CN110643860A - Ceramic membrane modified diamond/aluminum composite material and pressureless infiltration preparation process thereof - Google Patents
Ceramic membrane modified diamond/aluminum composite material and pressureless infiltration preparation process thereof Download PDFInfo
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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Abstract
The invention discloses a ceramic membrane modified diamond/aluminum composite material and a pressureless infiltration preparation process thereof, wherein the preparation process comprises the following steps: plating a ceramic film on the surface of the diamond powder, wherein the thickness of the film is 30-300 nm; and placing an aluminum alloy ingot on the diamond powder prefabricated body, and heating in a nitrogen atmosphere with the pressure of 0.08-0.15 MPa to obtain the diamond/aluminum composite material. The film layer is optimized in the form of the ceramic film, so that the composite material has better weather resistance, is not easy to attenuate under the conditions of damp heat, cold and hot shock and the like, and the attenuation of the heat conductivity of the product is less than 3 percent, which shows that the ceramic film on the surface of the diamond powder can inhibit the generation of harmful phase aluminum carbide, and the service reliability of the material is improved.
Description
Technical Field
The invention relates to a ceramic membrane modified diamond/aluminum composite material and a pressureless infiltration preparation process thereof.
Background
With the rapid development of the electrical, electronic and communication industries, various semiconductor laser elements and high-frequency elements are continuously developed to high power, high speed and high integration, the heat dissipation problem of the elements and the system is more and more prominent, and if the accumulated heat cannot be conducted or dissipated in time, the work is poor or even fails, which causes serious consequences.
In addition, in various semiconductor elements, the size of the element increases due to the increase in power of the element, and the problem of thermal expansion mismatch between the semiconductor element and the heat sink becomes remarkable. To solve these problems, researchers have sought to develop a thermally conductive material that combines high thermal conductivity with a matched coefficient of thermal expansion.
In the past, no matter how the thermal conductivity of the second generation and third generation metal electronic packaging materials is optimized, the thermal conductivity is difficult to reach 300W/(m.K), so that the development of metal electronic packaging materials with higher thermal conductivity is required.
Diamond has begun to receive attention from the electronic packaging industry as a material having extremely high thermal conductivity (thermal conductivity up to 2000W/(m · K)) and a relatively low thermal expansion coefficient, and as its price continues to decrease, large-scale application has begun to become practical. The diamond powder and the high-thermal-conductivity metal aluminum are compounded to obtain the diamond aluminum composite material, the heat conductivity and the thermal expansion coefficient of the diamond aluminum composite material are organically coordinated, the thermal conductivity higher than that of the electronic packaging materials of the previous generations is obtained, the thermal expansion coefficient matched with a semiconductor is also obtained, and the diamond aluminum composite material becomes a more advanced new generation of metal electronic packaging material in the current market.
The air pressure infiltration technology is one of the common technologies for preparing diamond aluminum composite materials at present and is characterized by vacuum environment, air pressure infiltration, infiltration temperature higher than the melting point of alloy and subsequent slow furnace cooling. The continuous change of pressure and temperature can be realized, the full contact between diamond and liquid aluminum alloy can be realized, the interface combination can be strengthened, and the prepared diamond/aluminum composite material has excellent performance.
Compared with the diamond aluminum composite material prepared by the pressure infiltration process, the pressureless infiltration process does not need pressurization, so that the requirement on equipment is low, the utilization rate of a furnace chamber is high, the targeted design can be performed, and the prepared diamond aluminum composite material has the outstanding advantages of low cost and high efficiency and is an industrialized technical scheme with more superiority.
Chinese invention patent ZL 201110194213.9 discloses a preparation method of a high volume fraction diamond/aluminum heat conduction function composite material, which adopts a salt bath coating method to coat Ti or Cr on diamond particles to obtain a coating with the thickness of 0.1-0.3 mu m, then diamond particle preforms are prepared, aluminum alloy is added, and the composite material is prepared under the nitrogen pressure of 0.6-1.5 MPa. The method has the advantages of high air pressure and high requirement on equipment, and is easy to cause uneven material preparation and poor density, thereby causing unstable material performance.
Disclosure of Invention
In order to overcome the defect that the thermal conductivity of the existing diamond/aluminum composite material is unstable, the invention aims to provide a preparation process of a ceramic membrane modified diamond/aluminum composite material.
It is another object of the present invention to provide a diamond/aluminum composite material produced by the above process.
The purpose of the invention is realized by the following technical scheme:
a pressureless infiltration preparation process of a diamond/aluminum composite material comprises the following steps:
(1) surface treatment of diamond powder
Plating a metal film or a silicon dioxide film on the surface of the diamond powder, and then placing the diamond powder under a vacuum condition and keeping the temperature at 1000 ℃ and 1400 ℃ for 5-10h to generate a ceramic film with the thickness of 30-300 nm; the surface treatment of diamond powder is one of the important solutions to the degradation of the properties of composite materials.
The ceramic membrane is a carbon compound, and the ceramic membrane comprises titanium carbide, tungsten carbide, molybdenum carbide, silicon carbide, chromium carbide, zirconium carbide and neodymium carbide;
the coating method can adopt the methods of the prior art such as magnetron sputtering, chemical plating, chemical vapor deposition, sol-gel and salt bath plating;
the bonding force between diamond and matrix aluminum alloy is weak, which is the main reason for poor performance of the diamond/aluminum composite material. The ceramic film on the surface of the diamond is a key transition phase, so that the interface bonding force can be effectively improved, the performance of the composite material is further improved, and the interface harmful phase Al can be inhibited4C3And (4) generating.
(2) Pressureless infiltration for preparing composite material
The diamond/aluminum composite material has a certain size and shape when used as a product. Due to the addition of diamond powder, the processability of the composite material is poor, and therefore, a direct forming mode is adopted, and the subsequent processing is reduced as much as possible.
In the invention, diamond powder is prepared into a prefabricated body with certain shape and strength in advance before the aluminum alloy is impregnated, and a binder is required.
Placing an aluminum alloy ingot on the diamond powder prefabricated body, and heating in a nitrogen atmosphere with the pressure of 0.08-0.15 MPa to obtain a diamond/aluminum composite material; the heating temperature and time are related to the type of alloy and the quality of the aluminum ingot;
the nitrogen gas has the function of reacting with magnesium element in the aluminum alloy, breaking a surface oxidation film which obstructs the flow of molten aluminum and promoting the penetration of aluminum liquid in the diamond powder prefabricated body. The invention adopts lower nitrogen pressure, which not only meets the reaction requirement, but also avoids the residue of nitrogen in the composite material, thereby reducing the density and the heat conductivity of the composite material.
In the step (1), the particle size of the diamond powder is 10-300 μm;
the diamond powder preform in the step (2) can be prepared by one of the following two methods:
firstly, diamond powder is put into a die and then compacted, and then high-temperature oxidation is carried out to obtain a prefabricated body;
mixing diamond powder and a binder, putting the mixture into a mould, and performing exhaust, pressurization and curing molding to obtain a prefabricated body; the curing temperature is different according to the type of the binder;
the diamond powder is mixed with a binder, and the binder accounts for 0.5-10.0% of the mass of the mixture. The volume fraction of the diamond powder is 50-75%, and the volume fraction of the diamond is related to the shape and the particle size distribution of the diamond powder and also related to the dosage of the binder;
the adhesive is one of the following:
TABLE 1 Binder composition
| Serial number | Binder composition |
| 1 | Polyacrylamide |
| 2 | Starch + polyvinyl alcohol |
| 3 | Graphite + polyvinyl alcohol |
| 4 | Paraffin and polyvinyl alcohol |
| 5 | Silica sol, glycerol and stearic acid |
| 6 | Silica sol and furan resin |
| 7 | Paraffin and stearic acid |
| 8 | Epoxy resin + ammonium dihydrogen phosphate |
The Al-Mg-Si alloy is preferably selected as the aluminum alloy in the step (2), wherein the mass fraction of Mg is 2-15%, and the mass fraction of Si is 5-25%;
the heating in the step (2) is carried out for 0.5-3.0 h at 780-1100 ℃; the temperature and time of heat preservation are related to the type of alloy and the quality of the aluminum ingot.
Compared with the prior art, the invention has the following advantages and effects:
1. the film layer is optimized in the form of the ceramic film, so that the composite material has better weather resistance, is not easy to attenuate under the conditions of damp heat, cold and hot shock and the like, and the attenuation of the heat conductivity of the product is less than 3 percent, which shows that the ceramic film on the surface of the diamond powder can inhibit the generation of harmful phase aluminum carbide, and the service reliability of the material is improved.
2. The invention solves the problems of high cost and low efficiency of the diamond aluminum composite material and the product thereof in the production and preparation process. The diamond aluminum composite material prepared by the pressureless infiltration process has excellent performance, meets the heat conduction and heat dissipation requirements of high-power electronic equipment, and is easy to control the product quality and stability.
Drawings
FIG. 1 is a scanning electron micrograph of the diamond/aluminum composite obtained in example 1.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto.
Example 1
A diamond/aluminum composite material adopts aluminum alloy of Al-5Mg-10Si, wherein the mass fraction of Mg is 5%, the mass fraction of Si is 10%, and the balance is Al.
The average grain diameter of the diamond powder is 170 mu m, the crystal form is better, the magnetron sputtering method is adopted to plate titanium on the diamond powder, and then the titanium carbide film is generated by vacuum heating. The specific method comprises the following steps: the target material of magnetron sputtering is a pure titanium target material with the purity of 99.99 percent, and the size of the target material is 50mm in thickness and 100mm in diameter. Sputtering pressure is 6-8 x 10-3Pa, Ar as sputtering gas, 0.9A of sputtering current, 600V of sputtering voltage, 300 ℃ of sputtering temperature and 3h of sputtering time. In order to ensure uniform diamond powder coating, the swing frequency of the sample holder is 0.5Hz, and the ultrasonic vibration frequency is 30 KHz. After plating a titanium film on the diamond powder, the degree of vacuum was 5X 10-3And (3) keeping the temperature of 1000 ℃ for 10h in a vacuum furnace with Pa, and generating a ceramic coating of titanium carbide by utilizing the reaction of titanium and diamond, wherein the thickness of the coating is 120 nm.
The adhesive for preparing the prefabricated body adopts silica sol and furan resin, and the mass of the adhesive is 2.8 percent of that of the diamond powder. Uniformly mixing the coated diamond powder and a binder, putting the mixture into a mould, vibrating and exhausting, applying a certain pressure to press the blank of the prefabricated body, solidifying, demoulding and taking out the prefabricated body. The mould forming method adopts isostatic pressing graphite as a mould material, and after the mould material is cooled along with a furnace, the mould is removed, and a product is taken out.
And placing an aluminum alloy ingot on the prefabricated body and placing the prefabricated body in an atmosphere furnace. Closing the furnace, starting to vacuumize, introducing nitrogen at 0.1MPa, and heating. When the temperature in the furnace reaches 950 ℃, the heat preservation is started, and the heat preservation is carried out for 1.5 h. After cooling with the furnace, the furnace is opened, and according to the product size, the excess aluminum alloy is mechanically processed to obtain the diamond-aluminum composite material, and fig. 1 is a scanning electron microscope photograph of the obtained diamond/aluminum composite material. The properties are shown in Table 2.
TABLE 2 test Properties of Diamond-Al composites
Because the ceramic film is plated on the surface of the diamond, the composite material has better weather resistance and is not easy to attenuate under the conditions of damp heat, cold and hot shock and the like. As shown in Table 2, under the damp-heat test conditions of 60 ℃, 85% humidity and 30 days standing, the attenuation of the thermal conductivity of the product is less than 3%, which shows that the TiC film on the surface of the diamond powder can inhibit the generation of harmful phase aluminum carbide and improve the service reliability of the material.
Example 2
A diamond/aluminum composite material comprises aluminum alloy Al-6Mg-12Si, wherein the mass fraction of Mg is 6%, the mass fraction of Si is 12%, and the balance is Al.
The diamond powder has the average grain diameter of 140 mu m and better crystal form, and adopts a magnetron sputtering method to plate W and then adopts a vacuum heating method to plate carbide on the surface of the diamond powder. The specific method comprises the following steps: the target material of magnetron sputtering is a pure W target material with the purity of 99.99 percent, and the size of the target material is 50mm in thickness and 100mm in diameter. Sputtering pressure is 6-8 x 10-3Pa, Ar as sputtering gas, 1A of sputtering current, 600V of sputtering voltage, 300 ℃ of sputtering temperature and 1.5h of sputtering time. In order to ensure uniform diamond powder coating, the swing frequency of the sample holder is 0.5Hz, and the ultrasonic vibration frequency is 30 KHz. After the diamond powder was coated with a W film, the degree of vacuum was 5X 10-3And (3) keeping the temperature of 1400 ℃ for 8h in a Pa vacuum furnace, and generating a tungsten carbide ceramic coating by utilizing the reaction of titanium and diamond, wherein the thickness of the coating is 40 nm.
The binder of the prefabricated body adopts epoxy resin and ammonium dihydrogen phosphate, and the mass of the binder is 1.5 percent of the mass of the diamond powder. Uniformly mixing the coated diamond powder and a binder, putting the mixture into a mould, vibrating and exhausting, applying a certain pressure to press the blank of the prefabricated body, solidifying, demoulding and taking out the prefabricated body.
And placing an aluminum alloy ingot on the prefabricated body and placing the prefabricated body in an atmosphere furnace. Closing the furnace, starting to vacuumize, introducing nitrogen, keeping the pressure at 0.12MPa, and starting to heat. When the temperature in the furnace reaches 960 ℃, heat preservation is started, and heat preservation is carried out for 1 h. After cooling with the furnace, the furnace was opened and, depending on the product size, the excess aluminum alloy was machined off to obtain a diamond-aluminum composite material having the properties shown in table 3.
TABLE 3 test Properties of Diamond-Al composites
Example 3
A diamond/aluminum composite material comprises aluminum alloy Al-7Mg-9Si, wherein the mass fraction of Mg is 7%, the mass fraction of Si is 9%, and the balance is Al.
The diamond powder has the average grain diameter of 240 mu m and better crystal form, and the surface of the diamond powder is coated with SiO by adopting a sol-gel method2And then generating silicon carbide on the surface of the diamond powder by a vacuum heating method. 30g diamond powder, 2ml oleic acid, 11ml ammonia and 110ml ethanol mixed, rapid stirring for 30min, then adding 400ml ethanol, 30ml ammonia and 10ml ethyl orthosilicate, rapid stirring for 2 hours. Then, the mixture was filtered, and the diamond powder was washed and dried at 60 ℃ for 2 hours. Then putting diamond powder into vacuum degree of 5X 10-3And (3) keeping the temperature of 1200 ℃ for 5h in a Pa vacuum furnace to generate a silicon carbide ceramic coating with the thickness of about 100 nm.
The binder of the prefabricated body is polyacrylamide, and the mass of the binder is 2.1 percent of that of the diamond powder. Uniformly mixing the coated diamond powder and a binder, putting the mixture into a mould, vibrating and exhausting, applying a certain pressure to press the blank of the prefabricated body, solidifying, demoulding and taking out the prefabricated body.
And placing an aluminum alloy ingot on the prefabricated body and placing the prefabricated body in an atmosphere furnace. Closing the furnace, starting to vacuumize, introducing nitrogen, keeping the pressure at 0.12MPa, and starting to heat. When the temperature in the furnace reaches 900 ℃, the heat preservation is started, and the heat preservation is carried out for 2 hours. After cooling with the furnace, the furnace was opened and the excess aluminum alloy was machined off according to the product size to obtain diamond-aluminum composite materials with properties as shown in table 4.
TABLE 4 test Properties of Diamond-Al composites
Example 4
A diamond/aluminum composite material comprises aluminum alloy Al-5Mg-15Si, wherein the mass fraction of Mg is 5%, the mass fraction of Si is 15%, and the balance is Al.
The average grain diameter of the diamond powder is 140 mu m, the crystal form is better, Cr is plated on the surface of the diamond powder by a salt bath method, and then chromium carbide is generated on the surface of the diamond powder by a vacuum heating method. The salt bath method comprises weighing 420 mesh Cr powder and diamond powder at the same volume ratio, mixing uniformly, placing into a crucible, covering the surface of the mixed powder with uniformly mixed chloride with the same mass as the diamond powder, wherein the chloride comprises NaCl and BaCl2The mass ratio of the two is 2: 1. heating to 950 ℃ in a resistance furnace, and keeping the temperature for 8 hours. And then taking out the powder, putting the powder into deionized water, heating and boiling the powder, removing mixed salt, drying the rest powder, putting the powder into a 180-mesh sieve, vibrating the powder for 30 minutes by using a vibrating screen machine, cleaning the diamond powder on the sieve by using acetone, and drying the diamond powder. After plating a Cr film on the diamond powder, the degree of vacuum was 5X 10-3Pa, and keeping the temperature at 1200 ℃ for 9.5h in a vacuum furnace, and generating a ceramic coating of chromium carbide by utilizing the reaction of chromium and diamond, wherein the film thickness is about 150 nm.
The binder of the prefabricated body adopts epoxy resin and ammonium dihydrogen phosphate, and the mass of the binder is 3.5 percent of the mass of diamond powder. Uniformly mixing the coated diamond powder and a binder, putting the mixture into a mould, vibrating and exhausting, applying a certain pressure to press the blank of the prefabricated body, solidifying, demoulding and taking out the prefabricated body.
And placing an aluminum alloy ingot on the prefabricated body and placing the prefabricated body in an atmosphere furnace. Closing the furnace, starting to vacuumize, introducing nitrogen, keeping the pressure at 0.1MPa, and starting to heat. When the temperature in the furnace reaches 870 ℃, the heat preservation is started and is carried out for 2 hours. After cooling with the furnace, the furnace was opened and, depending on the product size, the excess aluminum alloy was machined off to obtain diamond-aluminum composite materials with properties as shown in table 5.
TABLE 5 test Properties of Diamond aluminum composites
As can be seen from tables 3 to 5, the composite material has good weather resistance and is not easy to attenuate under the conditions of damp heat, cold and heat shock and the like because the film layer is a ceramic film. Under the damp-heat test condition of 60 ℃, humidity of 85% and standing for 30 days, the attenuation of the heat conductivity of the product is less than 3%, which shows that the ceramic film on the surface of the diamond powder can inhibit the generation of harmful phase aluminum carbide and improve the service reliability of the material.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A pressureless infiltration preparation process of a diamond/aluminum composite material is characterized by comprising the following steps:
(1) plating a metal film or a silicon dioxide film on the surface of the diamond powder, and then placing the diamond powder under a vacuum condition and keeping the temperature at 1000 ℃ and 1400 ℃ for 5-10h to generate a ceramic film with the thickness of 30-300 nm;
(2) and placing an aluminum alloy ingot on the diamond powder prefabricated body, and heating in a nitrogen atmosphere with the pressure of 0.08-0.15 MPa to obtain the diamond/aluminum composite material.
2. The process according to claim 1, characterized in that: the ceramic membrane in the step (1) is a carbon compound, and the ceramic membrane comprises titanium carbide, molybdenum carbide, tungsten carbide, silicon carbide, chromium carbide, zirconium carbide and neodymium carbide.
3. The process according to claim 1, characterized in that: and (2) plating the ceramic film in the step (1), wherein the plating method adopts magnetron sputtering, chemical plating, chemical vapor deposition, sol-gel or salt bath plating.
4. The process according to claim 1, characterized in that: in the step (1), the diamond powder has a particle size of 10-300 μm.
5. The process according to claim 1, characterized in that: the diamond powder preform in the step (2) is prepared by one of the following two methods:
firstly, diamond powder is put into a die and then compacted, and then high-temperature oxidation is carried out to obtain a prefabricated body;
secondly, diamond powder and a binder are mixed and put into a mould, and a prefabricated body is obtained after exhausting, pressurizing, curing and forming.
6. The process according to claim 5, characterized in that: the diamond powder is mixed with a binder, and the binder accounts for 0.5-10.0% of the mass of the mixture.
7. The process according to claim 5, characterized in that: the adhesive is one of the following:
TABLE 1 Binder composition
8. The process according to claim 1, characterized in that: the aluminum alloy in the step (2) is Al-Mg-Si alloy, wherein the mass fraction of Mg is 2-15%, and the mass fraction of Si is 5-25%.
9. The process according to claim 1, characterized in that: and (3) heating, namely preserving the heat at 780-1100 ℃ for 0.5-3.0 h.
10. A diamond/aluminum composite characterized by: is obtainable by the process according to any one of claims 1 to 9.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113547101A (en) * | 2021-07-21 | 2021-10-26 | 长飞光纤光缆股份有限公司 | Preparation method and product of high-thermal-conductivity diamond-aluminum-based composite material |
| CN114734039A (en) * | 2022-04-14 | 2022-07-12 | 南京瑞为新材料科技有限公司 | Diamond aluminum composite material and preparation method thereof |
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| CN114734039A (en) * | 2022-04-14 | 2022-07-12 | 南京瑞为新材料科技有限公司 | Diamond aluminum composite material and preparation method thereof |
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