CN112981163A - Preparation method of diamond-reinforced metal matrix composite with high surface precision and high reliability - Google Patents

Preparation method of diamond-reinforced metal matrix composite with high surface precision and high reliability Download PDF

Info

Publication number
CN112981163A
CN112981163A CN202110160248.4A CN202110160248A CN112981163A CN 112981163 A CN112981163 A CN 112981163A CN 202110160248 A CN202110160248 A CN 202110160248A CN 112981163 A CN112981163 A CN 112981163A
Authority
CN
China
Prior art keywords
diamond
metal matrix
composite material
steps
matrix composite
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202110160248.4A
Other languages
Chinese (zh)
Other versions
CN112981163B (en
Inventor
张强
孙凯
杨文澍
修子扬
周畅
陈国钦
武高辉
芶华松
姜龙涛
康鹏超
乔菁
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Harbin Institute of Technology
Original Assignee
Harbin Institute of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Harbin Institute of Technology filed Critical Harbin Institute of Technology
Priority to CN202110160248.4A priority Critical patent/CN112981163B/en
Publication of CN112981163A publication Critical patent/CN112981163A/en
Application granted granted Critical
Publication of CN112981163B publication Critical patent/CN112981163B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/10Alloys containing non-metals
    • C22C1/1036Alloys containing non-metals starting from a melt
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/17Metallic particles coated with metal
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/25Diamond
    • C01B32/28After-treatment, e.g. purification, irradiation, separation or recovery
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/10Alloys containing non-metals
    • C22C1/1005Pretreatment of the non-metallic additives
    • C22C1/1015Pretreatment of the non-metallic additives by preparing or treating a non-metallic additive preform
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/10Alloys containing non-metals
    • C22C1/1036Alloys containing non-metals starting from a melt
    • C22C1/1073Infiltration or casting under mechanical pressure, e.g. squeeze casting
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C26/00Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes

Abstract

A preparation method of a diamond reinforced metal matrix composite material with high surface precision and high reliability relates to the preparation of metal matrix composite materials. The purpose is to solve the problems of low surface precision and poor reliability of the diamond reinforced metal matrix composite. The method comprises the following steps: and paving diamond powder with the particle size of 5-20 microns at the bottom of the die, paving diamond powder with the particle size of 20-300 microns, paving the rest diamond powder with the particle size of 5-20 microns, compacting and cold-pressing to obtain a diamond blank, performing discharge plasma sintering, and performing pressure infiltration. The composite material prepared by the invention has high surface precision, thermal conductivity and reliability. The coatings on the surfaces of the diamonds are sintered together by utilizing spark plasma sintering to form a continuous three-dimensional connected network-shaped heat conduction path, so that the heat conduction performance of the prepared composite material is improved. The method is suitable for preparing the diamond reinforced metal matrix composite material.

Description

Preparation method of diamond-reinforced metal matrix composite with high surface precision and high reliability
Technical Field
The invention relates to a metal matrix composite material and a preparation method thereof.
Background
With the rapid development of electronic packaging technology, especially electronic products such as mobile phones, computers, televisions and the like are pursuing light and thin sizes, which means that the integration level of integrated circuits is higher and higher, and the sizes of electronic components are smaller and smaller, so that the heat productivity of the integrated circuits in unit area and unit time is larger and larger, and the burden of heat dissipation of electronic packaging materials is heavier and heavier. Therefore, high thermal conductivity is a necessary requirement for electronic packaging materials, and therefore, the development of new electronic packaging materials having high thermal conductivity, low density, and sufficient strength and rigidity is urgent. Diamond has excellent comprehensive thermophysical properties and is usually used as an ideal reinforcing phase to be combined with high-thermal-conductivity matrixes such as Ag, Al, Cu and the like to form a novel electronic packaging composite material.
With the increase of the diamond grain size, the thermal conductivity of the corresponding diamond is increased, but the increase of the diamond grain size causes the surface precision of the composite material to be reduced, so that how to obtain high thermal conductivity and simultaneously improve the surface precision of the composite material becomes one of the key problems of the diamond reinforced metal matrix composite material. Meanwhile, because diamond is easy to react with matrix metal to generate carbide with low thermal conductivity, the reliability of the composite material is reduced, so that how to improve the reliability of the composite material while keeping the high thermal conductivity of the composite material is also one of the key problems of the diamond reinforced metal matrix composite material.
Disclosure of Invention
The invention provides a preparation method of a diamond-enhanced metal-based composite material with high surface precision and high reliability, aiming at solving the problems of low surface precision and poor reliability of the existing diamond-enhanced metal-based composite material.
The preparation method of the diamond reinforced metal matrix composite material with high surface precision and high reliability comprises the following steps:
firstly, weighing materials: weighing 5-8% of diamond powder with the average particle size of 5-20 microns, 45-72% of diamond powder with the average particle size of 20-300 microns and the balance of metal matrix according to volume fraction;
the surfaces of the diamond powder with the average grain size of 5-20 mu m and the diamond powder with the average grain size of 20-300 mu m are provided with coatings; the coating material is W, Mo, Cr, Ti, etc.;
w, Mo, Cr and Ti are easy to react with diamond at high temperature to generate carbide, and the generated carbide is stable and does not cause obvious change of thermal conductivity after moist heat treatment.
Secondly, preparing a diamond preform:
spreading 50% of the diamond powder with the average particle size of 5-20 microns weighed in the step one on the bottom of the mold, and compacting; then, spreading diamond powder with the average particle size of 20-300 microns, which is weighed in the first step, and compacting the diamond powder; finally, flatly paving the rest diamond powder with the average grain diameter of 5-20 mu m weighed in the first step, and compacting; cold pressing to obtain a diamond blank; transferring the diamond blank belt mold to a discharge plasma sintering furnace, and performing discharge plasma sintering under the protection of vacuum or inert atmosphere to obtain a diamond preform;
thirdly, preheating and preparing a metal matrix: moving the diamond preform belt mold obtained in the step two to a heating furnace for preheating to obtain a preheated diamond preform; heating the metal matrix weighed in the step one to a temperature of 250-400 ℃ above the melting point under a protective atmosphere to obtain a molten metal matrix;
fourthly, liquid metal infiltration:
and (4) placing the diamond preform belt mold obtained in the third step on the table top of a press machine, pouring the molten metal matrix on the diamond preform in the mold, and performing pressure infiltration.
The invention has the following beneficial effects:
1. according to the invention, the diamond powder with a larger particle size of 20-300 microns is placed in the middle, and the diamond powder with a smaller particle size of 5-20 microns is placed outside, so that the prepared composite material can be ensured to have high surface precision and thermal conductivity.
2. The invention utilizes spark plasma sintering to sinter the coatings on the surfaces of the diamonds together to form a continuous three-dimensional connected network-shaped heat conduction path, thereby improving the heat conduction performance of the prepared composite material. The diamond surface coating is metal which is easy to react with diamond to generate carbide, and the generated carbide can not generate hydrolysis reaction with water and oxygen, so that the stability is high, and the reliability of the prepared composite material is improved. The diamond enhanced metal matrix composite material with the size of phi 100mm multiplied by 6mm prepared by the invention has the surface flatness of less than 5 mu m, the thermal conductivity of 1150W/(m.K), and the thermal conductivity is reduced by less than 0.1 percent after being treated in a damp-heat environment for 30 days;
3. the method has low cost, simple process method and easy operation, is suitable for large-batch preparation, is suitable for preparing the massive diamond reinforced metal matrix composite, and is easy to realize industrialized production and application; because the CVD method has high requirement on the atmosphere and the equipment has small volume of a uniform temperature area, the single yield is low and generally does not exceed 5g when the CVD method is adopted to deposit diamond on the foam metal template, and the single yield can reach 50g when the diamond is prepared by spark plasma sintering in a laboratory, so the method can obviously improve the single yield and the production efficiency.
4. Most of the existing preparation of carbide coatings is realized by a method of coating strong carbide forming elements such as W, Ti, Cr and the like on the surface of diamond, then carrying out vacuum high-temperature heat treatment, and converting coating metal into carbide, but the method generally needs heat preservation at high temperature for a long time, so that the graphitization of the diamond is caused.
Drawings
Fig. 1 is a structural picture of the diamond metal matrix composite with high reliability and high thermal conductivity obtained in example 1.
Detailed Description
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 diamond reinforced metal matrix composite material with high surface precision and high reliability comprises the following steps:
firstly, weighing materials: weighing 5-8% of diamond powder with the average particle size of 5-20 microns, 45-72% of diamond powder with the average particle size of 20-300 microns and the balance of metal matrix according to volume fraction;
the surfaces of the diamond powder with the average grain size of 5-20 mu m and the diamond powder with the average grain size of 20-300 mu m are provided with coatings; the coating material is W, Mo, Cr, Ti, etc.;
w, Mo, Cr and Ti are easy to react with diamond at high temperature to generate carbide, and the generated carbide is stable and does not cause obvious change of thermal conductivity after moist heat treatment.
Secondly, preparing a diamond preform:
spreading 50% of the diamond powder with the average particle size of 5-20 microns weighed in the step one on the bottom of the mold, and compacting; then, spreading diamond powder with the average particle size of 20-300 microns, which is weighed in the first step, and compacting the diamond powder; finally, flatly paving the rest diamond powder with the average grain diameter of 5-20 mu m weighed in the first step, and compacting; cold pressing to obtain a diamond blank; transferring the diamond blank belt mold to a discharge plasma sintering furnace, and performing discharge plasma sintering under the protection of vacuum or inert atmosphere to obtain a diamond preform;
thirdly, preheating and preparing a metal matrix: moving the diamond preform belt mold obtained in the step two to a heating furnace for preheating to obtain a preheated diamond preform; heating the metal matrix weighed in the step one to a temperature of 250-400 ℃ above the melting point under a protective atmosphere to obtain a molten metal matrix;
fourthly, liquid metal infiltration:
and (4) placing the diamond preform belt mold obtained in the third step on the table top of a press machine, pouring the molten metal matrix on the diamond preform in the mold, and performing pressure infiltration.
1. In the embodiment, the diamond powder with a larger particle size of 20-300 microns is placed in the middle, and the diamond powder with a smaller particle size of 5-20 microns is placed outside, so that the prepared composite material can have high surface precision and thermal conductivity.
2. In the embodiment, the coatings on the surfaces of the diamonds are sintered together by using spark plasma sintering to form a continuous three-dimensional connected network-shaped heat conduction passage, so that the heat conduction performance of the prepared composite material is improved. The diamond surface coating is metal which is easy to react with diamond to generate carbide, and the generated carbide can not generate hydrolysis reaction with water and oxygen, so that the stability is high, and the reliability of the prepared composite material is improved. The diamond enhanced metal matrix composite material prepared by the embodiment and having the size of phi 100mm multiplied by 6mm has the surface flatness of less than 5 mu m, the thermal conductivity reaches 1150W/(m.K), and the thermal conductivity is reduced by less than 0.1 percent after being treated in a damp-heat environment for 30 days;
3. the method has the advantages of low cost, simple process method, easy operation, suitability for large-batch preparation, suitability for preparation of large diamond reinforced metal matrix composite materials and easiness for realizing industrial production and application; because the CVD method has high requirements on atmosphere and the equipment has small volume of a uniform temperature area, the single yield is low and generally does not exceed 5g when the CVD method is adopted to deposit diamond on the foam metal template, and the single yield can reach 50g when the diamond is prepared by adopting spark plasma sintering in a laboratory, so that the method of the embodiment can obviously improve the single yield and improve the production efficiency.
4. At present, most of carbide coatings are prepared by coating strong carbide forming elements such as W, Ti, Cr and the like on the surfaces of diamonds and then carrying out vacuum high-temperature heat treatment to convert coating metals into carbides, but the method generally needs heat preservation at high temperature for a long time to cause graphitization of the diamonds.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: step one, the metal matrix is pure aluminum, aluminum alloy, pure copper or copper alloy.
The third concrete implementation mode: the second embodiment is different from the first embodiment in that: the aluminum alloy is one or a combination of more of Al-Si alloy, Al-Si-Cu alloy, Al-Cu-Mg alloy, Al-Zn-Cu alloy, Al-Zn-Mg-Cu alloy and Al-Si-Cu-Mg alloy; the copper alloy is one or a combination of more of Cu-Zn, Cu-Sn and Cu-Ni alloy.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: step two, the cold pressing process comprises the following steps: pressing to 2-5 MPa at a pressing speed of 5-60 mm/min, and maintaining the pressure for 2-5 min.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: and step two, the sintering temperature of the discharge plasma is as follows: the heating rate is 50-200 ℃/min, the sintering temperature is 1000-1500 ℃, the heat preservation time is 5-15 min, and the pulse condition is ton~toff=(2~10):1。
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: and step two, the inert atmosphere adopts argon, nitrogen or helium.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: step three, the preheating process comprises the following steps: heating the mixture from room temperature to 20-220 ℃ below the melting point of the metal matrix and preserving the heat for 0.5-2 h.
The specific implementation mode is eight: the present embodiment differs from one of the first to seventh embodiments in that: step four, the pressure infiltration process comprises the following steps: and (3) the pressure is 100-150 MPa, the infiltration speed is 1-3 mm/s, the molten metal is completely immersed into the diamond preform, then the diamond preform is cooled to room temperature, and demoulding is carried out after cooling, thus completing the preparation.
The specific implementation method nine: the present embodiment differs from the first to eighth embodiments in that: and fourthly, the cooling speed is 20-40 ℃/min.
The detailed implementation mode is ten: the present embodiment differs from one of the first to ninth embodiments in that: step one, the thickness of the coating is 10-50 nm.
Example 1:
the preparation method of the diamond reinforced metal matrix composite material with high surface precision and high reliability comprises the following steps:
firstly, weighing materials: weighing 8 percent of diamond powder with the average grain diameter of 5 mu m, 72 percent of diamond powder with the average grain diameter of 100 mu m and 20 percent of metal matrix according to volume fraction;
the surfaces of the diamond powder with the average grain diameter of 5 mu m and the diamond powder with the average grain diameter of 100 mu m are provided with coatings; the material of the coating is W, and the thickness of the coating is 20 nm; w is easy to react with diamond at high temperature to generate carbide, and the generated carbide is stable and does not cause obvious change of thermal conductivity after moist heat treatment.
The metal matrix is pure copper;
secondly, preparing a diamond preform:
spreading 50% of the diamond powder with the average particle size of 5 microns weighed in the step one on the bottom of the mold, and compacting; then, paving diamond powder with the average grain diameter of 100 mu m weighed in the first step, and compacting; finally, flatly paving the residual diamond powder with the average grain diameter of 5 mu m weighed in the first step, and compacting; cold pressing to obtain a diamond blank; transferring the diamond blank belt mold to a discharge plasma sintering furnace, and performing discharge plasma sintering under the protection of inert atmosphere to obtain a diamond preform;
the cold pressing process comprises the following steps: pressing to 2MPa at a pressing speed of 5mm/min, and maintaining the pressure for 2 min;
the spark plasma sintering temperature is as follows: the heating rate is 50 ℃/min, the sintering temperature is 1000 ℃, the heat preservation time is 10min, and the pulse condition is ton~toff=10:1;
The inert atmosphere adopts argon gas;
thirdly, preheating and preparing a metal matrix: moving the diamond preform belt mold obtained in the step two to a heating furnace for preheating to obtain a preheated diamond preform; heating the metal matrix weighed in the step one to 1350 ℃ under a protective atmosphere to obtain a molten metal matrix;
the preheating process comprises the following steps: heating from room temperature to 1050 ℃ and keeping the temperature for 0.5;
fourthly, liquid metal infiltration:
placing the diamond preform belt mold obtained in the third step on the table top of a press machine, pouring the molten metal matrix on the diamond preform in the mold, and performing pressure infiltration;
the pressure infiltration process comprises the following steps: the pressure is 100MPa, the infiltration speed is 1mm/s, the metal in the molten state is completely immersed into the diamond preform, the diamond preform is cooled to room temperature, and the diamond preform is demoulded after cooling to obtain the product;
the cooling rate was 20 ℃/min.
Fig. 1 is a structural picture of the diamond metal matrix composite with high reliability and high thermal conductivity obtained in example 1. As can be seen from FIG. 1, no significant voids were observed in the composite and the density of the composite was found to be 4.59g/m3The surface flatness of the cylindrical composite material with the bending strength of 408MPa and the diameter of 100mm multiplied by 6mm is less than 3 mu m, the thermal conductivity is 1150W/(m.K), and after 30 days of damp-heat environment treatment (carried out in a programmable constant temperature and humidity test box, the relative humidity is 90 percent and the temperature is 65 ℃ during the test), the thermal conductivity is reduced by 0.03 percent.
Example 2:
the preparation method of the diamond reinforced metal matrix composite material with high surface precision and high reliability comprises the following steps:
firstly, weighing materials: weighing 5 percent of diamond powder with the average grain diameter of 10 mu m, 45 percent of diamond powder with the average grain diameter of 50 mu m and 50 percent of metal matrix according to volume fraction;
the surfaces of the diamond powder with the average grain diameter of 10 mu m and the diamond powder with the average grain diameter of 50 mu m are provided with coatings; the coating material is Ti, and the thickness of the coating is 10 nm; ti is easy to react with diamond at high temperature to generate carbide, and the generated carbide is stable and does not cause obvious change of thermal conductivity after moist heat treatment.
The metal matrix is Cu-Sn alloy, and the mass fraction of Sn is 10%;
secondly, preparing a diamond preform:
spreading 50% of the diamond powder with the average particle size of 10 microns weighed in the step one on the bottom of the mold, and compacting; then, paving the diamond powder with the average grain diameter of 50 mu m weighed in the first step, and compacting; finally, flatly paving the rest diamond powder with the average grain diameter of 10 mu m weighed in the first step, and compacting; cold pressing to obtain a diamond blank; transferring the diamond blank belt mold to a discharge plasma sintering furnace, and performing discharge plasma sintering under the protection of inert atmosphere to obtain a diamond preform;
the cold pressing process comprises the following steps: pressing to 5MPa at a pressing speed of 10mm/min, and maintaining the pressure for 5 min;
the spark plasma sintering temperature is as follows: the heating rate is 100 ℃/min, the sintering temperature is 1200 ℃, the heat preservation time is 8min, and the pulse condition is ton~toff=5:1;
The inert atmosphere adopts argon gas;
thirdly, preheating and preparing a metal matrix: moving the diamond preform belt mold obtained in the step two to a heating furnace for preheating to obtain a preheated diamond preform; heating the metal matrix weighed in the step one to 1400 ℃ under a protective atmosphere to obtain a molten metal matrix;
the preheating process comprises the following steps: heating from room temperature to 1100 ℃ and preserving heat for 2 h;
fourthly, liquid metal infiltration:
placing the diamond preform belt mold obtained in the third step on the table top of a press machine, pouring the molten metal matrix on the diamond preform in the mold, and performing pressure infiltration;
the pressure infiltration process comprises the following steps: the pressure is 150MPa, the infiltration speed is 3mm/s, the metal in the molten state is completely immersed into the diamond preform, the diamond preform is cooled to room temperature, and the diamond preform is demoulded after cooling to obtain the product;
the cooling rate was 20 ℃/min.
The density of the obtained diamond reinforced metal matrix composite material is 6.09g/m through detection3The bending strength is 399MPa,
Figure BDA0002936254570000071
the surface flatness of the composite material is less than 4 mu m, the thermal conductivity is 1150W/(m.K), and after 30 days of damp-heat environment treatment, the thermal conductivity is reduced by 0.04 percent.
Example 3:
the preparation method of the diamond reinforced metal matrix composite material with high surface precision and high reliability comprises the following steps:
firstly, weighing materials: weighing 7 percent of diamond powder with the average grain diameter of 8 mu m, 63 percent of diamond powder with the average grain diameter of 150 mu m and 30 percent of metal matrix according to volume fraction;
the surfaces of the diamond powder with the average grain diameter of 8 mu m and the diamond powder with the average grain diameter of 150 mu m are provided with coatings; the material of the coating is W, and the thickness of the coating is 50 nm; w is easy to react with diamond at high temperature to generate carbide, and the generated carbide is stable and does not cause obvious change of thermal conductivity after moist heat treatment.
The metal matrix is pure aluminum;
secondly, preparing a diamond preform:
spreading 50% of the diamond powder with the average particle size of 8 microns weighed in the step one on the bottom of the mold, and compacting; then, spreading diamond powder with the average grain diameter of 150 mu m weighed in the first step, and compacting; finally, flatly paving the rest diamond powder with the average grain diameter of 8 mu m weighed in the first step, and compacting; cold pressing to obtain a diamond blank; transferring the diamond blank belt mold to a discharge plasma sintering furnace, and performing discharge plasma sintering under the protection of inert atmosphere to obtain a diamond preform;
the cold pressing process comprises the following steps: pressing to 5MPa at a pressing speed of 5mm/min, and maintaining the pressure for 2 min;
the spark plasma sintering temperature is as follows: the heating rate is 100 ℃/min, the sintering temperature is 1500 ℃, the heat preservation time is 2min, and the pulse condition is ton~toff=10:1;
The inert atmosphere adopts argon gas;
thirdly, preheating and preparing a metal matrix: moving the diamond preform belt mold obtained in the step two to a heating furnace for preheating to obtain a preheated diamond preform; heating the metal matrix weighed in the step one to 950 ℃ under a protective atmosphere to obtain a molten metal matrix;
the preheating process comprises the following steps: heating the mixture from room temperature to 500 ℃ and preserving the heat for 2 hours;
fourthly, liquid metal infiltration:
placing the diamond preform belt mold obtained in the third step on the table top of a press machine, pouring the molten metal matrix on the diamond preform in the mold, and performing pressure infiltration;
the pressure infiltration process comprises the following steps: the pressure is 100MPa, the infiltration speed is 2mm/s, the metal in the molten state is completely immersed into the diamond preform, the diamond preform is cooled to room temperature, and the diamond preform is demoulded after cooling to obtain the product;
the cooling rate was 20 ℃/min.
The diamond reinforced metal matrix composite obtained in example 3 had a density of 3.21g/m3The bending strength is 360MPa,
Figure BDA0002936254570000081
the surface flatness of the composite material is less than 3 mu m, the thermal conductivity is 920W/(m.K), and after 30 days of damp-heat environment treatment, the thermal conductivity isThe rate is reduced by 0.06%.

Claims (10)

1. A preparation method of a diamond enhanced metal matrix composite material with high surface precision and high reliability is characterized by comprising the following steps: the method comprises the following steps:
firstly, weighing materials: weighing 5-8% of diamond powder with the average particle size of 5-20 microns, 45-72% of diamond powder with the average particle size of 20-300 microns and the balance of metal matrix according to volume fraction;
the surfaces of the diamond powder with the average grain size of 5-20 mu m and the diamond powder with the average grain size of 20-300 mu m are provided with coatings; the coating material is W, Mo, Cr or Ti;
secondly, preparing a diamond preform:
spreading 50% of the diamond powder with the average particle size of 5-20 microns weighed in the step one on the bottom of the mold, and compacting; then, spreading diamond powder with the average particle size of 20-300 microns, which is weighed in the first step, and compacting the diamond powder; finally, flatly paving the rest diamond powder with the average grain diameter of 5-20 mu m weighed in the first step, and compacting; cold pressing to obtain a diamond blank; transferring the diamond blank belt mold to a discharge plasma sintering furnace, and performing discharge plasma sintering under the protection of vacuum or inert atmosphere to obtain a diamond preform;
thirdly, preheating and preparing a metal matrix: moving the diamond preform belt mold obtained in the step two to a heating furnace for preheating to obtain a preheated diamond preform; heating the metal matrix weighed in the step one to a temperature of 250-400 ℃ above the melting point under a protective atmosphere to obtain a molten metal matrix;
fourthly, liquid metal infiltration:
and (4) placing the diamond preform belt mold obtained in the third step on the table top of a press machine, pouring the molten metal matrix on the diamond preform in the mold, and performing pressure infiltration.
2. The method for preparing a diamond enhanced metal matrix composite material with high surface precision and high reliability according to claim 1, wherein the method comprises the following steps: step one, the metal matrix is pure aluminum, aluminum alloy, pure copper or copper alloy.
3. The method for preparing a diamond enhanced metal matrix composite material with high surface precision and high reliability according to claim 2, wherein: the aluminum alloy is one or a combination of more of Al-Si alloy, Al-Si-Cu alloy, Al-Cu-Mg alloy, Al-Zn-Cu alloy, Al-Zn-Mg-Cu alloy and Al-Si-Cu-Mg alloy; the copper alloy is one or a combination of more of Cu-Zn, Cu-Sn and Cu-Ni alloy.
4. The method for preparing a diamond enhanced metal matrix composite material with high surface precision and high reliability according to claim 1, wherein the method comprises the following steps: step two, the cold pressing process comprises the following steps: pressing to 2-5 MPa at a pressing speed of 5-60 mm/min, and maintaining the pressure for 2-5 min.
5. The method for preparing a diamond enhanced metal matrix composite material with high surface precision and high reliability according to claim 1, wherein the method comprises the following steps: and step two, the sintering temperature of the discharge plasma is as follows: the heating rate is 50-200 ℃/min, the sintering temperature is 1000-1500 ℃, the heat preservation time is 5-15 min, and the pulse condition is ton~toff=(2~10):1。
6. The method for preparing a diamond enhanced metal matrix composite material with high surface precision and high reliability according to claim 1, wherein the method comprises the following steps: and step two, the inert atmosphere adopts argon, nitrogen or helium.
7. The method for preparing a diamond enhanced metal matrix composite material with high surface precision and high reliability according to claim 1, wherein the method comprises the following steps: step three, the preheating process comprises the following steps: heating the mixture from room temperature to 20-220 ℃ below the melting point of the metal matrix and preserving the heat for 0.5-2 h.
8. The method for preparing a diamond enhanced metal matrix composite material with high surface precision and high reliability according to claim 1, wherein the method comprises the following steps: step four, the pressure infiltration process comprises the following steps: and (3) the pressure is 100-150 MPa, the infiltration speed is 1-3 mm/s, the molten metal is completely immersed into the diamond preform, then the diamond preform is cooled to room temperature, and demoulding is carried out after cooling, thus completing the preparation.
9. The method for preparing a diamond enhanced metal matrix composite material with high surface precision and high reliability according to claim 1, wherein the method comprises the following steps: and fourthly, the cooling speed is 20-40 ℃/min.
10. The method for preparing a diamond enhanced metal matrix composite material with high surface precision and high reliability according to claim 1, wherein the method comprises the following steps: step one, the thickness of the coating is 10-50 nm.
CN202110160248.4A 2021-02-05 2021-02-05 Preparation method of diamond-reinforced metal matrix composite with high surface precision and high reliability Active CN112981163B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110160248.4A CN112981163B (en) 2021-02-05 2021-02-05 Preparation method of diamond-reinforced metal matrix composite with high surface precision and high reliability

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110160248.4A CN112981163B (en) 2021-02-05 2021-02-05 Preparation method of diamond-reinforced metal matrix composite with high surface precision and high reliability

Publications (2)

Publication Number Publication Date
CN112981163A true CN112981163A (en) 2021-06-18
CN112981163B CN112981163B (en) 2021-11-26

Family

ID=76347924

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110160248.4A Active CN112981163B (en) 2021-02-05 2021-02-05 Preparation method of diamond-reinforced metal matrix composite with high surface precision and high reliability

Country Status (1)

Country Link
CN (1) CN112981163B (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115572961A (en) * 2022-10-20 2023-01-06 哈尔滨工业大学 Method for preparing high-thermal-conductivity diamond/metal-based composite material by microwave-assisted air pressure infiltration
CN116162819A (en) * 2023-03-23 2023-05-26 哈尔滨工业大学 Preparation method of multiphase interface high-heat-conductivity diamond/aluminum composite material
CN116408434A (en) * 2023-04-12 2023-07-11 哈尔滨工业大学 Preparation method of large-size special-shaped structure diamond/aluminum composite material
CN116516197A (en) * 2023-03-23 2023-08-01 哈尔滨工业大学 Preparation method of high-heat-conductivity diamond/metal composite material

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5783316A (en) * 1994-05-20 1998-07-21 Regents Of The University Of California Composite material having high thermal conductivity and process for fabricating same
US20100319900A1 (en) * 2009-10-21 2010-12-23 Andrey Mikhailovich Abyzov Composite material having high thermal conductivity nd process of fabricating same
CN102071332A (en) * 2010-11-23 2011-05-25 北京科技大学 Method for preparing diamond enhanced copper based composite with high volume fraction
JP2012117085A (en) * 2010-11-29 2012-06-21 Denki Kagaku Kogyo Kk Aluminum-diamond composite and method for producing the same
CN105112754A (en) * 2015-10-12 2015-12-02 中南大学 Metal-based composite material enhanced by three-dimensional networked diamond framework as well as preparation method
CN108179302A (en) * 2018-01-30 2018-06-19 哈尔滨工业大学 A kind of preparation method of high heat-conductive diamond/carbon/carbon-copper composite material
CN110117731A (en) * 2019-05-17 2019-08-13 北京科技大学 A kind of preparation method of superelevation thermal conductivity diamond particles reinforced aluminum matrix composites
CN110438444A (en) * 2019-08-27 2019-11-12 西安交通大学 A kind of plating tungsten diamond particles, tangsten plating process, its application and obtained diamond/copper composite material as copper-based reinforced phase
CN111304481A (en) * 2020-02-11 2020-06-19 中南大学 Infiltration preparation process of diamond-metal composite material and diamond-metal composite material

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5783316A (en) * 1994-05-20 1998-07-21 Regents Of The University Of California Composite material having high thermal conductivity and process for fabricating same
US20100319900A1 (en) * 2009-10-21 2010-12-23 Andrey Mikhailovich Abyzov Composite material having high thermal conductivity nd process of fabricating same
CN102071332A (en) * 2010-11-23 2011-05-25 北京科技大学 Method for preparing diamond enhanced copper based composite with high volume fraction
JP2012117085A (en) * 2010-11-29 2012-06-21 Denki Kagaku Kogyo Kk Aluminum-diamond composite and method for producing the same
CN105112754A (en) * 2015-10-12 2015-12-02 中南大学 Metal-based composite material enhanced by three-dimensional networked diamond framework as well as preparation method
CN108179302A (en) * 2018-01-30 2018-06-19 哈尔滨工业大学 A kind of preparation method of high heat-conductive diamond/carbon/carbon-copper composite material
CN110117731A (en) * 2019-05-17 2019-08-13 北京科技大学 A kind of preparation method of superelevation thermal conductivity diamond particles reinforced aluminum matrix composites
CN110438444A (en) * 2019-08-27 2019-11-12 西安交通大学 A kind of plating tungsten diamond particles, tangsten plating process, its application and obtained diamond/copper composite material as copper-based reinforced phase
CN111304481A (en) * 2020-02-11 2020-06-19 中南大学 Infiltration preparation process of diamond-metal composite material and diamond-metal composite material

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115572961A (en) * 2022-10-20 2023-01-06 哈尔滨工业大学 Method for preparing high-thermal-conductivity diamond/metal-based composite material by microwave-assisted air pressure infiltration
CN115572961B (en) * 2022-10-20 2023-05-23 哈尔滨工业大学 Method for preparing diamond composite material by microwave-assisted air pressure infiltration
CN116162819A (en) * 2023-03-23 2023-05-26 哈尔滨工业大学 Preparation method of multiphase interface high-heat-conductivity diamond/aluminum composite material
CN116516197A (en) * 2023-03-23 2023-08-01 哈尔滨工业大学 Preparation method of high-heat-conductivity diamond/metal composite material
CN116162819B (en) * 2023-03-23 2024-01-26 哈尔滨工业大学 Preparation method of multiphase interface high-heat-conductivity diamond/aluminum composite material
CN116516197B (en) * 2023-03-23 2024-02-27 哈尔滨工业大学 Preparation method of high-heat-conductivity diamond/metal composite material
CN116408434A (en) * 2023-04-12 2023-07-11 哈尔滨工业大学 Preparation method of large-size special-shaped structure diamond/aluminum composite material
CN116408434B (en) * 2023-04-12 2023-11-03 哈尔滨工业大学 Preparation method of large-size special-shaped structure diamond/aluminum composite material

Also Published As

Publication number Publication date
CN112981163B (en) 2021-11-26

Similar Documents

Publication Publication Date Title
CN112981163B (en) Preparation method of diamond-reinforced metal matrix composite with high surface precision and high reliability
CN112981164B (en) Preparation method of diamond reinforced metal matrix composite material with high reliability and high thermal conductivity
CN108746637B (en) Aluminum silicon/aluminum silicon carbide gradient composite material and preparation method thereof
JP4880447B2 (en) High thermal conductivity heat sink
CN102114541B (en) Preparation process of high volume fraction silicon particle enhanced aluminum based composite material
JP5275625B2 (en) Heat sink made of boron-containing diamond and copper composite
CN104694895B (en) W-Ti alloy target material and manufacturing method thereof
CN101831584A (en) High heat-conducting copper-based composite material and preparation method thereof
CN105483454B (en) A kind of preparation method of stratiform aluminum matrix composite used for electronic packaging
CN108179302A (en) A kind of preparation method of high heat-conductive diamond/carbon/carbon-copper composite material
US6123895A (en) Aluminum base member for semiconductor device containing a nitrogen rich surface and method for producing the same
CN108251733A (en) A kind of preparation method of high heat-conductive diamond/carbon/carbon-copper composite material
WO2017065139A1 (en) Aluminum-diamond composite and method for producing same
CN107058787A (en) A kind of method that graphene reinforced aluminum matrix composites are prepared by raw material of graphite microchip
CN113881875B (en) Three-dimensional framework structure metal reinforced aluminum matrix composite material and preparation method thereof
CN108774699A (en) Aluminium silicon/aluminium gold hard rock gradient composites and preparation method thereof
CN109759596B (en) Heterogeneous gradient composite material and preparation method thereof
CN114309596B (en) Preparation method of high-heat-conductivity surface-metallized diamond/copper composite substrate
SE535684C2 (en) Method of producing a gradient component of metal / cemented carbide
JP2014001439A (en) Composite member, method for manufacturing composite member and semiconductor device
CN102560204A (en) Silicon-aluminum bicontinuous composite material and preparation method thereof
CN109093113B (en) Rare earth intermetallic compound reinforced copper-based composite material and preparation method thereof
JP4228444B2 (en) Silicon carbide based composite material and method for producing the same
CN114807644B (en) Silicon-aluminum composite material and preparation method and application thereof
CN116408434B (en) Preparation method of large-size special-shaped structure diamond/aluminum composite material

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant