CN111748716A - Method for preparing Cu-Zr/Diamond copper-based composite material by using matrix alloying method - Google Patents
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- 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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- 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
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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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
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- B22F3/16—Both compacting and sintering in successive or repeated steps
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0824—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with a specific atomising fluid
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- 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
The invention provides a method for preparing a Cu-Zr/Diamond copper-based composite material by using a matrix alloying method, belonging to the technical field of copper-based composite materials; the copper-based composite material consists of 30-50% of Cu-Zr alloy and 50-70% of diamond particles; the preparation method comprises the following steps: preparing Cu-Zr alloy powder; fully mixing Cu-Zr alloy powder and pure diamond powder in a mixer with argon protection; pre-pressing and pre-sintering the mixed powder in a mould; finally, preparing the Cu-Zr/Diamond copper-based composite material in a hot-pressing sintering furnace in a hot-pressing sintering mode; the unique re-pressing and re-sintering process of the invention utilizes a secondary heating method, avoids long-time heating at high temperature, reduces the risk of graphitizing the diamond surface at high temperature, and provides guarantee for forming a perfect ZrC transition layer on the interface.
Description
Technical Field
The invention relates to the technical field of copper-based composite materials, in particular to a method for preparing a Cu-Zr/Diamond copper-based composite material by using a matrix alloying method.
Background
With the development of the next generation of integrated circuits and high power communication devices, the requirements for thermal management materials are becoming more and more strict, so effective heat dissipation is called as a key problem of the reliability of modern electronic, photoelectric and electronic devices. The diamond-copper-based composite material is mainly used for electronic packaging substrates, radiating fins and heat sinks, and is mainly characterized by being used for electronic devices with extremely high power density and extremely high radiating requirements. Therefore, the high-power RF, LD, LED and integrated circuit packaging has huge market potential and wide application prospect in the long-term market of high-power RF, LD, LED and integrated circuit packaging.
A common method for preparing diamond-copper composite materials is to improve the interface bonding performance by means of diamond surface metallization. The method for metallizing the surface of the diamond mainly comprises the steps of covering the surface of the diamond with a coating through some ways, wherein a Cr layer, a Ti layer, a Mo layer, a Zr layer and the like are mainly formed. Most Diamond-Cu manufacturers adopt a plating method, mainly including the technologies of magnetron sputtering, molten salt method, vacuum evaporation and the like, and the preparation method has complex process and higher cost, thereby limiting the wide use of the material.
Disclosure of Invention
Aiming at the problems, the invention provides a method for preparing a Cu-Zr/Diamond copper-based composite material by using a matrix alloying method; according to the invention, a ZrC transition layer is formed on the surface of the diamond by using a matrix alloying method, and alloy elements are introduced into a copper matrix by using a copper matrix metallization method, so that the mutual diffusion between metal and a reinforcement can be promoted by the subsequent hot-pressing sintering, the improvement of interface bonding is facilitated, and the densification and the improvement of interface strength of a composite material are promoted.
The technical scheme of the invention is as follows: a method for preparing a Cu-Zr/Diamond copper-based composite material by using a matrix alloying method comprises the following steps: 30-50% of Cu-Zr alloy and 50-70% of diamond particles, wherein the particle size of the diamond particles is 50-180 mu m;
the preparation method of the copper-based composite material comprises the following steps:
A. preparation of Cu-Zr alloy powder: fully mixing a raw material Cu and a raw material Zr in a mixer with argon protection, putting the mixture into a vacuum consumable arc melting furnace, and melting under the argon protection when the vacuum degree is pumped to reach a pH value less than or equal to 3 Pa: firstly, controlling the current at 200A and keeping for 3-5 min; then raising the current to 280-300A, and keeping for 1-2 min; then raising the current to 500-1000A, and keeping for 2-3 min; cooling to obtain a Cu-Zr alloy base block; then, putting the Cu-Zr alloy base block into a vacuum induction furnace, atomizing into a water atomization alloy material through a water atomization nozzle under the condition that the water pressure is 180-200 MPa after the Cu-Zr alloy base block is completely melted into a liquid state at 1900-2000 ℃, and then dehydrating and drying to obtain Cu-Zr alloy powder;
B. fully mixing Cu-Zr alloy powder and pure diamond powder in a mixer with argon protection according to the volume percentage;
C. pre-pressing and pre-sintering the mixed powder in a mould; wherein the compaction density is 60-80%;
D. and finally, preparing the Cu-Zr/Diamond copper-based composite material in a hot-pressing sintering furnace in a hot-pressing sintering mode.
Further, in the step A, the raw material Cu adopts an electrolytic copper block, and the raw material Zr adopts a high-purity zirconium block; mixing 0.5-3.5% of Zr and 96.5-99.5% of Cu according to mass percentage; the impurity content can be controlled from the source by adopting the raw materials with higher purity, and the influence of impurities on the performance of the prepared composite material is effectively avoided.
Further, in the step A, when the raw material Cu and the raw material Zr are smelted, after the raw materials are completely smelted, degassing treatment is carried out on the smelted raw material solution; the impurity gases contained in the raw material melt during melting can be effectively removed by degassing treatment.
Further, the degassing treatment is specifically as follows: treating the raw material solution for 120-150 s when the raw material is completely dissolved by using ultrasonic waves with the power of 800-950W and the frequency of 28-29 kHz; the traditional degassing mode is difficult to carry new impurities into the system during specific implementation, and the ultrasonic degassing treatment can ensure that the new impurities are not carried in on the basis of ensuring the degassing effect.
Further, the specific parameters of the pre-sintering in the step C are as follows: heating to 650-750 ℃ at a heating rate of 10 ℃/min, and preserving heat for 1-1.5 h; the sintering material can be more effectively densified through the heating up at a fixed heating up rate and the entering and exiting of the pre-sintering, so that the hot-pressing sintering at the later stage is facilitated.
Further, the specific parameters of the pre-sintering in the step C are as follows: heating to 750-960 ℃ at a heating rate of 30 ℃/min, and keeping the temperature for 0.5-1 h; the densification of the sintered object can be ensured at a higher and proper heating rate, and the temperature of the pre-sintering is closer to the hot-pressing sintering temperature in the later period, so that the graphitization of the diamond surface can be effectively avoided.
Further, the hot-pressing sintering parameters in the step D are as follows: and carrying out hot-pressing sintering under a vacuum condition, wherein the sintering temperature is 950-1100 ℃, the pressure is 50-80 MPa, and the heat preservation time is 0.5-1.5 h.
Compared with the prior art, the invention has the beneficial effects that:
1) a ZrC transition layer is formed on the surface of the diamond by utilizing a matrix alloying method, the thickness of ZrC can be adjusted by controlling the Zr content and subsequent sintering temperature and time, and the like, and meanwhile, the traditional expensive diamond surface coating method is omitted, and the cost is greatly saved.
2) The unique re-pressing and re-sintering process of the invention utilizes a secondary heating method, avoids long-time heating at high temperature, reduces the risk of graphitizing the diamond surface at high temperature, and provides guarantee for forming a perfect ZrC transition layer on the interface.
Drawings
FIG. 1 is a schematic view of interface bonding in the process of example 1 of the present invention;
FIG. 2 is a schematic view of interface bonding in the process of example 3 of the present invention.
Detailed Description
Example 1: raw materials: pure diamond particles having an average particle size of 80 μm, atomized pure copper powder.
Fully mixing diamond particles with the average particle size of 80 mu m and atomized pure copper powder, and performing pre-pressing sintering after mixing, wherein the sintering temperature is 690 ℃, and the compaction density is 75%. Carrying out hot-pressing sintering on the pre-sintered blank, wherein the related technical conditions of the hot-pressing sintering are as follows: hot-pressing sintering is carried out under the vacuum condition, the sintering temperature is 950 ℃, the pressure is 60MPa, and the heat preservation time is 0.5 h. The thermal conductivity of the prepared composite material was 182W/(m × K).
Example 2: raw materials: pure diamond particles having an average particle size of 80 μm, atomized Cu-0.6Zr powder.
Diamond particles with the average particle size of 80 microns and atomized Cu-0.6Zr powder are fully mixed, pre-pressing and sintering are carried out after mixing, the sintering temperature is 690 ℃, and the compaction density is 75%. Carrying out hot-pressing sintering on the pre-sintered blank, wherein the related technical conditions of the hot-pressing sintering are as follows: hot-pressing sintering is carried out under the vacuum condition, the sintering temperature is 1050 ℃, the pressure is 60MPa, and the heat preservation time is 0.5 h. The thermal conductivity of the prepared composite material is 480W/(m × K).
Example 3: raw materials: pure diamond particles having an average particle size of 80 μm, atomized Cu-1.4Zr powder.
Fully mixing diamond particles with the average particle size of 80 mu m and atomized Cu-1.4Zr powder, and performing pre-pressing sintering after mixing, wherein the sintering temperature is 780 ℃ and the compaction density is 75%. Carrying out hot-pressing sintering on the pre-sintered blank, wherein the related technical conditions of the hot-pressing sintering are as follows: hot-pressing sintering is carried out under the vacuum condition, the sintering temperature is 1050 ℃, the pressure is 60MPa, and the heat preservation time is 0.8 h. The thermal conductivity of the prepared composite material is 620W/(m × K).
Example 4: raw materials: pure diamond particles having an average particle size of 80 μm, atomized Cu-2.5Zr powder.
Diamond particles with the average particle size of 80 mu m and atomized Cu-2.5Zr powder are fully mixed, pre-pressing and sintering are carried out after mixing, the sintering temperature is 960 ℃, and the compaction density is 75%. Carrying out hot-pressing sintering on the pre-sintered blank, wherein the related technical conditions of the hot-pressing sintering are as follows: hot-pressing sintering is carried out under the vacuum condition, the sintering temperature is 1050 ℃, the pressure is 60MPa, and the heat preservation time is 1 h. The thermal conductivity of the prepared composite material is 520W/(m × K).
Example 5: raw materials: pure diamond particles having an average particle size of 80 μm, atomized Cu-1.4Zr powder.
Fully mixing diamond particles with the average particle size of 80 mu m and atomized Cu-1.4Zr powder, pre-pressing and sintering after mixing, raising the temperature to 780 ℃ at the temperature rise speed of 30 ℃/min, preserving the heat for 0.5h, and enabling the compaction density to be 75%. Carrying out hot-pressing sintering on the pre-sintered blank, wherein the related technical conditions of the hot-pressing sintering are as follows: hot-pressing sintering is carried out under the vacuum condition, the sintering temperature is 1050 ℃, the pressure is 60MPa, and the heat preservation time is 0.8 h. The thermal conductivity of the prepared composite material is 640W/(m × K).
Example 6: the rest of the operation and process parameters are the same as those of the example 1, except that:
raw materials: pure diamond particles with the average particle size of 80 mu m and atomized Cu-0.6Zr alloy powder;
the specific preparation method of the Cu-0.6Zr powder comprises the following steps: fully mixing 0.6 percent of raw material Zr and 99.4 percent of raw material Cu in a mixer with argon protection according to mass percent, putting the mixture into a vacuum consumable arc melting furnace, and melting under the argon protection when the vacuum degree is pumped to reach a pH value less than or equal to 3 Pa: firstly, controlling the current at 200A and keeping the current for 3 min; then the current is increased to 280A and kept for 1 min; then the current is increased to 500A and kept for 2 min; cooling to obtain a Cu-Zr alloy base block; then, the Cu-Zr alloy base block is placed in a vacuum induction furnace, after the Cu-Zr alloy base block is completely melted into liquid under the temperature of 1900 ℃, the Cu-Zr alloy base block is atomized into a water atomized alloy material through a water atomization nozzle under the condition that the water pressure is 180MPa, and then the Cu-Zr alloy powder is obtained after dehydration and drying. The thermal conductivity of the prepared composite material is 510W/(m × K).
Example 7: the rest of the operation and process parameters are the same as those of the example 1, except that:
raw materials: pure diamond particles with the average particle size of 80 mu m and atomized Cu-1.4Zr alloy powder;
the specific preparation method of the Cu-1.4Zr powder comprises the following steps: fully mixing 1.4% of Zr and 98.6% of Cu in a mixer with argon protection according to mass percent, putting the mixture into a vacuum consumable arc melting furnace, and melting under the argon protection when the vacuum degree is pumped to reach a pH value less than or equal to 3 Pa: firstly, controlling the current at 200A and keeping for 4 min; then the current is increased to 290A and kept for 1 min; then the current is increased to 800A and kept for 2 min; cooling to obtain a Cu-Zr alloy base block; then putting the Cu-Zr alloy base block into a vacuum induction furnace, atomizing the Cu-Zr alloy base block into a water atomization alloy material through a water atomization nozzle under the condition that the water pressure is 190MPa after the Cu-Zr alloy base block is completely melted into a liquid state at 1900 ℃, and then dehydrating and drying to obtain Cu-Zr alloy powder; when the raw material Cu and the raw material Zr are smelted, degassing treatment is carried out on a molten raw material solution after the raw materials are completely molten, and the method specifically comprises the following steps: the raw material solution was treated for 120 seconds with ultrasonic waves having a power of 900W and a frequency of 278kHz when the raw material was completely dissolved. The thermal conductivity of the prepared composite material is 640W/(m × K).
Example 8: the rest of the operation and process parameters are the same as those of the example 1, except that:
raw materials: pure diamond particles with the average particle size of 80 mu m and atomized Cu-2.5Zr alloy powder;
the specific preparation method of the Cu-02.5Zr powder comprises the following steps: fully mixing 2.5 percent of raw material Zr and 97.5 percent of raw material Cu in a mixer with argon protection according to mass percent, putting the mixture into a vacuum consumable arc melting furnace, and melting under the argon protection when the vacuum degree is pumped to reach a pH value less than or equal to 3 Pa: firstly, controlling the current at 200A and keeping for 5 min; then the current is increased to 300A and kept for 2 min; then the current is increased to 1000A and kept for 3 min; cooling to obtain a Cu-Zr alloy base block; then putting the Cu-Zr alloy base block into a vacuum induction furnace, atomizing the Cu-Zr alloy base block into a water atomized alloy material through a water atomization nozzle under the condition that the water pressure is 200MPa after the Cu-Zr alloy base block is completely melted into a liquid state at 2000 ℃, and then dehydrating and drying to obtain Cu-Zr alloy powder; when the raw material Cu and the raw material Zr are smelted, degassing treatment is carried out on a molten raw material solution after the raw materials are completely molten, and the method specifically comprises the following steps: the raw material solution was treated for 150 seconds with ultrasonic waves having a power of 850W and a frequency of 28kHz when the raw material was completely dissolved. The thermal conductivity of the prepared composite material is 550W/(m × K).
And (4) conclusion:
1. compared with the examples 2 to 7, the heat conductivity of the prepared composite material can be effectively improved by selecting the pure diamond particles and the CuZr powder as the raw materials in the example 1.
2. Compared with the examples 6, 7 and 8, the Cu-Zr alloy powder selected as the raw material has the advantages that the powder purity and the Zr element content in the powder influence the thermal conductivity of the prepared composite material; wherein, the thermal conductivity of the composite material can be improved by adopting the method of the embodiments 6, 7 and 8 to prepare the atomized Cu-Zr alloy powder; when the Zr element content is about 1.4, the thermal conductivity of the prepared composite material is optimal.
By comparing the examples 3 and 5, the thermal conductivity of the prepared composite material can be slightly improved by properly improving the parameters of the pre-sintering, but the effect is not very different.
Claims (7)
1. The method for preparing the Cu-Zr/Diamond copper-based composite material by using the matrix alloying method is characterized in that the composition and the volume percentage content of the copper-based composite material are as follows: 30-50% of Cu-Zr alloy and 50-70% of diamond particles, wherein the particle size of the diamond particles is 50-180 mu m;
the preparation method of the copper-based composite material comprises the following steps:
A. preparation of Cu-Zr alloy powder: fully mixing a raw material Cu and a raw material Zr in a mixer with argon protection, putting the mixture into a vacuum consumable arc melting furnace, and melting under the argon protection when the vacuum degree is pumped to reach a pH value less than or equal to 3 Pa: firstly, controlling the current at 200A and keeping for 3-5 min; then raising the current to 280-300A, and keeping for 1-2 min; then raising the current to 500-1000A, and keeping for 2-3 min; cooling to obtain a Cu-Zr alloy base block; then, putting the Cu-Zr alloy base block into a vacuum induction furnace, atomizing into a water atomization alloy material through a water atomization nozzle under the condition that the water pressure is 180-200 MPa after the Cu-Zr alloy base block is completely melted into a liquid state at 1900-2000 ℃, and then dehydrating and drying to obtain Cu-Zr alloy powder;
B. fully mixing Cu-Zr alloy powder and pure diamond powder in a mixer with argon protection according to the volume percentage;
C. pre-pressing and pre-sintering the mixed powder in a mould; wherein the compaction density is 60-80%;
D. and finally, preparing the Cu-Zr/Diamond copper-based composite material in a hot-pressing sintering furnace in a hot-pressing sintering mode.
2. The method for preparing Cu-Zr/Diamond copper-based composite material by matrix alloying according to claim 1, wherein in the step A, the raw material Cu is electrolytic copper block, and the raw material Zr is high-purity zirconium block; and 0.5-3.5% of Zr and 96.5-99.5% of Cu are mixed according to mass percentage.
3. The method for preparing Cu-Zr/Diamond copper-based composite material according to claim 1, wherein in step A, the molten raw material solution is degassed after the raw materials are all melted during the process of melting raw materials Cu and Zr.
4. The method for preparing the Cu-Zr/Diamond copper-based composite material by the matrix alloying method according to claim 1, wherein the specific parameters of the pre-sintering in the step C are as follows: heating to 650-750 ℃ at a heating rate of 10 ℃/min, and preserving heat for 1-1.5 h.
5. The method for preparing the Cu-Zr/Diamond copper-based composite material by the matrix alloying method according to claim 1, wherein the specific parameters of the pre-sintering in the step C are as follows: heating to 750-960 ℃ at a heating rate of 30 ℃/min, and preserving heat for 0.5-1 h.
6. The method for preparing the Cu-Zr/Diamond copper-based composite material by the matrix alloying method according to claim 1, wherein the specific parameters of the hot-pressing sintering in the step D are as follows: and carrying out hot-pressing sintering under a vacuum condition, wherein the sintering temperature is 950-1100 ℃, the pressure is 50-80 MPa, and the heat preservation time is 0.5-1.5 h.
7. The method for preparing a Cu-Zr/Diamond copper-based composite material according to claim 1, wherein the Diamond has Diamond particles with a particle size of 50 to 180 μm.
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| CN116329553A (en) * | 2023-02-23 | 2023-06-27 | 南京瑞为新材料科技有限公司 | Device and method for preparing diamond/metal composite material |
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| CN113445088A (en) * | 2021-06-28 | 2021-09-28 | 沈伟 | Vapor chamber with high heat absorption and preparation method thereof |
| CN113445088B (en) * | 2021-06-28 | 2021-12-14 | 沈伟 | Vapor chamber with high heat absorption and preparation method thereof |
| CN116329553A (en) * | 2023-02-23 | 2023-06-27 | 南京瑞为新材料科技有限公司 | Device and method for preparing diamond/metal composite material |
| CN116329553B (en) * | 2023-02-23 | 2024-04-16 | 南京瑞为新材料科技有限公司 | Device and method for preparing diamond/metal composite material |
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