CN115446307A - Preparation method of graphene-copper composite material - Google Patents

Preparation method of graphene-copper composite material Download PDF

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CN115446307A
CN115446307A CN202211156704.9A CN202211156704A CN115446307A CN 115446307 A CN115446307 A CN 115446307A CN 202211156704 A CN202211156704 A CN 202211156704A CN 115446307 A CN115446307 A CN 115446307A
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powder
graphene
mixed powder
copper
composite material
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CN115446307B (en
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张双宁
周俊
姚欢
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Changsha Saneway Electronic Materials Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/18Non-metallic particles coated with metal
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/12Metallic powder containing non-metallic particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02Compacting only
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24After-treatment of workpieces or articles
    • B22F3/26Impregnating
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

The invention provides a preparation method of a graphene-copper composite material, and belongs to the technical field of composite materials. According to the invention, a layer of metal with good wettability with copper is plated on the surface of graphene, then the plated graphene is pressed into a blank, and the copper is infiltrated into the material in an infiltration manner to form the composite material, so that the production efficiency of the material can be greatly improved, the raw material cost and the production cost are reduced, and the composite material with excellent heat conductivity is obtained.

Description

Preparation method of graphene-copper composite material
Technical Field
The invention relates to the field of composite materials, in particular to a preparation method of a graphene-copper composite material.
Background
Graphene is a carbon material with a special structure, and has excellent mechanical, thermal, electrical and other properties. However, due to the particularity of the graphene material, the graphene material cannot be used alone, and the graphene and other materials are usually made into a composite material to obtain better performance, wherein the graphene and copper composite material to obtain a high thermal and electrical conductivity material is an important application of the graphene material.
The common graphene/copper composite material usually needs graphene with a small number of layers to fully exert the performance advantages, and the graphene with a small number of layers is usually very expensive. In the prior art, the graphene-copper composite material is prepared by using an in-situ synthesis method, an electrostatic self-assembly method and the like, and the development of the graphene-copper material is greatly restricted by the problems of high cost, complex preparation method and low preparation efficiency.
The CN108160983B graphene copper-based composite material and the preparation method thereof adopt single-layer graphene oxide, and the cost of the single-layer graphene is high.
Disclosure of Invention
The invention provides a preparation method of a graphene-copper composite material, and aims to solve the problems in the background art.
In order to achieve the purpose, the surface of the graphene is coated with a layer of metal with good wettability with copper, the coated graphene is pressed into a blank, and the copper is infiltrated into the material in an infiltration mode to form the composite material, so that the production efficiency of the material can be greatly improved, the raw material cost and the production cost are reduced, and the material with excellent heat conductivity is obtained.
The embodiment of the invention provides a preparation method of a graphene-copper composite material, which comprises the following specific steps:
s1, filling metal powder into a graphite container, uniformly spreading, heating in an air atmosphere and preserving heat to obtain first mixed powder; the metal powder is tungsten powder or molybdenum powder;
s2, uniformly mixing the flaky graphene and the first mixed powder in proportion to obtain second mixed powder;
s3, filling the second mixed powder into a molybdenum container, and placing the molybdenum container in a vacuum furnace for plating to obtain third mixed powder;
s4, sieving the third mixed powder by using a vibrating sieving machine, and collecting powder which does not pass through a sieve;
s5, placing the powder which does not pass through the screen mesh into a coulter mixer, adding a forming agent, and stirring to obtain fourth mixed powder;
s6, filling the fourth mixed powder into a die for die pressing or isostatic pressing to obtain a blank;
s7, placing the blank into a molybdenum container, and placing the molybdenum container in a tubular furnace filled with hydrogen for heat treatment;
s8, flatly paving the heat-treated pressed blank on a graphite container, paving a copper sheet on the graphite container, and putting the pressed blank and the copper sheet into a vacuum furnace for sintering and infiltration to obtain the graphene/copper composite material.
Preferably, the particle size of the metal powder is less than 5 μm, and the mass ratio of the metal to the metal oxide is 1; the mass ratio of the flaky graphene to the metal oxide is (1-1); the addition of the copper sheet is 1.0-1.2 times of the filling gap amount.
Preferably, the first mixed powder in step S1 is W or WO 3 Mixture of (3) or Mo, moO 3 A mixture of (a). For example, the W powder is loaded into a boat and pushed into a tube furnace, and the W and WO powders are prepared by introducing air and keeping the temperature at 500 ℃ for 10min 3 And mixing the powders.
Preferably, the number of the scaly graphene sheets in step S2 is 5 to 30, more preferably 10, and the particle diameter is 5 μm or more.
Preferably, the mixing device in step S2 is a planetary mixer, a V-shaped mixer or a colter mixer.
Preferably, the plating conditions in step S3 are within 1Pa of vacuum degree, and may be 0.5Pa, 0.1Pa, 0.01Pa, temperature 800-1200 deg.C, and heat preservation for 1-4 h.
Preferably, the screen of the powder screening machine in the step S4 is a screen of 2300 meshes, and the powder screening time is 10-30 min. The separation method may be a centrifugal separation method, in addition to the sieving separation method.
Preferably, the forming agent in step S5 is paraffin, stearic acid or PEG2000, and the adding amount of the forming agent is 1/15-1/30 of the mass of the powder which does not pass through the screen.
Preferably, the pressure in step S6 is controlled to be 50 to 90% of porosity of the green powder. The pressed compact volume is 50-90% of the calculated volume of the theoretical density of the powder which does not pass through the screen.
Preferably, the heat treatment temperature in step S7 is 600 to 900 ℃, more preferably 800 ℃, and the temperature is kept for 6 to 12 hours, more preferably 8 hours. The heat treatment atmosphere is hydrogen, nitrogen, argon or carbon monoxide.
Preferably, the infiltration condition in step S8 is a vacuum atmosphere with a vacuum degree of 1Pa or less, the temperature is 1150 to 1300 ℃, more preferably 1250 ℃, and the infiltration time is 12 to 24 hours, more preferably 24 hours.
The scheme of the invention has the following beneficial effects:
according to the invention, a layer of metal with good wettability with copper is plated on the surface of graphene, then the plated graphene is pressed into a blank, and copper is infiltrated into the material in an infiltration manner to form the composite material.
The cost of the multilayer graphene is far lower than that of single-layer graphene, and the preparation method is simple, high in preparation efficiency, high in material density and good in heat conductivity, and is suitable for mass production.
Selecting WO 3 Firstly, W and Mo are easy to form a coating with graphene, secondly, the coating has better wettability to copper, and the copper can better infiltrate into a blank of graphene tungsten-plated material, so that the material density is higher. Graphene has excellent thermal conductivity, and copper is the best thermal conductivity of metals. The forming agent is selected from paraffin, PEG, stearic acid and the like, has good forming property, is easy to remove in the subsequent process, and does not influence the heat conductivity of the material.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
Fig. 1 is an SEM image of the flaky graphene in the first embodiment of the present invention;
fig. 2 is an SEM image of tungsten-plated graphene according to a first embodiment of the present invention;
fig. 3 is a cross-sectional SEM image of the graphene/copper composite material according to the first embodiment of the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantages of the present invention more apparent, the following detailed description is given with reference to the accompanying drawings and specific embodiments.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
The invention provides a preparation method of a graphene-copper composite material, aiming at the existing problems.
The embodiment of the invention provides a preparation method of a graphene-copper composite material, which comprises the following specific steps:
s1, filling metal powder into a graphite container, uniformly spreading, heating in an air atmosphere and preserving heat to obtain first mixed powder; the metal powder is tungsten powder or molybdenum powder;
s2, uniformly mixing the flaky graphene and the first mixed powder in proportion to obtain second mixed powder;
s3, filling the second mixed powder into a molybdenum container, and placing the molybdenum container in a vacuum furnace for plating to obtain third mixed powder;
s4, sieving the third mixed powder by using a vibrating sieving machine, and collecting powder which does not pass through a sieve;
s5, placing the powder which does not pass through the screen mesh into a coulter mixer, adding a forming agent, and stirring to obtain fourth mixed powder;
s6, filling the fourth mixed powder into a die for die pressing or isostatic pressing to obtain a blank;
s7, placing the blank into a molybdenum container, placing the molybdenum container into a tubular furnace filled with hydrogen, and carrying out heat treatment;
s8, flatly paving the heat-treated pressed blank on a graphite container, paving a copper sheet on the graphite container, and putting the pressed blank and the copper sheet into a vacuum furnace for sintering and infiltration to obtain the graphene/copper composite material.
Preferably, the particle size of the metal powder is less than 5 μm, and the mass ratio of the metal to the metal oxide is 1; the mass ratio of the flaky graphene to the metal oxide is 1-1; the addition amount of the copper sheet is 1.0-1.2 times of the filling gap amount.
Preferably, the first mixed powder in step S1 is W or WO 3 Mixture of (5) or Mo, moO 3 A mixture of (a). For example, the W powder is loaded into a boat and pushed into a tube furnace, and the W and WO powders are prepared by introducing air and keeping the temperature at 500 ℃ for 10min 3 And mixing the powders.
Preferably, in step S2, the number of the scaly graphene sheets is 5 to 30, more preferably 10, and the particle diameter is 5 μm or more.
Preferably, the mixing device in step S2 is a planetary mixer, a V-shaped mixer or a colter mixer.
Preferably, the plating conditions in step S3 are within 1Pa of vacuum degree, and may be 0.5Pa, 0.1Pa, 0.01Pa, temperature 800-1200 deg.C, and heat preservation for 1-4 h.
Preferably, the screen of the powder screening machine in the step S4 is a screen of 2300 meshes, and the powder screening time is 10-30 min. The separation method may be a centrifugal separation method, in addition to the sieving separation method.
Preferably, the forming agent in step S5 is paraffin, stearic acid or PEG2000, and the adding amount of the forming agent is 1/15-1/30 of the mass of the powder which does not pass through the screen.
Preferably, the pressure in step S6 is controlled to be 50 to 90% of the porosity of the powder compact. The pressed compact volume is 50-90% of the calculated volume of the theoretical density of the powder which does not pass through the screen.
Preferably, the heat treatment temperature in step S7 is 600 to 900 ℃, more preferably 800 ℃, and the temperature is kept for 6 to 12 hours, more preferably 8 hours. The heat treatment atmosphere is hydrogen, nitrogen, argon or carbon monoxide.
Preferably, the infiltration condition in step S8 is a vacuum atmosphere with a vacuum degree of 1Pa or less, the temperature is 1150 to 1300 ℃, more preferably 1250 ℃, and the infiltration time is 12 to 24 hours, more preferably 24 hours.
Example one
Preparing a 75 x 55 x 1.0mm tungsten-plated graphene/copper composite material, which comprises the following specific steps:
s1, filling 10kg of pure tungsten powder with D50 of 1 mu m into a graphite container, and uniformly spreading, wherein the powder filling thickness is 2cm. Heating to 500 ℃ in an air atmosphere and keeping the temperature for 10 minutes to obtain W and WO 3 Wherein the upper layer is yellow WO 3 The lower layer is grey W.
And S2, mixing the mixed powder with 2.5kg of flaky graphene (shown in figure 1) with 8-15 layers of sheet layers and 6 mu m of sheet diameter for 2h by using a V-shaped powder mixer to obtain uniform mixed powder.
And S3, putting the powder into a molybdenum container, and placing the molybdenum container in a vacuum furnace for plating, wherein the plating temperature is 1000 ℃, and the plating time is 4 hours.
And S4, sieving the coated powder by using a vibrating powder sieving machine, wherein the powder sieving machine adopts a 2300-mesh sieve, and the powder sieving time is 15min. The powder which can not pass through the screen is the tungsten-plated graphene powder (as shown in figure 2).
S5, adding the tungsten-plated graphene powder into a coulter mixer, adding 500mL of stearic acid, and stirring for 2h.
And S6, filling 50g of powder into a mold of 80 × 60mm, and adjusting the pressure until the thickness of the green compact is 1.8mm, namely the tungsten-plated graphene green compact contains about 30% of gaps for filling copper.
S7, placing the pressed green compact into a molybdenum container, placing the molybdenum container into a tube furnace filled with hydrogen, and carrying out heat treatment at 800 ℃ for 8 hours to remove a forming agent.
S8, flatly placing the blank after heat treatment on a graphite container, then placing a copper sheet with the weight of 27g on a pressed blank, then placing the pressed blank into a vacuum furnace, and sintering the pressed blank for 24 hours at 1250 ℃ under the air pressure of 0.1Pa to obtain a primary graphene-copper composite material.
And S9, subsequently processing the material to 75-55-1.0 mm tungsten-plated graphene/copper composite material by a grinding method, wherein the image structure is shown in figure 3, the density is better, and copper is better filled in the material. The density of the obtained material is 6.96g/cm 3 The thermal conductivity reaches 330W/mK.
Example two
Preparing a 70 x 40 x 5mm tungsten-plated graphene/copper composite material, which comprises the following specific steps:
s1, 5kg of pure tungsten powder with D50 of 1 mu m is filled into a graphite container and evenly spread, and the powder filling thickness is 1cm. Heating to 500 deg.C in air atmosphere, and maintaining for 10min to obtain container with surface layer powder oxidized into WO 3 W and WO 3 And (4) mixing the powder.
And S2, mixing the mixed powder with 2.5kg of flaky graphene (shown in figure 1) with the number of layers being 8-15 and the sheet diameter being about 6 microns for 2 hours by using a V-shaped powder mixer to obtain uniform mixed powder.
S3, putting the powder into a molybdenum container, and placing the molybdenum container in a vacuum furnace for plating, wherein the plating temperature is 1000 ℃, and the plating time is 2 hours.
And S4, sieving the coated powder by using a vibrating powder sieving machine, wherein the powder sieving machine adopts a 2300-mesh sieve, and the powder sieving time is 15min. The powder which can not pass through the screen is the tungsten-plated graphene powder (as shown in figure 2).
S5, adding the tungsten-plated graphene powder into a coulter mixer, adding 500mL of paraffin solution, and stirring for 1h.
And S6, filling 94.0g of powder into a mold with the thickness of 75 × 45mm, and adjusting the pressure until the thickness of the green compact is 6mm, namely, the tungsten-plated graphene green compact contains about 15% of gaps for filling copper.
S7, placing the pressed compact into a graphite container, placing the container into a tube furnace filled with hydrogen, and carrying out heat treatment at 800 ℃ for 8h to remove the forming agent.
S8, horizontally placing the blank after heat treatment on a graphite container, then placing a copper sheet with the weight of 27.5g on a pressed blank, then placing the pressed blank into a vacuum furnace, and sintering the pressed blank at 1250 ℃ for 24 hours under the air pressure of 0.1Pa to obtain a primary graphene-copper composite material.
And S9, subsequently processing the material to 70 x 40 x 5mm tungsten-plated graphene/copper composite material by grinding and other methods. The density of the obtained material is 5.66g/cm 3 The thermal conductivity reaches 310W/mK.
EXAMPLE III
Preparing an 80 x 10mm molybdenum-plated graphene/copper composite material, which comprises the following specific steps:
s1, filling 10kg of pure molybdenum powder with the D50 of 1 mu m into a graphite container, and uniformly spreading, wherein the powder filling thickness is 4cm. Heating to 500 ℃ in air atmosphere, and preserving heat for 30 minutes to obtain mixed powder of Mo and MoO3, wherein the surface layer powder in the container is oxidized into white MoO 3.
And S2, mixing the mixed powder with 2.5kg of flaky graphene (shown in figure 1) with 8-15 layers of sheet layers and 6 mu m of sheet diameter for 2h by using a V-shaped powder mixer to obtain uniform mixed powder.
S3, putting the powder into a molybdenum container, and placing the molybdenum container in a vacuum furnace for plating, wherein the plating temperature is 900 ℃, and the plating time is 4 hours.
And S4, sieving the coated powder by using a vibrating powder sieving machine, wherein the powder sieving machine adopts a 2300-mesh sieve, and the powder sieving time is 15min. The powder which can not pass through the screen is the molybdenum-plated graphene powder (as shown in figure 2).
S5, adding the tungsten-plated graphene powder into a coulter mixer, adding 500mL of stearic acid solution, and stirring for 1h.
And S6, filling 315.48g of powder into a mold with the thickness of 85 x 85mm, and adjusting the pressure until the thickness of the pressed compact is 11mm, namely, the molybdenum-plated graphene pressed compact contains about 15% of gaps for filling copper.
S7, filling the pressed green compact into a graphite container, filling the graphite container into a tubular furnace filled with hydrogen, and carrying out heat treatment at 800 ℃ for 8 hours to remove a forming agent.
S8, horizontally placing the blank after heat treatment on a graphite container, then placing a copper sheet with the weight of 106.1 on a pressed blank, then placing the pressed blank into a vacuum furnace, and sintering the pressed blank at 1250 ℃ for 24 hours under the air pressure of 0.1Pa to obtain a primary graphene-copper composite material.
S9, subsequently, the material is processed to 80-10 mm molybdenum-plated graphene/copper composite material by grinding and other methods, the structure photo of the composite material is shown in figure 3, the compactness is good, and copper is well filled into the material. The density of the obtained material is 5.17g/cm 3 The thermal conductivity reaches 280W/mK.
Comparative example 1
Adding 100g of multilayer graphene into 10kg of copper powder to obtain doped copper powder;
loading the doped copper powder obtained in the step 1 into a ball milling tank, and processing for 2 hours on a ball mill at the speed of 1000r/min to obtain graphene-copper composite powder;
putting the powder obtained in the step 2 into a die, and pressing the powder into a powder blank by 350T pressure;
putting the powder blank obtained in the step 3 into an SPS sintering furnace, and sintering for 30min at the pressure of 50Mpa and the temperature of 1000 ℃ to obtain a graphene-copper composite material;
machining the graphene-copper composite material obtained in the step (4) to obtain a required graphene-copper composite material;
the performance of the graphene-copper composite material is detected, and the density of the graphene-copper composite material is only 7.27g/cm 3 Only 84% of theoretical density, and the thermal conductivity is only 110W/mK due to the fact that the density is too low and ball milling causes certain damage to the graphene structure. And the hot-pressing sintering cost is higher compared with the conventional sintering.
While the foregoing is directed to the preferred embodiment of the present invention, it will be appreciated by those skilled in the art that various changes and modifications may be made therein without departing from the principles of the invention as set forth in the appended claims.

Claims (10)

1. A preparation method of a graphene-copper composite material is characterized by comprising the following steps:
s1, filling metal powder into a graphite container, uniformly spreading, heating in an air atmosphere and preserving heat to obtain first mixed powder; the metal powder is tungsten powder or molybdenum powder;
s2, uniformly mixing the flaky graphene and the first mixed powder in proportion to obtain second mixed powder;
s3, filling the second mixed powder into a molybdenum container, and placing the molybdenum container in a vacuum furnace for plating to obtain third mixed powder;
s4, sieving the third mixed powder by using a vibrating sieving machine, and collecting the powder which does not pass through the sieve;
s5, placing the powder which does not pass through the screen mesh in a coulter mixer, adding a forming agent, and stirring to obtain fourth mixed powder;
s6, filling the fourth mixed powder into a die for die pressing or isostatic pressing to obtain a blank;
s7, placing the blank into a molybdenum container, placing the molybdenum container into a tubular furnace filled with hydrogen, and carrying out heat treatment;
s8, laying the pressed compact after heat treatment on a graphite container, then laying a copper sheet upwards, and putting the pressed compact and the copper sheet together into a vacuum furnace for sintering infiltration to obtain the graphene/copper composite material.
2. The preparation method according to claim 1, wherein the metal powder has a particle size of less than 5 μm, and the mass ratio of metal to metal oxide is 1; the mass ratio of the flaky graphene to the metal oxide is (1-1); the addition amount of the copper sheet is 1.0-1.2 times of the filling gap amount.
3. The method according to claim 1, wherein the first mixed powder of step S1 is W or WO 3 Mixture of (5) or Mo, moO 3 A mixture of (a).
4. The production method according to claim 1, wherein the number of the flaky graphene sheets in step S2 is 5 to 30, and the particle diameter is 5 μm or more.
5. The method according to claim 1, wherein the plating conditions in step S3 are a vacuum degree of 1Pa or less, a temperature of 800-1200 ℃, and a temperature of 1-4 hours.
6. The preparation method according to claim 1, wherein the screen of the powder screening machine in the step S4 is a 2300-mesh screen, and the powder screening time is 10-30 min.
7. The method according to claim 1, wherein the forming agent in step S5 is paraffin, stearic acid or PEG2000, and the amount of the forming agent added is 1/15 to 1/30 of the mass of the powder which does not pass through the screen.
8. The method according to claim 1, wherein the pressure in step S6 is controlled to a powder compact porosity of 50 to 90%.
9. The method according to claim 1, wherein the heat treatment temperature in step S7 is 600-900 ℃ and the temperature is kept for 6-12 h.
10. The method according to claim 1, wherein the infiltration condition in step S8 is a vacuum atmosphere having a vacuum degree of 1Pa or less, the temperature is 1150-1300 ℃, and the infiltration time is 12-24 hours.
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