CN115261659A - Method for rapidly forming compact diamond metal matrix composite material component by two-step method - Google Patents
Method for rapidly forming compact diamond metal matrix composite material component by two-step method Download PDFInfo
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- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 104
- 239000010432 diamond Substances 0.000 title claims abstract description 104
- 238000000034 method Methods 0.000 title claims abstract description 84
- 239000011156 metal matrix composite Substances 0.000 title claims abstract description 31
- 239000000463 material Substances 0.000 title claims description 51
- 239000000843 powder Substances 0.000 claims abstract description 86
- 229910052751 metal Inorganic materials 0.000 claims abstract description 55
- 239000002184 metal Substances 0.000 claims abstract description 55
- 239000011248 coating agent Substances 0.000 claims abstract description 45
- 238000000576 coating method Methods 0.000 claims abstract description 45
- 230000001681 protective effect Effects 0.000 claims abstract description 27
- 239000012298 atmosphere Substances 0.000 claims abstract description 24
- 238000002156 mixing Methods 0.000 claims abstract description 22
- 238000000748 compression moulding Methods 0.000 claims abstract description 14
- 238000000280 densification Methods 0.000 claims abstract description 13
- 238000005245 sintering Methods 0.000 claims description 52
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 32
- 238000010438 heat treatment Methods 0.000 claims description 24
- 238000003825 pressing Methods 0.000 claims description 22
- 239000007789 gas Substances 0.000 claims description 17
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 16
- 239000011812 mixed powder Substances 0.000 claims description 14
- 238000005303 weighing Methods 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 12
- 238000011049 filling Methods 0.000 claims description 12
- 229910052721 tungsten Inorganic materials 0.000 claims description 10
- 239000012300 argon atmosphere Substances 0.000 claims description 8
- 238000005086 pumping Methods 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 6
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 4
- 238000011068 loading method Methods 0.000 claims description 3
- 229910000838 Al alloy Inorganic materials 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 2
- 239000002131 composite material Substances 0.000 description 33
- 229910052782 aluminium Inorganic materials 0.000 description 26
- 238000009715 pressure infiltration Methods 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 12
- 238000004519 manufacturing process Methods 0.000 description 11
- 238000002360 preparation method Methods 0.000 description 10
- 239000010949 copper Substances 0.000 description 9
- 239000007788 liquid Substances 0.000 description 9
- 229910052802 copper Inorganic materials 0.000 description 8
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 8
- 239000010937 tungsten Substances 0.000 description 8
- 230000008595 infiltration Effects 0.000 description 7
- 238000001764 infiltration Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 239000002002 slurry Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 5
- 230000007613 environmental effect Effects 0.000 description 5
- 239000010936 titanium Substances 0.000 description 5
- 229910052719 titanium Inorganic materials 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 230000017525 heat dissipation Effects 0.000 description 4
- 238000003754 machining Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 3
- 238000004134 energy conservation Methods 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- 238000009768 microwave sintering Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910001374 Invar Inorganic materials 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910000833 kovar Inorganic materials 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- -1 polyethylene Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 238000002490 spark plasma sintering Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000003685 thermal hair damage Effects 0.000 description 1
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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
-
- 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
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- 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
-
- 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
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
-
- 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
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1054—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by microwave
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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Abstract
A method for quickly forming a compact diamond metal matrix composite component by a two-step method relates to a method for forming a diamond metal matrix composite component. The method aims to solve the problem of low density of a diamond/metal matrix composite member containing a metal coating formed rapidly by microwave plasma. The method comprises the following steps: uniformly mixing diamond powder with a metal coating and metal powder through a powder mixing process, performing compression molding to obtain a pressed blank, performing microwave treatment under a protective atmosphere, and performing vacuum and microwave treatment to realize densification.
Description
Technical Field
The invention relates to a method for quickly forming a compact diamond metal matrix composite component by a two-step method.
Background
With the rapid development of the semiconductor industry, components are gradually developed towards the trend of miniaturization, light weight and integration, the heat generated inside the components in unit time is increased, the heat dissipation problem gradually becomes the key for restricting the development of the electronic technology, and in order to avoid the thermal damage of the components, the development of heat dissipation materials with excellent comprehensive performance is urgently needed. The traditional electronic packaging materials, such as Invar alloy, kovar alloy, W-Cu alloy, mo-Cu alloy and the like, have the defects of low heat conductivity and high density; although composite materials such as SiC/Al and Cf/Cu have the advantage of low density, the thermal conductivity (lower than 250W/(m.K)) of the composite materials is difficult to meet the increasing heat dissipation requirement. The diamond has the advantages of excellent heat conductivity, low thermal expansion coefficient, low density and the like, and the reinforced aluminum-based composite material has ultrahigh thermal conductivity and thermal expansion coefficient matched with a semiconductor substrate, can meet the heat dissipation requirement of ultrahigh-power electronic components, and is a hotspot of the current heat management material research.
At present, the main methods for preparing diamond/aluminum-based composite materials in laboratories and industrial production are Spark Plasma Sintering (SPS), gas Pressure Infiltration (GPI), high temperature High Pressure (HPHT), vacuum Hot Pressing (VHP), microwave plasma sintering, and the like. According to the survey, the method comprises the following steps: the multifunctionality of equipment and the capacity of pulse current need to be increased when a large-size product is required to be manufactured by the discharge plasma sintering method, so that the equipment cost can be obviously increased; the gas infiltration method has complex equipment, high price and strict requirements on operation conditions; the high temperature and high pressure method can cause defects and gaps of the material to cause the thermal conductivity to be lower than the theoretical expected value; the vacuum hot pressing method has the advantages of expensive equipment, short service life of the die, various consumable materials and high cost, and in addition, the further improvement of the heat conductivity of the composite material is limited due to the fact that only single-shaft pressurization is available; the material prepared by the microwave plasma sintering method is limited by the problem of density, and the thermal conductivity of the composite material can be further improved. Therefore, developing a process method for preparing the composite material in batches with low cost, high density, large scale and multiple shapes is an important technology for the diamond/metal matrix composite material to mature.
Disclosure of Invention
The invention provides a method for quickly forming a compact diamond metal-based composite material component by a two-step method, aiming at solving the problem of low density of a diamond/metal-based composite material component containing a metal coating formed by quickly forming microwave plasma.
The method for quickly forming the compact diamond metal matrix composite material component by the two-step method comprises the following steps:
1. weighing:
weighing diamond powder and metal powder with a metal coating;
step one, the thickness of the metal coating is 20-300 nm;
step one, the volume of the diamond powder with the metal coating is 40-60% of the total volume of the diamond powder with the metal coating and the metal powder;
2. mixing powder:
uniformly mixing the diamond powder with the metal coating obtained in the step one and metal powder by a powder mixing process to obtain mixed powder;
3. and (3) compression molding:
putting the mixed powder obtained in the step two into a die, transferring the die into a press machine, and applying pressure to perform compression molding to obtain a pressed blank; wherein, the purpose of the compression molding is to reduce the gaps among the powder and increase the contact area;
thirdly, the pressure of the press machine in the compression molding is 0.5-20 MPa;
step three, the mould is a simple-shaped mould or a complex-shaped mould; the cavity of the simple-shaped mold is round, square, flaky, cake-shaped and the like, the cavity of the complex-shaped mold is provided with holes, bosses and the like, and the heights of the bosses are 0.1-1 mm;
4. plasma sintering:
placing the pressing blank obtained in the third step on a tray, loading the tray into a furnace, vacuumizing the furnace, filling protective atmosphere with certain pressure, performing microwave treatment in the protective atmosphere, ionizing low-pressure gas (protective atmosphere gas) by using microwave to form plasma, using the plasma as a heating source, and sintering diamond powder with a metal coating and metal powder together; then cooling to room temperature along with the furnace, and demoulding; the purpose of vacuumizing is to remove oxygen in the furnace and prevent powder from oxidative deterioration;
5. microwave rapid heating densification treatment:
and (4) pumping the sintering furnace in the fourth step to vacuum again, then carrying out microwave treatment under the vacuum condition, wherein the microwave acts on the material under the vacuum condition, alternating electromagnetism enables dipoles inside the material to be repeatedly turned, strong vibration and friction are generated, the material is rapidly heated, the component is further densified, then the material is cooled to room temperature along with the furnace, and demolding is carried out.
The invention has the following beneficial effects:
1. the invention provides a method for quickly preparing a compact diamond metal matrix composite component by using a two-step method of plasma sintering and microwave quick heating, which comprises the steps of firstly forming plasma by using microwave ionization protective gas, taking the plasma as a heating source, enabling the environmental temperature of a blank body in the plasma to be very high instantly, and quickly finishing primary sintering after the blank body is heated to a certain temperature; then the reaction device is vacuumized, and the microwave sintering technology is utilized to further heat the material, so as to achieve the purpose of improving the density; finally, the high-heat-conductivity diamond/metal matrix composite material with uniform components and high density is obtained.
2. When the diamond metal matrix composite is prepared by sintering, pressure is not required to be applied, so that the requirement on microwave plasma sintering equipment is low, and a large number of composite components can be prepared simultaneously;
3. the invention only needs to use the die to press the mixed powder of the diamond and the metal powder into the pressed compact with the target shape at room temperature, has lower requirement on pressed compact equipment, is beneficial to reducing the production cost and improving the production efficiency;
4. the member prepared by the method can meet the requirement of practical use only by performing simple secondary machining such as checking, assembling, deburring and the like, the material prepared by the traditional composite material preparation method can obtain the required member only by performing complex secondary machining such as cutting, polishing and the like, and the embodiment can greatly reduce the production procedures and effectively improve the production efficiency.
5. The invention can prepare the structural component of different shapes, the applicable scope is wide, compared with the traditional preparation technology, the invention can obtain the material of different shapes only by changing the shape of the mould, it is easy to regulate and control;
6. the method has the advantages of simple process, easy operation, no need of using chemical reagents harmful to the environment, energy conservation, environmental protection, low cost and easy realization of industrial production and application.
7. The diamond/metal matrix composite material and the member thereof prepared by the invention have the advantages that the performance meets the use requirement, the material performance is high, the preparation period is short, the price is greatly reduced, the problems of insufficient performance, high preparation cost, long preparation period and the like of the existing diamond/metal matrix composite material are solved, and the market requirement can be better met.
Description of the drawings:
FIG. 1 is an SEM photograph of a tungsten-plated diamond/aluminum composite material prepared 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: in the first embodiment, material weighing:
weighing diamond powder and metal powder with a metal coating;
step one, the thickness of the metal coating is 20-300 nm;
step one, the volume of the diamond powder with the metal coating is 40-60% of the total volume of the diamond powder with the metal coating and the metal powder;
2. mixing powder:
uniformly mixing the diamond powder with the metal coating obtained in the step one and metal powder by a powder mixing process to obtain mixed powder;
3. and (3) pressing and forming:
putting the mixed powder obtained in the step two into a die, transferring the die into a press machine, and applying pressure to perform compression molding to obtain a pressed blank; wherein, the purpose of the compression molding is to reduce the gaps among the powder and increase the contact area;
thirdly, the pressure of the press machine in the compression molding is 0.5-20 MPa;
step three, the mould is a simple-shaped mould or a complex-shaped mould; the cavity of the simple-shaped mold is round, square, flaky, cake-shaped and the like, the cavity of the complex-shaped mold is provided with holes, bosses and the like, and the heights of the bosses are 0.1-1 mm;
4. plasma sintering:
placing the pressing blank obtained in the third step on a tray, loading the tray into a furnace, vacuumizing the furnace, filling protective atmosphere with certain pressure, performing microwave treatment in the protective atmosphere, ionizing low-pressure gas (protective atmosphere gas) by using microwave to form plasma, using the plasma as a heating source, and sintering diamond powder with a metal coating and metal powder together; then cooling to room temperature along with the furnace, and demoulding; the purpose of vacuumizing is to remove oxygen in the furnace and prevent powder from oxidative deterioration;
5. microwave rapid heating densification treatment:
and (4) pumping the sintering furnace in the fourth step to vacuum again, then carrying out microwave treatment under the vacuum condition, wherein the microwave acts on the material under the vacuum condition, alternating electromagnetism enables dipoles inside the material to be repeatedly turned, strong vibration and friction are generated, the material is rapidly heated, the component is further densified, then the material is cooled to room temperature along with the furnace, and demolding is carried out.
The embodiment has the following beneficial effects:
1. the method of the embodiment provides a method for quickly forming a compact diamond metal matrix composite component by a two-step method, and the method comprises the steps of firstly ionizing gas by using a microwave plasma technology to form microwave plasma, taking the plasma as a heating source, enabling the environmental temperature of a blank body in the plasma to reach a very high temperature instantly, and quickly finishing primary sintering after the blank body is heated to a certain temperature; then the reaction device is vacuumized, and the microwave sintering technology is utilized to further heat the material, so as to achieve the purpose of improving the density; finally, the high-heat-conductivity diamond metal-based composite material with uniform components and high density is obtained.
2. In the embodiment, when the diamond metal matrix composite is prepared by sintering, pressure is not required to be applied, so that the requirement on microwave plasma sintering equipment is low, and a large number of composite components can be prepared simultaneously;
3. according to the embodiment, the mixed powder of the diamond and the metal powder is pressed into the pressed blank with the target shape only by using the die at room temperature, so that the requirement on pressed blank equipment is low, the production cost is reduced, and the production efficiency is improved;
4. the component prepared by the embodiment can meet the requirement of practical use only by carrying out simple secondary machining such as checking, assembling and deburring, the material prepared by the existing composite material preparation method can obtain the required component only by carrying out complex secondary machining such as cutting and polishing, and the embodiment can greatly reduce production procedures and effectively improve production efficiency.
5. The embodiment can be used for preparing components in different shapes, has a wide application range, and can obtain materials in different shapes only by changing the shape of the die, so that the embodiment is easy to regulate and control;
6. the method has the advantages of simple process, easy operation, no need of using chemical reagents harmful to the environment, energy conservation, environmental protection, low cost and easy realization of industrial production and application.
7. The diamond/metal matrix composite material and the member thereof prepared by the embodiment have the advantages that the performance meets the use requirement, the preparation period is short, the price is greatly reduced, the problems of high preparation cost, long preparation period and the like of the existing diamond/metal matrix composite material are solved, and the market requirement can be better met.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: step one, the metal powder is pure aluminum powder, aluminum alloy powder, pure copper powder or copper alloy powder.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: step one, the metal coating is one of W, ti, cr and Mo, and the thickness of the metal coating is 20-300 nm.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: the diamond powder has a particle size of 50-200 μm, and the metal powder has a particle size of 5-20 μm.
The fifth concrete implementation mode is as follows: the difference between this embodiment and one of the first to fourth embodiments is: and fourthly, the tray is made of wave-transmitting materials such as alumina, polyethylene and the like.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: step four, vacuumizing until the vacuum degree is 0-10-3Pa；
The seventh concrete implementation mode: the difference between this embodiment and one of the first to sixth embodiments is: the protective atmosphere in the step four is nitrogen atmosphere, argon atmosphere or helium atmosphere; the pressure of the protective atmosphere is 1-100 Pa.
The specific implementation mode eight: the present embodiment differs from one of the first to seventh embodiments in that: and fourthly, during microwave treatment, the microwave frequency is 2450MHz, the microwave power is 6-24 KW, and the microwave treatment time is 1-10 min.
The specific implementation method nine: the present embodiment differs from the first to eighth embodiments in that: step five, vacuumizing until the vacuum degree is 0-10-3Pa。
The detailed implementation mode is ten: the present embodiment differs from one of the first to ninth embodiments in that: and fifthly, the microwave frequency during microwave treatment is 2450MHz, the microwave treatment power is 6-24 KW, and the microwave treatment time is 5-15 min.
The following examples were used to demonstrate the beneficial effects of the present invention:
example 1:
the method for rapidly forming the compact diamond metal matrix composite component by the two-step method comprises the following steps:
1. weighing:
weighing diamond powder with a tungsten coating and pure aluminum powder;
step one, the thickness of the tungsten coating is 100nm;
firstly, the grain diameter of the diamond powder is 200 mu m;
step one, the grain diameter of the pure aluminum powder is 5 mu m;
step one, the volume of the diamond powder with the metal coating is 40 percent of the total volume of the diamond powder with the metal coating and the metal powder;
2. mixing powder:
uniformly mixing the diamond powder and the copper powder obtained in the step one in a slurry powder mixing mode, and then drying the mixture to obtain mixed powder, wherein the slurry is water;
3. and (3) pressing and forming:
filling the mixed powder obtained in the step two into a mold with the length of 30mm, the width of 30mm and the height of 30mm, putting the mold into a press machine, and applying the pressure of 5MPa to perform compression molding to obtain a pressed blank;
4. plasma sintering:
putting the pressing blank formed by pressing in the step three on an alumina tray, putting the pressing blank in a furnace, firstly vacuumizing, then filling protective atmosphere with certain pressure, carrying out continuous microwave treatment in the protective atmosphere, forming plasma by utilizing microwave ionization low-pressure gas, taking the plasma as a heating source, and sintering diamond powder with a metal coating and metal powder together; then cooling to room temperature along with the furnace, and demoulding;
the vacuum pumping is carried out until the vacuum degree is 10-3Pa。
The protective atmosphere is argon atmosphere; the pressure of the argon atmosphere is 100Pa;
the microwave frequency is 2450MHz, the microwave power is 12KW and the microwave treatment time is 2min;
5. microwave rapid heating densification treatment:
pumping the sintering furnace in the fourth step to vacuum again, then carrying out microwave treatment under the vacuum condition, wherein the microwave acts on the material under the vacuum condition, alternating electromagnetism enables dipoles inside the material to be repeatedly turned to generate strong vibration and friction, so that the material is rapidly heated to further densify the component, then cooling to room temperature along with the furnace, and demolding;
step five, vacuumizing to the vacuum degree of 10-3Pa；
And fifthly, the microwave frequency during microwave treatment is 2450MHz, the microwave treatment power is 24KW, and the microwave treatment time is 5min.
The tungsten-plated diamond/aluminum composite material member of 30mm x 30mm, which took 32 minutes for the treatment method according to example 1 (evacuation and protective gas filling time was 20 minutes, plasma sintering was 2 minutes, evacuation time was 5 minutes again, microwave rapid heating was 5 minutes), was tested to have a density of 96% and a thermal conductivity of 575W/(m · K). The preparation method has the advantages of one-step forming, simple process, high energy utilization rate, energy conservation, environmental protection and lower cost. FIG. 1 is an SEM photograph of a tungsten-plated diamond/aluminum composite material prepared in example 1. FIG. 1 is an SEM photograph of a tungsten-plated diamond/aluminum composite material prepared in example 1. Figure 1 shows that the composite material has good sintering and high density.
Comparative example 1: according to the same components and process, material weighing, powder mixing, press forming and plasma sintering are carried out, namely, the plasma sintering in the fourth step is carried out only once without the microwave rapid heating densification treatment in the fifth subsequent step, the time is taken for 22 minutes (the time for vacuumizing and inflating is 20 minutes, and the plasma sintering time is 2 minutes), a 30mm x 30mm tungsten-plated diamond/aluminum composite material component can be obtained through sintering, and the compactness of the component is only 87%, and the thermal conductivity is 510W/(m.K) through testing. Compared with the one-step plasma sintering forming process of the comparative example 1, the density of the material can be improved by 9%, the thermal conductivity is improved by 12%, only 10min of microwave rapid heating densification treatment is added, but the performance is obviously improved, and the application range is wider.
Comparative example 2: the diamond/pure aluminum composite material is prepared by adopting 200-micron diamond powder with a 100-nm tungsten coating and pure aluminum as raw materials through pressure infiltration, wherein diamond with a tungsten carbide coating is placed in a mold during pressure infiltration, liquid pure aluminum at 850 ℃ is poured into the mold, 5MPa pressure is applied through a press machine to enable the liquid pure aluminum to be slowly infiltrated into gaps of diamond particles, the pressure is kept for 15min after infiltration, then, the furnace is cooled to the room temperature, and demolding is carried out, so that the diamond/aluminum composite material with the diamond volume fraction of 40% is obtained. Calculating that the process of aluminum melting, liquid infiltration and final cooling to room temperature takes 18 hours; the test shows that the thermal conductivity of the diamond/aluminum composite material is 582W/(m.K); compared with the traditional pressure infiltration process of the comparative example 2, the heat conductivity of the embodiment 1 is only reduced by 1%, the sintering process of the embodiment 1 only takes 32 minutes, the sintering process is greatly shortened by 18 hours compared with the pressure infiltration process, and the production efficiency is greatly improved.
Example 2:
the method for quickly forming the compact diamond metal matrix composite component by the two-step method comprises the following steps:
1. weighing:
weighing diamond powder and pure aluminum powder with a tungsten coating;
step one, the thickness of the tungsten coating is 50nm;
step one, the grain diameter of the diamond powder is 100 mu m;
step one, the grain diameter of the pure aluminum powder is 15 mu m
Step one, the volume of the diamond powder with the tungsten coating is 60 percent of the total volume of the diamond powder with the tungsten coating and pure aluminum powder;
2. mixing powder:
uniformly mixing the diamond powder and the copper powder obtained in the step one by a slurry powder mixing mode, and then drying, wherein the slurry is water, so as to obtain mixed powder;
3. and (3) pressing and forming:
filling the mixed powder obtained in the second step into a die with the diameter of 50mm multiplied by 5mm, putting the die into a press machine, and applying the pressure of 10MPa to carry out compression molding to obtain a pressed blank;
4. plasma sintering:
putting the pressing blank formed by pressing in the step three on an alumina tray, putting the pressing blank in a furnace, vacuumizing, filling protective atmosphere with certain pressure, performing continuous pulse microwave treatment in the protective atmosphere, ionizing low-pressure gas by using microwave to form plasma, taking the plasma as a heating source, and sintering diamond powder with a metal coating and metal powder together; then cooling to room temperature along with the furnace, and demoulding;
the vacuum degree is 0.5 multiplied by 10-3Pa；
The protective atmosphere is argon atmosphere; the pressure of the argon atmosphere is 50Pa;
the microwave frequency during the microwave treatment is 2450MHz, the microwave treatment power is 6KW, and the microwave treatment time is 4min;
5. microwave rapid heating densification treatment:
pumping the sintering furnace in the fourth step to vacuum again, then carrying out microwave treatment under the vacuum condition, wherein the microwave acts on the material under the vacuum condition, alternating electromagnetism enables dipoles inside the material to be repeatedly turned to generate strong vibration and friction, so that the material is rapidly heated to further densify the component, then cooling to room temperature along with the furnace, and demolding;
step five, vacuumizing until the vacuum degree is 0.5 multiplied by 10-3Pa；
And fifthly, the microwave frequency during microwave treatment is 2450MHz, the microwave treatment power is 6KW, and the microwave treatment time is 15min.
The treatment method according to example 2 took 44 minutes (evacuation and protective gas charging time was 20 minutes, plasma sintering was 4 minutes, evacuation time was 5 minutes again, microwave rapid heating was 15 minutes) and a tungsten-plated diamond/aluminum composite member of 50mm × 50mm × 5mm, which had been tested to achieve 97% compactness and 622W/(m · K) thermal conductivity, was obtained by sintering.
Comparative example 3: according to the same components and process, the materials are weighed, the powder is mixed, the pressing forming and the plasma sintering are carried out, namely the plasma sintering in the fourth step is carried out only once without the microwave rapid heating densification treatment in the fifth step, the tungsten-plated diamond/aluminum composite material member with the thickness of 50mm multiplied by 5mm can be obtained by sintering after 24 minutes (the vacuumizing and gas filling time is 20 minutes, and the plasma sintering time is 4 minutes), and the member has the compactness of only 91 percent and the thermal conductivity of 580W/(m.K) through tests. Compared with the one-step plasma sintering forming process of the comparative example 3, the density of the material can be improved by 6%, the thermal conductivity is improved by 7%, only 20min microwave rapid heating densification treatment is added, but the performance is obviously improved, and the application range is wider.
Comparative example 4: the diamond/pure aluminum composite material is prepared by adopting 100-micron diamond powder with a 50nm tungsten coating and pure aluminum as raw materials through pressure infiltration, wherein diamond with a tungsten carbide coating is placed in a mold during pressure infiltration, liquid pure aluminum at 850 ℃ is poured into the mold, 15MPa pressure is applied through a press machine to enable the liquid pure aluminum to be slowly infiltrated into gaps of diamond particles, the pressure is kept for 15min after infiltration, then, the furnace is cooled to the room temperature, and demolding is carried out, so that the diamond/aluminum composite material with the diamond volume fraction of 60% is obtained. Calculating that the process of aluminum melting, liquid aluminum infiltration and final cooling to room temperature takes 18 hours; the test shows that the thermal conductivity of the diamond/aluminum composite material is 625W/(m.K);
compared with the traditional pressure infiltration process of the comparative example 4, the thermal conductivity of the embodiment 2 is only 0.5 percent lower, the sintering process of the embodiment 2 only takes 44 minutes, the time is greatly shortened compared with 18 hours of the pressure infiltration process, and the production efficiency is greatly improved.
Example 3:
the method for quickly forming the compact diamond metal matrix composite component by the two-step method comprises the following steps:
1. weighing:
weighing diamond powder and pure copper powder with a titanium coating;
step one, the thickness of the titanium coating is 200nm;
step one, the grain diameter of the diamond powder is 100 mu m;
step one, the grain diameter of the pure copper powder is 5 mu m
Step one, the volume of the diamond powder with the titanium coating is 50 percent of the total volume of the diamond powder with the titanium coating and the pure copper powder;
2. mixing powder:
uniformly mixing the diamond powder and the copper powder obtained in the step one in a slurry powder mixing mode, and then drying the mixture to obtain mixed powder, wherein the slurry is water;
3. and (3) compression molding:
putting the mixed powder obtained in the step two into a die with a boss with the height of 1mm and the diameter of 50mm multiplied by 10mm, putting the die into a press machine, and applying the pressure of 20MPa to perform compression molding to obtain a pressing blank;
4. plasma sintering:
putting the pressing blank formed by pressing in the step three on an alumina tray, putting the pressing blank in a furnace, firstly vacuumizing, then filling protective atmosphere with certain pressure, carrying out continuous microwave treatment in the protective atmosphere, forming plasma by utilizing microwave ionization low-pressure gas, taking the plasma as a heating source, and sintering diamond powder with a metal coating and metal powder together; then cooling to room temperature along with the furnace, and demoulding;
the vacuum degree of the vacuum is 10-4Pa；
The protective atmosphere is argon atmosphere; the pressure of the argon atmosphere is 10Pa;
the microwave frequency during microwave treatment is 2450MHz, the microwave treatment power is 24KW, and the treatment time is 10min;
5. microwave rapid heating densification treatment:
pumping the sintering furnace in the fourth step to vacuum again, then carrying out microwave treatment under the vacuum condition, wherein the microwaves act on the material under the vacuum condition, alternating electromagnetism enables dipoles inside the material to be repeatedly turned, strong vibration and friction are generated, the material is rapidly heated, the component is further densified, then the component is cooled to room temperature along with the furnace, and demoulding is carried out;
fifthly, vacuumizing to the vacuum degree of 10-4Pa；
And fifthly, the microwave frequency during microwave treatment is 2450MHz, the microwave treatment power is 24KW, and the microwave treatment time is 10min.
The tungsten-plated diamond/copper composite material member 50mm x 10mm with a boss 1mm high can be sintered by the treatment method of example 3, which takes 50 minutes (evacuation and protective gas filling time is 25 minutes, plasma sintering time is 10 minutes, evacuation time is 5 minutes again, microwave rapid heating time is 10 minutes), and the member has a density of 97% and a thermal conductivity of 738W/(m.K) as tested.
Comparative example 5: weighing materials, mixing powder, pressing and sintering by plasma according to the same components and process, namely only performing plasma sintering in the fourth step once without performing microwave rapid heating densification treatment in the fifth step, wherein the tungsten-plated diamond/copper composite material member with a boss with the height of 1mm can be obtained by sintering after the time is 35 minutes (the time for vacuumizing and filling protective gas is 25 minutes, and the plasma sintering time is 10 minutes), the density of the member is only 92 percent through tests, and the thermal conductivity is 700W/(m.K). Compared with the one-step plasma sintering forming process of the comparative example 5, the density of the material can be improved by 5%, the thermal conductivity is improved by 5%, only 15min microwave rapid heating densification treatment is added, but the performance is obviously improved, and the application range is wider.
Comparative example 6: the diamond/pure aluminum composite material is prepared by adopting 100-micron diamond powder with a 200nm titanium coating and pure copper as raw materials through pressure infiltration, wherein diamond with a tungsten carbide coating is placed in a mold during pressure infiltration, liquid pure copper at 1350 ℃ is poured into the mold, 25MPa pressure is applied through a press machine to enable the liquid copper to be slowly infiltrated into gaps of diamond particles, the pressure is maintained for 20min after infiltration, then furnace cooling is carried out to room temperature, and demolding is carried out to obtain the diamond/copper composite material with the diamond volume fraction of 50%. Calculating that the processes of copper melting, liquid infiltration and final cooling to room temperature take 25 hours; the test shows that the thermal conductivity of the diamond/copper composite material is 742W/(m.K); compared with the traditional pressure infiltration process of the comparative example 6, the heat conductivity of the embodiment 3 is only 0.5 percent lower, the sintering process of the embodiment 3 only takes 50 minutes, the time is greatly shortened compared with 25 hours of the pressure infiltration process, and the production efficiency is greatly improved.
Claims (10)
1. A method for rapidly forming a compact diamond metal matrix composite component by a two-step method is characterized by comprising the following steps of: the method for quickly forming the compact diamond metal matrix composite component by the two-step method comprises the following steps:
1. weighing:
weighing diamond powder and metal powder with a metal coating;
step one, the thickness of the metal coating is 20-300 nm;
step one, the volume of the diamond powder with the metal coating is 40-60% of the total volume of the diamond powder with the metal coating and the metal powder;
2. mixing powder:
uniformly mixing the diamond powder with the metal coating obtained in the step one and metal powder through a powder mixing process to obtain mixed powder;
3. and (3) pressing and forming:
putting the mixed powder obtained in the step two into a die, transferring the die into a press machine, and applying pressure to perform compression molding to obtain a pressed blank;
thirdly, the pressure of the press machine in the compression molding is 0.5-20 MPa;
step three, the mould is a simple-shaped mould or a complex-shaped mould; the cavity of the simple-shaped mold is round, square, flaky or cake-shaped, the cavity of the complex-shaped mold is provided with a hole or a boss, and the height of the boss is 0.1-1 mm;
4. plasma sintering:
placing the pressing blank obtained in the third step on a tray, loading the tray into a furnace, vacuumizing the furnace, filling protective atmosphere with certain pressure, performing microwave treatment in the protective atmosphere, ionizing low-pressure gas by using microwave to form plasma, using the plasma as a heating source, and sintering diamond powder with a metal coating and metal powder together; then cooling to room temperature along with the furnace, and demoulding;
5. microwave rapid heating densification treatment:
and (4) pumping the sintering furnace in the fourth step to vacuum again, then carrying out microwave treatment under the vacuum condition, wherein the microwave acts on the material under the vacuum condition, alternating electromagnetism enables dipoles inside the material to be repeatedly turned, strong vibration and friction are generated, the material is rapidly heated, the component is further densified, then the material is cooled to room temperature along with the furnace, and demolding is carried out.
2. The two-step process for rapid prototyping a densified diamond metal matrix composite component as set forth in claim 1 wherein: step one, the metal powder is pure aluminum powder, aluminum alloy powder, pure copper powder or copper alloy powder.
3. The two-step process rapid prototyping densified diamond metal matrix composite component of claim 1 wherein: step one, the metal coating is one of W, ti, cr and Mo.
4. The two-step process for rapid prototyping a densified diamond metal matrix composite component as set forth in claim 1 wherein: firstly, the grain diameter of the diamond powder is 50-200 mu m; in the first step, the particle size of the metal powder is 5-20 μm.
5. The two-step process for rapid prototyping a densified diamond metal matrix composite component as set forth in claim 1 wherein: and fourthly, the tray is made of a wave-transmitting material.
6. The two-step process for rapid prototyping a densified diamond metal matrix composite component as set forth in claim 1 wherein: step four, vacuumizing until the vacuum degree is 0-10-3Pa。
7. The two-step process for rapid prototyping a densified diamond metal matrix composite component as set forth in claim 1 wherein: the protective atmosphere in the step four is nitrogen atmosphere, argon atmosphere or helium atmosphere; the pressure of the protective atmosphere is 1-100 Pa.
8. The two-step process for rapid prototyping a densified diamond metal matrix composite component as set forth in claim 1 wherein: and step four, during microwave treatment, the microwave frequency is 2450MHz, the microwave power is 6-24 KW, and the microwave treatment time is 1-10 min.
9. The two-step process for rapid prototyping a densified diamond metal matrix composite component as set forth in claim 1 wherein: step five, vacuumizing to vacuumThe degree is 0 to 10-3Pa。
10. The two-step process for rapid prototyping a densified diamond metal matrix composite component as set forth in claim 1 wherein: and fifthly, the microwave frequency during microwave treatment is 2450MHz, the microwave treatment power is 6-24 KW, and the microwave treatment time is 5-15 min.
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| US6011248A (en) * | 1996-07-26 | 2000-01-04 | Dennis; Mahlon Denton | Method and apparatus for fabrication and sintering composite inserts |
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| CN111590080A (en) * | 2020-05-21 | 2020-08-28 | 南京航空航天大学 | Method for rapidly preparing titanium-plated diamond copper composite material by SPS |
| CN112974797A (en) * | 2021-02-07 | 2021-06-18 | 哈尔滨工业大学 | Method for preparing high-bonding-strength carbide coating on diamond surface by utilizing microwaves |
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| US6011248A (en) * | 1996-07-26 | 2000-01-04 | Dennis; Mahlon Denton | Method and apparatus for fabrication and sintering composite inserts |
| WO2010034492A1 (en) * | 2008-09-26 | 2010-04-01 | Wendt Gmbh | Microwave plasma sintering |
| CN105112707A (en) * | 2015-08-28 | 2015-12-02 | 昆明理工大学 | Preparation method of diamond/aluminum composite material |
| CN110202131A (en) * | 2019-07-12 | 2019-09-06 | 河南工业大学 | A kind of preparation method of diamond composition |
| CN111590080A (en) * | 2020-05-21 | 2020-08-28 | 南京航空航天大学 | Method for rapidly preparing titanium-plated diamond copper composite material by SPS |
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