High-content ceramic / metal composite material and preparation method thereof

Through high-frequency pulse current rolling technology, the problem of poor heterointerface connection during the rolling process of high-content ceramic/metal composite materials is solved, and the healing of microgaps and microcracks of heterointerfaces is achieved, which improves the overall performance of the material.

CN120249724AActive Publication Date: 2025-07-04TAIYUAN UNIVERSITY OF TECHNOLOGY

Patent Information

Application Number
CN202510742309.6
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-06-05
Publication Date
2025-07-04
Estimated Expiration
2045-06-05

AI Technical Summary

Technical Problem

During the rolling process of high-content ceramic/metal composite materials, the difference in physical and chemical properties between the ceramic particles and the metal matrix makes it difficult to achieve complete wetting of the heterogeneous interface, there are micro gaps and micro cracks, and traditional rolling methods are difficult to avoid cracking.

Method used

High-frequency pulse current rolling technology is adopted to assist in the heterogeneous interface between ceramic particles and metal matrix during the rolling process through the skin effect and proximity effect of high-frequency pulse current, combining the ampere force and hot compressive stress generated by the magnetic field to promote microgap healing.

Benefits of technology

It significantly improves the coordinated plastic deformation capability of the heterogeneous interface of ceramic particles/metal matrix, improves the quality of heterogeneous interface connection, reduces micro gaps and microcracks, and improves the overall performance of the material.

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Abstract

The invention belongs to the technical field of post-treatment of ceramic / metal composite materials, and particularly relates to a high-content ceramic / metal composite material and a preparation method thereof. In order to reduce the existence of micro gaps on the surface of the ceramic / metal composite material and improve the performance of the ceramic / metal composite material, a high-content ceramic / metal composite material blank is prepared by adopting a spark plasma sintering method, and then high-frequency pulse current is added to assist rolling; and finally, the high-content ceramic / metal composite material with micro-gap healing and improved performance is obtained.
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Description

Technical Field

[0001] The present invention belongs to the technical field of post-treatment of ceramic / metal composites, and particularly relates to a high-content ceramic / metal composite material and a preparation method thereof. Background Art

[0002] With the progress of science and technology and the rapid development of key equipment fields, high-content ceramic / metal composite materials have become advanced materials integrating functions and structures. They have the advantages of low density, high hardness, wear resistance, good thermal conductivity, good thermal stability, and will not crack due to sudden cooling or heating. They have broad application prospects in the fields of aerospace, nuclear power, and transportation. Taking nuclear power as an example, since the spent fuel discharged from the fuel compartment of a nuclear reactor has extremely strong α, β, and γ radioactivity and is accompanied by a certain amount of neutron emission, harsh requirements are put forward for the neutron absorption material of the spent fuel compartment of a nuclear power plant. If the performance of the neutron absorption material fails to meet the neutron absorption requirements or is damaged, a chain nuclear fission reaction will be triggered, bringing great harm. Boron (B) element has a high thermal neutron capture cross-section and is considered an ideal neutron absorption material. In nature, most B elements exist in the form of B4C ceramics. However, it is difficult to directly prepare B4C ceramics into plates and the cost is very high. Moreover, the high hardness of B4C ceramics also leads to higher subsequent processing difficulty. Therefore, the B4C / Al composite material prepared by adding a high content of B4C ceramics to a soft aluminum alloy can meet the performance requirements of the service environment at the same time.

[0003] Currently, when adding a high content of ceramic particles to a metal matrix, the uniform distribution of ceramic particles is the key technical problem that needs to be solved first. Due to the large differences in physical and chemical properties such as density and thermal expansion coefficient between ceramic particles and the metal matrix, the use of liquid-phase forming technology cannot avoid the occurrence of phenomena such as floating and aggregation of ceramic particles. Moreover, due to the melting-solidification process, harmful reaction products generated at the heterogeneous interface of the ceramic / metal matrix are harmful to the improvement of the overall performance of the material. On the contrary, powder metallurgy solid-phase forming technology can achieve uniform particle distribution and reduction of harmful products at a temperature lower than the melting point of the matrix, and is considered an ideal forming technology. However, there are the following problems in the traditional rolling forming of high-content ceramic / metal composite billets into plates: 1) The physical and chemical properties between ceramic particles and the metal matrix are quite different, and it is difficult to achieve complete wetting at the heterogeneous interface of the ceramic / metal matrix, resulting in a low bonding quality at the heterogeneous interface and the existence of a certain number of micro-gaps; 2) The ceramic particles are hard, and mainly rotate and flow with the matrix during the rolling deformation process. It is difficult to achieve coordinated plastic deformation at the heterogeneous interface of the ceramic particle / metal matrix, and micro-gaps and micro-cracks will be further generated at the heterogeneous interface; 3) Even if a certain metallurgical bonding is achieved between the ceramic particles and the metal matrix, the micro-gaps caused by the differences in their physical and chemical properties still make it difficult to avoid the phenomenon of rolling cracking of the plate. Summary of the Invention

[0004] The present invention provides a high-content ceramic / metal composite material and a preparation method thereof for solving the above problems. During the process of rolling a blank of a traditional high-content ceramic / metal composite material into a plate, a high-frequency pulsed current is added for assisted rolling treatment. By utilizing the skin effect and proximity effect of the high-frequency pulsed current, the closure connection of the micro-gaps and micro-cracks at the heterogeneous interface between ceramic particles and the metal matrix is realized, and the electroplastic effect can significantly improve the coordinated plastic deformation ability of the heterogeneous interface between ceramic particles and the metal matrix; the situation of "external heat - internal cold" in traditional heat treatment is changed, so that the blank of the high-content ceramic / metal composite material is uniformly heated during the rolling process, and the problem of large difference in the healing of the heterogeneous junction surface is improved; in the case of rolling stress generated during rolling, the Ampere force generated by the magnetic field generated by the high-frequency pulsed current and the hot pressing stress act together on the micro-gaps on the surface of the high-content ceramic / metal composite material, promoting the healing of the micro-gaps on the surface of the high-content ceramic / metal composite material, and obtaining a high-content ceramic / metal composite material with relatively excellent comprehensive performance.

[0005] To achieve the above object, the present invention adopts the following technical solutions: The present invention provides a preparation method of a high-content ceramic / metal composite material, comprising the following steps: Step 1, select ceramic particles and aluminum alloy powder; Step 2, uniformly mix the selected ceramic particles and aluminum alloy powder, and perform drying and impurity removal treatment to obtain a mixed powder; Step 3, load the mixed powder into a graphite mold in a vacuum glove box, and perform pre-pressing treatment to obtain a powder block; Step 4, perform spark plasma sintering on the powder block to obtain a blank; Step 5, polish the blank to obtain a high-content ceramic / metal composite material specimen; Step 6, clamp the high-content ceramic / metal composite material specimen to a high-frequency pulsed current rolling test bench through a fixture, and deploy a thermocouple and an infrared thermal imager; Step 7, adjust the high-frequency pulsed current based on the temperature measurement results of the thermocouple and the infrared thermal imager, and perform high-frequency pulsed current rolling treatment; Step 8, polish the specimen after high-frequency pulsed current rolling treatment to obtain a high-content ceramic / metal composite material.

[0006] Further, in the step 1, the ceramic particles are boron carbide ceramic particles with a particle size of 5 - 8 µm; the aluminum alloy powder is 7075 aluminum alloy powder with a particle size of 5 - 25 µm; the purity of both the boron carbide ceramic particles and the 7075 aluminum alloy powder is ≥99.99%.

[0007] Further, in step 2, the selected ceramic particles and aluminum alloy powder are mixed evenly, specifically as follows: Put the selected ceramic particles and aluminum alloy powder into a stainless steel ball milling tank, and use a planetary ball mill to mix the powder. The mass ratio of ceramic particles to aluminum alloy powder is 2 - 5:95 - 98; the mass ratio of balls:materials:solvent is 5:1:1; zirconia balls are selected as the balls, anhydrous ethanol is used as the solvent, the ball milling speed is 150 - 300 rad / min, and the ball milling time is 10 - 12 hours, with 5 - 6 hours of forward rotation and 5 - 6 hours of reverse rotation; In step 2, the drying and impurity removal treatment is carried out in a vacuum drying oven. The drying temperature is 100 - 150 °C, and the drying time is 6 - 12 hours.

[0008] Further, in step 3, the pre - pressing treatment is carried out using a press, with a pressure of 40 - 60 MPa and a holding time of 3 - 5 min, so that the relative density of the mixed powder reaches more than 60%.

[0009] Further, in step 4, spark plasma sintering is carried out using an SPS sintering device. The pressure applied during sintering is 45 - 55 MPa, the sintering temperature is 500 - 600 °C, the heating rate is 20 - 30 °C / min, the graphite mold is insulated with carbon felt around it, and the insulation time is 5 - 10 min.

[0010] Further, in step 5, the grinding and polishing are specifically as follows: Sand the workpiece successively with sandpapers from 120# to 1500#, and then use an alcohol solution with a volume fraction of 75% to clean the surface of the ground blank.

[0011] Further, in step 6, the thermocouple and infrared thermal imager are deployed, specifically as follows: Lap the thermocouple on the surface of the high - content ceramic / metal composite material specimen to obtain the surface temperature, and use an infrared thermal imager to observe the overall temperature distribution of the high - content ceramic / metal composite material specimen.

[0012] Further, in step 7, the high - frequency pulsed current is adjusted based on the temperature measurement results of the thermocouple and infrared thermal imager, and high - frequency pulsed current rolling treatment is carried out, including: The pulse frequency of the high - frequency pulsed current is 10 kHz - 20 kHz, the pulse width is 25 - 45 ms, the reduction per pass of rolling is controlled, and it is rolled back and forth in the same direction for multiple times. The rolling speed is 10 - 15 mm / min, the temperature of the high - frequency pulsed current rolling treatment is 240 - 270 °C, and the specimen is rapidly water - cooled after the high - frequency pulsed current rolling treatment.

[0013] Further, in step 8, the grinding and polishing are specifically as follows: Polish successively with sandpapers numbered 120# to 1500#, and then use an alcohol solution with a volume fraction of 75% to clean the surface of the polished specimen.

[0014] The present invention also provides a high-content ceramic / metal composite material prepared by the preparation method of the high-content ceramic / metal composite material described above.

[0015] Compared with the prior art, the present invention has the following advantages: 1. For the high-content ceramic / metal composite material, the present invention innovatively proposes a new idea of using high-frequency pulsed current rolling to heal the micro-gaps at the heterogeneous interfaces of the composite material. Compared with the traditional hot rolling of "external heat - internal cold", it effectively improves the problem of uneven heating of the overall composite material and the poor connection quality of the ceramic / metal heterogeneous interfaces in different healing regions.

[0016] 2. The proximity effect of the high-frequency pulsed current is conducive to the wetting and spreading of the metal matrix on the ceramic particles when the current concentrates on flowing through the ceramic / metal heterogeneous interface, effectively improving the connection quality at the heterogeneous interface of the ceramic / metal.

[0017] 3. The present invention uses high-frequency pulsed current rolling treatment, which greatly enhances the healing effect of the micro-gaps at the ceramic / metal heterogeneous interface. The specific reasons are as follows: 1) The non-thermal effect of the high-frequency pulsed current can effectively improve the plastic deformation ability of the matrix, which is conducive to the high-quality bonding of the heterogeneous interface; 2) The rolling compressive stress effectively closes the micro-gaps at the heterogeneous interface; 3) The proximity effect of the high-frequency pulsed current generates an instantaneous high temperature, and a large thermal compressive stress will be generated at the interface, further promoting the closure of the micro-gaps at the interface. Description of the Drawings

[0018] Figure 1 It is a comparison diagram of the high-content ceramic / metal composite materials prepared in Example 1, Example 2, and Example 3.

[0019] Figure 2 It is a crack morphology diagram of the healing region of the high-content ceramic / metal composite material prepared in Example 1.

[0020] Figure 3 It is a crack morphology diagram of the healing region of the high-content ceramic / metal composite material prepared in Example 2.

[0021] Figure 4 It is a crack morphology diagram of the healing region of the high-content ceramic / metal composite material prepared in Example 3.

[0022] Figure 5 It is a columnar comparison diagram of the density and relative density of the high-content ceramic / metal composite materials prepared in Example 1, Example 2, and Example 3.

[0023] Figure 6 Bar chart for comparing the grain sizes of the high-content ceramic / metal composites prepared in Example 1, Example 2, and Example 3.

[0024] Figure 7 Microhardness comparison diagram of the high-content ceramic / metal composites prepared in Example 1, Example 2, and Example 3. Detailed implementation manners

[0025] In order to further elaborate on the technical solution of the present invention, the present invention will be further described below through examples. Example 1

[0026] A preparation method of a high-content ceramic / metal composite material. The high-content ceramic / metal composite material blank is prepared by spark plasma sintering method, and then hot rolling treatment is carried out without high-frequency pulse current treatment. The method includes the following steps: Step 1, select ceramic particles and aluminum alloy powder. The ceramic particles are boron carbide ceramic particles with a particle size of 5 µm; the aluminum alloy powder is 7075 aluminum alloy powder with a particle size of 15 µm; the purity of the boron carbide ceramic particles and 7075 aluminum alloy powder is ≥ 99.99%; Step 2, mix the selected ceramic particles and aluminum alloy powder evenly, and perform drying and impurity removal treatment to obtain mixed powder; Mixing the selected ceramic particles and aluminum alloy powder evenly specifically means: putting the selected ceramic particles and aluminum alloy powder into a stainless steel ball milling tank, using a planetary ball mill to mix the powder. The mass ratio of ceramic particles to aluminum alloy powder is 5:95; the mass ratio of balls:materials:solvent is 5:1:1; the balls are zirconia balls, the solvent is anhydrous ethanol, the ball milling speed is 200 rad / min, and the ball milling time is 10 hours, with 5 hours of forward rotation and 5 hours of reverse rotation; The drying and impurity removal treatment is carried out in a vacuum drying oven. The drying temperature is 120 °C and the drying time is 6 hours; Step 3, put the mixed powder into a graphite mold in a vacuum glove box. Graphite paper is padded on both the upper and lower parts of the graphite mold to seal and prevent the mixed powder from leaking and conduct electricity, and perform pre-pressing treatment to obtain a powder block; The pre-pressing treatment is carried out by a press, with a pressure of 50 MPa and a holding time of 4 min to make the density of the mixed powder reach more than 60%; Step 4, perform spark plasma sintering on the powder block to obtain a blank; The spark plasma sintering specifically is: the spark plasma sintering uses an SPS sintering device. The pressure applied during sintering is 50 MPa, the sintering temperature is 500 °C, the heating rate is 25 °C / min, the graphite mold is insulated with carbon felt around, and the insulation time is 7 min; Step 5: Grind and polish the blank. Sand it successively with sandpapers of 120# to 1500#, and then clean the surface of the ground blank with an alcohol solution with a volume fraction of 75% to obtain a high-content ceramic / metal composite material specimen. Step 6: Heat the high-content ceramic / metal composite material specimen to 310°C in a resistance furnace and perform hot rolling treatment on it. Control the reduction per pass of each rolling to be 3% (i.e., 0.15 mm), and roll back and forth 10 times in the same direction. The total reduction is 30%, and the thickness of the specimen is reduced by 1.5 mm. After the hot rolling treatment, perform rapid water cooling. Step 7: Grind and polish the high-content ceramic / metal composite material specimen after the hot rolling treatment. Sand it successively with sandpapers of 120# to 1500#, and then clean the surface of the ground specimen with an alcohol solution with a volume fraction of 75% to obtain a high-content ceramic / metal composite material. Example 2

[0027] A preparation method of a high-content ceramic / metal composite material. The high-content ceramic / metal composite material blank is prepared by spark plasma sintering method, and then hot rolling treatment is carried out first and high-frequency pulse current treatment is carried out later, including the following steps: Steps 1 to 6: The same as Example 1. Step 7: Clamp the high-content ceramic / metal composite material specimen after the hot rolling treatment to the high-frequency pulse current test bench through a fixture, and deploy a thermocouple and an infrared thermal imager. Specifically: The thermocouple uses a contact thermocouple, which is lapped on the surface of the high-content ceramic / metal composite material specimen to obtain the surface temperature (ensure good contact between the thermocouple and the specimen). The overall temperature distribution of the high-content ceramic / metal composite material specimen is observed by using an infrared thermal imager, which can ensure the uniform improvement of the performance of each part of the specimen after treatment. Step 8: Adjust the high-frequency pulse current based on the temperature measurement results of the thermocouple and the infrared thermal imager, and perform high-frequency pulse current treatment. Reasonable high-frequency pulse current treatment parameters are the premise for the healing of the micro-gap at the interface of the high-content ceramic / metal composite material specimen. Starting from the perspective of pulse energy, after optimization and adjustment, the pulse frequency of this high-frequency pulse current is 15 kHz, the pulse width is 30 ms, the temperature of the high-frequency pulse current treatment is 250°C, and after the high-frequency pulse current treatment, perform rapid water cooling. Step 9: Grind and polish the specimen after the high-frequency pulse current treatment. Sand it successively with sandpapers of 120# to 1500#, and then clean the surface of the ground specimen with an alcohol solution with a volume fraction of 75% to obtain a high-content ceramic / metal composite material. Example 3

[0028] A preparation method of a high-content ceramic / metal composite material. The high-content ceramic / metal composite material blank is prepared by spark plasma sintering method, and then high-frequency pulse current treatment and hot rolling treatment are carried out synchronously (i.e., high-frequency pulse current rolling treatment), including the following steps: Steps 1 to 5 are the same as those in Example 1; Step 6: Clamp the high-content ceramic / metal composite material specimen to the high-frequency pulse current rolling test bench through a fixture, and deploy a thermocouple and an infrared thermal imager; Specifically: The thermocouple uses a contact thermocouple, which is lapped on the surface of the high-content ceramic / metal composite material specimen to obtain the surface temperature (ensure good contact between the thermocouple and the specimen). The infrared thermal imager is used to observe the overall temperature distribution of the high-content ceramic / metal composite material specimen, which can ensure the uniform improvement of the performance of each part of the specimen after treatment; Step 7: Adjust the high-frequency pulse current based on the temperature measurement results of the thermocouple and the infrared thermal imager, and carry out high-frequency pulse current rolling treatment; Reasonable high-frequency pulse current treatment parameters and rolling treatment parameters are the premise for the healing of the interface micro-gap of the high-content ceramic / metal composite material specimen. Starting from the perspective of pulse energy, after optimization and adjustment, the pulse frequency of the high-frequency pulse current in this time is 15 kHz, the pulse width is 30 ms, the reduction per rolling is controlled at 3% (i.e., 0.15 mm), reciprocating rolling is carried out 10 times in the same direction, the total reduction is 30%, the thickness of the specimen is reduced by 1.5 mm, the rolling speed is 10 mm / min, the temperature of the high-frequency pulse current rolling treatment is 250 °C, and the specimen is rapidly water-cooled after the high-frequency pulse current rolling treatment; Step 8: Grind and polish the specimen after high-frequency pulse current rolling treatment, use sandpaper from 120# to 1500# to grind in sequence, and then clean the surface of the ground specimen with an alcohol solution with a volume fraction of 75% to obtain the high-content ceramic / metal composite material.

[0029] Figure 1 It is a comparison diagram of the high-content ceramic / metal composite materials prepared in Example 1, Example 2, and Example 3. It can be seen that there is no obvious difference in the high-content ceramic / metal composite materials prepared in the three examples, all of which are dark gray, and the overall shape is a regular oval.

[0030] Figures 2 to 4 They are respectively the crack morphology diagrams of the healing areas of the high-content ceramic / metal composite materials prepared in Example 1, Example 2, and Example 3. It can be seen that the internal micro-cracks in the healing areas of the high-content ceramic / metal composite materials prepared in the three examples become discontinuous, and there are multiple healing areas, among which the crack healing effect of Example 3 is better than that of Example 1 and 2.

[0031] Figure 5Column chart comparing the density and relative density of the high-content ceramic / metal composites prepared in Example 1, Example 2, and Example 3. It can be seen that the density of the high-content ceramic / metal composite prepared in Example 1 is 2.7189 g / cm 3 , and the relative density is 99.21%; the density of the high-content ceramic / metal composite prepared in Example 2 is 2.7034 g / cm 3 , and the relative density is 98.89%; the density of the high-content ceramic / metal composite prepared in Example 3 is 2.7213 g / cm 3 , and the relative density is 99.57%.

[0032] Figure 6 Column chart comparing the grain sizes of the high-content ceramic / metal composites prepared in Example 1, Example 2, and Example 3. It can be seen that for the high-content ceramic / metal composite prepared in Example 1, the proportion of grains with a size of 0 - 3 µm is 76.8%, the proportion of grains with a size of 3 - 6 µm is 20.1%, and the proportion of grains with a size greater than 6 µm is 3.1%, and the average grain size is 2.4717 µm; for the high-content ceramic / metal composite prepared in Example 2, the proportion of grains with a size of 0 - 3 µm is 78.5%, the proportion of grains with a size of 3 - 6 µm is 18.7%, and the proportion of grains with a size greater than 6 µm is 2.8%, and the average grain size is 2.3981 µm; for the high-content ceramic / metal composite prepared in Example 3, the proportion of grains with a size of 0 - 3 µm is 82.3%, the proportion of grains with a size of 3 - 6 µm is 15.8%, and the proportion of grains with a size greater than 6 µm is 1.9%, and the average grain size is 2.2875 µm.

[0033] Figure 7 Microhardness comparison chart of the high-content ceramic / metal composites prepared in Example 1, Example 2, and Example 3. It can be seen that the microhardness of the high-content ceramic / metal composite prepared in Example 1 is 1.453 GPa; the microhardness of the high-content ceramic / metal composite prepared in Example 2 is 1.486 GPa; the microhardness of the high-content ceramic / metal composite prepared in Example 3 is 1.513 GPa. Example 4

[0034] A preparation method of a high-content ceramic / metal composite. The high-content ceramic / metal composite blank is prepared by spark plasma sintering, and then high-frequency pulse current treatment and hot rolling treatment are carried out simultaneously (i.e., high-frequency pulse current rolling treatment), including the following steps: Step 1, select ceramic particles and aluminum alloy powder. The ceramic particles are boron carbide ceramic particles with a particle size of 8 µm; the aluminum alloy powder is 7075 aluminum alloy powder with a particle size of 25 µm; the purity of both the boron carbide ceramic particles and the 7075 aluminum alloy powder is ≥99.99%; Step 2: Mix the selected ceramic particles and aluminum alloy powder evenly, and then perform drying and impurity removal treatments to obtain mixed powder; Mixing the selected ceramic particles and aluminum alloy powder evenly specifically means: putting the selected ceramic particles and aluminum alloy powder into a stainless steel ball milling tank, and using a planetary ball mill to mix the powder. The mass ratio of ceramic particles to aluminum alloy powder is 2:98; the mass ratio of balls:materials:solvent is 5:1:1; zirconia balls are selected as the balls, anhydrous ethanol is used as the solvent, the ball milling speed is 300 rad / min, and the ball milling time is 12 hours, with 6 hours of forward rotation and 6 hours of reverse rotation; The drying and impurity removal treatments are carried out in a vacuum drying oven. The drying temperature is 150 °C and the drying time is 8 hours; Step 3: Load the mixed powder into a graphite mold inside a vacuum glove box. Graphite paper is placed on both the top and bottom of the graphite mold to seal and prevent the leakage of the mixed powder and conduct electricity, and then perform pre-pressing treatment to obtain a powder block; The pre-pressing treatment is carried out using a press. The pressure is 60 MPa and it is maintained for 3 min to make the relative density of the mixed powder reach more than 60%; Step 4: Perform spark plasma sintering on the powder block to obtain a blank; The spark plasma sintering specifically means: using an SPS sintering device for spark plasma sintering. The pressure applied during sintering is 55 MPa, the sintering temperature is 550 °C, the heating rate is 30 °C / min, and the graphite mold is insulated with carbon felt around it. The insulation time is 5 min; Step 5: Grind and polish the blank. Use sandpaper from 120# to 1500# to grind it in sequence, and then use an alcohol solution with a volume fraction of 75% to clean the surface of the ground blank to obtain a high-content ceramic / metal composite material specimen; Step 6: Clamp the high-content ceramic / metal composite material specimen to a high-frequency pulsed current rolling test bench through a fixture, and deploy a thermocouple and an infrared thermal imager; Specifically: a contact thermocouple is used as the thermocouple, which is lapped on the surface of the high-content ceramic / metal composite material specimen to obtain the surface temperature (ensuring good contact between the thermocouple and the specimen). An infrared thermal imager is used to observe the overall temperature distribution of the high-content ceramic / metal composite material specimen, which can ensure the uniform improvement of the performance of each part of the specimen after treatment; Step 7: Adjust the high-frequency pulsed current based on the temperature measurement results of the thermocouple and the infrared thermal imager, and perform high-frequency pulsed current rolling treatment; Reasonable high-frequency pulse current treatment parameters and rolling treatment parameters are the prerequisites for the interfacial micro-gap healing of high-content ceramic / metal composite specimens. From the perspective of pulse energy, after optimization and adjustment, the pulse frequency of the high-frequency pulse current in this experiment is 20 kHz, the pulse width is 25 ms, the reduction per rolling is controlled at 3% (i.e., 0.15 mm), rolling back and forth 10 times in the same direction, the total reduction is 30%, the thickness of the specimen is reduced by 1.5 mm, the rolling speed is 15 mm / min, the temperature of the high-frequency pulse current rolling treatment is 270 °C, and the specimen is rapidly water-cooled after the high-frequency pulse current rolling treatment; Step 8, polish the specimen after high-frequency pulse current rolling treatment, polish it successively with 120# to 1500# sandpaper, and then clean the surface of the polished specimen with an alcohol solution with a volume fraction of 75% to obtain a high-content ceramic / metal composite material. Example 5

[0035] A preparation method of a high-content ceramic / metal composite material, using spark plasma sintering to prepare a high-content ceramic / metal composite material blank, and then synchronously performing high-frequency pulse current treatment and hot rolling treatment (i.e., high-frequency pulse current rolling treatment), including the following steps: Step 1, select ceramic particles and aluminum alloy powder. The ceramic particles are boron carbide ceramic particles with a particle size of 6 µm; the aluminum alloy powder is 7075 aluminum alloy powder with a particle size of 5 µm; the purity of both the boron carbide ceramic particles and the 7075 aluminum alloy powder is ≥99.99%; Step 2, mix the selected ceramic particles and aluminum alloy powder evenly, and perform drying and impurity removal treatment to obtain a mixed powder; Mixing the selected ceramic particles and aluminum alloy powder evenly specifically means: putting the selected ceramic particles and aluminum alloy powder into a stainless steel ball milling tank, using a planetary ball mill for powder mixing, the mass ratio of ceramic particles to aluminum alloy powder is 4:96; the mass ratio of balls:materials:solvent is 5:1:1; the balls are zirconia balls, the solvent is anhydrous ethanol, the ball milling speed is 150 rad / min, and the ball milling time is 11 hours, with 5 hours of forward rotation and 6 hours of reverse rotation; The drying and impurity removal treatment is carried out in a vacuum drying oven, the drying temperature is 100 °C, and the drying time is 12 hours; Step 3, load the mixed powder into a graphite mold in a vacuum glove box, and pad graphite paper on both the upper and lower parts of the graphite mold to seal and prevent the mixed powder from leaking and conduct electricity, and perform pre-pressing treatment to obtain a powder block; The pre-pressing treatment is carried out using a press, the pressure is 40 MPa, and it is maintained for 5 min to make the density of the mixed powder reach more than 60%; Step 4, perform spark plasma sintering on the powder block to obtain a blank; The spark plasma sintering is specifically as follows: The SPS sintering equipment is used for spark plasma sintering. During sintering, the applied pressure is 45 MPa, the sintering temperature is 550 °C, the heating rate is 20 °C / min, the graphite mold is insulated with carbon felt around it, and the insulation time is 10 min; Step 5: Grind and polish the blank. Grind it successively with sandpapers from 120# to 1500#, and then clean the surface of the ground blank with an alcohol solution with a volume fraction of 75% to obtain a high-content ceramic / metal composite material specimen; Step 6: Clamp the high-content ceramic / metal composite material specimen to the high-frequency pulsed current rolling test bench through a fixture, and deploy the thermocouple and the infrared thermal imager; Specifically: A contact thermocouple is used. It is lapped on the surface of the high-content ceramic / metal composite material specimen to obtain the surface temperature (ensuring good contact between the thermocouple and the specimen). The infrared thermal imager is used to observe the overall temperature distribution of the high-content ceramic / metal composite material specimen, which can ensure the uniform improvement of the properties of each part of the specimen after treatment; Step 7: Adjust the high-frequency pulsed current based on the temperature measurement results of the thermocouple and the infrared thermal imager, and perform high-frequency pulsed current rolling treatment; Reasonable high-frequency pulsed current treatment parameters and rolling treatment parameters are the premise for the interface micro-gap healing of the high-content ceramic / metal composite material specimen. Starting from the perspective of pulse energy, after optimization and adjustment, the pulse frequency of the high-frequency pulsed current in this time is 10 kHz, the pulse width is 45 ms, the reduction per rolling is controlled to be 3% (i.e., 0.15 mm), reciprocally roll 10 times in the same direction, the total reduction is 30%, the thickness of the specimen is reduced by 1.5 mm, the rolling speed is 12 mm / min, the temperature of the high-frequency pulsed current rolling treatment is 240 °C, and the specimen is rapidly water-cooled after the high-frequency pulsed current rolling treatment; Step 8: Grind and polish the specimen after the high-frequency pulsed current rolling treatment. Grind it successively with sandpapers from 120# to 1500#, and then clean the surface of the ground specimen with an alcohol solution with a volume fraction of 75% to obtain the high-content ceramic / metal composite material.

[0036] The above shows and describes the main features and advantages of the present invention. For those skilled in the art, it is obvious that the present invention is not limited to the details of the above exemplary embodiments, and can be implemented in other specific forms without departing from the spirit or basic features of the present invention. Therefore, from any point of view, the embodiments should be regarded as exemplary and non-limiting. The scope of the present invention is defined by the appended claims rather than the above description. Therefore, it is intended to include all changes falling within the meaning and scope of the equivalent elements of the claims in the present invention.

[0037] In addition, it should be understood that although this specification is described according to embodiments, not every embodiment only contains an independent technical solution. This narrative way of the specification is only for clarity. Those skilled in the art should regard the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. A preparation method of a high-content ceramic / metal composite material, characterized in that, It includes the following steps: Step 1: Select ceramic particles and aluminum alloy powder; Step 2: Mix the selected ceramic particles and aluminum alloy powder evenly, and conduct drying and impurity removal treatment to obtain mixed powder; Step 3: Load the mixed powder into a graphite mold in a vacuum glove box and conduct pre-pressing treatment to obtain a powder block; Step 4: Conduct spark plasma sintering on the powder block to obtain a blank; Step 5: Grind and polish the blank to obtain a high-content ceramic / metal composite material specimen; Step 6: Clamp the high-content ceramic / metal composite material specimen to a high-frequency pulsed current rolling test bench through a fixture, and deploy a thermocouple and an infrared thermal imager; Step 7: Adjust the high-frequency pulsed current based on the temperature measurement results of the thermocouple and the infrared thermal imager, and conduct high-frequency pulsed current rolling treatment; Step 8: Grind and polish the specimen after high-frequency pulsed current rolling treatment to obtain a high-content ceramic / metal composite material.

2. The preparation method of a high-content ceramic / metal composite material according to claim 1, wherein In Step 1, boron carbide ceramic particles with a particle size of 5 - 8 µm are selected as the ceramic particles; 7075 aluminum alloy powder with a particle size of 5 - 25 µm is selected as the aluminum alloy powder; the purity of both the boron carbide ceramic particles and the 7075 aluminum alloy powder is ≥99.99%.

3. The preparation method of a high-content ceramic / metal composite material according to claim 1, characterized in that, In Step 2, mixing the selected ceramic particles and aluminum alloy powder evenly specifically includes: Put the selected ceramic particles and aluminum alloy powder into a stainless steel ball milling tank, and use a planetary ball mill to mix the powder. The mass ratio of ceramic particles to aluminum alloy powder is 2 - 5:95 - 98; the mass ratio of balls:materials:solvent is 5:1:1; zirconia balls are selected as the balls, anhydrous ethanol is used as the solvent, the ball milling speed is 150 - 300 rad / min, and the ball milling time is 10 - 12 hours, with 5 - 6 hours of forward rotation and 5 - 6 hours of reverse rotation; In Step 2, the drying and impurity removal treatment is carried out in a vacuum drying oven, the drying temperature is 100 - 150 °C, and the drying time is 6 - 12 hours.

4. The preparation method of a high-content ceramic / metal composite material according to claim 1, characterized in that, In Step 3, the pre-pressing treatment is carried out using a press, the pressure is 40 - 60 MPa, and it is maintained for 3 - 5 min to make the density of the mixed powder reach more than 60%.

5. The preparation method of a high-content ceramic / metal composite material according to claim 1, characterized in that, In Step 4, spark plasma sintering is carried out using an SPS sintering device. The pressure applied during sintering is 45 - 55 MPa, the sintering temperature is 500 - 600 °C, the heating rate is 20 - 30 °C / min, the graphite mold is insulated with carbon felt around it, and the insulation time is 5 - 10 min.

6. The preparation method of a high-content ceramic / metal composite material according to claim 1, characterized in that, In Step 5, grinding and polishing specifically includes: Use sandpaper from 120# to 1500# to grind in sequence, and then use an alcohol solution with a volume fraction of 75% to clean the surface of the ground blank.

7. The preparation method of a high-content ceramic / metal composite material according to claim 1, characterized in that, In Step 6, deploying the thermocouple and the infrared thermal imager specifically includes: Lap the thermocouple on the surface of the high-content ceramic / metal composite material specimen to obtain the surface temperature, and use an infrared thermal imager to observe the overall temperature distribution of the high-content ceramic / metal composite material specimen.

8. The preparation method of a high-content ceramic / metal composite material according to claim 1, characterized in that, In Step 7, adjusting the high-frequency pulsed current based on the temperature measurement results of the thermocouple and the infrared thermal imager, and conducting high-frequency pulsed current rolling treatment includes: The pulse frequency of the high-frequency pulsed current is 10 kHz to 20 kHz, the pulse width is 25 to 45 ms, the reduction per pass of rolling is controlled, and rolling is carried out reciprocally multiple times in the same direction. The rolling speed is 10 to 15 mm / min, the temperature of the high-frequency pulsed current rolling treatment is 240 to 270 °C, and the specimen is rapidly water-cooled after the high-frequency pulsed current rolling treatment is completed.

9. The preparation method of a high-content ceramic / metal composite material according to claim 1, characterized in that, In step 8, the grinding and polishing are specifically as follows: Sandpapers with grit sizes from 120# to 1500# are used for grinding in sequence, and then the surface of the ground specimen is cleaned with an alcohol solution with a volume fraction of 75%.

10. A high-content ceramic / metal composite material prepared by the method for preparing a high-content ceramic / metal composite material according to any one of claims 1 to 9.

Citation Information

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