CN108179302B - preparation method of high-thermal-conductivity diamond/copper composite material - Google Patents
preparation method of high-thermal-conductivity diamond/copper composite material Download PDFInfo
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- CN108179302B CN108179302B CN201810089819.8A CN201810089819A CN108179302B CN 108179302 B CN108179302 B CN 108179302B CN 201810089819 A CN201810089819 A CN 201810089819A CN 108179302 B CN108179302 B CN 108179302B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1005—Pretreatment of the non-metallic additives
- C22C1/1015—Pretreatment of the non-metallic additives by preparing or treating a non-metallic additive preform
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1005—Pretreatment of the non-metallic additives
- C22C1/1015—Pretreatment of the non-metallic additives by preparing or treating a non-metallic additive preform
- C22C1/1021—Pretreatment of the non-metallic additives by preparing or treating a non-metallic additive preform the preform being ceramic
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
Abstract
A preparation method of a high-thermal-conductivity diamond/copper composite material relates to a preparation method of a composite material. The invention aims to solve the problem that the existing preparation method of the diamond copper composite material cannot realize near-net-shape, high-quality and large-batch preparation of large-size sheet samples. The preparation method comprises the following steps: putting diamond powder into a mould, compacting to prepare a prefabricated body, placing the prefabricated body in a crucible, placing pure copper or massive copper alloy on the upper part of the prefabricated body, vacuumizing, heating to melt copper under the protection of inert gas, pressurizing and impregnating, maintaining pressure, cooling, releasing pressure, and finally demoulding. Has the advantages that: the method can realize high-efficiency mass production, has high mechanical property and high yield, can prepare large-size thin slice sample pieces, improves the thermal conductivity of the sample pieces, has low preparation cost and low impurity content, and can repeatedly use the forming die and the crucible. The invention is suitable for preparing the high-thermal-conductivity diamond/copper composite material.
Description
Technical Field
The invention relates to a preparation method of a composite material.
background
the high-quality diamond is a substance with the highest heat conductivity known in the world at present, can reach 1800 plus 2000W/(m.K), is an insulator at room temperature, has the characteristics of low dielectric constant, low thermal expansion coefficient and the like, but the single diamond is not easy to be made into a packaging material, has high cost, is ideally made into a metal-based composite material, the metal copper has excellent electric conductivity and heat conductivity, the heat conductivity of the metal copper is 404W/(m.K), the thermal expansion coefficient is 16.8 multiplied by 10 -6/K, and the diamond/copper-based composite material has the advantages of higher heat conductivity than the traditional metal alloy and aluminum nitride ceramic material, the thermal expansion coefficient is matched with a semiconductor material, the heat conductivity is matched with the seawater, the seawater is resistant to corrosion and fog and the like, so the electronic packaging material is suitable for the phased array radar packaging material, and the phased array packaging material.
The difficulty of the preparation of the diamond/copper-based composite material is as follows: (1) the wettability of diamond and copper is poor, and the wetting angle of diamond and copper is 145 degrees at 1150 ℃; (2) diamond and copper have no solid phase reaction at high temperature, and carbon has no solid solubility in copper, so that a compact composite material is difficult to sinter. The wettability of diamond and copper can be improved to a certain extent by modifying the surface of diamond, for example, adding a strong carbide forming element, but the modification also brings a new problem of increasing interface thermal resistance, and influences the thermal conductivity and the thermal expansion coefficient of the diamond/copper-based composite material. (3) The problem of diamond graphitization, diamond 773K or less may be completely graphitized in air. Under the vacuum condition, 970K-1670K diamond begins to generate partial graphitization phenomenon, and when the temperature is higher than 2070K, the diamond is completely graphitized.
The existing diamond reinforced copper-based composite material mainly comprises the following preparation methods: pressure infiltration method/high pressure infiltration method, SPS plasma discharge sintering method, powder metallurgy method, air pressure infiltration method, and the like. The thermal conductivity of the Diamond/CuCr0.8 composite material prepared by the Guo-Hongkong project group of Beijing institute of nonferrous metals is 620W/m.K. The equipment required by the pressure infiltration method is a vacuum hot-pressing infiltration furnace, and the pressure of gas required by the pressure infiltration method is megapascal (MPa). The Guo hong subject group of Beijing institute of nonferrous metals also adopts a high-pressure infiltration method to prepare a Diamond/CuCr0.8 composite material, the heat conductivity reaches 700W/m.K, the method enables partial Diamond to realize glomerocryst, but the Diamond is partially crushed in the preparation process of the method and can influence the stability and reliability of the material, the required equipment is special equipment, particularly six-side ultrahigh-pressure equipment, and the required pressure is gigapascal (GPa) level. And the prepared composite material is limited in small-size sample pieces for experiments, and large-scale batch production is not easy to realize. Northern Dajiacheng and the like also report a diamond composite material with high heat conductivity and low thermal expansion coefficient and a preparation method thereof, a high-temperature and high-pressure infiltration method is adopted, ultrahigh-pressure infiltration sintering is required to be carried out at 500-2000 ℃ and under the pressure of 2-8 GPa, and the method also belongs to a high-pressure infiltration method. The diamond/copper boron and diamond/copper zirconium composite material prepared by the high-temperature high-pressure infiltration method reported by HooJen et al of Beijing university of science and technology also belongs to a high-pressure infiltration method. Is limited by the volume of the internal cavity of the cubic apparatus, and the yield of the diamond/copper-based composite material prepared by adopting the high-pressure infiltration method is lower. The Spark Plasma Sintering (SPS) process has the advantages of high temperature rise speed, short preparation period and the like, but the composite material prepared by the method has low density, so the thermal conductivity is not high, and a sheet sample with the thickness less than 1mm is difficult to prepare. In the discharge sintering process, the upper pressure head and the lower pressure head are electrodes, and the sample is too thin, which is equivalent to short circuit, so that the sintering process with controlled temperature, time and pressure cannot be completed. Generally, when the material is prepared by the method, protective atmosphere is filled, the protective atmosphere is remained in the material, a large number of closed holes are reserved, and further, the density is low and the interface has pores, so that the thermal conductivity of the composite material is low. The reaction time of the powder metallurgy method is longer, and impurities are easily introduced in the ball milling and powder mixing process of the powder metallurgy method, so that the high-quality preparation of the diamond/copper-based composite material is difficult to realize; compared with other methods, particularly the air pressure infiltration method, the powder metallurgy method has the advantages that diamond powder is not tightly packed, so that the preparation of the diamond/copper-based composite material with high volume fraction is difficult. Compared with the material prepared by the air pressure infiltration method, the diamond/copper composite material prepared by the powder metallurgy method has lower thermal conductivity under the condition of the same diamond particle size and volume fraction. In summary, the existing preparation method of the diamond/copper composite material can not realize the near net shape of a large-size thin sheet sample and is difficult to realize the high-quality and large-batch preparation.
Disclosure of Invention
The invention aims to solve the problem that the existing preparation method of the diamond/copper composite material cannot realize near-net-shape, high-quality and large-batch preparation of large-size sheet samples, and provides a preparation method of a high-thermal-conductivity diamond/copper-based composite material.
the preparation method of the high-thermal-conductivity diamond/copper-based composite material is carried out according to the following steps:
the method comprises the following steps: weighing diamond raw powder coated with a coating layer on the surface, filling the diamond raw powder into a forming die, and performing tap compaction treatment to prepare a prefabricated body; placing the prefabricated body in a crucible, placing massive pure copper or massive copper alloy on the upper part of the prefabricated body in the crucible, and placing the crucible in an air pressure infiltration furnace;
Or weighing diamond raw powder, filling the diamond raw powder into a forming die, and performing compaction treatment to prepare a prefabricated body; placing the prefabricated body in a crucible, placing the massive copper alloy on the upper part of the prefabricated body in the crucible, and placing the crucible in an air pressure infiltration furnace;
during the vibration compaction treatment, the forming die is placed on an ultrasonic vibration plate and is vibrated for 5-15 minutes at the frequency of 20-30 kHz;
the material of the coating layer is W, Cr, Mo or Ti; the thickness of the coating layer is 50-5000 nm;
the diameter of the diamond powder raw powder or the diamond raw powder coated with the coating layer on the surface is 50-400 mu m;
the forming die is made of high-purity graphite or isostatic pressing graphite;
the crucible is made of high-purity graphite or isostatic pressing graphite;
the mass ratio of the blocky pure copper or blocky copper alloy to the diamond raw powder with the surface coated with the coating layer after the tap treatment is (0.85-2.07): 1;
the mass ratio of the massive copper alloy to the diamond raw powder after the jolt ramming treatment is (0.85-2.07): 1;
The bulk copper alloy is made of copper-zirconium alloy, copper-chromium alloy, copper-titanium alloy or copper-boron alloy;
Because copper and graphite are not wetted, the crucible and the forming die are not damaged in the contact process of the copper solution at high temperature and high pressure, and the forming die and the crucible can be repeatedly used;
step two: vacuumizing the air pressure infiltration furnace until the vacuum degree is 0.1-1 Pa;
wherein the purpose of vacuumizing is to exhaust residual gas in the preform;
step three: heating the air pressure infiltration furnace to 100-250 ℃ above the melting point of the blocky pure copper or blocky copper alloy under the protection of inert gas, and keeping the temperature for 1-3 h; the pressure intensity of the inert gas is 0.1-1 MPa;
introducing 0.1-1 MPa inert gas in the melting process of copper or copper alloy to prevent loss of the molten copper or copper alloy due to excessive evaporation, wherein the evaporation behavior of the copper or copper alloy is related to air pressure, and the higher the pressure is, the slower the evaporation speed is; melting pure copper or copper alloy in an inert gas protective atmosphere and keeping the pure copper or copper alloy in a molten state, and meanwhile, enabling the copper or copper alloy melt to flow downwards into a crucible to wrap the prefabricated body and isolate gas;
step four: introducing inert gas into the air pressure infiltration furnace, maintaining the pressure, cooling after the pressure maintaining is finished, releasing the pressure and demolding to finish the process;
The pressure of the inert gas is 1-10 MPa; the pressure maintaining time is 10 min-3 h; the cooling speed is 3-5 ℃/min;
and introducing high-pressure inert gas into the air pressure infiltration furnace and maintaining the pressure to enable the molten pure copper or copper alloy melt to flow into the forming die from the gate of the forming die and infiltrate into the gaps of the diamond powder.
The principle and the beneficial effects of the invention are as follows:
1. the invention adopts the air pressure infiltration and near net forming process to make diamond powder and the die into a prefabricated body, thereby having high forming precision and uniform stress. Compared with the existing high-pressure infiltration technology which adopts GPa-grade pressure and six-surface-top equipment to prepare the composite material, the method has small pressure, protects the sample piece through the die, does not damage the sample piece, and ensures that the sample piece does not generate internal cracks in the preparation process, so the preparation yield is high, the preparation efficiency is high, the high-quality mass production of large-size thin-sheet sample pieces required by wide practical application can be realized, and the thickness of the sample piece prepared by the method is 0.5-3 mm; compared with a six-side-jacking device, the air pressure infiltration furnace has the advantages that the furnace inner space is large, and high-efficiency mass production can be realized by reasonably arranging the positions of the sample pieces and designing the die;
2. The diamond/copper composite material prepared by the prior art has weak interface combination, and the interface layer has pores or is discontinuous, so that the thermal conductivity and the mechanical property of the composite material are very low, and the thermal expansion coefficient is very high. In the process of preparing the high-thermal-conductivity diamond/copper composite material, the diamond reinforcement body reacts with the coating elements to generate coating element carbide, and the diamond reinforcement body reacts with the elements in the alloy to generate alloy element carbide, so that a compact and continuous carbide interface layer is generated on the interface layer of the diamond reinforcement body and the matrix alloy. The interface combination between the reinforcement and the matrix is promoted, and the interface thermal resistance is reduced, so that the thermal conductivity of the integral composite material is improved;
3. the high-thermal-conductivity diamond/copper composite material prepared by plating a titanium layer with the thickness of 1000 nanometers on the surface of diamond powder with the particle size of 100 micrometers and compounding the titanium layer with CuCr0.5 alloy has the thermal conductivity of 530W/m.K, and the average thermal expansion coefficient of 6.5 multiplied by 10 -6/K when the ambient temperature is 30-100 ℃;
4. the method prevents the loss of the molten copper or copper alloy due to excessive evaporation by heating in a protective atmosphere, greatly reduces the consumption of the copper or copper alloy and reduces the preparation cost of the composite material;
5. the invention removes the residual gas in the prefabricated body and the alloy by vacuumizing before infiltration; then, the alloy melt completely wraps the prefabricated body and isolates gas through gas pressurization and permeation, and then the alloy fully permeates into the prefabricated body under the air pressure; finally, the solidification process is effectively fed by pressure maintaining and cooling, and shrinkage cavities in the composite material are avoided;
6. in the preparation process of the prefabricated body, no binder is added, so that the impurity content is low;
7. because copper and graphite are not wet, the crucible and the forming mold which are made of high-purity graphite or isostatic pressure graphite are not damaged in the contact process of the crucible and the forming mold with the copper solution at high temperature and high pressure, and the forming mold and the crucible can be repeatedly used;
8. When the existing diamond/copper composite material is prepared, if the volume fraction of the diamond reinforcement body is too high, the channel for alloy melt to flow is narrower, pores are easy to form, the density of the material is further reduced, and the thermal conductivity and the mechanical property of the prepared diamond/copper composite material are also reduced. Because the temperature field is uniformly and stably controlled to be 100-250 ℃ above the melting point of pure copper or copper alloy and the melt of the copper or copper alloy has good fluidity, the diamond/copper composite material with the diamond powder reinforcement with the highest volume fraction of 75% can be prepared, the volume fraction of the diamond powder reinforcement is improved, the tissue structure is not damaged, and the thermophysical property and the mechanical property of the diamond/copper composite material are not influenced.
Drawings
FIG. 1 is a schematic view showing a process for producing a highly thermally conductive diamond/copper composite member according to example 1; in the figure, step a is a state when the bulk copper alloy in the atmospheric pressure infiltration furnace is not melted, step b is a state when the bulk copper alloy in the atmospheric pressure infiltration furnace is melted, and step c is a state after the bulk copper alloy in the atmospheric pressure infiltration furnace is solidified, and in the figure, 1 represents the atmospheric pressure infiltration furnace, 2 represents the preform core mold, 3 represents the crucible, and 4 represents the bulk copper alloy;
Fig. 2 is a schematic structural view of a forming mold used in the process of preparing the high thermal conductivity diamond/copper composite material and the member in example 1, in which fig. 1 is a gate, 2 is a mold cavity, and 3 is a mold main body;
FIG. 3 is a photograph of a fracture scan of the high thermal conductive diamond/copper composite prepared in example 1;
FIG. 4 is a graph of the interface morphology of the high thermal conductivity diamond/copper composite material prepared in example 1, wherein 1 is chromium carbide and 2 is titanium carbide;
Fig. 5 is a three-point bending performance graph of the high thermal conductive diamond/copper composite materials prepared in example 1 and comparative example 1, in which curve 1 is a three-point bending performance curve of the high thermal conductive diamond/copper composite material prepared in example 1, and curve 2 is a three-point bending performance curve of the diamond/copper composite material prepared in comparative example 1;
FIG. 6 is a graph of the interface morphology of the high thermal conductivity diamond/copper composite material prepared in example 2, wherein 1 is chromium carbide and 2 is tungsten carbide;
FIG. 7 is a side view of a high thermal conductivity diamond/copper composite member prepared in example 2;
FIG. 8 is a schematic representation of a high thermal conductivity diamond/copper composite member prepared in example 2;
fig. 9 is an interface topography of the high thermal conductivity diamond/copper composite prepared in example 5, in which fig. 1 is chromium carbide.
the specific implementation mode is as follows:
the technical scheme of the invention is not limited to the specific embodiments listed below, and any reasonable combination of the specific embodiments is included.
the first embodiment is as follows: the preparation method of the high-thermal-conductivity diamond/copper composite material is carried out according to the following steps:
The method comprises the following steps: weighing diamond raw powder coated with a coating layer on the surface, filling the diamond raw powder into a forming die, and performing tap compaction treatment to prepare a prefabricated body; placing the prefabricated body in a crucible, placing massive pure copper or massive copper alloy on the upper part of the prefabricated body in the crucible, and placing the crucible in an air pressure infiltration furnace; or weighing diamond raw powder, filling the diamond raw powder into a forming die, and performing compaction treatment to prepare a prefabricated body; placing the prefabricated body in a crucible, placing the massive copper alloy on the upper part of the prefabricated body in the crucible, and placing the crucible in an air pressure infiltration furnace;
the forming die is made of high-purity graphite or isostatic pressing graphite;
the crucible is made of high-purity graphite or isostatic pressing graphite;
step two: vacuumizing the air pressure infiltration furnace until the vacuum degree is 0.1-1 Pa;
step three: heating the air pressure infiltration furnace to 100-250 ℃ above the melting point of the blocky pure copper or blocky copper alloy under the protection of inert gas, and keeping the temperature for 1-3 h;
the pressure intensity of the inert gas is 0.1-1 MPa;
step four: introducing inert gas into the air pressure infiltration furnace, maintaining the pressure, cooling after the pressure maintaining is finished, releasing the pressure and demolding to finish the process;
the pressure of the inert gas is 1-10 MPa;
The pressure maintaining time is 10 min-3 h.
the principle and the beneficial effects of the implementation mode are as follows:
1. the embodiment adopts the air pressure infiltration and near net forming process, diamond powder and a die are made into a prefabricated body, the forming precision is high, and the stress is uniform. Compared with the existing high-pressure infiltration technology which adopts GPa-grade pressure and six-surface-top equipment to prepare the composite material, the method of the embodiment has small pressure, protects the sample piece through the die, does not damage the sample piece, and ensures that the sample piece does not generate internal cracks in the preparation process, so the preparation yield is high, the preparation efficiency is high, the high-quality mass production of large-size thin-sheet sample pieces required by wide practical application can be realized, and the thickness of the sample piece prepared by the embodiment is 0.5-3 mm; compared with a six-side-top device, the air pressure infiltration furnace used in the embodiment has a large furnace space, and high-efficiency mass production can be realized by reasonably arranging the positions of the sample pieces and designing the die;
2. the diamond/copper composite material prepared by the prior art has weak interface combination, and the interface layer has pores or is discontinuous, so that the thermal conductivity and the mechanical property of the composite material are very low, and the thermal expansion coefficient is very high. In the process of preparing the high-thermal-conductivity diamond/copper composite material, the diamond reinforcement body reacts with the coating elements to generate coating element carbide, and the diamond reinforcement body reacts with the elements in the alloy to generate alloy element carbide, so that a compact and continuous carbide interface layer is generated on the interface layer of the diamond reinforcement body and the matrix alloy. The interface combination between the reinforcement and the matrix is promoted, and the interface thermal resistance is reduced, so that the thermal conductivity of the integral composite material is improved;
3. the high-thermal-conductivity diamond/copper composite material prepared by plating a titanium layer with the thickness of 1000 nanometers on the surface of diamond powder with the particle size of 100 micrometers and compounding the titanium layer with CuCr0.5 alloy has the thermal conductivity of 530W/m.K, and the average thermal expansion coefficient of 6.5 multiplied by 10 -6/K when the ambient temperature is 30-100 ℃;
4. according to the method, the molten copper or copper alloy is prevented from being excessively evaporated and lost by heating in the protective atmosphere, so that the using amount of the copper or copper alloy is greatly reduced, and the preparation cost of the composite material is reduced;
5. in the embodiment, residual gas in the prefabricated body and the alloy is removed by vacuumizing before permeation; then, the alloy melt completely wraps the prefabricated body and isolates gas through gas pressurization and permeation, and then the alloy fully permeates into the prefabricated body under the air pressure; finally, the solidification process is effectively fed by pressure maintaining and cooling, and shrinkage cavities in the composite material are avoided;
6. in the preparation process of the preform in the embodiment, no binder is added, so that the impurity content is low;
7. because copper and graphite are not wet, the crucible and the forming mold which are made of high-purity graphite or isostatic pressure graphite are not damaged in the contact process of the crucible and the forming mold with the copper solution at high temperature and high pressure, and the forming mold and the crucible can be repeatedly used;
8. When the existing diamond/copper composite material is prepared, if the volume fraction of the diamond reinforcement body is too high, the channel for alloy melt to flow is narrower, pores are easy to form, the density of the material is further reduced, and the thermal conductivity and the mechanical property of the prepared diamond/copper composite material are also reduced. In the embodiment, the temperature field is uniformly and stably controlled to be 100-250 ℃ above the melting point of pure copper or copper alloy, and the copper or copper alloy melt has good fluidity, so that the diamond/copper composite material with the diamond powder reinforcement body with the highest volume fraction of 75% can be prepared, the volume fraction of the diamond powder reinforcement body is improved, the tissue structure is not damaged, and the thermophysical property and the mechanical property of the diamond/copper composite material are not influenced.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: step one, the mass ratio of the massive pure copper or the massive copper alloy to the diamond raw powder which is subjected to the tap treatment and is coated with the coating layer on the surface is (0.85-2.07): 1. other steps and parameters are the same as in the first embodiment.
the third concrete implementation mode: step one, the mass ratio of the massive copper alloy to the diamond raw powder after the tap treatment is (0.85-2.07): 1. other steps and parameters are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: and step one, during the compaction treatment, placing the forming die on an ultrasonic oscillation plate, and vibrating for 5-15 minutes at the frequency of 20-30 kHz. Other steps and parameters are the same as in one of the first to third embodiments.
the fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: step one, the diameter of the diamond powder raw powder or the diamond powder coated with the coating layer on the surface is 50-400 mu m. Other steps and parameters are the same as in one of the first to fourth embodiments.
the sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: : the material of the bulk copper alloy in the first step is copper-zirconium alloy, copper-chromium alloy, copper-titanium alloy or copper-boron alloy. Other steps and parameters are the same as in one of the first to fifth embodiments.
the seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: step one, the material of the coating layer is W, Cr, Mo or Ti. Other steps and parameters are the same as in one of the first to sixth embodiments.
the specific implementation mode is eight: the present embodiment differs from one of the first to seventh embodiments in that: step one, the thickness of the coating layer is 50-5000 nm. Other steps and parameters are the same as in one of the first to seventh embodiments.
the specific implementation method nine: the present embodiment differs from the first to eighth embodiments in that: and step three, heating the air pressure infiltration furnace to 250 ℃ above the melting point of the blocky pure copper or blocky copper alloy under the protection of inert gas, and keeping the temperature for 2 hours. Other steps and parameters are the same as in one of the first to eighth embodiments.
the detailed implementation mode is ten: the present embodiment differs from one of the first to ninth embodiments in that: and fourthly, the cooling speed is 3-5 ℃/min. Other steps and parameters are the same as in one of the first to ninth embodiments.
the following examples were used to demonstrate the beneficial effects of the present invention:
example 1:
the preparation method of the high-thermal-conductivity diamond/copper-based composite material is carried out according to the following steps:
the method comprises the following steps: weighing diamond raw powder coated with a coating layer on the surface, filling the diamond raw powder into a forming die, and performing tap compaction treatment to prepare a prefabricated body; placing the prefabricated body in a crucible, placing the massive copper alloy on the upper part of the prefabricated body in the crucible, and placing the crucible in an air pressure infiltration furnace;
during the vibration compaction treatment, the forming die is placed on an ultrasonic vibration plate and is vibrated for 10 minutes at the frequency of 28 kHz;
the coating layer is made of Ti;
The thickness of the coating layer is 1000 nm;
The diameter of the diamond raw powder coated with the coating layer on the surface is 100 mu m;
the forming die is made of high-purity graphite;
the crucible is made of high-purity graphite;
the mass ratio of the massive copper alloy to the diamond raw powder which is subjected to the tap compaction and coated with the coating layer on the surface is 1.37: 1;
the bulk copper alloy is made of 0.5-1.1 wt.% chromium-containing copper-chromium alloy;
step two: vacuumizing the air pressure infiltration furnace until the vacuum degree is 1 Pa;
Step three: heating the air pressure infiltration furnace to 1200 ℃ above the melting point of the blocky pure copper or blocky copper alloy under the protection of inert gas, and preserving heat for 1 h; the pressure intensity of the inert gas is 0.1 MPa;
Step four: introducing inert gas into the air pressure infiltration furnace, maintaining the pressure, cooling after the pressure maintaining is finished, releasing the pressure and demolding to finish the process;
The pressure of the inert gas is 1 MPa; the pressure maintaining time is 1 h; the cooling speed is 3 ℃/min;
The density of the diamond/copper-based composite material prepared by the embodiment is 5.53g/cm 3, the volume fraction of the diamond reinforcement in the composite material is 62%, the thermal diffusivity of the composite material is 220.598/mm 2, the thermal conductivity is 530W/m.K, the average thermal expansion coefficient from room temperature (30 ℃) to 100 ℃ is 6.5 x 10 -6/K, the average thermal expansion coefficient from room temperature (30 ℃) to 200 ℃ is 6.8 x 10 -6/K, and the bending strength is 320 MPa.
FIG. 1 is a schematic view showing a process for producing a highly thermally conductive diamond/copper composite member according to example 1; in the figure, step a is a state when the bulk copper alloy in the atmospheric pressure infiltration furnace is not melted, step b is a state when the bulk copper alloy in the atmospheric pressure infiltration furnace is melted, and step c is a state after the bulk copper alloy in the atmospheric pressure infiltration furnace is solidified, and in the figure, 1 represents the atmospheric pressure infiltration furnace, 2 represents the preform core mold, 3 represents the crucible, and 4 represents the bulk copper alloy; fig. 2 is a schematic structural view of a forming mold used in the process of preparing the high thermal conductivity diamond/copper composite material and the member in example 1, in which fig. 1 is a gate, 2 is a mold cavity, and 3 is a mold main body; FIG. 3 is a photograph of a fracture scan of the high thermal conductive diamond/copper composite prepared in example 1; as seen from fig. 3, the copper-chromium alloy was adhered to the diamond particles, and thus in the high thermal conductive diamond/copper composite material prepared in example 1, titanium plating improved the wettability of diamond and copper; FIG. 4 is a graph of the interface morphology of the high thermal conductivity diamond/copper composite material prepared in example 1, wherein 1 is chromium carbide and 2 is titanium carbide; as shown in fig. 4, the diamond/copper-chromium alloy interface layer of the high thermal conductivity diamond/copper composite material is composed of two layers of carbide, namely titanium carbide and chromium carbide, the titanium carbide layer is on the inner side, the titanium carbide crystal grains are fine and discontinuous, the thickness of the titanium carbide layer is about 200-700 nm, and the titanium carbide layer grows towards one side of the diamond; the chromium carbide layer is arranged on the outer side, the chromium carbide grains are thick and continuous, the thickness of the chromium carbide layer is 0.6-1.6 mu m, and the chromium carbide layer grows towards one side of the copper alloy;
comparative example 1:
the preparation method of the high-thermal-conductivity diamond/copper-based composite material comprises the following steps:
The method comprises the following steps: weighing diamond powder raw powder, filling the diamond powder raw powder into a forming die, and performing compaction treatment to prepare a prefabricated body; placing the prefabricated body in a crucible, placing massive pure copper on the upper part of the prefabricated body in the crucible, and placing the crucible in an air pressure infiltration furnace;
during the vibration compaction treatment, the forming die is placed on an ultrasonic vibration plate and is vibrated for 10 minutes at the frequency of 28 kHz;
the diameter of the diamond powder raw powder is 100 mu m;
The forming die is made of high-purity graphite;
the crucible is made of high-purity graphite;
The mass ratio of the massive pure copper to the diamond raw powder after the tap treatment is 1.37: 1;
step two: vacuumizing the air pressure infiltration furnace until the vacuum degree is 1 Pa;
step three: heating the air pressure infiltration furnace to 1200 ℃ above the melting point of the massive pure copper under the protection of inert gas, and preserving heat for 1 h; the pressure intensity of the inert gas is 0.1 MPa;
step four: introducing inert gas into the air pressure infiltration furnace, maintaining the pressure, cooling after the pressure maintaining is finished, releasing the pressure and demolding to finish the process;
the pressure of the inert gas is 1 MPa; the pressure maintaining time is 1 h; the cooling speed is 3 ℃/min;
The diamond/copper-based composite material prepared in comparative example 1 had a density of 5.39g/cm 3, a thermal diffusivity of 83.784/mm 2, a thermal conductivity of 197.567W/m.K, an average thermal expansion coefficient of 13.1X 10 -6/K at room temperature (30 ℃) to 100 ℃, an average thermal expansion coefficient of 15.4X 10 -6/K at room temperature (30 ℃) to 200 ℃, and a bending strength of 56 MPa.
fig. 5 is a three-point bending performance graph of the high thermal conductive diamond/copper composite materials prepared in example 1 and comparative example 1, in which curve 1 is a three-point bending performance curve of the high thermal conductive diamond/copper composite material prepared in example 1, and curve 2 is a three-point bending performance curve of the diamond/copper composite material prepared in comparative example 1;
as can be seen in fig. 5, the mechanical properties of the high thermal conductivity diamond/copper composite material prepared in example 1 are significantly improved after the interface is improved;
example 2:
The preparation method of the high-thermal-conductivity diamond/copper-based composite material is carried out according to the following steps:
the method comprises the following steps: weighing diamond raw powder coated with a coating layer on the surface, filling the diamond raw powder into a forming die, and performing tap compaction treatment to prepare a prefabricated body; placing the prefabricated body in a crucible, placing the massive copper alloy on the upper part of the prefabricated body in the crucible, and placing the crucible in an air pressure infiltration furnace;
during the vibration compaction treatment, the forming die is placed on an ultrasonic vibration plate and is vibrated for 10 minutes at the frequency of 28 kHz;
the coating layer is made of W;
the thickness of the coating layer is 100 nm;
the diameter of the diamond raw powder coated with the coating layer on the surface is 100 mu m;
the forming die is made of high-purity graphite;
the crucible is made of high-purity graphite;
the mass ratio of the bulk copper alloy to the diamond raw powder with the surface coated with the coating layer after the tap treatment is 1.69: 1;
The bulk copper alloy is made of 0.5-1.1 wt.% chromium-containing copper-chromium alloy;
step two: vacuumizing the air pressure infiltration furnace until the vacuum degree is 1 Pa;
step three: heating the air pressure infiltration furnace to 1300 ℃ above the melting point of the blocky pure copper or blocky copper alloy under the protection of inert gas, and preserving heat for 1 h; the pressure intensity of the inert gas is 0.1 MPa;
step four: introducing inert gas into the air pressure infiltration furnace, maintaining the pressure, cooling after the pressure maintaining is finished, releasing the pressure and demolding to finish the process;
The pressure of the inert gas is 1 MPa; the pressure maintaining time is 1 h; the cooling speed is 3 ℃/min;
the volume fraction of diamond reinforcement in the composite material prepared in example 2 is 65.3%, the density of the composite material is 5.37g/cm 3, the thermal diffusivity is 226.478/mm 2, the thermal conductivity is 533W/m.K, and the thermal expansion coefficient is 8.5 multiplied by 10 -6/K, fig. 6 is an interface morphology graph of the high thermal conductivity diamond/copper composite material prepared in example 2, 1 is chromium carbide and 2 is tungsten carbide, fig. 6 shows that the interface layer of the diamond/copper-chromium alloy in the high thermal conductivity diamond/copper composite material prepared in example 2 is composed of tungsten carbide and chromium carbide, fig. 7 is a lateral real object graph of the high thermal conductivity diamond/copper composite material prepared in example 2, fig. 8 is a front view of the high thermal conductivity diamond/copper composite material prepared in example 2, and the high thermal conductivity diamond/copper composite material prepared in example 2 is a square sheet shape, the thickness is 1.54mm, and the side length of the square is 80 mm.
example 3:
the preparation method of the high-thermal-conductivity diamond/copper-based composite material is carried out according to the following steps:
the method comprises the following steps: weighing diamond raw powder coated with a coating layer on the surface, filling the diamond raw powder into a forming die, and performing tap compaction treatment to prepare a prefabricated body; placing the prefabricated body in a crucible, placing the massive copper alloy on the upper part of the prefabricated body in the crucible, and placing the crucible in an air pressure infiltration furnace;
during the vibration compaction treatment, the forming die is placed on an ultrasonic vibration plate and is vibrated for 10 minutes at the frequency of 28 kHz;
The coating layer is made of Cr;
the thickness of the coating layer is 100 nm;
The diameter of the diamond raw powder coated with the coating layer on the surface is 100 mu m;
The forming die is made of high-purity graphite;
the crucible is made of high-purity graphite;
The mass ratio of the bulk copper alloy to the diamond raw powder with the surface coated with the coating layer after the tap treatment is 2.07: 1;
the bulk copper alloy is made of 0.5-1.1 wt.% chromium-containing copper-chromium alloy;
step two: vacuumizing the air pressure infiltration furnace until the vacuum degree is 1 Pa;
step three: heating the air pressure infiltration furnace to 1200 ℃ above the melting point of the blocky pure copper or blocky copper alloy under the protection of inert gas, and preserving heat for 1 h; the pressure intensity of the inert gas is 0.1 MPa;
step four: introducing inert gas into the air pressure infiltration furnace, maintaining the pressure, cooling after the pressure maintaining is finished, releasing the pressure and demolding to finish the process;
the pressure of the inert gas is 1 MPa; the pressure maintaining time is 10 min; the cooling speed is 3 ℃/min;
the high-thermal-conductivity diamond/copper composite material member prepared in example 3 is in the shape of a square sheet, the thickness of the diamond/copper composite material member is 0.8mm, the side length of the square sheet is 100mm, the volume fraction of the diamond reinforcement in the composite material is 65%, the density of the composite material is 5.38g/cm 3, the thermal diffusion coefficient is 195.748/mm 2, the thermal conductivity is 461W/m.K, and the thermal expansion coefficient is 7.5 multiplied by 10 -6/K.
example 4:
the preparation method of the high-thermal-conductivity diamond/copper-based composite material is carried out according to the following steps:
The method comprises the following steps: weighing diamond raw powder coated with a coating layer on the surface, filling the diamond raw powder into a forming die, and performing tap compaction treatment to prepare a prefabricated body; placing the prefabricated body in a crucible, placing the massive copper alloy on the upper part of the prefabricated body in the crucible, and placing the crucible in an air pressure infiltration furnace;
During the vibration compaction treatment, the forming die is placed on an ultrasonic vibration plate and is vibrated for 10 minutes at the frequency of 28 kHz;
the material of the coating layer is Mo;
the thickness of the coating layer is 100 nm;
the diameter of the diamond raw powder coated with the coating layer on the surface is 100 mu m;
The forming die is made of high-purity graphite;
the crucible is made of high-purity graphite;
the mass ratio of the massive copper alloy to the diamond raw powder which is subjected to the tap treatment and is coated with the coating layer on the surface is 0.85: 1;
the bulk copper alloy is made of 0.5-1.1 wt.% chromium-containing copper-chromium alloy;
Step two: vacuumizing the air pressure infiltration furnace until the vacuum degree is 1 Pa;
step three: heating the air pressure infiltration furnace to 1300 ℃ above the melting point of the blocky pure copper or blocky copper alloy under the protection of inert gas, and preserving heat for 1 h; the pressure intensity of the inert gas is 0.1 MPa;
step four: introducing inert gas into the air pressure infiltration furnace, maintaining the pressure, cooling after the pressure maintaining is finished, releasing the pressure and demolding to finish the process;
the pressure of the inert gas is 1 MPa; the pressure maintaining time is 10 min; the cooling speed is 3 ℃/min;
the diamond/copper composite material component with high thermal conductivity prepared in the embodiment 4 is in a square sheet shape, the thickness of the diamond/copper composite material component is 1.0mm, the side length of a square is 100mm, the volume fraction of a diamond reinforcement in the composite material is 65%, the density of the composite material is 5.39g/cm 3, the thermal diffusion coefficient is 182.239/mm 2, the thermal conductivity is 430W/m.K, and the thermal expansion coefficient is 9.8 multiplied by 10 -6/K;
Example 5:
the preparation method of the high-thermal-conductivity diamond/copper-based composite material is carried out according to the following steps:
the method comprises the following steps: weighing diamond raw powder, filling the diamond raw powder into a forming die, and performing compaction treatment to prepare a prefabricated body; placing the prefabricated body in a crucible, placing the massive copper alloy on the upper part of the prefabricated body in the crucible, and placing the crucible in an air pressure infiltration furnace;
during the vibration compaction treatment, the forming die is placed on an ultrasonic vibration plate and is vibrated for 10 minutes at the frequency of 28 kHz;
the diameter of the diamond raw powder is 100 mu m;
the forming die is made of high-purity graphite;
the crucible is made of high-purity graphite;
The mass ratio of the massive copper alloy to the diamond raw powder which is subjected to the tap compaction and coated with the coating layer on the surface is 1.09: 1;
the bulk copper alloy is made of 0.5-1.1 wt.% chromium-containing copper-chromium alloy;
step two: vacuumizing the air pressure infiltration furnace until the vacuum degree is 1 Pa;
step three: heating the air pressure infiltration furnace to 1300 ℃ above the melting point of the blocky pure copper or blocky copper alloy under the protection of inert gas, and preserving heat for 1 h; the pressure intensity of the inert gas is 0.1 MPa;
Step four: introducing inert gas into the air pressure infiltration furnace, maintaining the pressure, cooling after the pressure maintaining is finished, releasing the pressure and demolding to finish the process;
The pressure of the inert gas is 1 MPa; the pressure maintaining time is 10 min; the cooling speed is 3 ℃/min;
the high-thermal-conductivity diamond/copper composite material member prepared in example 5 is in a square sheet shape, the thickness of the diamond/copper composite material member is 1.0mm, the side length of a square is 100mm, the volume fraction of diamond reinforcement in the composite material is 65%, the density of the composite material is 5.39g/cm 3, the thermal diffusivity is 218.492/mm 2, the thermal conductivity is 515W/m.K, and the thermal expansion coefficient is 7.2 × 10 -6/K, and fig. 9 is an interface morphology diagram of the high-thermal-conductivity diamond/copper composite material prepared in example 5, wherein 1 in the diagram is chromium carbide.
Claims (8)
1. a preparation method of a high-thermal-conductivity diamond/copper composite material is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: weighing diamond powder, filling the diamond powder into a forming die, and performing compaction treatment to prepare a prefabricated body;
during the vibration compaction treatment, the forming die is placed on an ultrasonic vibration plate and is vibrated for 5 ~ 15 minutes at the frequency of 20 ~ 30kHz 30;
The surface of the diamond powder is coated with a coating layer;
the material of the coating layer is W, Cr, Mo or Ti;
step two: placing the prefabricated body in a crucible, placing massive pure copper or massive copper alloy on the upper part of the prefabricated body in the crucible, and placing the crucible in an air pressure infiltration furnace;
the forming die is made of high-purity graphite or isostatic pressing graphite;
the crucible is made of high-purity graphite or isostatic pressing graphite;
the bulk copper alloy is made of copper-zirconium alloy, copper-chromium alloy, copper-titanium alloy or copper-boron alloy;
the mass ratio of the bulk copper alloy to the diamond powder after the tap treatment is (0.85 ~ 2.07.07) to 1;
step three, vacuumizing the air pressure infiltration furnace until the vacuum degree is 0.1 ~ 1 Pa;
step four, heating the air pressure infiltration furnace to 100 ~ 250 ℃ above the melting point of the blocky pure copper or the blocky copper alloy under the protection of inert gas, and preserving heat for 1h ~ 3h, wherein the pressure of the inert gas is 0.1 ~ 1 MPa;
introducing inert gas into the air pressure infiltration furnace, maintaining the pressure, cooling after the pressure maintaining is finished, relieving the pressure and demolding to obtain a square flaky high-heat-conductivity diamond/copper composite material member with the side length of 100mm and the thickness of 0.5 ~ 3 mm;
The pressure of the inert gas is 1 ~ 10MPa, and the pressure maintaining time is 10min ~ 3 h.
2. the method for preparing a diamond/copper composite material with high thermal conductivity as claimed in claim 1, wherein the thickness of the coating layer in the first step is 50 ~ 5000 nm.
3. the method for preparing a diamond/copper composite material with high thermal conductivity according to claim 1, wherein the diameter of the diamond powder in the first step is 50 ~ 400 μm.
4. the method for preparing a diamond/copper composite material with high thermal conductivity according to claim 1, wherein the cooling rate in the fifth step is 3 ~ 5 ℃/min.
5. a preparation method of a high-thermal-conductivity diamond/copper composite material is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: weighing diamond powder, filling the diamond powder into a forming die, and performing compaction treatment to prepare a prefabricated body;
During the vibration compaction treatment, the forming die is placed on an ultrasonic vibration plate and is vibrated for 5 ~ 15 minutes at the frequency of 20 ~ 30kHz 30;
The diamond powder is raw diamond powder;
Step two: placing the prefabricated body in a crucible, placing the massive copper alloy on the upper part of the prefabricated body in the crucible, and placing the crucible in an air pressure infiltration furnace;
the forming die is made of high-purity graphite or isostatic pressing graphite; the crucible is made of high-purity graphite or isostatic pressing graphite;
the bulk copper alloy is made of copper-zirconium alloy, copper-chromium alloy, copper-titanium alloy or copper-boron alloy;
the mass ratio of the bulk copper alloy to the diamond powder after the tap treatment is (0.85 ~ 2.07.07) to 1;
step three, vacuumizing the air pressure infiltration furnace until the vacuum degree is 0.1 ~ 1 Pa;
Step four, heating the air pressure infiltration furnace to 100 ~ 250 ℃ above the melting point of the bulk copper alloy under the protection of inert gas, and preserving heat for 1h ~ 3h, wherein the pressure of the inert gas is 0.1 ~ 1 MPa;
introducing inert gas into the air pressure infiltration furnace, maintaining the pressure, cooling after the pressure maintaining is finished, relieving the pressure and demolding to obtain a square flaky high-heat-conductivity diamond/copper composite material member with the side length of 100mm and the thickness of 0.5 ~ 3 mm;
The pressure of the inert gas is 1 ~ 10MPa, and the pressure maintaining time is 10min ~ 3 h.
6. the method for preparing a high thermal conductive diamond/copper composite material according to claim 5, wherein: step one, during the compaction treatment, the forming die is placed on an ultrasonic oscillation plate and vibrated for 10 minutes at the frequency of 28 kHz.
7. the method for preparing a diamond/copper composite material with high thermal conductivity according to claim 5, wherein the diameter of the diamond powder in the first step is 50 ~ 400 μm.
8. the method for preparing a diamond/copper composite material with high thermal conductivity according to claim 5, wherein the cooling rate in the fifth step is 3 ~ 5 ℃/min.
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