CN110699567B - Silicon carbide particle reinforced aluminum matrix composite and preparation method thereof - Google Patents
Silicon carbide particle reinforced aluminum matrix composite and preparation method thereof Download PDFInfo
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- CN110699567B CN110699567B CN201910998985.4A CN201910998985A CN110699567B CN 110699567 B CN110699567 B CN 110699567B CN 201910998985 A CN201910998985 A CN 201910998985A CN 110699567 B CN110699567 B CN 110699567B
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1005—Pretreatment of the non-metallic additives
- C22C1/101—Pretreatment of the non-metallic additives by coating
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
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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
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
- C22C1/1047—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
- C22C21/02—Alloys based on aluminium with silicon as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- 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
Abstract
The invention provides a silicon carbide particle reinforced aluminum matrix composite and a preparation method thereof, belonging to the field of composite preparation. The preparation method provided by the invention comprises the following steps: adding TiO into the mixture2And after the sol and the SiC powder are sequentially subjected to first mixing and calcination, the sol and the SiC powder are sequentially subjected to second mixing and casting with molten aluminum alloy, so that the SiC particle reinforced aluminum matrix composite is obtained. The invention adds TiO2After mixing the sol with SiC powder and calcining, TiO2Reacts with SiC to generate TiC and SiO2TiC and SiO formed2The SiC/Al transition layer has good wettability with Al in molten aluminum alloy, can effectively improve the interface bonding of SiC and molten Al, avoids the occurrence of interface reaction, and improves the dispersibility of SiC particle reinforcement in the aluminum matrix composite.
Description
Technical Field
The invention relates to the field of composite material preparation, in particular to a silicon carbide particle reinforced aluminum matrix composite material and a preparation method thereof.
Background
Silicon carbide (SiC) has the advantages of high melting point, high hardness, high elastic modulus, low manufacturing cost, and the like. The ZL101 alloy is used as a novel Al-Si casting alloy, and is widely applied to the fields of automobile manufacturing and aerospace due to the advantages of good casting fluidity, good air tightness, small shrinkage, strong corrosion resistance and the like. The silicon carbide particle reinforced aluminum matrix composite material has the advantages of excellent thermal conductivity, low expansion coefficient, high specific strength and specific stiffness, abrasion resistance and the like, is widely applied to the fields of aerospace, automobiles, electronic packaging and military equipment, and becomes a research hotspot of metal matrix composite materials.
The commonly used methods for preparing SiC aluminum matrix composite materials at present include powder metallurgy, stirring casting, extrusion casting, vacuum pressure infiltration, spray deposition and the like. Wherein, the compactness of the composite material prepared by the powder metallurgy method is poor, and secondary processing is needed to improve the performance of the composite material; the extrusion casting method is easy to cause the damage of the prefabricated member in the extrusion and infiltration process, and simultaneously, the particles are difficult to infiltrate into the metal melt in the infiltration process, the wettability is poor, the preparation is difficult, and the strength of the manufactured prefabricated member is not high; the vacuum pressure infiltration method is prepared under the conditions of vacuum and high pressure, the obtained composite material can have structural defects such as air holes and the like, and the uniform distribution of reinforcement particles in the subsequent spray deposition process cannot be ensured, so that the prepared material has all defects and the spray deposition thickness is thinner; the jet deposition method has high preparation cost and high requirements on preparation equipment.
Disclosure of Invention
In view of the above, the present invention is directed to a silicon carbide particle reinforced aluminum matrix composite and a method for preparing the same. The SiC particle reinforcement in the silicon carbide reinforced aluminum-based composite material prepared by the preparation method provided by the invention has good wettability with an aluminum-based material, the dispersibility of the SiC particle reinforcement in the aluminum-based material is good, and the mechanical property of the aluminum-based composite material is excellent.
In order to achieve the above purpose, the invention provides the following technical scheme:
the invention provides a preparation method of a SiC particle reinforced aluminum matrix composite, which comprises the following steps:
adding TiO into the mixture2And after the sol and the SiC powder are sequentially subjected to first mixing and calcination, the sol and the SiC powder are sequentially subjected to second mixing and casting with molten aluminum alloy, so that the SiC particle reinforced aluminum matrix composite is obtained.
Preferably, the mass ratio of the SiC powder to the molten aluminum alloy is 1-11: 100, and the SiC powder and the TiO are mixed2The dosage ratio of the sol is 1 g: 10-50 mL.
Preferably, the temperature of the molten aluminum alloy is 740-790 ℃.
Preferably, the material of the molten aluminum alloy is ZL101 or ZL 102.
Preferably, the particle size of the SiC powder is 0.5-3 μm.
Preferably, the calcining temperature is 400-500 ℃ and the calcining time is 2-3 h.
Preferably, the SiC powder further comprises a pretreatment before use, the pretreatment comprising the steps of:
and sequentially cleaning and drying the SiC powder to obtain the pretreated SiC powder.
The invention also provides the SiC particle reinforced aluminum-based composite material prepared by the preparation method in the technical scheme, which comprises an aluminum alloy matrix, the SiC particle reinforcement and eutectic silicon, wherein the SiC particle reinforcement and the eutectic silicon are dispersed in the aluminum alloy matrix, and the surface of the SiC particle reinforcement is coated with TiC and SiO2。
The invention provides a preparation method of a SiC particle reinforced aluminum matrix composite, which comprises the following steps: adding TiO into the mixture2And after the sol and the SiC powder are sequentially subjected to first mixing and calcination, the sol and the SiC powder are sequentially subjected to second mixing and casting with molten aluminum alloy, so that the SiC particle reinforced aluminum matrix composite is obtained. The invention adds TiO2Mixing the sol with SiC powder to obtain TiO2Uniformly coating the SiC powder surface with TiO after calcination2Reacts with SiC to generate TiC and SiO2TiC and SiO formed2The SiC particle reinforcement material has good wettability with Al in molten aluminum alloy as a transition layer, can effectively improve the interface bonding of SiC and molten Al, avoids the occurrence of interface reaction, and improves the dispersibility of SiC particle reinforcement in the aluminum matrix composite material. The invention adopts the stirring casting method to prepare the SiC particle reinforced aluminum matrix composite material, has simple process and low cost, and can realize large-scale batch production. The embodiment result shows that SiC particles in the SiC particle reinforced aluminum matrix composite material prepared by the invention are uniformly distributed, and the SiC particle reinforced aluminum matrix composite material has excellent mechanical property, the Brinell hardness is 80-95 HB, and the tensile strength is 210-230 MPa.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
FIG. 1 shows TiO prepared in example 12XRD pattern of the coated SiC composite powder;
FIG. 2 is an XRD pattern of a SiC particle-reinforced aluminum matrix composite obtained in example 1;
FIG. 3 is a metallographic structure diagram of a SiC particle-reinforced aluminum matrix composite obtained in example 1;
FIG. 4 is a metallographic structure diagram of the SiC particle-reinforced aluminum matrix composite obtained in example 2.
Detailed Description
The invention provides a preparation method of a SiC particle reinforced aluminum matrix composite, which comprises the following steps:
adding TiO into the mixture2And after the sol and the SiC powder are sequentially subjected to first mixing and calcination, the sol and the SiC powder are sequentially subjected to second mixing and casting with molten aluminum alloy, so that the SiC particle reinforced aluminum matrix composite is obtained.
According to the invention, the SiC powder is preferably cleaned and dried in sequence and then is mixed with the TiO powder2The sol is subjected to a first mixing and calcination in sequence.
In the present invention, the particle diameter of the SiC powder is preferably 0.5 to 3 μm, and more preferably 1 to 2 μm. The specific source of the SiC powder is not particularly limited in the invention, and the conventional commercial products in the field can be adopted.
In the invention, the SiC powder is preferably subjected to first cleaning in an ethanol solution and under ultrasonic conditions in sequence, and then subjected to second cleaning in distilled water. In the present invention, the mass concentration of the ethanol solution is preferably 40% to 60%. The conditions of the ultrasound are not particularly limited in the present invention, and the ultrasound conditions known to those skilled in the art may be used. In the present invention, the number of times of the second washing is preferably 2 to 3 times. The specific operation of the cleaning is not particularly limited in the present invention, and a cleaning method known to those skilled in the art may be used.
In the invention, the drying temperature is preferably 80-100 ℃, and the drying time is preferably 6-12 h. The specific operation mode of the drying is not particularly limited, and the drying mode known to those skilled in the art can be adopted.
After drying is finished, the invention preferably cools the product obtained after drying along with the furnace.
In the present invention, the TiO is2The sol is preferably prepared by a process comprising the steps of:
mixing ethyl titanate and first absolute ethyl alcohol to carry out a first reaction to obtain a first reaction solution;
mixing distilled water, second absolute ethyl alcohol and glacial acetic acid to carry out second reaction to obtain a second reaction solution;
mixing the first reaction solution and the second reaction solution for a third reaction, and aging to obtain TiO2And (3) sol.
According to the invention, ethyl titanate and first absolute ethyl alcohol are mixed for a first reaction to obtain a first reaction solution. In the invention, the volume ratio of the ethyl titanate to the first absolute ethyl alcohol is preferably 15-20: 40-60 mL. The sources of the ethyl titanate and the first absolute ethyl alcohol are not particularly limited, and conventional commercial products in the field can be adopted. In the invention, the first reaction is preferably carried out under the condition of magnetic stirring, the speed of the magnetic stirring is preferably 1800-2000 rpm, and the time is preferably 30-60 min. According to the invention, the ethyl titanate is preferably dripped into the first absolute ethyl alcohol; in the present invention, the dropping rate of the ethyl titanate is not particularly limited, and a dropping rate known in the art may be used.
According to the invention, distilled water, second absolute ethyl alcohol and glacial acetic acid are mixed for second reaction to obtain a second reaction solution. In the invention, the volume ratio of the distilled water, the second absolute ethyl alcohol and the glacial acetic acid is preferably 4-8: 40-80: 8-15. The sources of the distilled water, the second absolute ethyl alcohol and the glacial acetic acid are not particularly limited, and the conventional commercial products in the field can be adopted. In the invention, the second reaction is preferably carried out under the condition of magnetic stirring, the speed of the magnetic stirring is preferably 1000-1500 rpm, and the time is preferably 20-30 min.
After the first reaction solution and the second reaction solution are obtained, the first reaction solution and the second reaction solution are mixed for a third reaction and are aged to obtain TiO2And (3) sol. In the invention, the third reaction is preferably carried out under the condition of magnetic stirring, the speed of the magnetic stirring is preferably 1800-2000 rpm, and the time is preferably 2-3 h. The present invention preferably adds the second reaction solution to the first reaction solution. In the present invention, the aging is carried outThe time of (2) is preferably 8-12 h. The aging method is not particularly limited in the present invention, and the aging operation known to those skilled in the art may be used. TiO prepared by the invention2The sol has good stability compared with other TiO2The sol can be effectively coated on the surface of the SiC powder.
In the invention, TiO is mixed with2Sequentially carrying out first mixing and calcination on the sol and the SiC powder, and then carrying out second mixing and casting on the sol and the SiC powder and molten aluminum alloy to obtain TiO2Wrapping SiC particle reinforced aluminum matrix composite.
In the invention, the mass ratio of the SiC powder to the molten aluminum alloy is preferably 1-11: 100, more preferably 3-7: 100, and the SiC powder and the TiO powder are mixed together2The amount ratio of the sol is preferably 1 g: 10 to 50mL, more preferably 1 g: 20-40 mL. In the present invention, the first mixing is preferably performed by adding the SiC powder to TiO with stirring2In the sol, the stirring speed is preferably 500-1000 rpm, and the time is preferably 1-2 h.
After the first mixing is completed, the present invention preferably filters, washes and dries the resulting mixed product. In the present invention, the filtration is preferably vacuum filtration. The specific operation mode of the washing is not particularly limited in the present invention, and a washing mode known to those skilled in the art may be adopted. In the invention, the drying temperature is preferably 80-100 ℃, and the drying time is preferably 10-16 h. The specific operation of the drying is not particularly limited in the present invention, and a mixing method known to those skilled in the art may be adopted.
The first mixing and separating step is preferably repeated, and the number of times of repetition is preferably 2-3 times. The invention leads TiO to be mixed for a plurality of times2Deposited and firmly wrapped on the surface of the SiC powder.
In the invention, the calcination temperature is preferably 400-500 ℃, the calcination time is preferably 2-3 h, and the heating rate is preferably 3-6 ℃/min. The invention leads TiO coated on the surface of SiC powder to be calcined2Reacts with SiC powder to generate TiC and SiO2TiC formed andSiO2the SiC particle reinforcement material has good wettability with Al in molten aluminum alloy as a transition layer, can effectively improve the interface bonding of SiC and molten Al, avoids the occurrence of interface reaction, and improves the dispersibility of SiC particle reinforcement in the aluminum matrix composite material.
In the invention, the material of the molten aluminum alloy is preferably ZL101 or ZL102, and the temperature of the molten aluminum alloy is preferably 740-790 ℃. The specific source of the molten aluminum alloy is not particularly limited, and the conventional commercial products in the field can be adopted.
In the invention, the second mixing is preferably electric stirring, the speed of the electric stirring is preferably 300-500 rpm, and the time is preferably 10-20 min.
After the second mixing is finished, the obtained mixed product is preferably subjected to degassing and deslagging in sequence and then is cast. The present invention is not particularly limited to the specific operation of the degassing and deslagging process, and the degassing and deslagging process known to those skilled in the art may be used. The present invention is not particularly limited to the specific operation of the casting, and the casting method known to those skilled in the art may be used.
The invention also provides the SiC particle reinforced aluminum-based composite material prepared by the preparation method in the technical scheme, which comprises an aluminum alloy matrix, the SiC particle reinforcement and eutectic silicon, wherein the SiC particle reinforcement and the eutectic silicon are dispersed in the aluminum alloy matrix, and the surface of the SiC particle reinforcement is coated with TiC and SiO2. In the invention, the mass percentage of the SiC particle reinforcement body in the SiC particle reinforced aluminum matrix composite material is preferably 1-11%.
The following will explain the SiC particle reinforced aluminum matrix composite material and the preparation method thereof provided by the present invention in detail with reference to the examples, but they should not be construed as limiting the scope of the present invention.
Example 1
(1) Washing 10g of SiC powder (0.5-1 μm) with 50% by mass absolute ethanol solution under ultrasonic conditions, and washing with distilled water for 2 times; and drying the cleaned SiC powder at the constant temperature of 80 ℃ for 8 h.
(2) Under magnetic stirring, 16mL of butyl titanate is dropwise added into 40mL of absolute ethyl alcohol, magnetic stirring is continued for 30min, the stirring speed is 1800 rpm, and the prepared solution is called solution A; putting 5mL of distilled water, 50mL of absolute ethyl alcohol and 10mL of glacial acetic acid into a magnetic stirrer, and magnetically stirring for 30min at the stirring speed of 1000 revolutions per minute to obtain a uniformly stirred solution B; slowly adding the solution B into the solution A under the magnetic stirring, continuously stirring for 2 hours at the stirring speed of 1800 rpm, and aging the solution to obtain TiO2And (3) sol.
(3) 10g of the SiC particles obtained in the step (1) were put into 500mL of the TiO prepared in the step (2)2Stirring the sol continuously at the stirring speed of 600 rpm for 1.5h, separating and taking out SiC, and drying at the temperature of 80 ℃.
(4) Repeating the step (3) for 2 times to obtain TiO2After wrapping the SiC particles, calcining for 2h at 400 ℃.
(5) Preheating a crucible in a resistance furnace at 200 ℃ for 30 minutes, putting ZL101 aluminum alloy into the crucible in the resistance furnace, heating the resistance furnace to 750 ℃, adding the SiC powder obtained in the step (4) (the adding amount of the SiC powder accounts for 5% of the mass of the ZL101 aluminum alloy) after the alloy is melted, fully stirring, and pouring the melt into a metal mold after degassing and deslagging to obtain the SiC particle reinforced ZL101 composite material.
The obtained SiC particle reinforced ZL101 composite material is subjected to mechanical property test, and the tensile strength is 220MPa and the Brinell hardness is 90 HB.
FIG. 1 shows TiO prepared in example 12The XRD pattern of the coated SiC composite powder shows that the SiC surface is coated with a layer of TiO2And part of TiO after the composite powder is calcined2Reacts with SiC to generate TiC and SiO2。
Fig. 2 is an XRD chart of the SiC particle-reinforced aluminum matrix composite material obtained in example 1, and it can be seen from fig. 2 that the SiC particle-reinforced ZL101 composite material obtained in this example mainly has an Al phase, Si phase, SiC phase and TiC phase.
Fig. 3 is a metallographic structure diagram of the SiC particle reinforced aluminum matrix composite prepared in example 1, and it can be seen from the diagram that SiC particle reinforcements are uniformly distributed in the aluminum matrix composite, the boundary of SiC particles is clear, the occurrence of interface reaction is effectively avoided, and eutectic silicon is in a short rod shape.
Example 2
(1) Washing 10g of SiC powder (1-2 μm) with 50% by mass absolute ethanol solution under ultrasonic conditions, and washing with distilled water for 2 times; and drying the cleaned SiC powder at the constant temperature of 80 ℃ for 10 hours.
(2) Under magnetic stirring, dropwise adding 17mL of butyl titanate into 50mL of absolute ethyl alcohol, continuing magnetic stirring for 30min at a stirring speed of 2000 r/min, and calling the prepared solution as solution A; putting 8mL of distilled water, 70mL of absolute ethyl alcohol and 15mL of glacial acetic acid into a magnetic stirrer, and magnetically stirring for 30min at the stirring speed of 1500 revolutions per minute to obtain a uniformly stirred solution B; slowly adding the solution B into the solution A under magnetic stirring, continuously stirring for 2 hours at the stirring speed of 2000 r/min, and aging the solution to obtain TiO2And (3) sol.
(3) 10g of the SiC particles obtained in the step (1) were put into 500mL of the TiO prepared in the step (2)2Stirring the sol continuously at the stirring speed of 600 rpm for 1h, separating and taking out SiC, and drying at the temperature of 90 ℃.
(4) Repeating the step (3) for 3 times to obtain TiO2After wrapping the SiC particles, calcining for 2h at 450 ℃.
(5) Preheating a crucible in a resistance furnace at 200 ℃ for 30 minutes, putting ZL101 aluminum alloy into the crucible in the resistance furnace, heating the resistance furnace to 750 ℃, adding SiC powder (the adding amount of the SiC powder accounts for 3% of the mass of the ZL101 aluminum alloy) obtained in the step (4) after the alloy is melted, fully stirring, and pouring the melt into a metal mold after degassing and deslagging to obtain the SiC particle reinforced ZL101 composite material.
The obtained SiC particle reinforced ZL101 composite material is subjected to mechanical property test, and the tensile strength is 210MPa and the Brinell hardness is 90 HB.
Fig. 4 is a metallographic structure diagram of the SiC particle reinforced aluminum matrix composite prepared in example 2, and it can be seen from the diagram that the SiC particle reinforcements are uniformly distributed in the aluminum matrix composite, the boundary of the SiC particles is clear, and the occurrence of interface reaction is effectively avoided.
Example 3
(1) Washing 10g of SiC powder (2-3 μm) with 50% by mass absolute ethanol solution under ultrasonic conditions, and washing with distilled water for 2 times; and drying the cleaned SiC powder at the constant temperature of 80 ℃ for 10 hours.
(2) Under magnetic stirring, dropwise adding 17mL of butyl titanate into 40mL of absolute ethyl alcohol, continuing magnetic stirring for 30min at a stirring speed of 2000 r/min, and calling the prepared solution as solution A; putting 10mL of distilled water, 80mL of absolute ethyl alcohol and 12mL of glacial acetic acid into a magnetic stirrer, and magnetically stirring for 30min at the stirring speed of 1500 revolutions per minute to obtain a uniformly stirred solution B; slowly adding the solution B into the solution A under magnetic stirring, continuously stirring for 2 hours at the stirring speed of 2000 r/min, and aging the solution to obtain TiO2And (3) sol.
(3) 10g of the SiC particles obtained in the step (1) were put into 500mL of the TiO prepared in the step (2)2Stirring the sol continuously at a stirring speed of 600 rpm for 1h, separating and taking out SiC, and drying at 80 ℃.
(4) Repeating the step (3) for 2 times to obtain TiO2After wrapping the SiC particles, calcining for 2h at 500 ℃.
(5) Preheating a crucible in a resistance furnace at 200 ℃ for 30 minutes, putting ZL101 aluminum alloy into the crucible in the resistance furnace, heating the resistance furnace to 750 ℃, adding SiC powder (the adding amount of the SiC powder accounts for 7% of the mass of the ZL101 aluminum alloy) obtained in the step (4) after the alloy is melted, fully stirring, degassing and deslagging the melt, and pouring the melt into a metal mold to obtain the SiC particle reinforced ZL101 composite material.
The obtained SiC particle reinforced ZL101 composite material is subjected to mechanical property test, and the tensile strength is 225MPa, and the Brinell hardness is 95 HB.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (7)
1. A preparation method of a SiC particle reinforced aluminum matrix composite is characterized by comprising the following steps:
adding TiO into the mixture2After the sol and the SiC powder are sequentially subjected to first mixing and calcination, the sol and the SiC powder are sequentially subjected to second mixing and casting with molten aluminum alloy to obtain a SiC particle reinforced aluminum matrix composite;
the calcining temperature is 400-500 ℃, and the time is 2-3 h.
2. The preparation method according to claim 1, wherein the mass ratio of the SiC powder to the molten aluminum alloy is 1-11: 100, and the SiC powder and the TiO are mixed together2The dosage ratio of the sol is 1 g: 10-50 mL.
3. The preparation method according to claim 1, wherein the temperature of the molten aluminum alloy is 740 to 790 ℃.
4. The method as claimed in any one of claims 1 to 3, wherein the molten aluminum alloy is ZL101 or ZL 102.
5. The production method according to claim 1 or 2, wherein the particle diameter of the SiC powder is 0.5 to 3 μm.
6. The method according to claim 1, wherein the SiC powder further comprises a pretreatment before use, the pretreatment comprising the steps of:
and sequentially cleaning and drying the SiC powder to obtain the pretreated SiC powder.
7. The SiC particle reinforced aluminum matrix composite material prepared by the preparation method of any one of claims 1 to 6, which is characterized by comprising an aluminum alloy matrix, a SiC particle reinforcement and eutectic silicon, wherein the SiC particle reinforcement and the eutectic silicon are dispersed in the aluminum alloy matrix, and the surface of the SiC particle reinforcement is coated with TiC and SiO2。
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