CN110144506B - Preparation method of diamond copper-based composite material - Google Patents
Preparation method of diamond copper-based composite material Download PDFInfo
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- CN110144506B CN110144506B CN201910597544.3A CN201910597544A CN110144506B CN 110144506 B CN110144506 B CN 110144506B CN 201910597544 A CN201910597544 A CN 201910597544A CN 110144506 B CN110144506 B CN 110144506B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
- C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
Abstract
The invention discloses a preparation method of a diamond copper-based composite material, which comprises the following raw materials in percentage by weight: 20-50% of diamond, 0.5-2.5% of zirconium, 0.02-0.05% of erbium, 0.01-0.05% of niobium, 0.01-0.05% of tantalum, 0.5-1.5% of rare earth coupling agent, 1-3% of aluminum-zirconium coupling agent and the balance of copper. The preparation method comprises the following steps: adding diamond, zirconium, erbium, niobium, tantalum, rare earth coupling agent, aluminum-zirconium coupling agent and grinding balls into a ball milling tank for ball milling to obtain mixed powder; heating the mixed powder to 700-; and (3) carrying out plasma discharge sintering on the pressed compact to obtain the diamond copper-based composite material. The thermal conductivity of the diamond copper-based composite material prepared by the invention reaches more than 520W/(m.K), the thermal expansion coefficient is lower than 3.0 x 10 < -6 > m/K, and the diamond copper-based composite material can be used as an excellent electronic packaging material and has wide market prospect.
Description
Technical Field
The invention relates to the technical field of heat conduction materials, in particular to a preparation method of a diamond copper-based composite material.
Background
The diamond/copper composite material which takes diamond as a reinforcing phase and copper as a matrix material realizes high thermal conductivity and adjustable thermal expansion by adjusting the volume fraction of the diamond, can meet the requirements of system heat dissipation and assembly processes, and is a novel electronic packaging material with great competitiveness. With the development of electronic packaging materials towards miniaturization, light weight and high performance, the working temperature of a circuit is continuously increased, and the heating rate of a system unit volume is continuously increased, so that the system is unstable in operation. In order to obtain stable performance, heat dissipation conditions must be improved, so that the importance of electronic packaging in the field of microelectronics is continuously increased, and along with the increasing demand of new electronic packaging materials, the research of packaging materials with high thermal conductivity is a demand of the current market.
However, the preparation of the diamond/copper composite material has the following difficulties: the problem that the wettability of diamond and copper is very poor is that the surface of diamond is not easily wetted by metal and solder, so that the diamond cannot be connected with other materials, and the application of the diamond in the electronic packaging industry is seriously hindered. The wettability of diamond with copper is improved by diamond surface modification, such as adding strong carbon compound elements (W, B, Ti, Cr). However, the modification also brings a new problem of increasing the interface thermal resistance, and influences the thermal conductivity and the thermal expansion coefficient of the diamond/copper composite material.
The above background disclosure is only for the purpose of assisting understanding of the inventive concept and technical solutions of the present invention, and does not necessarily belong to the prior art of the present patent application, and should not be used for evaluating the novelty and inventive step of the present application in the case that there is no clear evidence that the above content is disclosed at the filing date of the present patent application.
Disclosure of Invention
The invention provides a preparation method of a novel diamond copper-based composite material, aiming at solving the problems of poor wettability and poor thermal conductivity of diamond and copper. The diamond copper-based composite material prepared by the invention has the characteristics of high thermal conductivity and low expansion coefficient, and can be widely applied to electronic packaging materials.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the diamond copper-based composite material is prepared from the following raw materials in percentage by weight: 20-50% of diamond, 0.5-2.5% of zirconium, 0.02-0.05% of erbium, 0.01-0.05% of niobium, 0.01-0.05% of tantalum, 0.5-1.5% of rare earth coupling agent, 1-3% of aluminum-zirconium coupling agent and the balance of copper.
The invention also provides a preparation method of the diamond copper-based composite material, which comprises the following steps:
(1) weighing the raw materials according to the proportion, adding the diamond, the zirconium, the erbium, the niobium, the tantalum, the rare earth coupling agent, the aluminum-zirconium coupling agent and the grinding ball into a ball milling tank, and carrying out ball milling to obtain mixed powder;
(2) heating the mixed powder to 700-900 ℃ under the protection of inert gas, preserving the heat for 1-3h, and then pressing and forming to obtain a pressed blank;
(3) and (3) carrying out plasma discharge sintering on the pressed compact to obtain the diamond copper-based composite material.
Preferably, the grinding ball is a zirconia grinding ball, and the ball-to-material ratio is 5-10: 1.
Preferably, the ball milling is performed for 2-4h at the rotating speed of 300-500 r/min.
Preferably, the rare earth coupling agent is a WOT type rare earth coupling agent and is a commercially available product.
Preferably, the press forming is press forming under a pressure of 30 to 50 MPa.
Preferably, the plasma discharge sintering is carried out at 1050-1150 ℃ and 30-40MPa for 3-5 h.
Preferably, the diamond, zirconium, erbium, niobium and tantalum have a particle size of 50 μm or less.
Compared with the prior art, the invention has the advantages and beneficial effects that:
1. the thermal conductivity of the diamond copper-based composite material prepared by the invention reaches more than 520W/(m.K), and the thermal expansion coefficient is lower than 3.0 multiplied by 10-6m/k, can be used as an excellent electronic packaging material, and has wide market prospect.
2. The addition of the aluminum-zirconium coupling agent and the rare earth coupling agent can improve the interfacial wettability of diamond and copper, improve the interfacial bonding force among materials and maintain the performances of high thermal conductivity and low expansion coefficient on the diamond-copper-based composite material.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments. It should be emphasized that the following description is merely exemplary in nature and is not intended to limit the scope of the invention or its application.
Example 1
The diamond copper-based composite material is prepared from the following raw materials in percentage by weight: 35% of diamond, 1.5% of zirconium, 0.03% of erbium, 0.02% of niobium, 0.03% of tantalum, 1.2% of rare earth coupling agent, 2% of aluminum-zirconium coupling agent and the balance of copper. The preparation method comprises the following steps:
(1) weighing the raw materials according to the proportion, adding diamond, zirconium, erbium, niobium, tantalum, rare earth coupling agent and aluminum-zirconium coupling agent, adding zirconia grinding balls into a ball-milling tank according to the ball-material ratio of 8:1, and ball-milling for 3 hours at the rotating speed of 300r/min to obtain mixed powder;
(2) heating the mixed powder to 850 ℃ under the protection of argon, preserving heat for 2.5 hours, and then pressing and forming under the pressure of 40Mpa to obtain a pressed blank;
(3) and (3) sintering the pressed compact for 5h under the conditions of temperature of 1050 ℃ and pressure of 40MPa and the like by electron discharge to obtain the diamond copper-based composite material.
The thermal conductivity of the diamond copper-based composite material prepared by the invention is 649W/(m.K), and the thermal expansion coefficient is 1.94 multiplied by 10-6m/K。
Example 2
The diamond copper-based composite material is prepared from the following raw materials in percentage by weight: 42% of diamond, 1.8% of zirconium, 0.05% of erbium, 0.01% of niobium, 0.03% of tantalum, 0.8% of rare earth coupling agent, 1.2% of aluminum-zirconium coupling agent and the balance of copper. The preparation method comprises the following steps:
(1) weighing the raw materials according to the proportion, adding diamond, zirconium, erbium, niobium, tantalum, rare earth coupling agent and aluminum-zirconium coupling agent, adding zirconia grinding balls into a ball-milling tank according to the ball-material ratio of 5:1, and ball-milling for 2.5 hours at the rotating speed of 500r/min to obtain mixed powder;
(2) heating the mixed powder to 900 ℃ under the protection of argon, preserving heat for 1.5h, and then pressing and forming under the pressure of 35Mpa to obtain a pressed blank;
(3) and (3) sintering the pressed compact for 4h at 1100 ℃ and under the pressure of 35MPa by equal electronic discharge to obtain the diamond copper-based composite material.
The diamond copper-based composite material prepared by the invention has the thermal conductivity of 532W/(m.K) and the thermal expansion coefficient of 2.84 multiplied by 10-6m/K。
Example 3
The diamond copper-based composite material is prepared from the following raw materials in percentage by weight: 28% of diamond, 2.4% of zirconium, 0.03% of erbium, 0.02% of niobium, 0.01% of tantalum, 1.5% of rare earth coupling agent, 2.5% of aluminum-zirconium coupling agent and the balance of copper. The preparation method comprises the following steps:
(1) weighing the raw materials according to the proportion, adding diamond, zirconium, erbium, niobium, tantalum, rare earth coupling agent and aluminum-zirconium coupling agent, adding zirconia grinding balls into a ball-milling tank according to the ball-material ratio of 10:1, and ball-milling for 3.5 hours at the rotating speed of 400r/min to obtain mixed powder;
(2) heating the mixed powder to 750 ℃ under the protection of argon, preserving heat for 3 hours, and then pressing and forming under the pressure of 40Mpa to obtain a pressed blank;
(3) and (3) sintering the pressed compact for 5h under the conditions of temperature of 1050 ℃ and pressure of 30MPa and the like by electron discharge to obtain the diamond copper-based composite material.
The diamond copper-based composite material prepared by the invention has the thermal conductivity 578W/(m.K) and the thermal expansion coefficient 2.11 multiplied by 10-6m/K。
Example 4
The diamond copper-based composite material is prepared from the following raw materials in percentage by weight: 41% of diamond, 0.8% of zirconium, 0.04% of erbium, 0.03% of niobium, 0.02% of tantalum, 1.0% of rare earth coupling agent, 1.5% of aluminum-zirconium coupling agent and the balance of copper. The preparation method comprises the following steps:
(1) weighing the raw materials according to the proportion, adding diamond, zirconium, erbium, niobium, tantalum, rare earth coupling agent and aluminum-zirconium coupling agent, adding zirconia grinding balls into a ball-milling tank according to the ball-material ratio of 7:1, and ball-milling for 4 hours at the rotating speed of 350r/min to obtain mixed powder;
(2) heating the mixed powder to 850 ℃ under the protection of argon, preserving heat for 1.5h, and then pressing and forming under the pressure of 35Mpa to obtain a pressed blank;
(3) and (3) sintering the pressed compact for 4h at 1100 ℃ and 40MPa by equal-electron discharge to obtain the diamond copper-based composite material.
The diamond copper-based composite material prepared by the invention has the thermal conductivity 541W/(m.K) and the thermal expansion coefficient of 2.65 multiplied by 10-6m/K。
Example 5
The diamond copper-based composite material is prepared from the following raw materials in percentage by weight: 28% of diamond, 1.8% of zirconium, 0.02% of erbium, 0.05% of niobium, 0.03% of tantalum, 1.2% of rare earth coupling agent, 2% of aluminum-zirconium coupling agent and the balance of copper. The preparation method comprises the following steps:
(1) weighing the raw materials according to the proportion, adding diamond, zirconium, erbium, niobium, tantalum, rare earth coupling agent and aluminum-zirconium coupling agent, adding zirconia grinding balls into a ball-milling tank according to the ball-material ratio of 5:1, and ball-milling for 3 hours at the rotating speed of 450r/min to obtain mixed powder;
(2) heating the mixed powder to 750 ℃ under the protection of argon, preserving heat for 2.5h, and then pressing and forming under the pressure of 30Mpa to obtain a pressed blank;
(3) and (3) sintering the pressed compact for 5h under the conditions of temperature of 1050 ℃ and pressure of 40MPa and the like by electron discharge to obtain the diamond copper-based composite material.
The diamond copper-based composite material prepared by the invention has the thermal conductivity 588W/(m.K) and the thermal expansion coefficient of 2.32 multiplied by 10-6m/K。
The foregoing is a more detailed description of the invention in connection with specific/preferred embodiments and is not intended to limit the practice of the invention to those descriptions. It will be apparent to those skilled in the art that various substitutions and modifications can be made to the described embodiments without departing from the spirit of the invention, and such substitutions and modifications are to be considered as within the scope of the invention.
Claims (4)
1. A preparation method of a diamond copper-based composite material is characterized by comprising the following steps: the composite material is prepared from the following raw materials in percentage by weight: 20-50% of diamond, 0.5-2.5% of zirconium, 0.02-0.05% of erbium, 0.01-0.05% of niobium, 0.01-0.05% of tantalum, 0.5-1.5% of rare earth coupling agent, 1-3% of aluminum-zirconium coupling agent and the balance of copper;
the preparation method comprises the following steps:
(1) weighing the raw materials according to the proportion, adding the diamond, the zirconium, the erbium, the niobium, the tantalum, the rare earth coupling agent, the aluminum-zirconium coupling agent and the grinding ball into a ball milling tank, and carrying out ball milling to obtain mixed powder;
(2) heating the mixed powder to 700-900 ℃ under the protection of inert gas, preserving the heat for 1-3h, and then pressing and forming to obtain a pressed blank;
(3) carrying out plasma discharge sintering on the pressed compact to obtain a diamond copper-based composite material;
the grinding balls are zirconia grinding balls, and the ball material ratio is 5-10: 1;
the rare earth coupling agent is a WOT type rare earth coupling agent;
the plasma discharge sintering is carried out for 3-5h at the temperature of 1050-1150 ℃ and the pressure of 30-40 MPa.
2. The method for producing a diamond copper-based composite material according to claim 1, characterized in that: the ball milling is carried out for 2-4h at the rotating speed of 300-500 r/min.
3. The method for producing a diamond copper-based composite material according to claim 1, characterized in that: the compression molding is compression molding under the pressure of 30-50 MPa.
4. The method for producing a diamond copper-based composite material according to claim 1, characterized in that: the grain diameter of the diamond, the zirconium, the erbium, the niobium and the tantalum is less than 50 mu m.
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| CN111676385A (en) * | 2020-05-20 | 2020-09-18 | 东南大学 | Preparation method of low-cost high-thermal-conductivity diamond copper composite material |
| CN112877563B (en) * | 2021-02-23 | 2022-05-10 | 郑州华晶金刚石股份有限公司 | Diamond/copper composite material and preparation method thereof |
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| CN101139515B (en) * | 2007-05-18 | 2010-08-18 | 中南大学 | High heat-conductive diamond-copper composite encapsulating material and method for making same |
| CN101649400B (en) * | 2009-07-20 | 2011-04-20 | 温州宏丰电工合金股份有限公司 | Diamond reinforced metal-base composite material for electronic packaging and preparation method thereof |
| WO2011049479A1 (en) * | 2009-10-21 | 2011-04-28 | Andrey Mikhailovich Abyzov | Composite material having high thermal conductivity and process of fabricating same |
| JP5896400B2 (en) * | 2011-11-25 | 2016-03-30 | トーメイダイヤ株式会社 | Diamond-containing heat sink material and method for producing the same |
| CN103489665B (en) * | 2013-10-08 | 2016-04-27 | 哈尔滨东大高新材料股份有限公司 | The preparation method of high breaking low-voltage electrical apparatus contact material, the preparation method of high breaking low-voltage electrical apparatus composite contact material |
| CN104060117A (en) * | 2014-07-08 | 2014-09-24 | 武汉理工大学 | Preparation method for diamond/copper-based composite material |
| CN106633662A (en) * | 2016-12-27 | 2017-05-10 | 铜陵市铜峰光电科技有限公司 | Diamond powder-copper powder high-heat-conductivity composite material for LED (Light Emitting Diode) and preparation method of diamond powder-copper powder high-heat-conductivity composite material |
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