CN115582547A - Cu/C/SiC composite material and preparation method thereof - Google Patents

Cu/C/SiC composite material and preparation method thereof Download PDF

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CN115582547A
CN115582547A CN202211274146.6A CN202211274146A CN115582547A CN 115582547 A CN115582547 A CN 115582547A CN 202211274146 A CN202211274146 A CN 202211274146A CN 115582547 A CN115582547 A CN 115582547A
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microwave
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CN115582547B (en
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张锐
关莉
张圆圆
王海龙
白爽
李明亮
闵志宇
董宾宾
高前程
赵世龙
宋勃震
范冰冰
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Zhengzhou University of Aeronautics
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Zhengzhou University of Aeronautics
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/12—Metallic powder containing non-metallic particles
    • 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
    • B22F3/02—Compacting only
    • 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
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
    • C22C32/0052—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
    • C22C32/0063—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides based on SiC
    • 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
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
    • 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
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    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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    • Y02E30/30—Nuclear fission reactors

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Abstract

The invention belongs to the technical field of metal matrix composite materials, and discloses a Cu/C/SiC composite material and a preparation method thereof, wherein the preparation method comprises the following steps: coated with SiO on the surface 2 ‑Cu 2 Taking SiC particles of an O interface modification phase as a precursor, and uniformly mixing the precursor, cu powder and graphite powder by ball milling to obtain composite powder; prepressing the composite powder to prepare a blank to obtain a blank body; and uniformly placing a microwave wave-transmitting material around the blank, and then carrying out microwave treatment at the temperature of 700-1000 ℃ for 10-30 min to obtain the Cu/C/SiC composite material. The invention adopts the method of introducing into Cu/SiC composite powderThe graphite can form microwave hot spots through the coupling effect with microwaves in the microwave sintering process, accumulate heat, improve the diffusion rate of an atomic interface and realize the rapid preparation of the Cu/C/SiC composite material at a low temperature.

Description

Cu/C/SiC composite material and preparation method thereof
Technical Field
The invention relates to the technical field of metal matrix composite materials, in particular to a Cu/C/SiC composite material and a preparation method thereof.
Background
Metal copper itself has excellent electrical conductivity, thermal conductivity, corrosion resistance, fatigue resistance, and the like, and is widely used in the fields of electronics, electric appliances, and the like. However, the mechanical properties and high temperature resistance of copper metal are poor, which limits the further development and application of copper metal.
In order to solve the problems, the prior art mainly adopts methods such as powder metallurgy, composite casting, mechanical alloying and the like to process copper into a composite material so as to improve the comprehensive performance of the metal copper and expand the application of the metal copper.
However, in the above method, the long-term heat retention of the powder metallurgy method causes softening of copper, thereby causing distortion of crystal junctions; the composite casting method requires high-temperature melting of metal, and the preparation process is complex and is not suitable for large-scale production; the mechanical alloying method improves the surface energy of the composite powder through high-energy ball milling, thereby promoting sintering, but the high-speed and long-time ball milling process can cause mechanical crushing of particles and generate lattice defects. That is to say, the preparation method generally has the problems of complex sintering procedure, long preparation period, low energy utilization rate, serious pollution of solvent and the like.
Therefore, the invention provides a Cu/C/SiC composite material and a preparation method thereof.
Disclosure of Invention
In order to solve the defects in the prior art, the invention provides a Cu/C/SiC metal matrix composite material and a preparation method thereof. According to the invention, graphite is introduced into the Cu/SiC composite powder, and the interface of SiC and Cu is modified by the graphite, so that the performance of the Cu/SiC composite material can be obviously improved, and in the microwave sintering process, the graphite has good wave absorbing performance and can cooperate with the SiC powder, heat is accumulated through the coupling effect of the graphite and the microwave, a microwave hot spot is formed, and the diffusion efficiency of an atomic interface is improved.
The Cu/C/SiC metal matrix composite material and the preparation method thereof are realized by the following technical scheme:
the first purpose of the invention is to provide a preparation method of a Cu/C/SiC metal matrix composite material, which comprises the following steps:
step 1, coating SiO on the surface 2 -Cu 2 Taking SiC particles of an O interface modification phase as a precursor, and uniformly mixing the precursor, cu powder and graphite powder by ball milling to obtain composite powder;
step 2, prepressing the composite powder to prepare a blank to obtain a blank body; and uniformly placing a microwave wave-transmitting material around the blank, and then carrying out microwave treatment at the temperature of 700-1000 ℃ for 10-30 min to obtain the Cu/C/SiC composite material.
Further, the mass ratio of the precursor powder to the Cu powder and the graphite powder is (2-3).
Further, the precursor is prepared by the following steps:
uniformly dispersing SiC powder in silicon by adopting a sol-gel methodPutting the mixed solution of ethyl acetate, ethanol and water into a water bath temperature of 38-42 ℃, stirring and preserving heat for 1.5-2.5 h to ensure that a layer of SiO is coated on the surface of the SiC powder 2 Then ammonia water solution is used for adjusting the pH value of the solution to 11-12, and Cu is added 2 Continuously stirring the O powder at the water bath temperature of 38-42 ℃ and keeping the temperature for 0.8-1.2 h to ensure that the Cu is 2 O powder and SiO coated on the surface 2 Reaction of SiC to form SiC/SiO 2 -Cu 2 O composite gel, and then freeze-drying at the temperature of-130 to-115 ℃ for 12 to 30 hours to obtain the precursor.
Further, the Cu 2 The mass ratio of the O powder to the tetraethoxysilane is 0.05-0.25;
the dosage ratio of the SiC powder to the ethyl orthosilicate is 1mg;
the volume ratio of the ethyl orthosilicate to the ethanol to the water is 1.
Furthermore, the frequency of the microwave treatment is 300 MHz-300 GHz.
Furthermore, the wavelength of the microwave treatment is 1 mm-1 m, and the power is 0-15 kW.
Further, the ball-material ratio of the ball milling treatment is 2-10, the rotating speed is 150-300 r/min, and the particle size of the composite powder after the ball milling treatment is 0.5-1 μm.
Furthermore, the prepressing blank is formed by adopting a uniaxial pressing mode, and the pressure is 3-30 MPa.
Furthermore, the melting point of the microwave-transparent material is 1200-1800 ℃, and the volume ratio of the microwave-transparent material to the blank body is 4-10.
Further, the particle size of the microwave transmission material is 40-120 meshes.
The second purpose of the invention is to provide a Cu/C/SiC composite material prepared by the preparation method.
The second purpose of the invention is to provide a Cu/C/SiC metal matrix composite material prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, graphite is introduced into Cu/SiC composite powder, the graphite is an allotrope of carbon, has the characteristics of high temperature resistance, electric conduction, heat conduction, lubricity and the like, is stable in chemical property, has a special lamellar structure, can be used as a solid lubricant, and can form a surface lubricating layer under the action of self lubrication when being subjected to external stress and friction force, so that the friction coefficient is reduced, and the wear resistance of the material is improved; and the Cu matrix and the SiC move relatively, so that the internal stress of the material is released, the generation and the expansion of cracks are reduced, and the performance of the composite material is improved.
The surface of the invention is coated with SiO 2 -Cu 2 Taking the SiC material of O as a precursor, and uniformly mixing precursor powder, cu powder and graphite powder together by adopting mechanical ball milling to obtain composite powder; subsequently, microwave sintering is performed in cooperation with the microwave-transparent material. In the microwave sintering process, the graphite has good wave absorbing performance, can form microwave hot spots through the coupling effect with microwaves, accumulate heat, improve the diffusion rate of an atomic interface, realize the rapid preparation of a Cu/C/SiC composite material at a low temperature, and wrap SiO on the surface of SiC 2 The material is a wave-transparent material, and can fix microwaves, so that more microwaves reach the surface of SiC particles, the impedance matching between SiC and the microwaves is regulated and controlled, the sintering is promoted, and the Cu/C/SiC composite material is prepared quickly and efficiently.
The preparation method is simple and easy to operate, has short preparation period, can greatly utilize microwave energy, improves the energy utilization rate, and is favorable for large-scale production and preparation.
Drawings
FIG. 1 is a temperature rise graph of a microwave sintered Cu/C/SiC composite material of example 1 of the present invention.
FIG. 2 is an XRD pattern of the Cu/C/SiC powder raw material used for microwave sintering in examples 1 and 2 of the present invention.
FIG. 3 is an XRD pattern of the microwave sintered Cu/C/SiC composite material obtained in examples 1 and 2 of the present invention.
FIG. 4 is an SEM photograph of the composite powder in example 1 of the present invention.
FIG. 5 is an SEM photograph of a microwave sintered Cu/C/SiC composite material obtained in example 1 of the present invention.
FIG. 6 is an SEM photograph of a microwave sintered Cu/C/SiC composite material obtained in example 2 of the present invention.
Detailed Description
As described in the background art, the preparation method of the copper-based material in the prior art generally has the problems of complex sintering procedure, long preparation period, low energy utilization rate, serious pollution and the like. Therefore, the inventor tries to provide a novel and environment-friendly method for preparing copper-based materials, so as to shorten the preparation period and improve the energy utilization rate. The inventors tried to apply the microwave sintering technique to the preparation of copper-based materials, but the inventors considered that microwave radiation of metal copper is reflected during the microwave heating process, resulting in poor bonding of copper with the second phase material and inefficient use of microwaves, resulting in difficulty in applying the microwave sintering technique to the efficient preparation of copper-based composite materials. In order to overcome the technical problem, the inventor adopts the technical scheme that graphite is introduced into Cu/SiC composite powder, and the interface of SiC and Cu is modified by the graphite, so that the performance of the Cu/SiC composite material can be obviously improved, and in the microwave sintering process, the graphite has good wave-absorbing performance, and can accumulate heat through the coupling effect with microwaves, form microwave hot spots and improve the diffusion efficiency of an atomic interface. In addition, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention.
It should be noted that the experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials used are commercially available, unless otherwise specified.
Example 1
The embodiment provides a Cu/C/SiC composite material, and a preparation method thereof is as follows:
s1, preparing precursor powder by adopting a sol-gel method:
uniformly dispersing SiC powder in a mixed solution of tetraethoxysilane, ethanol and water, stirring at the water bath temperature of 40 ℃, and preserving heat for 2 hours to hydrolyze the tetraethoxysilanePost-formed SiO 2 Wrapping the SiC surface; then adjusting the pH value of the solution to 11-12 by ammonia water, and adding Cu 2 Keeping the temperature of the O powder at the water bath temperature of 40 ℃ and stirring for 1h to ensure that the Cu 2 SiO coated on surface of O and SiC 2 Act to form SiO on the SiC surface 2 -Cu 2 O, and further obtaining SiC/SiO 2 -Cu 2 O composite gel, followed by SiC/SiO 2 -Cu 2 Freeze-drying the O composite gel at-130 ℃ for 24h to obtain precursor powder;
wherein the volume ratio of the ethyl orthosilicate to the ethanol to the water is 1;
the dosage ratio of the SiC powder to the tetraethoxysilane is 1mg;
the Cu 2 The mass ratio of the O powder to the tetraethoxysilane is 0.1.
S2, preparing composite powder:
respectively weighing the precursor powder, cu powder and graphite powder according to the mass ratio of the precursor powder to the Cu powder to the graphite powder of 2.5.
S3, microwave sintering treatment:
weighing 45g of the composite powder, pressing into 3 identical blanks in a cylindrical tabletting mold at room temperature, and maintaining the pressure for 1min under the pressure of 3MPa, wherein the diameter of each blank is 30mm, and the thickness of each blank is 3mm.
Sintering the block by using microwave and attaching a heat insulation structure; by means of SiO 2 The particles are used as microwave wave-transmitting materials to be buried around the blank body to prevent high-temperature oxidation; the sintering temperature is 900 ℃, the temperature is kept for 20min, the wavelength range of the microwave is 0.5m, the frequency range is 100GHz, the power is set to be 0-15 kw/min, and the heating rate is 10-20 ℃/min; and obtaining the Cu/C/SiC composite material.
And the temperature rise curve in the microwave sintering process is shown in figure 1, and it can be seen that through microwave heating, the temperature of the sample rises to 670 ℃ in the 7 th minute, and the sintering temperature is controlled to be about 900 ℃ by regulating and controlling the microwave input power, after the temperature is stabilized in the 15 th minute, the heat preservation time is 20min, and the whole process is about 35 min. Compared with the traditional sintering, the microwave sintering greatly shortens the sintering time.
Example 2
This example provides a Cu/C/SiC composite material, and the preparation method thereof differs from that of example 1 only in that:
in this example, the microwave sintering temperature was 1000 ℃.
Example 3
This example provides a Cu/C/SiC composite material, and the preparation method thereof differs from example 1 only in that:
in the embodiment, the dosage ratio of the SiC powder to the ethyl orthosilicate is 1mg;
the mass ratio of the precursor powder to the Cu powder to the graphite powder is 2;
the frequency of the microwave treatment was 915MHz.
Example 4
This example provides a Cu/C/SiC composite material, and the preparation method thereof differs from example 1 only in that:
in this embodiment, the dosage ratio of the SiC powder to the tetraethoxysilane is 1mg;
the mass ratio of the precursor powder to the Cu powder to the graphite powder is 3;
the frequency of the microwave treatment was 2.45GHz.
Example 5
This example provides a Cu/C/SiC composite material, and the preparation method thereof differs from example 1 only in that:
in the embodiment, the ball-to-material ratio of the ball milling treatment is 2;
the prepressing blank is formed by adopting a single shaft pressing mode, and the pressure is 3MPa;
the volume ratio of the microwave permeable material to the green body is 4;
the particle size of the microwave transmission material is 40 meshes.
Example 6
This example provides a Cu/C/SiC composite material, and the preparation method thereof differs from example 1 only in that:
in the embodiment, the ball-to-material ratio of the ball milling treatment is 10, the rotating speed is 300r/min, and the particle size of the composite powder after the ball milling treatment is 0.5 μm;
the prepressing blank is formed by adopting a single shaft pressing mode, and the pressure is 30MPa;
the volume ratio of the microwave permeable material to the green body is 10;
the particle size of the microwave transmission material is 120 meshes.
Test section
To illustrate the relevant properties of the Cu/C/SiC composites prepared in accordance with the present invention, the following tests were performed on the composites provided in examples 1-2.
(I) X-ray diffraction test
XRD test was carried out on the Cu/C/SiC composite material obtained in examples 1 to 2 using a SmartLab type X-ray diffraction analyzer (XRD) of Japan science and electric machines corporation, and the test results are shown in FIGS. 2 and 3, respectively.
As can be seen from FIG. 2, the composite powder prepared by the sol-gel method and the wet ball milling method has high purity and no impurities. The prepared precursor powder has high quality, and can ensure that a Cu/C/SiC composite material with excellent performance is formed after the subsequent sintering process.
As can be seen from FIG. 3, the Cu/C/SiC composite material prepared by microwave sintering and heat preservation at 900-1000 ℃ for 20min has high pattern peak, and the fired sample has high crystalline phase content and large crystal grains. The interface modification phase wrapped on the SiC surface by the sol-gel method is also shown, but under the action of high-temperature air, part of Cu is oxidized to generate CuO and the like.
(II) scanning electron microscope testing
The microstructure of the composite powder of example 1 and the microstructure of the Cu/C/SiC composite material obtained in examples 1 to 2 were measured by a JSM-7001F Scanning Electron Microscope (SEM) from Japan Electron Ltd. The results are shown in FIGS. 4 to 6, respectively.
Fig. 4 shows the micro-morphology of the composite powder of example 1, and it can be seen that the composite powder prepared by the sol-gel method and the wet ball milling method has relatively uniform dispersion of the Cu and SiC simple substances, but has a relatively low interface bonding degree and a powder particle size of about 1 μm.
FIG. 5 shows the micro-morphology of example 1, and it can be seen that the interface bonding strength of Cu and SiC is improved, and SiC is attached to part of the surface of Cu and forms a tight bond between the Cu and SiC of the Cu/C/SiC composite material prepared by microwave sintering and heat preservation at 900 ℃ for 20 min.
FIG. 6 shows the microstructure of example 2, which shows that the interface bonding strength of Cu and SiC is stronger in the Cu/C/SiC composite material prepared by holding at 1000 ℃ for 20min compared with the sample sintered at 900 ℃, and most of Cu and SiC are bonded more tightly with the increase of temperature.
It is to be understood that the above-described embodiments are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.

Claims (10)

1. A preparation method of a Cu/C/SiC composite material is characterized by comprising the following steps:
step 1, coating SiO on the surface 2 -Cu 2 Taking SiC particles of an O interface modification phase as a precursor, and uniformly mixing the precursor, cu powder and graphite powder by ball milling to obtain composite powder;
step 2, prepressing the composite powder to prepare a blank to obtain a blank body; and uniformly placing a microwave wave-transmitting material around the blank, and then carrying out microwave treatment at the temperature of 700-1000 ℃ for 10-30 min to obtain the Cu/C/SiC composite material.
2. The preparation method according to claim 1, wherein the mass ratio of the precursor powder to the Cu powder to the graphite powder is 2 to 3.
3. The method of claim 1, wherein the precursor is prepared by:
uniformly dispersing SiC powder in a mixed solution of ethyl orthosilicate, ethanol and water by adopting a sol-gel method, stirring and preserving heat for 1.5-2.5 h at the temperature of 38-42 ℃, adjusting the pH value of the solution to 11-12, adding Cu 2 And continuously stirring the O powder at the temperature of between 38 and 42 ℃ and preserving the heat for 0.8 to 1.2 hours, and freeze-drying to obtain the precursor.
4. The method of claim 3, wherein the Cu 2 The mass ratio of the O powder to the tetraethoxysilane is 0.05-0.25;
the dosage ratio of the SiC powder to the tetraethoxysilane is 1mg;
the volume ratio of the ethyl orthosilicate to the ethanol to the water is 1.
5. The method of claim 1, wherein the microwave treatment has a frequency of 300MHz to 300GHz, a wavelength of 1mm to 1m, and a power of 0 to 15kW.
6. The preparation method of claim 1, wherein the ball-milling treatment has a ball-to-material ratio of 2-10, a rotation speed of 150-300 r/min, and a particle size of the composite powder after ball-milling treatment is 0.5-1 μm.
7. The production method according to claim 1, wherein the preliminary press molding is performed by uniaxial press molding at a pressure of 3 to 30MPa.
8. The preparation method according to claim 1, wherein the melting point of the microwave transparent material is 1200 to 1800 ℃, and the volume ratio of the microwave transparent material to the green body is 4 to 10.
9. The method of claim 1, wherein the microwave transparent material has a particle size of 40 to 120 mesh.
10. A Cu/C/SiC composite material produced by the production method according to any one of claims 1 to 9.
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