CN112981164B - Preparation method of diamond reinforced metal matrix composite material with high reliability and high thermal conductivity - Google Patents
Preparation method of diamond reinforced metal matrix composite material with high reliability and high thermal conductivityDownload PDFInfo
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- 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
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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- 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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- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
- C22C1/1073—Infiltration or casting under mechanical pressure, e.g. squeeze casting
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
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Abstract
Translated fromChinese
Description
Technical Field
The invention relates to a preparation method of a composite material.
Background
Semiconductor technology is rapidly developed nowadays, chip integration is higher and higher, heat dissipation capacity is higher and higher, and heat dissipation requirements for heat dissipation plates are also more and more strict, for example, high-power diodes and circuits with high integration level have high heat productivity and extremely high performance requirements. As is known, the integration level and power density of electronic components are higher and higher, and the performance of chips is inevitably reduced when a large amount of heat is generated during the operation of integrated circuits and the temperature thereof is continuously increased. Some traditional heat conducting materials have the problems of low heat conductivity or high density and cannot meet the requirements of high heat conductivity and low quality at present, so that a novel heat conducting material diamond reinforced metal matrix composite material is produced at the same time, diamond has excellent heat conductivity and can be used as a reinforcement, and the material not only has high heat conductivity, but also has a thermal expansion coefficient which is well matched with a chip, and is an ideal heat management material. Diamond is an ideal reinforcement for metal matrix composites due to its various excellent properties. At present, the discontinuous diamond reinforced metal matrix composite material obtains better heat-conducting property. Such as diamond copper composites, diamond aluminum composites, and the like, the thermal conductivity of these composites is significantly improved over the corresponding metal matrix.
But the non-continuous diamond structure in the metal matrix composite material causes the interruption of the diamond heat conduction path, thereby limiting the further improvement of the thermal conductivity of the composite material. While the reaction between the diamond and the metal matrix can lead to a decrease in the reliability of the composite. For example, the interface product generated by the reaction of diamond and matrix aluminum is easy to generate hydrolysis reaction with water and oxygen, so that more pores, cracks and other defects are caused, the heat-conducting property of the composite material is greatly reduced, and the reliability is reduced.
According to the existing method, after the diamond is deposited on the foam metal template by adopting a chemical vapor deposition method, the diamond can realize the continuity of a heat conduction path through the foam metal template, and the diamond reinforced aluminum composite material is obtained after the aluminum is infiltrated.
Disclosure of Invention
The invention aims to solve the problems that the heat conduction channel in the composite material is interrupted due to the discontinuity of diamond in the existing diamond-reinforced metal-based composite material, so that the heat conduction rate is reduced, the heat conduction rate of the composite material is low, and the reliability is reduced due to the generation of carbide by diamond and metal, and provides a preparation method of a diamond-reinforced metal-based composite material with high reliability and high heat conduction.
The preparation method of the diamond reinforced metal matrix composite material with high reliability and high heat conductivity is carried out according to the following steps:
the preparation method of the diamond reinforced metal matrix composite material with high reliability and high heat conductivity is carried out according to the following steps:
firstly, weighing materials: weighing 50-95% diamond powder and 5-50% metal matrix according to volume fraction;
the diamond powder surface is provided with a coating;
the diamond powder surface coating is made of W, Mo, Cr, Ti and the like, and the thickness of the coating is 10-50 nm; 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:
putting diamond powder into a graphite mould, and carrying out 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 250-350 ℃ 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. 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 reinforced metal matrix composite material prepared by the invention has excellent heat conductivity, and the heat conductivity can reach 1350W/(m.K) at most; the diamond composite material has high reliability, and the heat conductivity of the diamond composite material is reduced by less than 0.1% after being treated in a damp and hot environment for 30 days;
2. 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 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.
3. 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 composite material obtained in example 1, and a in the figure is the composite material 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 reliability and high heat conductivity is carried out according to the following steps:
firstly, weighing materials: weighing 50-95% diamond powder and 5-50% metal matrix according to volume fraction;
the diamond powder surface is provided with a coating;
the diamond powder surface coating is made of W, Mo, Cr, Ti and the like, and the thickness of the coating is 10-50 nm; 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:
putting diamond powder into a graphite mould, and carrying out 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 250-350 ℃ 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 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 reinforced metal matrix composite material prepared by the embodiment has excellent heat conductivity, and the heat conductivity reaches 1350W/(m.K) at most; the diamond composite material has high reliability, and the heat conductivity of the diamond composite material is reduced by less than 0.1% after being treated in a damp and hot environment for 30 days;
2. 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.
3. 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: the average grain diameter of the diamond powder in the first step is 20-300 mu m.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: step one, the metal matrix is pure aluminum, aluminum alloy, pure copper or copper alloy.
The fourth concrete implementation mode: the third difference between the present embodiment and the specific embodiment is 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 fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: step two, the cold pressing process comprises the following steps: pressing to 6-10 MPa at a pressing speed of 5-60 mm/min, and maintaining the pressure for 2-5 min.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth 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 5-10 min, and the pulse condition is ton～toff＝(2～10):1。
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: and step two, the inert atmosphere adopts argon, nitrogen or helium.
The specific implementation mode is eight: the present embodiment differs from one of the first to seventh embodiments in that: step three, the preheating process comprises the following steps: heating the mixture from room temperature to 20-200 ℃ below the melting point of the metal matrix and keeping the temperature for 0.5-2 h.
The specific implementation method nine: the present embodiment differs from the first to eighth embodiments in that: step four, the pressure infiltration process comprises the following steps: the pressure is 100-150 MPa, the infiltration speed is 1-3 mm/s, and after the molten metal is completely immersed into the diamond preform, the diamond preform is cooled to room temperature, and demoulding is carried out after cooling.
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 20-40 ℃/min.
Example 1:
the preparation method of the diamond reinforced metal matrix composite material with high reliability and high heat conductivity is carried out according to the following steps:
firstly, weighing materials: weighing 95% of diamond powder and 5% of metal matrix according to volume fraction;
the diamond powder surface is provided with a coating;
the average grain diameter of the diamond powder is 50 μm;
the diamond powder surface coating material is W, and the coating thickness 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:
putting diamond powder into a graphite mould, and carrying out cold pressing to obtain a diamond blank; transferring the diamond blank belt mold to a discharge plasma sintering furnace, and performing discharge plasma sintering in vacuum to obtain a diamond preform;
the cold pressing process comprises the following steps: pressing to 6MPa 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 1200 ℃, the heat preservation time is 5min, and the pulse condition is ton～toff＝2:1；
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 the mixture from room temperature to 1000 ℃ and preserving the heat for 1 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 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 3.78g/m3The bending strength is 400MPa, the thermal conductivity is 1350W/(m.K), and after 30-day 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 ℃ in the test process), the thermal conductivity is reduced by 0.03 percent.
Example 2:
the preparation method of the diamond reinforced metal matrix composite material with high reliability and high heat conductivity is carried out according to the following steps:
firstly, weighing materials: weighing 50% diamond powder and 50% metal matrix according to volume fraction;
the diamond powder surface is provided with a coating;
the average grain diameter of the diamond powder is 100 mu m;
the coating material on the surface of the diamond powder 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 is Cu-Zn alloy, and the mass fraction of Zn is 10%;
secondly, preparing a diamond preform:
putting diamond powder into a graphite mould, and carrying out 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 8MPa at a pressing speed of 10mm/min, and maintaining the pressure for 3 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 10min, and the pulse condition is ton～toff＝2:1；
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 the mixture from room temperature to 1000 ℃ and preserving the heat for 1 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 40 ℃/min.
The density of the obtained diamond reinforced metal matrix composite material is 6.15g/m through detection3The bending strength is 386MPa, the thermal conductivity is 1150W/(m.K), and after 30 days of damp-heat environment treatment, the thermal conductivity is reduced by 0.05 percent.
Example 3:
the preparation method of the diamond reinforced metal matrix composite material with high reliability and high heat conductivity is carried out according to the following steps:
firstly, weighing materials: weighing 70% of diamond powder and 30% of metal matrix according to volume fraction;
the diamond powder surface is provided with a coating;
the average grain diameter of the diamond powder is 100 mu m;
the diamond powder surface coating material is W, and the coating thickness 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:
putting diamond powder into a graphite mould, and carrying out cold pressing to obtain a diamond blank; transferring the diamond blank belt mold to a discharge plasma sintering furnace, and performing discharge plasma sintering in vacuum to obtain a diamond preform;
the cold pressing process comprises the following steps: pressing to 10MPa at a pressing speed of 20mm/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 1400 ℃, the heat preservation time is 5min, and the pulse condition is ton～toff＝2:1；
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 from room temperature to 600 ℃ and keeping the temperature for 0.5 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 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, the thermal conductivity is 920W/(m.K), and after 30 days of damp-heat environment treatment, the thermal conductivity is reduced by 0.08 percent.
Claims (9)
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| CN115213409B (en)* | 2022-07-11 | 2024-02-20 | 哈尔滨工业大学 | Method for rapidly forming diamond/metal matrix composite member by utilizing microwave plasma |
| CN115513435B (en)* | 2022-10-09 | 2024-01-30 | 哈尔滨工业大学 | Preparation method of biomass charcoal/magnesium composite material for magnesium battery cathode |
| 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 |
| CN116162819B (en)* | 2023-03-23 | 2024-01-26 | 哈尔滨工业大学 | A method for preparing multi-phase interface high thermal conductivity diamond/aluminum composite materials |
| CN116393677B (en)* | 2023-04-07 | 2023-11-03 | 哈尔滨工业大学 | Method for preparing diamond/aluminum composite material by high-flux near-net forming |
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| DE102015206241B4 (en)* | 2015-04-08 | 2018-10-25 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | SiC-diamond composite material and process for its production |
| CN107739948B (en)* | 2017-10-31 | 2019-05-17 | 哈尔滨工业大学 | A kind of diamond/aluminum composite material and its high efficiency preparation method |
| CN107760951B (en)* | 2017-10-31 | 2019-05-17 | 哈尔滨工业大学 | A kind of diamond/aluminum composite material and its low cost preparation method |
| CN108179302B (en)* | 2018-01-30 | 2019-12-10 | 哈尔滨工业大学 | A kind of preparation method of high thermal conductivity diamond/copper composite material |
| CN108251733A (en)* | 2018-01-30 | 2018-07-06 | 哈尔滨工业大学 | A kind of preparation method of high heat-conductive diamond/carbon/carbon-copper composite material |
| CN110438444B (en)* | 2019-08-27 | 2020-10-27 | 西安交通大学 | A kind of tungsten-plated diamond particle, tungsten-plating method, its application as copper-based reinforcing phase and obtained diamond/copper composite material |
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