CN112935249A - Efficient preparation method of diamond/metal-based composite material - Google Patents

Efficient preparation method of diamond/metal-based composite material Download PDF

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CN112935249A
CN112935249A CN202110186963.5A CN202110186963A CN112935249A CN 112935249 A CN112935249 A CN 112935249A CN 202110186963 A CN202110186963 A CN 202110186963A CN 112935249 A CN112935249 A CN 112935249A
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diamond
temperature
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coating
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CN112935249B (en
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梁雪
李会
杨文澍
修子扬
武高辉
陈国钦
周畅
芶华松
姜龙涛
康鹏超
乔菁
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Harbin Institute of Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02—Compacting only
    • B22F3/093—Compacting only using vibrations or friction
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D23/00—Casting processes not provided for in groups B22D1/00 - B22D21/00
    • B22D23/04—Casting by dipping
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • 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
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • B22F2003/248—Thermal after-treatment

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Abstract

An efficient preparation method of a diamond/metal matrix composite material relates to a preparation method of a diamond/metal matrix composite material. The method aims to solve the problems that the existing method for preparing the carbide coating on the surface of the diamond has large energy loss, the diamond is easy to be graphitized and the process is complex. Weighing diamond powder with a metal coating, filling the diamond powder into a graphite mould, compacting, performing low-temperature diffusion treatment and high-temperature reaction treatment, and infiltrating under air pressure. According to the invention, the diamond is subjected to low-temperature long-time diffusion and high-temperature short-time reaction treatment by changing a preheating temperature curve, the high-temperature short-time reaction avoids the diamond from graphitizing, a compact carbide coating is synthesized in situ on the surface of the diamond in the preparation process of the composite material, the energy loss is reduced, the process is simple, the efficiency is high, the product quality and stability are easy to control, the cost is low, and the industrial production and application are easy to realize. The invention is suitable for preparing diamond/metal matrix composite materials.

Description

Efficient preparation method of diamond/metal-based composite material
Technical Field
The invention relates to a preparation method of a diamond/metal matrix composite material.
Background
With the rapid development of semiconductor technology, the integration level of electronic components is higher and higher, electronic power devices are gradually developed towards miniaturization, light weight and high power density, and the heat dissipation problem becomes the key for restricting the efficiency and reliability of electronic equipment. The traditional materials such as Invar, Kovar alloy, W-Cu, Mo-Cu and the like have the defects of low heat conductivity and high density; SiCpThe composite material such as/Al has the advantages of low density, adjustable thermal expansion coefficient and the like, but at present, the thermal conductivity (lower than 250W/(m.K)) of the composite material is difficult to meet the increasing heat dissipation requirement. The diamond has the advantages of excellent heat-conducting property, low thermal expansion coefficient, low density and the like, the reinforced metal-based composite material has ultrahigh thermal conductivity and thermal expansion coefficient matched with a semiconductor substrate, can meet the heat dissipation requirement of ultrahigh-power electronic components, and is a hotspot of the current heat management material research。
In practical application, the heat-dissipating performance of the heat-management material is required to be good, and the stability of the material is also required to be high. At present, the main problems of the diamond/metal matrix composite material are that the interface bonding of diamond and metal is weak and the debonding is easy. On one hand, the debonding interface can cause the interface thermal resistance of the composite material to be improved, so that the heat conducting performance of the composite material is reduced; on the other hand, the debonded interface may also act as a crack source, thereby reducing the reliability of the composite material. The existing method for regulating and controlling the diamond/aluminum composite material interface structure mainly comprises technological method optimization, matrix alloying, diamond surface coating treatment and the like. Compared with other methods, the diamond surface coating treatment can realize the improvement of the interface structure on the premise of not damaging the heat conductivity of the matrix, and common coating materials comprise W, Ti, Mo, Cr and other metals and carbide coatings thereof. Compared with metals such as W, Ti, the carbide of the metal has better stability at high temperature, is not easy to dissolve in a metal matrix, generally has higher thermal conductivity, and is a more effective coating material.
In order to ensure that the prepared carbide coating and the diamond have good interface combination, the carbide coating on the surface of the diamond must be prepared by chemical reaction with the diamond, the conventional treatment method is to promote W, Ti and other metals to react with the diamond at high temperature, and the high-temperature heat treatment method has large energy loss, and the diamond is usually subjected to graphite conversion at high temperature, so that the intrinsic heat conductivity of the diamond is reduced, and the comprehensive performance of the composite material is not favorable. In addition, the process for preparing the coating is complex, expensive and difficult to mass-produce. Therefore, how to synthesize the carbide coating in situ at relatively low temperature by improving the preparation process and prepare the diamond/metal matrix composite material with high thermal conductivity and high reliability in the preparation process is an important technology for fully utilizing the excellent thermal property of the diamond.
Disclosure of Invention
The invention provides an efficient preparation method of a diamond/metal matrix composite material, aiming at solving the problems that the existing method for preparing a carbide coating on the surface of diamond has large energy loss, the diamond is easy to be graphitized and the process is complex.
The efficient preparation method of the diamond/metal matrix composite material is carried out according to the following steps:
firstly, weighing and filling:
weighing diamond powder with a metal coating, filling the diamond powder into a cavity of a graphite mold, and compacting the diamond powder by using an ultrasonic vibration table;
the metal coating is one of W, Ti, Cr and Mo;
secondly, low-temperature diffusion treatment:
placing the forming mould filled with diamond powder into a vacuum air pressure infiltration furnace, and heating to a low-temperature diffusion temperature for low-temperature diffusion treatment;
when the metal of the coating is W, the low-temperature diffusion temperature is 700-750 ℃, and the heat preservation time is 6-12 h;
when the metal of the coating is Ti, the low-temperature diffusion temperature is 650-700 ℃, and the heat preservation time is 5-10 h;
when the metal of the coating is Cr, the low-temperature diffusion temperature is 450-500 ℃, and the heat preservation time is 4-8 h;
when the metal of the coating is Mo, the temperature of a low-temperature diffusion region is 700-750 ℃, and the heat preservation time is 5-10 h;
in the process of low-temperature diffusion treatment at a low-temperature diffusion temperature, carbon atoms are promoted to be fully diffused in the metal coating by keeping the temperature for a long time, the generation rate of carbide depends on the reaction temperature and the diffusion rate of the carbon atoms, the sufficient diffusion of the carbon atoms at a relatively low temperature can reduce the retention time of the carbon atoms at a high temperature, and the graphitization of diamond is avoided; the low-temperature diffusion temperature is selected according to the condition that the temperature is slightly lower than the graphitization transformation temperature of the diamond under vacuum, and the heat preservation time is determined by the diffusion rate of carbon in the coating metal and the thickness of the coating metal;
thirdly, high-temperature reaction treatment:
after the low-temperature diffusion treatment, heating the forming die filled with diamond powder to a high-temperature reaction temperature for high-temperature reaction treatment;
when the metal of the coating is W, the high-temperature reaction temperature is 900-950 ℃, and the heat preservation time is 30-60 min;
when the metal of the coating is Ti, the high-temperature reaction temperature is 750-800 ℃, and the heat preservation time is 30-60 min;
when the metal of the coating is Cr, the high-temperature reaction temperature is 600-650 ℃, and the heat preservation time is 30-60 min;
when the metal of the coating is Mo, the temperature of the high-temperature reaction zone is 800-850 ℃, and the heat preservation time is 30-60 min;
during the high-temperature reaction treatment at the high-temperature reaction temperature, the purpose of short-time heat preservation is to promote the diamond to react with the surface coating metal thereof to generate a carbide coating in situ, so that the formation of the carbide is ensured and the generation of a graphite layer is avoided. The high temperature reaction temperature is selected based on the formation temperature of the carbide of the plating metal;
fourthly, air pressure infiltration:
and heating the matrix metal to obtain molten metal, pouring the molten metal into a forming die subjected to high-temperature reaction treatment, and performing vacuum pressure infiltration to obtain the diamond/metal matrix composite.
The invention has the following beneficial effects:
1. the invention provides a high-efficiency preparation method of a diamond/metal matrix composite, which comprises the steps of carrying out low-temperature long-time diffusion and high-temperature short-time reaction treatment on a diamond by changing a preheating temperature curve, avoiding the graphitization of the diamond by the short-time high-temperature reaction treatment, synthesizing a compact carbide coating on the surface of the diamond in situ in the preparation process of the composite, completing the preparation of the carbide coating and the preheating of the diamond by the low-temperature diffusion treatment and the high-temperature reaction treatment at the same time, combining the preparation process of the diamond surface coating and the preparation process of the composite, reducing the energy loss, having simple process, high efficiency, easy control of the quality and stability of a product, low cost and easy realization of industrial production and application;
2. the method is suitable for preparing the carbide coating on the surface of the diamond with the particle size of 30-120 mu m, the wettability between diamond powder and a metal matrix is improved by the carbide coating, the density of the prepared diamond/aluminum composite material reaches more than 99.8 percent, and the preparation of the high-heat-conductivity diamond/aluminum composite material is realized; the thermal conductivity of the diamond/aluminum composite material prepared by the method, which is composed of industrial pure aluminum 1060 and diamond with a tungsten carbide coating, reaches 744W/(m.K); the thermal conductivity of the diamond/aluminum composite material consisting of the AlSi10 aluminum alloy and the diamond with the titanium carbide coating reaches 682W/(m.K); the thermal conductivity of the diamond/aluminum composite material consisting of 2024 aluminum alloy and diamond with chromium carbide coating reaches 692W/(m.K);
3. the method can obtain a compact carbide coating with the thickness of 20-500 nm on the surface of the diamond, the thickness of the coating can be regulated and controlled by controlling the thickness of the metal coating on the surface of the diamond, the carbide coating effectively improves the interface bonding of the diamond/metal matrix composite material, greatly improves the interface bonding strength, and simultaneously avoids the easily-hydrolyzed phase Al4C3The composite material has higher reliability, the performance is not easy to attenuate under severe service conditions such as cold and hot shock, damp and hot and the like, and the attenuation amplitude of the thermal conductivity is controlled within 3 percent.
Description of the drawings:
FIG. 1 is a metallographic picture of a diamond/aluminum composite prepared in example 1;
FIG. 2 is an interfacial SEM photograph of the diamond/aluminum composite prepared in example 1;
fig. 3 is an XRD pattern of the diamond/aluminum composite prepared in example 1.
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 efficient preparation method of the diamond/metal matrix composite material is carried out according to the following steps:
firstly, weighing and filling:
weighing diamond powder with a metal coating, filling the diamond powder into a cavity of a graphite mold, and compacting the diamond powder by using an ultrasonic vibration table;
the metal coating is one of W, Ti, Cr and Mo;
secondly, low-temperature diffusion treatment:
placing the forming mould filled with diamond powder into a vacuum air pressure infiltration furnace, and heating to a low-temperature diffusion temperature for low-temperature diffusion treatment;
when the metal of the coating is W, the low-temperature diffusion temperature is 700-750 ℃, and the heat preservation time is 6-12 h;
when the metal of the coating is Ti, the low-temperature diffusion temperature is 650-700 ℃, and the heat preservation time is 5-10 h;
when the metal of the coating is Cr, the low-temperature diffusion temperature is 450-500 ℃, and the heat preservation time is 4-8 h;
when the metal of the coating is Mo, the temperature of a low-temperature diffusion region is 700-750 ℃, and the heat preservation time is 5-10 h;
thirdly, high-temperature reaction treatment:
after the low-temperature diffusion treatment, heating the forming die filled with diamond powder to a high-temperature reaction temperature for high-temperature reaction treatment;
when the metal of the coating is W, the high-temperature reaction temperature is 900-950 ℃, and the heat preservation time is 30-60 min;
when the metal of the coating is Ti, the high-temperature reaction temperature is 750-800 ℃, and the heat preservation time is 30-60 min;
when the metal of the coating is Cr, the high-temperature reaction temperature is 600-650 ℃, and the heat preservation time is 30-60 min;
when the metal of the coating is Mo, the temperature of the high-temperature reaction zone is 800-850 ℃, and the heat preservation time is 30-60 min;
fourthly, air pressure infiltration:
and heating the matrix metal to obtain molten metal, pouring the molten metal into a forming die subjected to high-temperature reaction treatment, and performing vacuum pressure infiltration to obtain the diamond/metal matrix composite.
The embodiment has the following beneficial effects:
1. the embodiment provides an efficient preparation method of a diamond/metal matrix composite, the diamond is subjected to low-temperature long-time diffusion and high-temperature short-time reaction treatment by changing a preheating temperature curve, graphitization of the diamond is avoided by the short-time high-temperature reaction treatment, a compact carbide coating is synthesized in situ on the surface of the diamond in the preparation process of the composite, the preparation of the carbide coating and the preheating of the diamond are completed simultaneously by the low-temperature diffusion treatment and the high-temperature reaction treatment, the preparation process of the diamond surface coating and the preparation process of the composite are combined, the energy loss is reduced, the process is simple, the efficiency is high, the product quality and the stability are easy to control, the cost is low, and the industrial production and application are easy to realize;
2. the embodiment is suitable for preparing the carbide coating on the surface of the diamond with the grain size of 30-120 mu m, the wettability between diamond powder and a metal matrix is improved by the carbide coating, the density of the prepared diamond/aluminum composite material reaches more than 99.8 percent, and the preparation of the high-heat-conductivity diamond/aluminum composite material is realized; the thermal conductivity of the diamond/aluminum composite material prepared by the method of the embodiment and composed of industrial pure aluminum 1060 and diamond with a tungsten carbide coating reaches 744W/(m.K); the thermal conductivity of the diamond/aluminum composite material consisting of the AlSi10 aluminum alloy and the diamond with the titanium carbide coating reaches 682W/(m.K); the thermal conductivity of the diamond/aluminum composite material consisting of 2024 aluminum alloy and diamond with chromium carbide coating reaches 692W/(m.K);
3. the embodiment can obtain the compact carbide coating with the thickness range of 20-500 nm on the surface of the diamond, the thickness of the coating can be regulated and controlled by controlling the thickness of the metal coating on the surface of the diamond, the interface bonding of the diamond/metal matrix composite material is effectively improved by the carbide coating, the interface bonding strength is greatly improved, and meanwhile, the easily-hydrolyzed phase Al is avoided4C3The composite material has higher reliability, the performance is not easy to attenuate under severe service conditions such as cold and hot shock, damp and hot and the like, and the attenuation amplitude of the thermal conductivity is controlled within 3 percent.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the thickness of the metal coating layer in the first step is 20-500 nm.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the particle size of the diamond powder in the first step is 30-120 mu m.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: step one, the crystal form of the diamond powder is one of single form and poly form or a mixture of two of the single form and the poly form in any proportion.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: and the temperature rise rate is 5-10 ℃/min when the material is heated to the low-temperature diffusion temperature in the second step.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: and in the third step, the heating rate is 15-20 ℃/min when the reaction is heated to the high-temperature reaction temperature.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: and fourthly, the base metal is one of pure aluminum, aluminum alloy, pure copper and copper alloy.
The specific implementation mode is eight: the present embodiment differs from one of the first to seventh embodiments in that: and fourthly, heating the base metal at a temperature of 100-300 ℃ above the melting point of the base metal.
The specific implementation method nine: the present embodiment differs from the first to eighth embodiments in that: step four, the vacuum pressure infiltration process comprises the following steps: pressurizing the air pressure in the infiltration furnace to 20MPa at the pressurizing rate of 1MPa/min, wherein the infiltration rate is 5mm/min, and the pressure maintaining time is 15 min; the vacuum degree in the infiltration furnace is less than 10-2Pa。
The detailed implementation mode is ten: the present embodiment differs from one of the first to ninth embodiments in that: and step four, after the vacuum air pressure infiltration is finished, maintaining the pressure of the forming die at 20MPa for 90min, cooling the forming die along with the furnace to 300 ℃, taking out the forming die from the furnace, and finally demolding.
The following examples were used to demonstrate the beneficial effects of the present invention:
example 1:
the efficient preparation method of the diamond/metal matrix composite material is carried out according to the following steps:
firstly, weighing and filling:
weighing 20.00g of diamond powder with a metal coating, filling the diamond powder into a cavity of a graphite mold, and compacting the diamond powder by using an ultrasonic vibration table;
the metal coating is a W coating; the thickness of the metal coating is 100 nm;
the grain diameter of the diamond powder is 100 mu m; the diamond powder is in a hexaoctahedral poly-crystal form and comprises two crystal faces (111) and (100);
secondly, low-temperature diffusion treatment:
placing the forming mould filled with diamond powder into a vacuum air pressure infiltration furnace, and heating to a low-temperature diffusion temperature for low-temperature diffusion treatment;
the heating rate during the low-temperature diffusion treatment is 10 ℃/min, the low-temperature diffusion temperature is 750 ℃, and the heat preservation time is 8 h;
thirdly, high-temperature reaction treatment:
after the low-temperature diffusion treatment, heating the forming die filled with diamond powder to a high-temperature reaction temperature for high-temperature reaction treatment;
the heating rate during the high-temperature reaction treatment is 20 ℃/min, the high-temperature reaction temperature is 950 ℃, and the heat preservation time is 30 min;
fourthly, air pressure infiltration:
heating a base metal to obtain molten metal, pouring the molten metal into a forming die subjected to high-temperature reaction treatment, and performing vacuum pressure infiltration to obtain a diamond/metal matrix composite;
the base metal is pure aluminum with the grade of 1060; the heating temperature of the matrix metal is 850 ℃;
the vacuum air pressure infiltration process comprises the following steps: pressurizing the air pressure in the infiltration furnace to 20MPa at the pressurizing rate of 1MPa/min, and keeping the pressure for 15 min; the vacuum degree in the infiltration furnace is less than 10-2Pa; after the vacuum air pressure infiltration is finished, maintaining the pressure of the forming die at 20MPa for 90min, cooling the forming die along with the furnace, taking the forming die out of the furnace after cooling to 300 ℃, and finally demoulding;
the preparation method of example 1 can form a compact tungsten carbide coating on the surface of diamond, and the coating thicknessThe volume fraction of diamond in the prepared diamond/aluminum composite material is 58 percent and the density of the composite material is 3.24g/cm, wherein the volume fraction is 100nm3The thermal conductivity is 744W/(m.K), the three-point bending strength is 324MPa, and the thermal expansion coefficient is 6.0-7.0 x 10 at 20-100 DEG C-6and/K, the thermal conductivity decay rate is less than 3 percent when the material is placed for 60 days under the damp and hot conditions that the temperature is 80 ℃ and the humidity is 90 percent R.H. In contrast, the same process is adopted, the diamond is not coated, the thermal conductivity of the obtained diamond/aluminum composite material is 556W/(m.K), the three-point bending strength is 245MPa, and the thermal expansion coefficient is 8.0-9.0 multiplied by 10 at 20-100 DEG C-6K, a thermal conductivity decay rate of 17% after being placed for 60 days under a humid and hot condition with a temperature of 80 ℃ and a humidity of 90% R.H.
FIG. 1 is a metallographic picture of a diamond/aluminum composite prepared in example 1; as can be seen from FIG. 1, the diamond particles are uniformly distributed in the composite material, and the composite material is compact and has no defects such as holes and cracks; FIG. 2 is an interfacial SEM photograph of the diamond/aluminum composite prepared in example 1; as can be seen from FIG. 2, the interface of the composite material is well combined, the tungsten carbide coating is continuous and uniform, and the matrix metal and the diamond are tightly combined together; FIG. 3 is an XRD pattern of the diamond/aluminum composite prepared in example 1; it can be seen from fig. 3 that the composite phase is composed of aluminum, diamond, tungsten carbide and no by-products are produced during the preparation process.
Example 2:
the efficient preparation method of the diamond/metal matrix composite material is carried out according to the following steps:
firstly, weighing and filling:
weighing 20.00g of diamond powder with a metal coating, filling the diamond powder into a cavity of a graphite mold, and compacting the diamond powder by using an ultrasonic vibration table;
the metal coating is a Ti coating; the thickness of the metal coating is 100 nm;
the grain diameter of the diamond powder is 100 mu m; the diamond powder is in a hexaoctahedral poly-crystal form and comprises two crystal faces (111) and (100);
secondly, low-temperature diffusion treatment:
placing the forming mould filled with diamond powder into a vacuum air pressure infiltration furnace, and heating to a low-temperature diffusion temperature for low-temperature diffusion treatment;
the heating rate during the low-temperature diffusion treatment is 10 ℃/min, the low-temperature diffusion temperature is 700 ℃, and the heat preservation time is 8 h;
third, high temperature reaction treatment
After the low-temperature diffusion treatment, heating the forming die filled with diamond powder to a high-temperature reaction temperature for high-temperature reaction treatment;
the heating rate during the high-temperature reaction treatment is 20 ℃/min, the high-temperature reaction temperature is 800 ℃, and the heat preservation time is 30 min;
fourthly, air pressure infiltration:
heating a base metal to obtain molten metal, pouring the molten metal into a forming die subjected to high-temperature reaction treatment, and performing vacuum pressure infiltration to obtain a diamond/metal matrix composite;
the base metal is AlSi10 aluminum alloy; the heating temperature of the matrix metal is 800 ℃;
the vacuum air pressure infiltration process comprises the following steps: the pressure in the infiltration furnace is pressurized to 20MPa at a pressurizing rate of 1MPa/min, and the pressure maintaining time is 15 min. The vacuum degree in the infiltration furnace is less than 10-2Pa; after the vacuum air pressure infiltration is finished, maintaining the pressure of the forming die at 20MPa for 90min, cooling the forming die along with the furnace, taking the forming die out of the furnace after cooling to 300 ℃, and finally demoulding;
the preparation method of example 2 can form a compact titanium carbide coating on the surface of diamond, the coating thickness is 100nm, the diamond volume fraction in the prepared diamond/aluminum composite material with the titanium carbide coating is 60%, and the density of the composite material is 3.33g/cm3The thermal conductivity is 682W/(m.K), the three-point bending strength is 334MPa, and the thermal expansion coefficient is 6.5-7.5 multiplied by 10 at 20-100 DEG C-6and/K, the thermal conductivity decay rate is less than 3 percent when the material is placed for 60 days under the damp and hot conditions that the temperature is 80 ℃ and the humidity is 90 percent R.H. In contrast, the same process is adopted, the diamond is not coated, the thermal conductivity of the obtained diamond/aluminum composite material is 556W/(m.K), and the three-point bending strength is 556W245MPa and a thermal expansion coefficient of 8.0 to 9.0 x 10 at 20 to 100 DEG C-6K, a thermal conductivity decay rate of 17% after being placed for 60 days under a humid and hot condition with a temperature of 80 ℃ and a humidity of 90% R.H.
Example 3:
the efficient preparation method of the diamond/metal matrix composite material is carried out according to the following steps:
firstly, weighing and filling:
weighing 20.00g of diamond powder with a metal coating, filling the diamond powder into a cavity of a graphite mold, and compacting the diamond powder by using an ultrasonic vibration table;
the metal coating is a Cr coating; the thickness of the metal coating is 100 nm;
the grain diameter of the diamond powder is 100 mu m; the diamond powder is in a hexaoctahedral poly-crystal form and comprises two crystal faces (111) and (100);
secondly, low-temperature diffusion treatment:
placing the forming mould filled with diamond powder into a vacuum air pressure infiltration furnace, and heating to a low-temperature diffusion temperature for low-temperature diffusion treatment;
the heating rate during the low-temperature diffusion treatment is 10 ℃/min, the low-temperature diffusion temperature is 500 ℃, and the heat preservation time is 6 h;
thirdly, high-temperature reaction treatment:
after the low-temperature diffusion treatment, heating the forming die filled with diamond powder to a high-temperature reaction temperature for high-temperature reaction treatment;
the heating rate during the high-temperature reaction treatment is 20 ℃/min, the high-temperature reaction temperature is 650 ℃, and the heat preservation time is 30 min;
fourthly, air pressure infiltration:
heating a base metal to obtain molten metal, pouring the molten metal into a forming die subjected to high-temperature reaction treatment, and performing vacuum pressure infiltration to obtain a diamond/metal matrix composite;
the base metal is 2024 aluminum alloy; the heating temperature of the matrix metal is 800 ℃;
the vacuum air pressure infiltration process comprises the following steps: gas in the infiltration furnacePressurizing to 20MPa at a pressurizing rate of 1MPa/min, maintaining the pressure for 5min, and controlling the vacuum degree in the infiltration furnace to be less than 10-2Pa; after the vacuum air pressure infiltration is finished, maintaining the pressure of the forming die at 20MPa for 90min, cooling the forming die along with the furnace, taking the forming die out of the furnace after cooling to 300 ℃, and finally demoulding;
the preparation method of example 3 can form a compact chromium carbide coating on the surface of diamond, the coating thickness is 100nm, the diamond volume fraction in the prepared diamond/aluminum composite material with the chromium carbide coating is 58%, and the density of the composite material is 3.26g/cm3The thermal conductivity is 692W/(m.K), the three-point bending strength is 313MPa, and the thermal expansion coefficient is 6.0-7.0 multiplied by 10 at 20-100 DEG C-6and/K, the thermal conductivity decay rate is less than 3 percent when the material is placed for 60 days under the damp and hot conditions that the temperature is 80 ℃ and the humidity is 90 percent R.H. In contrast, the same process is adopted, the diamond is not coated, the thermal conductivity of the obtained diamond/aluminum composite material is 556W/(m.K), the three-point bending strength is 245MPa, and the thermal expansion coefficient is 8.0-9.0 multiplied by 10 at 20-100 DEG C-6K, a thermal conductivity decay rate of 17% after being placed for 60 days under a humid and hot condition with a temperature of 80 ℃ and a humidity of 90% R.H.

Claims (10)

1. A high-efficiency preparation method of a diamond/metal matrix composite material is characterized by comprising the following steps: the efficient preparation method of the diamond/metal matrix composite material comprises the following steps:
firstly, weighing and filling:
weighing diamond powder with a metal coating, filling the diamond powder into a cavity of a graphite mold, and compacting the diamond powder by using an ultrasonic vibration table;
the metal coating is one of W, Ti, Cr and Mo;
secondly, low-temperature diffusion treatment:
placing the forming mould filled with diamond powder into a vacuum air pressure infiltration furnace, and heating to a low-temperature diffusion temperature for low-temperature diffusion treatment;
when the metal of the coating is W, the low-temperature diffusion temperature is 700-750 ℃, and the heat preservation time is 6-12 h;
when the metal of the coating is Ti, the low-temperature diffusion temperature is 650-700 ℃, and the heat preservation time is 5-10 h;
when the metal of the coating is Cr, the low-temperature diffusion temperature is 450-500 ℃, and the heat preservation time is 4-8 h;
when the metal of the coating is Mo, the temperature of a low-temperature diffusion region is 700-750 ℃, and the heat preservation time is 5-10 h;
thirdly, high-temperature reaction treatment:
after the low-temperature diffusion treatment, heating the forming die filled with diamond powder to a high-temperature reaction temperature for high-temperature reaction treatment;
when the metal of the coating is W, the high-temperature reaction temperature is 900-950 ℃, and the heat preservation time is 30-60 min;
when the metal of the coating is Ti, the high-temperature reaction temperature is 750-800 ℃, and the heat preservation time is 30-60 min;
when the metal of the coating is Cr, the high-temperature reaction temperature is 600-650 ℃, and the heat preservation time is 30-60 min;
when the metal of the coating is Mo, the temperature of the high-temperature reaction zone is 800-850 ℃, and the heat preservation time is 30-60 min;
fourthly, air pressure infiltration:
and heating the matrix metal to obtain molten metal, pouring the molten metal into a forming die subjected to high-temperature reaction treatment, and performing vacuum pressure infiltration to obtain the diamond/metal matrix composite.
2. The method for efficiently producing a diamond/metal matrix composite according to claim 1, wherein: the thickness of the metal coating layer in the first step is 20-500 nm.
3. The method for efficiently producing a diamond/metal matrix composite according to claim 1, wherein: the particle size of the diamond powder in the first step is 30-120 mu m.
4. The method for efficiently producing a diamond/metal matrix composite according to claim 1, wherein: step one, the crystal form of the diamond powder is one of single form and poly form or a mixture of two of the single form and the poly form in any proportion.
5. The method for efficiently producing a diamond/metal matrix composite according to claim 1, wherein: and the temperature rise rate is 5-10 ℃/min when the material is heated to the low-temperature diffusion temperature in the second step.
6. The method for efficiently producing a diamond/metal matrix composite according to claim 1, wherein: and in the third step, the heating rate is 15-20 ℃/min when the reaction is heated to the high-temperature reaction temperature.
7. The method for efficiently producing a diamond/metal matrix composite according to claim 1, wherein: and fourthly, the base metal is one of pure aluminum, aluminum alloy, pure copper and copper alloy.
8. The method for efficiently producing a diamond/metal matrix composite according to claim 1, wherein: and fourthly, heating the base metal at a temperature of 100-300 ℃ above the melting point of the base metal.
9. The method for efficiently producing a diamond/metal matrix composite according to claim 1, wherein: step four, the vacuum pressure infiltration process comprises the following steps: pressurizing the air pressure in the infiltration furnace to 20MPa at the pressurizing rate of 1MPa/min, wherein the infiltration rate is 5mm/min, and the pressure maintaining time is 15 min; the vacuum degree in the infiltration furnace is less than 10-2Pa。
10. The method for efficiently producing a diamond/metal matrix composite according to claim 1, wherein: and step four, after the vacuum air pressure infiltration is finished, maintaining the pressure of the forming die at 20MPa for 90min, cooling the forming die along with the furnace to 300 ℃, taking out the forming die from the furnace, and finally demolding.
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