coating technology, etc. Among them, magnetron sputtering is to vaporize titanium into ions, introduce inert gas under vacuum conditions, and accelerate the coating of titanium ions on the diamond surface to form a film through the action of electric and magnetic fields; vacuum evaporation coating is to place titanium in a material boat, apply electricity to increase the temperature to vaporize it, and then deposit the vapor on the diamond surface after cooling; vacuum micro-evaporation coating is to allow diamond to contact highly activated titanium metal under certain vacuum and temperature conditions, so that the titanium surface atoms react with the diamond surface to form a compound.
[0067] Further, aerosolized spherical electrolytic copper powder is a high-performance metal powder having the advantages of aerosolized copper powder and electrolytic copper powder. In the present embodiment, the preparation of the powder is achieved by electrolysis, with a refined copper plate as an anode, a red copper plate as a cathode, and copper sulfate and sulfuric acid solution as an electrolyte. After energization, copper dissolves into the electrolyte from the anode and is then deposited and precipitated on the cathode to form electrolytic copper powder. The copper powder obtained by electrolysis or the copper raw material is directly heated and melted, and then the molten copper liquid stream is broken into fine droplets with high-pressure gas (such as inert gases such as nitrogen). These droplets are rapidly condensed in a cold environment to form aerosolized spherical copper powder.
[0068] In this embodiment, the powder is further dried, and the drying is preferably performed in a vacuum drying oven; specifically, the mixture is dried in a vacuum drying oven at 90° C. for 1 hour to obtain a mixed powder.
[0069] Furthermore, the mixed powder is cold sprayed on a copper substrate to obtain a diamond-reinforced copper-based material layer on the surface of the copper substrate;
[0070] Specifically, the copper substrate preferably includes a copper alloy substrate, more preferably a copper substrate; the present invention has no special requirements for the size of the copper substrate, and a size commonly used by those skilled in the art can be selected; a copper substrate with a size (length, width, and height) of 200×50×5 mm is polished with 36 mesh, 240 mesh, 400 mesh, 800 mesh, 1200 mesh, 2000 mesh, 3000 mesh, and 5000 mesh sandpaper in sequence, and polished with a 0.5 μm diamond spray polishing agent until there are no obvious scratches on the surface, and the surface-treated copper substrate is cleaned with acetone and alcohol until there are no impurities on the surface;
[0071] The particle size of the titanium-coated diamond powder is 60 to 120 μm, and the titanium coating amount of the titanium-coated diamond powder is 10 wt% of the titanium-coated diamond powder. The particle size of the atomized spherical electrolytic copper powder is 5 to 60 μm, the purity is ≥99.9%, and the oxygen content is ≤600 ppm. Preferably, the particle size of the titanium-coated diamond powder is 90 μm, and the particle size of the atomized spherical electrolytic copper powder is 30 μm. The morphology of the atomized spherical electrolytic copper powder is as follows: Figure 1 As shown in the figure, it can be seen that the sphericity of the gas-atomized spherical electrolytic copper powder is very high, and it is approximately spherical. The titanium coating amount of the titanium-coated diamond powder used in the embodiment is 20wt%, and its morphology is as follows Figure 2 As shown, it can be seen that the shape of the titanium-coated diamond powder on the surface is similar to that of pebbles and has irregular morphology.
[0072] The mixed powder was cold sprayed on a surface-treated copper substrate to obtain a diamond-reinforced copper-based material layer on the copper substrate surface. The working gas pressure was 5 MPa, the powder feeding gas pressure was 3 MPa, the working gas temperature was 700°C, the vertical distance between the spray gun muzzle and the copper substrate was 20 mm, and the spray gun movement speed was 20 mm / s.
[0073] The cold spray gun used in this embodiment is of model PCS-1000L, the gas supply equipment is a POG series high-pressure volumetric powder feeder, model POG-2030, and both the working gas and the powder supply gas are nitrogen with a purity of 99.9%.
[0074] The copper substrate coated with the diamond-reinforced copper-based material layer was removed by wire cutting to obtain a diamond-reinforced copper-based layer. Impurities on the surface of the diamond-reinforced copper-based layer were first cleaned with an acetone solution and then cleaned with alcohol to obtain a diamond-reinforced copper-based material with an average thickness of 10 mm.
[0075] Example 5
[0076] This embodiment provides a titanium-plated diamond-reinforced copper-based material, which is prepared using the preparation methods provided in Examples 1 to 4.
[0077] Existing technology uses copper-coated diamonds combined with atomized spherical electrolytic copper powder to produce diamond-reinforced copper-based materials. However, the copper-diamond bond in the copper-coated diamond is relatively poor, making it susceptible to breakage during high-speed deposition.
[0078] In this embodiment, a metal compound layer is formed when titanium is plated on the surface of the diamond, and titanium and copper can also have a good bond. The titanium in the titanium-plated diamond has a good bond with the diamond, and it is easier to combine with copper powder during deposition, thereby improving the deposition effect of the diamond and exerting the thermal conductivity of the diamond.
[0079] For diamond-reinforced copper-based composite materials, the larger the diamond, the better its thermal conductivity, but it may be more prone to breakage during the deposition process. In this embodiment, the spraying temperature is increased to soften the copper powder, and titanium is plated on the diamond surface to improve the diamond bonding ability, thereby promoting more diamond deposition in the copper and improving thermal conductivity.
[0080] The porosity, thermal conductivity and sample thickness of the diamond-reinforced copper-based materials obtained by the preparation methods of Examples 1-4 were tested respectively.
[0081] Testing the porosity of diamond-reinforced copper-based materials
[0082] First, the porosity was calculated as follows: cross-sectional photographs of some diamond-reinforced copper-based materials were taken using a scanning electron microscope, and the voids in the SEM tissue images were marked using imageJ software. The ratio of the total area of the voids to the total area of the test area was calculated to obtain the area fraction, and the porosity of the diamond-reinforced copper-based material was obtained. The porosities of the diamond-reinforced copper-based materials obtained in Examples 1 to 4 are shown in Table 1:
[0083] Table 1 Porosity of diamond-reinforced copper-based materials prepared in Examples 1 to 4
[0084] Example Example 1 Example 2 Example 3 Example 4 Porosity 0.8% 0.7% 0.6% 0.7%
[0085] Based on the data in Table 1, Figure 3-Figure 6 It can be seen from the content shown in that the porosity of the materials prepared in Examples 1 to 4 is less than 1%, the porosity is low, the density is high, and the thermal conductivity of the material can be effectively improved.
[0086] Testing the thermal conductivity of diamond-enhanced copper-based materials
[0087] The thermal conductivity of different samples was tested using a laser thermal conductivity meter (NETZSCH LFA 457) to obtain the thermal conductivity of the diamond-enhanced copper-based material. The thermal conductivity of the diamond-enhanced copper-based material obtained by Examples 1 to 4 is shown in Table 2:
[0088] Table 2 Thermal conductivity of diamond-enhanced copper-based materials prepared in Examples 1 to 4
[0089]
[0090] It can be seen from Table 2 that the diamond-reinforced copper-based materials prepared in Examples 1 to 4 have relatively high thermal conductivity.
[0091] Testing the Deposition Effect of Diamond-Enhanced Copper-Based Materials
[0092] The thickness of samples of different types was measured and compared to obtain the deposition effect of diamond-enhanced copper-based materials. The thickness of samples of Examples 1 to 4 is shown in Table 3:
[0093] Table 1 Thickness of samples prepared in Examples 1 to 3
[0094] Example Example 1 Example 2 Example 3 Example 4 Sample thickness 5.19mm 5.32mm 5.47mm 5.48mm
[0095] It can be seen from Table 3 that the diamond-reinforced copper-based materials prepared in Examples 1 to 4 have a higher deposition effect.
[0096] Comparative Example
[0097] This embodiment adopts the solution in the prior art, and the specific solution is as follows:
[0098] The surface copper-plated diamond powder is mixed with atomized spherical electrolytic copper powder and dried, and then cold sprayed on a copper substrate to obtain a diamond-reinforced copper-based material layer on the surface of the copper substrate. The copper substrate is then removed to obtain a diamond-reinforced copper-based material.
[0099] The mass ratio of the atomized spherical electrolytic copper powder to the surface copper-plated diamond powder is 80:20; the mixed powder is cold sprayed on a copper substrate to obtain a diamond-reinforced copper-based material layer on the surface of the copper substrate, wherein the temperature of the working gas used for cold spraying is 500°C; in the diamond-reinforced copper-based material layer, the mass of the surface copper-plated diamond powder accounts for 20%.
[0100] Other process steps and process parameters remain the same as those in Example 1.
[0101] After analyzing the performance of the obtained copper-plated diamond reinforced copper-based material, it was found that its thermal conductivity was 253.3 W / (m·k), and the sample thickness of the copper-plated diamond reinforced copper-based material was 4.97 mm.
[0102] After analysis, it can be seen that in this embodiment, by mixing surface titanium-coated diamond powder with atomized spherical electrolytic copper powder and combining it with relevant preparation processes, its lowest thermal conductivity is 292.4W / (m·k). When the surface copper-coated diamond powder is mixed with atomized spherical electrolytic copper powder and dried, its thermal conductivity is 253.3W / (m·k). It can be seen that by adopting the solution of this embodiment, the thermal conductivity of the diamond-reinforced copper-based material can be effectively improved.
[0103] Similarly, in this embodiment, by mixing titanium-coated diamond powder with atomized spherical electrolytic copper powder and combining the relevant preparation processes, the minimum sample thickness was 5.19 mm. When copper-coated diamond powder and atomized spherical electrolytic copper powder were mixed and dried, the sample thickness was 4.97 mm. This demonstrates that the solution of this embodiment can effectively increase the sample thickness of diamond-reinforced copper-based materials.
[0104] In summary, the products obtained in Examples 1-4 have higher thermal conductivity and better deposition effect.
[0105] The above description is merely a preferred embodiment of the present invention and does not constitute any limitation thereto. It should be noted that those skilled in the art may make various improvements and modifications without departing from the principles of the present invention, and such improvements and modifications shall also be considered within the scope of protection of the present invention.
Claims
1. A method for preparing a titanium-plated diamond-reinforced copper-based material, characterized in that: The following steps are involved: Mixing titanium-coated diamond powder with atomized spherical electrolytic copper powder, wherein the mass ratio of the atomized spherical electrolytic copper powder to the titanium-coated diamond powder is 80:20; The mixed powder is cold sprayed on a copper substrate to obtain a diamond-reinforced copper-based material layer on the surface of the copper substrate, wherein the temperature of the working gas used in the cold spraying is 500-700°C; In the diamond-reinforced copper-based material layer, the mass proportion of the surface titanium-plated diamond powder is 20%.
2. The preparation method according to claim 1, characterized in that The average thickness of the diamond-reinforced copper-based material layer is 2 to 10 mm.
3. The preparation method according to claim 1, characterized in that The particle size of the titanium-coated diamond powder is 60-120 μm, and the titanium coating amount is 10 wt % of the titanium-coated diamond powder.
4. The preparation method according to claim 3, characterized in that The particle size of the gas-atomized spherical electrolytic copper powder is 5 to 60 μm, the purity is ≥99.9%, and the oxygen content is ≤600 ppm.
5. The preparation method according to claim 1, characterized in that The working gas used in the cold spraying process is nitrogen, and the pressure of the working gas is 5 MPa.
6. The preparation method according to claim 5, characterized in that The purity of the nitrogen is 99.9% to 99.99%.
7. The preparation method according to claim 1 or 5, characterized in that The vertical distance between the muzzle of the cold spraying gun and the copper substrate is 20 mm, and the moving speed of the spray gun is 20 mm / s.
8. The preparation method according to claim 1, characterized in that Also includes: The obtained diamond-reinforced copper-based material layer is cut and separated from the copper substrate.
9. A diamond-reinforced copper-based material, characterized in that: The preparation method according to any one of claims 1 to 8 is used.
Citation Information
Patent Citations
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