CN118270789A - Recovery process of aluminum-based silicon carbide composite material - Google Patents
Recovery process of aluminum-based silicon carbide composite material Download PDFInfo
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 113
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
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- BYFGZMCJNACEKR-UHFFFAOYSA-N aluminium(i) oxide Chemical compound [Al]O[Al] BYFGZMCJNACEKR-UHFFFAOYSA-N 0.000 description 4
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Abstract
The application relates to the technical field of aluminum-based silicon carbide composite material recovery, in particular to an aluminum-based silicon carbide composite material recovery process. The recovery process of the aluminum-based silicon carbide composite material comprises the following steps: the method comprises the steps of firstly cleaning the surface of the recovered aluminum-based silicon carbide waste, then fully dissolving the recovered aluminum-based silicon carbide waste subjected to surface cleaning in acid liquor, performing ultrasonic dispersion treatment, performing reduced pressure filtration after the ultrasonic dispersion treatment is finished to obtain liquid-phase aluminum salt aqueous solution and solid-phase silicon carbide, and respectively performing water-based and compound cleaning liquid ultrasonic cleaning, water washing and vacuum drying treatment on the solid-phase silicon carbide to obtain the recovered silicon carbide powder with high purity. The method can fully recycle the silicon carbide, and the recycled silicon carbide meets the use requirement of the IGBT aluminum-based silicon carbide board, so that the production cost of the IGBT aluminum-based silicon carbide board can be effectively reduced, and the method is beneficial to the industrialized development of semiconductors.
Description
Technical Field
The application relates to the technical field of aluminum-based silicon carbide composite material recovery, in particular to an aluminum-based silicon carbide composite material recovery process.
Background
The aluminum-based silicon carbide composite material has the advantages of higher specific strength, wear resistance, low density, higher heat conductivity and the like, and is widely applied to important fields such as aerospace, automobile industry, consumer electronics and the like. The high-volume aluminum-based silicon carbide material is mainly used in the field of semiconductors, such as IGBT aluminum-based silicon carbide plates for semiconductors. The high-volume aluminum-based silicon carbide material has high purity and high content to silicon carbide filler, so that the production cost of the IGBT aluminum-based silicon carbide board is high, and the industrialized popularization of the IGBT aluminum-based silicon carbide board is not facilitated.
At present, the recycling of waste materials and defective products thereof generated in the processing process of the IGBT aluminum-based silicon carbide board is a great difficulty. The recovered IGBT aluminum-based silicon carbide waste is treated by adopting a conventional melting recovery process, and although part of aluminum and aluminum alloy materials thereof can be recovered, impurity components connected by chemical bonds are reserved on the surface of the recovered silicon carbide, so that the purity of the recovered silicon carbide is lower, and the recovered silicon carbide cannot be applied to the IGBT aluminum-based silicon carbide plate. Therefore, silicon carbide obtained by the melt recovery process is generally used for 3C digital electronic materials and automobile parts. In summary, the recovery process in the prior art cannot recover high-purity silicon carbide, so that the production cost of the IGBT aluminum-based silicon carbide board is high, and the industrial popularization of the IGBT aluminum-based silicon carbide board is not facilitated. Therefore, the application provides the recovery process of the aluminum-based silicon carbide composite material, silicon carbide can be fully recovered, the recovered silicon carbide meets the use requirement of the IGBT aluminum-based silicon carbide board, the production cost of the IGBT aluminum-based silicon carbide board can be effectively reduced, and the industrial development of semiconductors is facilitated.
Disclosure of Invention
In order to solve the technical problems, the application provides a recycling process of an aluminum-based silicon carbide composite material.
The application provides a recovery process of an aluminum-based silicon carbide composite material, which is realized by the following technical scheme:
the recovery process of the aluminum-based silicon carbide composite material comprises the following steps:
Recovering aluminum-based silicon carbide waste materials for surface cleaning, and removing organic matters and oxide impurities attached to the surfaces;
fully dissolving the aluminum-based silicon carbide waste subjected to surface cleaning in an acid solution, wherein the acid solution is 0.5-3.0mol/L nitric acid aqueous solution or 0.5-3mol/L hydrochloric acid aqueous solution or 0.5-3mol/L sulfuric acid aqueous solution, and fully and uniformly mixing to obtain a mixed solution;
Step three, performing ultrasonic dispersion treatment on the obtained mixed solution, wherein the ultrasonic frequency is 40-80kHz, the ultrasonic power is 800-2000W, and after ultrasonic treatment for 20-40min, the liquid phase aluminum salt aqueous solution and the solid phase silicon carbide can be separated by decompression and filtration;
Step four, washing the solid-phase silicon carbide in the step three by distilled water at least twice, uniformly mixing the solid-phase silicon carbide subjected to distilled water washing and the compound cleaning liquid according to the mass ratio of 1 (4-9), carrying out ultrasonic dispersion treatment for 15-30min, and then washing by distilled water at least twice, wherein the obtained solid-phase silicon carbide is subjected to vacuum drying treatment to obtain the recovered silicon carbide powder with high purity;
the compound cleaning liquid comprises an acidic nonionic surfactant and nitric acid;
Simultaneously, carrying out electrolytic impurity removal treatment on the liquid-phase aluminum salt aqueous solution, removing impurity metal salt in the liquid-phase aluminum salt aqueous solution, adding sodium hydroxide aqueous solution into the aluminum salt aqueous solution obtained after the electrolytic impurity removal treatment to fully precipitate aluminum ions in the aluminum salt aqueous solution, carrying out solid-liquid separation to obtain liquid-phase and solid-phase aluminum hydroxide, carrying out liquid-phase distillation to remove water to obtain sodium salt, drying the solid-phase aluminum hydroxide, grinding to obtain aluminum hydroxide powder, and carrying out calcination and ball milling treatment on the aluminum hydroxide powder to obtain aluminum oxide powder.
By adopting the technical scheme, the silicon carbide can be fully recovered, the recovered silicon carbide meets the use requirement of the IGBT aluminum-based silicon carbide plate, the production cost of the IGBT aluminum-based silicon carbide plate can be effectively reduced, and the semiconductor industrialization development is facilitated.
Preferably, the acid liquor in the second step is 1-2mol/L hydrochloric acid aqueous solution.
By adopting the technical scheme, sodium salt generated in the subsequent step four is convenient to recycle.
Preferably, in the second step, the aluminum-based silicon carbide waste after surface cleaning is crushed and screened to obtain 325-800 mesh screen discharge, the 325-800 mesh screen discharge is placed in acid liquor, the 325-800 mesh screen discharge is fully dissolved by stirring and mixing at 200-400rpm/min, then the acid liquor is continuously added dropwise under stirring at 200-400rpm/min to adjust the pH value to 3-5, and the mixed liquor is obtained.
By adopting the technical scheme, the recovery process efficiency of the aluminum-based silicon carbide composite material can be effectively improved.
Preferably, the obtained mixed solution is subjected to ultrasonic dispersion treatment with ultrasonic frequency of 60-80kHz and ultrasonic power of 1200-2000W for 30-40min, and then is subjected to reduced pressure filtration and separation to obtain liquid phase aluminum salt aqueous solution and solid phase silicon carbide.
By adopting the technical scheme, the surface cleanliness of the prepared solid-phase silicon carbide can be ensured.
Preferably, in the fourth step, distilled water is adopted to clean the solid-phase silicon carbide in the third step for three times, the solid-phase silicon carbide which is cleaned by distilled water and the compound cleaning liquid are uniformly mixed according to the mass ratio of 1 (7-9), the ultrasonic dispersion treatment is carried out for 30min, the ultrasonic frequency is 60-80kHz, the ultrasonic power is 1200-2000W, the distilled water is used for cleaning for three times after the ultrasonic cleaning is finished, the obtained solid-phase silicon carbide is subjected to vacuum drying treatment, the vacuum drying temperature is 100-120 ℃, the pressure is 0.01-0.1Pa, and the high-purity recovered silicon carbide powder is obtained after the vacuum drying is carried out for 6-8 hours.
Preferably, the compound cleaning liquid is mainly prepared from 3-8 parts of acidic nonionic surfactant, 1-8 parts of nitric acid and 80-100 parts of distilled water; the acidic nonionic surfactant is at least one of alkylphenol ethoxylate OP-10, peregal 0, fatty alcohol ether sulfate AES and alkylbenzene sulfonate LAS.
Preferably, the compound cleaning liquid is mainly prepared from 4 parts of acidic nonionic surfactant, 6 parts of nitric acid and 90 parts of distilled water.
By adopting the technical scheme, the recovered silicon carbide meets the use requirement of the IGBT aluminum-based silicon carbide board, can effectively reduce the production cost of the IGBT aluminum-based silicon carbide board, and is beneficial to the industrialized development of semiconductors.
Preferably, the electrolytic impurity removal treatment of the liquid-phase aluminum salt aqueous solution in the fourth step is specifically as follows: the anode material and the cathode material are graphite columns, liquid phase aluminum salt aqueous solution is used as electrolyte, electrons are obtained from the cathode graphite columns in the electrolysis process, impurity metals in the liquid phase aluminum salt aqueous solution are separated out and attached to the surfaces of the cathode graphite columns, electrons are lost from the anode graphite columns in the electrolysis process, and the anodic electrolysis reaction is as follows: 2H 2O-4e=4H++O2, electrolysis until bubbles are generated near the cathode graphite column, the cathode electrolysis reaction is as follows: and 2H 2O+2e=2OH-+H2, stopping electrolysis, and performing reduced pressure filtration treatment on the obtained electrolyte to obtain the aluminum salt aqueous solution after the electrolytic impurity removal treatment.
By adopting the technical scheme, the electrolytic precipitable impurity metal in the liquid-phase aluminum salt aqueous solution is effectively treated.
Preferably, the method further comprises a step five of carrying out surface chemical vapor deposition CVD treatment on the recovered silicon carbide powder with high purity obtained in the step four, wherein nano aluminum metal clusters are deposited on the surface of the recovered silicon carbide powder, and the method specifically comprises the following steps: the aluminum salt aqueous solution after the electrolytic impurity removal treatment and the high-purity recovered silicon carbide powder obtained in the step four are subjected to the magnetic stirring for 20-30min at 160-240rpm/min until aluminum ions in the aluminum salt aqueous solution are completely precipitated, then the magnetic stirring for 60-80min at 160-240rpm/min is continued, and the aluminum salt aqueous solution is kept stand for 20-24h to obtain Al (OH) 3/silicon carbide binary colloid, and the Al (OH) 3/silicon carbide binary colloid is subjected to washing for at least three times by distilled water and then subjected to vacuum suction filtration to obtain solid powder; placing the obtained solid powder in a vacuum drying oven, drying at 100-125 ℃ for 8-12h, then transferring into an atmosphere tube furnace for calcining treatment, heating to 550-680 ℃ at 5-20 ℃/min under air atmosphere, calcining for 3-5h to obtain Al2O 3/silicon carbide composite powder, then introducing hydrogen-argon mixed gas into the atmosphere tube furnace, wherein the volume ratio of hydrogen to argon is 1 (3-7), reducing at 550-680 ℃ for 3-5h, opening the furnace for natural cooling to room temperature, and finally performing planetary ball milling treatment to obtain the high-purity recovered silicon carbide powder with the particle diameter of 0.5-5 microns and the surface doped with nano aluminum metal clusters.
Preferably, the method further comprises a step five of carrying out surface doping modification treatment on the recovered silicon carbide powder with high purity obtained in the step four, wherein the surface doping modification treatment is specifically as follows: firstly, preparing a surface modified multi-wall carbon nano tube; then adding the surface modified multi-wall carbon nano tube and polyvinylpyrrolidone prepared in the first step into the prepared Ag (2E 4 MI) 2Ac complex solution, wherein the mass ratio of the surface modified multi-wall carbon nano tube to the polyvinylpyrrolidone is 1 (0.8-1.2), the mass ratio of the surface modified multi-wall carbon nano tube to the Ag (2E 4 MI) 2Ac complex solution is 1 (80-120), the content of the Ag (2E 4 MI) 2Ac complex in the Ag (2E 4 MI) 2Ac complex solution is 0.6-1.2wt%, and after ultrasonic dispersion for 2-6 hours, adding the obtained high-purity recycled silicon carbide powder into the fourth step, and continuously performing ultrasonic dispersion for 30-60min to obtain a dispersion liquid, wherein the mass ratio of the recycled silicon carbide powder to the surface modified multi-wall carbon nano tube is 1 (20-100); then, the obtained dispersion liquid is distilled under reduced pressure to remove the solid matters of the organic solution in the Ag (2E 4 MI) 2Ac complex solution; and (3) carrying out high-temperature sintering treatment on the obtained solid, sintering at 210-220 ℃ for 3-5 hours to obtain a blocky solid, and carrying out jet milling treatment on the obtained blocky solid to obtain the silicon carbide composite powder with the surface doped with the multiwall carbon nanotube.
By adopting the technical scheme, the interface compatibility of the silicon carbide subjected to surface modification and the aluminum substrate is relatively excellent, the compactness, the uniformity and the physical and chemical properties of the prepared IGBT aluminum-based silicon carbide plate are improved, the comprehensive product quality of the IGBT aluminum-based silicon carbide plate can be improved, and the development of semiconductor industrialization is facilitated.
In summary, the application has the following advantages:
1. the method can fully recycle the silicon carbide, and the recycled silicon carbide meets the use requirement of the IGBT aluminum-based silicon carbide board, so that the production cost of the IGBT aluminum-based silicon carbide board can be effectively reduced, and the method is beneficial to the industrialized development of semiconductors.
2. The recovery method is relatively simple, has lower embodiment difficulty, not only can effectively recover the high-purity silicon carbide material, but also can fully recover and recycle the aluminum and aluminum alloy materials in the IGBT aluminum-based silicon carbide waste.
3. According to the application, the surface modification treatment is carried out on the silicon carbide, the interface compatibility of the obtained surface doped modified silicon carbide and an aluminum substrate is relatively excellent, the compactness, the uniformity and the physical and chemical properties of the prepared IGBT aluminum-based silicon carbide plate are improved, the comprehensive product quality of the IGBT aluminum-based silicon carbide plate can be further improved, and the development of semiconductor industrialization is deduced.
Detailed Description
For a further understanding of the present invention, preferred embodiments of the present invention are described below in conjunction with examples and comparative examples.
Examples
The recovery process of the aluminum-based silicon carbide composite material comprises the following steps:
Recovering aluminum-based silicon carbide waste materials for surface cleaning, and removing organic matters and oxide impurities attached to the surfaces;
fully dissolving the aluminum-based silicon carbide waste subjected to surface cleaning in an acid solution, wherein the acid solution is 0.5-3.0mol/L nitric acid aqueous solution or 0.5-3mol/L hydrochloric acid aqueous solution or 0.5-3mol/L sulfuric acid aqueous solution, and fully and uniformly mixing to obtain a mixed solution;
Step three, performing ultrasonic dispersion treatment on the obtained mixed solution, wherein the ultrasonic frequency is 40-80kHz, the ultrasonic power is 800-2000W, and after ultrasonic treatment for 20-40min, the liquid phase aluminum salt aqueous solution and the solid phase silicon carbide can be separated by decompression and filtration;
Step four, washing the solid-phase silicon carbide in the step three by distilled water at least twice, uniformly mixing the solid-phase silicon carbide subjected to distilled water washing and the compound cleaning liquid according to the mass ratio of 1 (4-9), carrying out ultrasonic dispersion treatment for 15-30min, and then washing by distilled water at least twice, wherein the obtained solid-phase silicon carbide is subjected to vacuum drying treatment to obtain the recovered silicon carbide powder with high purity;
The compound cleaning liquid comprises an acidic nonionic surfactant and nitric acid;
Simultaneously, carrying out electrolytic impurity removal treatment on the liquid-phase aluminum salt aqueous solution, removing impurity metal salt in the liquid-phase aluminum salt aqueous solution, adding sodium hydroxide aqueous solution into the aluminum salt aqueous solution obtained after the electrolytic impurity removal treatment to fully precipitate aluminum ions in the aluminum salt aqueous solution, carrying out solid-liquid separation to obtain liquid-phase and solid-phase aluminum hydroxide, carrying out liquid-phase distillation to remove water to obtain sodium salt, drying the solid-phase aluminum hydroxide, grinding to obtain aluminum hydroxide powder, and carrying out calcination and ball milling treatment on the aluminum hydroxide powder to obtain aluminum oxide powder.
Preferably, the acid solution in the second step is 1-2mol/L hydrochloric acid aqueous solution.
Preferably, in the second step, firstly crushing and screening the aluminum-based silicon carbide waste with the surface cleaned to obtain 325-800-mesh screen discharge, placing the 325-800-mesh screen discharge into acid liquor, stirring and mixing at 200-400rpm/min to enable the 325-800-mesh screen discharge to be fully dissolved, and then continuously stirring at 200-400rpm/min, dropwise adding acid liquor to adjust the pH value to 3-5, thus obtaining the mixed liquor.
Preferably, in the third step, the obtained mixed solution is subjected to ultrasonic dispersion treatment, the ultrasonic frequency is 60-80kHz, the ultrasonic power is 1200-2000W, after ultrasonic treatment is carried out for 30-40min, the liquid phase aluminum salt aqueous solution and the solid phase silicon carbide can be separated by decompression and filtration.
Preferably, step four, washing the solid phase silicon carbide in step three by distilled water for three times, uniformly mixing the solid phase silicon carbide subjected to distilled water washing and the compound cleaning liquid according to the mass ratio of 1 (7-9), performing ultrasonic dispersion treatment for 30min, performing ultrasonic frequency of 60-80kHz, performing ultrasonic power of 1200-2000W, washing the solid phase silicon carbide three times by distilled water after the ultrasonic washing is finished, performing vacuum drying treatment on the obtained solid phase silicon carbide, performing vacuum drying at the temperature of 100-120 ℃ and the pressure of 0.01-0.1Pa, and performing vacuum drying for 6-8 hours to obtain the high-purity recovered silicon carbide powder.
Preferably, the compound cleaning liquid is mainly prepared from 3-8 parts of acidic nonionic surfactant, 1-8 parts of nitric acid and 80-100 parts of distilled water; the acidic nonionic surfactant is at least one of alkylphenol ethoxylate OP-10, peregal 0, fatty alcohol ether sulfate AES and alkylbenzene sulfonate LAS. Further preferably, the compound cleaning liquid is mainly prepared from 4 parts of acidic nonionic surfactant, 6 parts of nitric acid and 90 parts of distilled water.
Preferably, the electrolytic impurity removal treatment of the liquid-phase aluminum salt aqueous solution in the fourth step is specifically as follows: the anode material and the cathode material are graphite columns, liquid phase aluminum salt aqueous solution is used as electrolyte, electrons are obtained from the cathode graphite columns in the electrolysis process, impurity metals in the liquid phase aluminum salt aqueous solution are separated out and attached to the surfaces of the cathode graphite columns, electrons are lost from the anode graphite columns in the electrolysis process, and the anodic electrolysis reaction is as follows: 2H 2O-4e=4h++ O2, electrolysis until bubbles are generated near the cathode graphite column, the cathode electrolysis reaction is as follows: stopping electrolysis if 2H2O+2e=2OH- +H2, and performing reduced pressure filtration treatment on the obtained electrolyte to obtain the aluminum salt aqueous solution after the electrolytic impurity removal treatment.
In order to obtain silicon carbide with relatively good interface compatibility with aluminum matrix, the recovered silicon carbide powder with high purity obtained in the step four is subjected to surface chemical vapor deposition CVD treatment, and nano aluminum metal clusters are deposited on the surface of the recovered silicon carbide powder, and the method specifically comprises the following steps: the aluminum salt aqueous solution after the electrolytic impurity removal treatment and the high-purity recovered silicon carbide powder obtained in the step four are subjected to the step four, wherein the mass of aluminum ions in the aluminum salt aqueous solution is equal to 0.05-0.20 times of the mass of the recovered silicon carbide powder, the magnetic stirring is carried out for 20-30min at 160-240rpm/min, then sodium hydroxide aqueous solution with the concentration of 4-8wt% is added until the aluminum ions in the aluminum salt aqueous solution are completely precipitated, then the magnetic stirring is carried out for 60-80min at 160-240rpm/min continuously, the mixture is kept stand for 20-24h, and then Al (OH) 3/silicon carbide binary colloid can be obtained, the Al (OH) 3/silicon carbide binary colloid is washed for at least three times by distilled water, and then the vacuum suction filtration is carried out to obtain solid powder; placing the obtained solid powder in a vacuum drying oven, drying at 100-125 ℃ for 8-12h, then transferring into an atmosphere tube furnace for calcining treatment, heating to 550-680 ℃ at 5-20 ℃/min under air atmosphere, calcining for 3-5h to obtain Al2O 3/silicon carbide composite powder, then introducing hydrogen-argon mixed gas into the atmosphere tube furnace, wherein the volume ratio of hydrogen to argon is 1 (3-7), reducing at 550-680 ℃ for 3-5h, opening the furnace for natural cooling to room temperature, and finally performing planetary ball milling treatment to obtain the high-purity recovered silicon carbide powder with the particle diameter of 0.5-5 microns and the surface doped with nano aluminum metal clusters.
In order to obtain silicon carbide with relatively good interface compatibility with an aluminum matrix, the recovered silicon carbide powder with high purity obtained in the fourth step can be subjected to surface doping modification treatment, and the method specifically comprises the following steps: firstly, preparing a surface modified multi-wall carbon nano tube; then adding the surface modified multi-wall carbon nano tube and polyvinylpyrrolidone prepared in the first step into the prepared Ag (2E 4 MI) 2Ac complex solution, wherein the mass ratio of the surface modified multi-wall carbon nano tube to the polyvinylpyrrolidone is1 (0.8-1.2), the mass ratio of the surface modified multi-wall carbon nano tube to the Ag (2E 4 MI) 2Ac complex solution is1 (80-120), the content of the Ag (2E 4 MI) 2Ac complex in the Ag (2E 4 MI) 2Ac complex solution is 0.6-1.2wt%, and after ultrasonic dispersion for 2-6 hours, adding the obtained high-purity recycled silicon carbide powder into the fourth step, and continuously performing ultrasonic dispersion for 30-60min to obtain a dispersion liquid, wherein the mass ratio of the recycled silicon carbide powder to the surface modified multi-wall carbon nano tube is1 (20-100); then, the obtained dispersion liquid is distilled under reduced pressure to remove the solid matters of the organic solution in the Ag (2E 4 MI) 2Ac complex solution; and (3) carrying out high-temperature sintering treatment on the obtained solid, sintering at 210-220 ℃ for 3-5 hours to obtain a blocky solid, and carrying out jet milling treatment on the obtained blocky solid to obtain the silicon carbide composite powder with the surface doped with the multiwall carbon nanotube.
Example 1: the recovery process of the aluminum-based silicon carbide composite material comprises the following steps:
Firstly, selecting waste materials generated in the processing process of IGBT aluminum-based silicon carbide plates and defective IGBT aluminum-based silicon carbide plates as recovered aluminum-based silicon carbide waste materials, carrying out recovery treatment, wherein the delivery calibration content of silicon carbide in the recovered aluminum-based silicon carbide waste materials is 60.4wt%, the balance is 6063 aluminum alloy, carrying out surface cleaning on the recovered aluminum-based silicon carbide waste materials, adopting an acetone aqueous solution with the concentration of 10wt% to soak the recovered aluminum-based silicon carbide waste materials for 5min, taking out deionized water, washing 2 times, soaking in a nonionic surfactant aqueous solution with the pH value of 4.8-5 (1 part of alkylphenol ethoxylate OP-10, 1 part of peregal 0 and 20 parts of deionized water are uniformly mixed, then dropwise adding 1mol/L hydrochloric acid aqueous solution, and adjusting the pH value of a system to be 4.8-5 to prepare a nonionic surfactant aqueous solution), and removing organic matters and oxide impurities attached to the surface of the recovered aluminum-based silicon carbide waste materials;
Fully dissolving the recovered aluminum-based silicon carbide waste subjected to surface cleaning in 2mol/L hydrochloric acid aqueous solution, wherein 1kg of recovered aluminum-based silicon carbide waste adopts 22.2kg of 2mol/L hydrochloric acid aqueous solution, and mechanically stirring for 2 hours at 240rpm/min externally, so that the recovered aluminum-based silicon carbide waste can be fully dissolved, and a mixed solution is obtained;
Step three, performing ultrasonic dispersion treatment on the obtained mixed solution, wherein the ultrasonic frequency is 75kHz, the ultrasonic power is 1600W, and after 30 minutes of ultrasonic treatment, performing reduced pressure filtration by adopting an ultrafiltration membrane to obtain a liquid phase aluminum salt aqueous solution and solid phase silicon carbide;
Meanwhile, preparing a compound cleaning solution, namely stirring and mixing 1 part of OP-10, 1 part of peregal 0, 2 parts of fatty alcohol ether sulfate AES, 6 parts of nitric acid and 90 parts of distilled water for 10 minutes at a rotating speed of 200rpm/min to prepare the compound cleaning solution;
Step four, washing the solid-phase silicon carbide in the step three by distilled water for three times, uniformly mixing the solid-phase silicon carbide subjected to distilled water washing with the compound cleaning liquid prepared in the step three according to the mass ratio of 1:4, carrying out ultrasonic dispersion treatment for 20min, carrying out ultrasonic frequency of 75kHz, carrying out ultrasonic power of 1600W, carrying out ultrasonic washing for three times by using distilled water after the ultrasonic washing is finished, carrying out vacuum drying treatment on the obtained solid-phase silicon carbide, setting the vacuum drying temperature to 120 ℃, setting the pressure to 0.1Pa, and carrying out vacuum drying for 8h to obtain high-purity recovered silicon carbide powder;
Simultaneously, carrying out electrolytic impurity removal treatment on the liquid phase aluminum salt aqueous solution obtained in the step three, wherein the electrolytic impurity removal treatment is specifically as follows: the anode material and the cathode material are graphite columns, liquid phase aluminum salt aqueous solution is used as electrolyte, electrons are obtained from the cathode graphite columns in the electrolysis process, impurity metals in the liquid phase aluminum salt aqueous solution are separated out and attached to the surfaces of the cathode graphite columns, electrons are lost from the anode graphite columns in the electrolysis process, and the anodic electrolysis reaction is as follows: 2H 2O-4e=4H++O2, electrolysis until bubbles are generated near the cathode graphite column, the cathode electrolysis reaction is as follows: 2H 2O+2e=2OH-+H2, stopping electrolysis, performing reduced pressure filtration treatment on the obtained electrolyte to obtain aluminum salt water solution after the electrolytic impurity removal treatment, adding 2mol/L sodium hydroxide water solution into the aluminum salt water solution after the electrolytic impurity removal treatment to enable aluminum ions in the aluminum salt water solution to be fully precipitated, performing solid-liquid separation treatment at a system pH value of 7-7.1, performing reduced pressure filtration by using an ultrafiltration membrane to obtain liquid phase and solid phase aluminum hydroxide, heating the obtained liquid phase to 100 ℃ to remove distillation to obtain sodium salt, drying the solid phase aluminum hydroxide at 80 ℃ for 6 hours, grinding to obtain aluminum hydroxide powder of 300-800 meshes, and performing calcination and ball milling treatment on the obtained aluminum hydroxide powder to obtain aluminum oxide powder of 325-2000 meshes.
Example 2 differs from example 1 in that: crushing and screening the aluminum-based silicon carbide waste subjected to surface cleaning to obtain 325-mesh sieve discharge, adopting 22kg of 2mol/L hydrochloric acid aqueous solution for 1kg of recovered aluminum-based silicon carbide waste, placing the 325-mesh sieve discharge into the 2mol/L hydrochloric acid aqueous solution, stirring and mixing for 1h at 240rpm/min to fully dissolve the 325-mesh sieve discharge, continuing to deliver the 2mol/L hydrochloric acid aqueous solution under 240rpm/min stirring, and adjusting the pH value of the system to 3-3.2 to obtain the mixed solution.
Example 3 differs from example 1 in that: crushing and screening the aluminum-based silicon carbide waste subjected to surface cleaning to obtain 800-mesh sieve discharge, adopting 22kg of 2mol/L hydrochloric acid aqueous solution for 1kg of recovered aluminum-based silicon carbide waste, placing the 800-mesh sieve discharge into the 2mol/L hydrochloric acid aqueous solution, stirring and mixing for 40min at 240rpm/min to fully dissolve the 800-mesh sieve discharge, continuing delivering the 2mol/L hydrochloric acid aqueous solution under stirring at 240rpm/min, and adjusting the pH value of the system to 3-3.2 to obtain the mixed solution.
Example 4 differs from example 1 in that: and step four, washing the solid-phase silicon carbide in the step three by distilled water for three times, uniformly mixing the solid-phase silicon carbide subjected to distilled water washing with the compound cleaning liquid prepared in the step three according to the mass ratio of 1:7, performing ultrasonic dispersion treatment for 30min, performing ultrasonic frequency of 75kHz, performing ultrasonic power of 1600W, performing ultrasonic washing with distilled water for three times after the completion of ultrasonic washing, performing vacuum drying treatment on the obtained solid-phase silicon carbide, performing vacuum drying at 120 ℃, setting the pressure of 0.1Pa, and performing vacuum drying for 8 hours to obtain the high-purity recovered silicon carbide powder.
Example 5 differs from example 1 in that: the preparation method of the aluminum-based silicon carbide composite material recovery process further comprises a step five of carrying out surface chemical vapor deposition CVD treatment on the recovered silicon carbide powder with high purity obtained in the step four, wherein nano aluminum metal clusters are deposited on the surface of the recovered silicon carbide powder, and the preparation method specifically comprises the following steps: the aluminum salt aqueous solution after the electrolytic impurity removal treatment and the high-purity recovered silicon carbide powder obtained in the fourth step are subjected to the fourth step, wherein the mass of aluminum ions in the aluminum salt aqueous solution is equal to 0.08 times that of the recovered silicon carbide powder, the magnetic stirring is carried out for 30min at 240rpm/min, then the sodium hydroxide aqueous solution with the concentration of 5wt% is added until the aluminum ions in the aluminum salt aqueous solution are completely precipitated, then the magnetic stirring is carried out for 80min at 240rpm/min continuously, the Al (OH) 3/silicon carbide binary colloid is obtained after standing for 24h, the Al (OH) 3/silicon carbide binary colloid is washed for three times by distilled water, and then the solid powder is obtained through the vacuum suction filtration; the obtained solid powder is placed in a vacuum drying oven to be dried for 10 hours at 120 ℃, then the solid powder is transferred to an atmosphere tube furnace to be calcined, the temperature is raised to 600 ℃ at 20 ℃/min under the air atmosphere to be calcined for 4 hours to obtain Al 2O3/silicon carbide composite powder, then hydrogen-argon mixed gas is introduced into the atmosphere tube furnace, the volume ratio of hydrogen to argon in the hydrogen-argon mixed gas is 1:4, the temperature is maintained at 600 ℃ to be subjected to reduction reaction for 4 hours, the solid powder is opened to be naturally cooled to the room temperature, finally, the solid powder is subjected to planetary ball milling treatment, zirconium oxide is taken as a grinding ball, and ball milling is carried out for 30 minutes at the rotating speed of 60rpm/min to obtain the recovered silicon carbide powder with high purity of the surface doped nano aluminum metal clusters with the particle size of D 50 =5.0 microns.
Example 6 differs from example 5 in that: the mass of aluminum ions in the aluminum salt aqueous solution is equal to 0.16 times of the mass of the recovered silicon carbide powder.
Example 7 differs from example 1 in that: the preparation method of the aluminum-based silicon carbide composite material recovery process further comprises a fifth step of carrying out surface doping modification treatment on the recovered silicon carbide powder with high purity obtained in the fourth step, wherein the surface doping modification treatment comprises the following steps of:
S5.1, preparing the surface modified multi-wall carbon nano tube: dispersing 1g of amination multiwall carbon nanotube (Jiangsu Xianfeng nano materials science and technology Co., ltd., diameter: 8-15nm; inner diameter: 3-5nm; length: 50um; purity: 95%, color: black; amino content: 0.45wt%; SSA: 233m 2/g) in 500g of distilled water; 1.5g KOH was dissolved in 250g distilled water to prepare a KOH solution; mixing the multiwall carbon nanotube dispersion liquid with KOH solution, and then stirring at 80 ℃ and drying to obtain multiwall carbon nanotube/KOH powder with surface alkali treatment; placing the obtained multi-wall carbon nano tube/KOH powder into a crucible A, placing 5.0g of aluminum chloride into a crucible B, loading the crucible A into a downstream region of a tube furnace, loading the crucible B into an upstream region of the tube furnace, sealing the tube furnace, heating the upstream region of the tube furnace to 500 ℃ from room temperature at a heating rate of 10 ℃/min for 60min under argon atmosphere, and heating the downstream region of the tube furnace to 600 ℃ from room temperature at a heating rate of 12 ℃/min for 60min to obtain a metal monoatomic doped multi-wall carbon nano tube precursor; adding a metal monoatomic doped multiwall carbon nanotube precursor into dilute hydrochloric acid with the concentration of 1.0mol/L, stirring, vacuum filtering, washing with distilled water, and drying to obtain a monoatomic aluminum doped multiwall carbon nanotube;
Meanwhile, preparing Ag (2E 4 MI) 2 Ac complex solution, adding 2.2g of 2-ethyl-4-methylimidazole 2E4MI and 1.67g of silver acetate AgAc into 530g of dichloromethane at room temperature, and magnetically stirring at 200rpm for 120min to obtain clear and transparent Ag (2E 4 MI) 2 Ac complex solution;
S5.2, adding 5.0g of the surface modified multi-wall carbon nano tube and 5.0g of polyvinylpyrrolidone prepared in the first step into the Ag (2E 4 MI) 2 Ac complex solution, performing ultrasonic dispersion treatment for 5.0h, wherein the ultrasonic frequency is 44kHz, the ultrasonic power is 1200W, adding 40g of superfine silicon carbide powder (alpha superfine high-purity nano silicon carbide powder with the average particle size of 1-3 microns, which is customized by Ningbo Bei Gaer new material Co., ltd., CAS:409-21-2, the density of 3.25 g/cm), continuing ultrasonic dispersion for 60min, and the ultrasonic frequency is 44kHz and the ultrasonic power is 1200W, thereby obtaining a dispersion;
S5.3, distilling the obtained dispersion liquid under reduced pressure to remove dichloromethane to obtain a solid, performing high-temperature sintering treatment on the obtained solid, sintering at 215 ℃ for 5 hours to obtain a blocky solid, and performing jet milling treatment on the blocky solid to obtain the surface aluminum nanocluster modified silicon carbide powder with the average particle size of 1-8 mu m.
Example 8 differs from example 7 in that: s5.2, adding 5.0g of the surface modified multi-wall carbon nano tube and 5.0g of polyvinylpyrrolidone prepared in the first step into the Ag (2E 4 MI) 2Ac complex solution, performing ultrasonic dispersion treatment for 5.0h, wherein the ultrasonic frequency is 44kHz, the ultrasonic power is 1200W, and adding 60g of superfine silicon carbide powder (alpha superfine high-purity nano silicon carbide powder with the average particle size of 1-3 microns, which is manufactured by Ningbo Bei Gaer New material Co., ltd., CAS:409-21-2, the density of 3.25 g/cm), continuing ultrasonic dispersion for 60min, and the ultrasonic frequency is 44kHz, the ultrasonic power is 1200W, thereby obtaining a dispersion liquid.
Comparative example
Comparative example 1 differs from example 1 in that: and step four, washing the solid-phase silicon carbide in the step three by distilled water for three times, uniformly mixing the solid-phase silicon carbide subjected to distilled water washing with the compound cleaning liquid prepared in the step three according to the mass ratio of 1:15, performing ultrasonic dispersion treatment for 30min, performing ultrasonic frequency of 75kHz, performing ultrasonic power of 1600W, performing ultrasonic washing with distilled water for three times after the completion of ultrasonic washing, performing vacuum drying treatment on the obtained solid-phase silicon carbide, performing vacuum drying at 120 ℃, setting the pressure of 0.1Pa, and performing vacuum drying for 8 hours to obtain the high-purity recovered silicon carbide powder.
Comparative example 2 differs from example 1 in that: the preparation method of the compound cleaning liquid in the fourth step comprises the following steps: 1 part of OP-10, 1 part of peregal 0, 2 parts of fatty alcohol ether sulfate AES and 96 parts of distilled water are stirred and mixed for 10min at the rotating speed of 200rpm/min to prepare the compound cleaning liquid.
Comparative example 3 differs from example 1 in that: the preparation method of the compound cleaning liquid in the fourth step comprises the following steps: 6 parts of nitric acid and 94 parts of distilled water are stirred and mixed for 10 minutes at the rotating speed of 200rpm/min, and then the compound cleaning liquid is prepared.
Comparative example 4 differs from example 1 in that: in the recovery process of the aluminum-based silicon carbide composite material, the first treatment is carried out, and the second treatment is directly carried out.
Comparative example 5 differs from example 1 in that: the recovery process of the aluminum-based silicon carbide composite material comprises the following steps: step one, selecting waste materials generated in the processing process of IGBT aluminum-based silicon carbide plates and defective IGBT aluminum-based silicon carbide plates as recovered aluminum-based silicon carbide waste materials to be recovered, wherein the recovered aluminum-based silicon carbide waste materials have a factory calibration content of 60.4wt% of silicon carbide, the balance is 6063 aluminum alloy, carrying out surface cleaning on the recovered aluminum-based silicon carbide waste materials, soaking the recovered aluminum-based silicon carbide waste materials for 5min by adopting an acetone aqueous solution with the concentration of 10wt%, taking out deionized water, washing 2 times, soaking in a nonionic surfactant aqueous solution (1 part of alkylphenol ethoxylate OP-10, 1 part of peregal 0 and 20 parts of deionized water, uniformly mixing, then dropwise adding a 1mol/L hydrochloric acid aqueous solution, and adjusting the pH value of a system to be 4.8-5 to prepare a nonionic surfactant aqueous solution) to remove organic matters and oxide impurities attached to the surface of the recovered aluminum-based silicon carbide waste materials; heating the recovered aluminum-based silicon carbide waste obtained in the first step to 720 ℃, melting the recovered aluminum-based silicon carbide waste to obtain a fluid alloy liquid, and carrying out solid-liquid separation treatment on the obtained fluid alloy liquid to obtain a liquid alloy liquid and solid silicon carbide powder; and thirdly, grinding the solid silicon carbide powder to obtain the finished product recovered silicon carbide powder with the particle size of 10-35 microns.
Comparative example 6 was ultrafine silicon carbide powder (alpha ultrafine high-purity nano silicon carbide powder with an average particle size of 1-3 μm, CAS:409-21-2, density 3.25g/cm, manufactured by Ningbo Bei Gaer New Material Co., ltd.), i.e. a new material.
Performance test
The test samples of the IGBT aluminum-based silicon carbide board were prepared as follows: step one, weighing 60 parts of the silicon carbide powder recovered in examples 1-8 and comparative examples 1-5, respectively mixing with 40 parts of 6063 aluminum alloy powder (average grain size 30-53 mu m manufactured by Beijing optical focusing win-win technology Co., ltd.) uniformly, and performing ball milling for 1h at 200rpm/min to obtain mixed alloy powder; step two, placing the mixed alloy powder in the step one into a forming die for cold isostatic pressing forming, wherein the forming temperature is room temperature, the actual measured temperature is 22.3 ℃, and the forming pressure is as follows: pressurizing to 100MPa with 20MPa/s, maintaining the pressure for 10s, pressurizing to 200MPa with 10 MPa/s, maintaining the pressure for 20s, pressurizing to 300MPa with 5MPa/s, maintaining the pressure for 20s, pressurizing to 400MPa with 2MPa/s, maintaining the pressure for 30s, pressurizing to 500MPa with 1MPa/s, maintaining the pressure for 30s, then reducing the pressure to 200MPa with 5MPa/s, maintaining the pressure for 30s, reducing the pressure to 0MPa with 20MPa/s, and forming the finished product at a speed of 4mm/s to obtain the prefabricated plate; step three, performing rapid sintering treatment on the obtained finished prefabricated plate under the protection of nitrogen, heating up to 680 ℃ at the sintering heating rate of 200 ℃/min, preserving heat for 2.0h, cooling down to 540 ℃ at the speed of 10 ℃/min, preserving heat for 120min, and naturally cooling down to room temperature after opening a furnace, thus obtaining a semi-finished product; step four, quenching and aging treatment are carried out on the semi-finished product, and quenching parameters are as follows: heating to 480+/-0.5 ℃ at 25 ℃ per minute, preserving heat for 45min, quenching with water to room temperature, repeating the quenching operation for three times, and carrying out aging treatment, wherein the aging treatment parameters are as follows: heating to 185 ℃ at 20 ℃/min, preserving heat for 3 hours, opening a furnace, naturally cooling to room temperature, polishing burrs, and obtaining test samples 1-8 and comparison samples 1-5 of the finished IGBT aluminum-based silicon carbide board.
1. The elongation and elastic modulus were measured by using a universal tensile tester of HH11013YZUFY according to GB/T228.1-2010. 2. The heat conductivity coefficient performance is measured according to GB/T3651-2008-metal high temperature heat conductivity coefficient. 3. The density test was determined by volumetric methods. 4. The expansion coefficient is according to GB/T1039-2019 test method for thermal expansion coefficient of aluminum and aluminum alloy. 5. Flexural strength was measured according to GB/T232-2010.
TABLE 1 test parameter tables for IGBT aluminum-based silicon carbide boards made of recovered silicon carbide powder in examples 1-8 and comparative examples 1-5
In summary, the recovery process provided by the application can fully recover silicon carbide, and the recovered silicon carbide meets the use requirement of the IGBT aluminum-based silicon carbide board, so that the production cost of the IGBT aluminum-based silicon carbide board can be effectively reduced, and the semiconductor industrialization development is facilitated.
The present embodiment is only for explanation of the present application and is not to be construed as limiting the present application, and modifications to the present embodiment, which may not creatively contribute to the present application as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present application.
Claims (10)
1. A recycling process of an aluminum-based silicon carbide composite material is characterized by comprising the following steps of: the method comprises the following steps:
Recovering aluminum-based silicon carbide waste materials for surface cleaning, and removing organic matters and oxide impurities attached to the surfaces;
fully dissolving the aluminum-based silicon carbide waste subjected to surface cleaning in an acid solution, wherein the acid solution is 0.5-3.0mol/L nitric acid aqueous solution or 0.5-3mol/L hydrochloric acid aqueous solution or 0.5-3mol/L sulfuric acid aqueous solution, and fully and uniformly mixing to obtain a mixed solution;
Step three, performing ultrasonic dispersion treatment on the obtained mixed solution, wherein the ultrasonic frequency is 40-80kHz, the ultrasonic power is 800-2000W, and after ultrasonic treatment for 20-40min, the liquid phase aluminum salt aqueous solution and the solid phase silicon carbide can be separated by decompression and filtration;
Step four, washing the solid-phase silicon carbide in the step three by distilled water at least twice, uniformly mixing the solid-phase silicon carbide subjected to distilled water washing and the compound cleaning liquid according to the mass ratio of 1 (4-9), carrying out ultrasonic dispersion treatment for 15-30min, and then washing by distilled water at least twice, wherein the obtained solid-phase silicon carbide is subjected to vacuum drying treatment to obtain the recovered silicon carbide powder with high purity;
the compound cleaning liquid comprises an acidic nonionic surfactant and nitric acid;
Simultaneously, carrying out electrolytic impurity removal treatment on the liquid-phase aluminum salt aqueous solution, removing impurity metal salt in the liquid-phase aluminum salt aqueous solution, adding sodium hydroxide aqueous solution into the aluminum salt aqueous solution obtained after the electrolytic impurity removal treatment to fully precipitate aluminum ions in the aluminum salt aqueous solution, carrying out solid-liquid separation to obtain liquid-phase and solid-phase aluminum hydroxide, carrying out liquid-phase distillation to remove water to obtain sodium salt, drying the solid-phase aluminum hydroxide, grinding to obtain aluminum hydroxide powder, and carrying out calcination and ball milling treatment on the aluminum hydroxide powder to obtain aluminum oxide powder.
2. The recycling process of aluminum-based silicon carbide composite material according to claim 1, wherein: the acid liquor in the second step is 1-2mol/L hydrochloric acid aqueous solution.
3. The recycling process of an aluminum-based silicon carbide composite material according to claim 1 or 2, wherein: in the second step, firstly crushing and screening the aluminum-based silicon carbide waste subjected to surface cleaning to obtain 325-800-mesh screen discharge, placing the 325-800-mesh screen discharge into acid liquor, stirring and mixing at 200-400rpm/min to fully dissolve the 325-800-mesh screen discharge, and then continuously stirring at 200-400rpm/min, dropwise adding acid liquor to adjust the pH value to 3-5, thus obtaining the mixed liquor.
4. The recycling process of aluminum-based silicon carbide composite material according to claim 1, wherein: and thirdly, performing ultrasonic dispersion treatment on the obtained mixed solution, wherein the ultrasonic frequency is 60-80kHz, the ultrasonic power is 1200-2000W, and after 30-40min of ultrasonic treatment, the liquid phase aluminum salt aqueous solution and the solid phase silicon carbide can be separated by decompression and filtration.
5. The recycling process of aluminum-based silicon carbide composite material according to claim 1, wherein: and step four, washing the solid-phase silicon carbide in the step three by distilled water for three times, uniformly mixing the solid-phase silicon carbide subjected to distilled water washing and the compound cleaning liquid according to the mass ratio of 1 (7-9), performing ultrasonic dispersion treatment for 30min, performing ultrasonic frequency of 60-80kHz, performing ultrasonic power of 1200-2000W, washing the solid-phase silicon carbide for three times by distilled water after the ultrasonic washing is finished, performing vacuum drying treatment on the obtained solid-phase silicon carbide, and performing vacuum drying for 6-8h at the vacuum drying temperature of 100-120 ℃ and the pressure of 0.01-0.1Pa to obtain the high-purity recovered silicon carbide powder.
6. The recycling process of aluminum-based silicon carbide composite material according to claim 5, wherein: the compound cleaning liquid is mainly prepared from 3-8 parts of acidic nonionic surfactant, 1-8 parts of nitric acid and 80-100 parts of distilled water; the acidic nonionic surfactant is at least one of alkylphenol ethoxylate OP-10, peregal 0, fatty alcohol ether sulfate AES and alkylbenzene sulfonate LAS.
7. The recycling process of aluminum-based silicon carbide composite material according to claim 6, wherein: the compound cleaning liquid is mainly prepared from 4 parts of acidic nonionic surfactant, 6 parts of nitric acid and 90 parts of distilled water.
8. The recycling process of aluminum-based silicon carbide composite material according to claim 1, wherein: the electrolytic impurity removal treatment of the liquid-phase aluminum salt aqueous solution in the step four is specifically as follows: the anode material and the cathode material are graphite columns, liquid phase aluminum salt aqueous solution is used as electrolyte, electrons are obtained from the cathode graphite columns in the electrolysis process, impurity metals in the liquid phase aluminum salt aqueous solution are separated out and attached to the surfaces of the cathode graphite columns, electrons are lost from the anode graphite columns in the electrolysis process, and the anodic electrolysis reaction is as follows: 2H 2O-4e=4H++O2, electrolysis until bubbles are generated near the cathode graphite column, the cathode electrolysis reaction is as follows: and 2H 2O+2e=2OH-+H2, stopping electrolysis, and performing reduced pressure filtration treatment on the obtained electrolyte to obtain the aluminum salt aqueous solution after the electrolytic impurity removal treatment.
9. The recycling process of aluminum-based silicon carbide composite material according to claim 1, wherein: the method further comprises a step five of carrying out surface chemical vapor deposition CVD treatment on the recovered silicon carbide powder with high purity obtained in the step four, wherein nano aluminum metal clusters are deposited on the surface of the recovered silicon carbide powder, and the method specifically comprises the following steps: the aluminum salt aqueous solution after the electrolytic impurity removal treatment and the high-purity recovered silicon carbide powder obtained in the fourth step are subjected to magnetic stirring for 20-30min at 160-240rpm/min until aluminum ions in the aluminum salt aqueous solution are completely precipitated, then the magnetic stirring for 60-80min at 160-240rpm/min is continued, and standing is carried out for 20-24h to obtain Al (OH) 3/silicon carbide binary colloid, at least three times of washing is carried out on the Al (OH) 3/silicon carbide binary colloid by distilled water, and then the solid powder is obtained by vacuum suction filtration; placing the obtained solid powder in a vacuum drying oven, drying at 100-125 ℃ for 8-12h, then transferring into an atmosphere tube furnace for calcining treatment, heating to 550-680 ℃ at 5-20 ℃/min under air atmosphere, calcining for 3-5h to obtain Al 2O3/silicon carbide composite powder, then introducing hydrogen-argon mixed gas into the atmosphere tube furnace, wherein the volume ratio of hydrogen to argon is 1 (3-7), reducing at 550-680 ℃ for 3-5h, opening the furnace for natural cooling to room temperature, and finally performing planetary ball milling treatment to obtain the high-purity recovered silicon carbide powder with the particle size of 0.5-5 microns and the surface doped with nano aluminum metal clusters.
10. The recycling process of aluminum-based silicon carbide composite material according to claim 1, wherein: the method also comprises a step five of carrying out surface doping modification treatment on the recovered silicon carbide powder with high purity obtained in the step four, and specifically comprises the following steps: firstly, preparing a surface modified multi-wall carbon nano tube; then adding the surface modified multi-wall carbon nano tube and polyvinylpyrrolidone prepared in the first step into the Ag (2E 4 MI) 2 Ac complex solution, wherein the mass ratio of the surface modified multi-wall carbon nano tube to the polyvinylpyrrolidone is 1 (0.8-1.2), the mass ratio of the surface modified multi-wall carbon nano tube to the Ag (2E 4 MI) 2 Ac complex solution is 1 (80-120), the content of the Ag (2E 4 MI) 2 Ac complex in the Ag (2E 4 MI) 2 Ac complex solution is 0.6-1.2wt%, and after ultrasonic dispersion is carried out for 2-6 hours, the recovered silicon carbide powder with high purity is obtained in the fourth step, the mass ratio of the recovered silicon carbide powder to the surface modified multi-wall carbon nano tube is 1 (20-100), and continuing ultrasonic dispersion for 30-60min to obtain a dispersion liquid; then, the obtained dispersion liquid is distilled under reduced pressure to remove the solid matters of the organic solution in the Ag (2E 4 MI) 2 Ac complex solution; and (3) carrying out high-temperature sintering treatment on the obtained solid, sintering at 210-220 ℃ for 3-5 hours to obtain a blocky solid, and carrying out jet milling treatment on the obtained blocky solid to obtain the silicon carbide composite powder with the surface doped with the multiwall carbon nanotube.
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| CN101244823A (en) * | 2008-02-20 | 2008-08-20 | 江南大学 | Method for recycling silicon carbide from by-product in silicon slice cutting process |
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| CN116288384A (en) * | 2023-01-06 | 2023-06-23 | 广东誉品实业有限公司 | Pickling solution for removing ash on surface of aluminum-based silicon carbide composite material |
| CN118086800A (en) * | 2024-04-26 | 2024-05-28 | 广州众山功能材料有限公司 | High-strength high-toughness aluminum-based silicon carbide composite material and preparation process thereof |
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| CN101244823A (en) * | 2008-02-20 | 2008-08-20 | 江南大学 | Method for recycling silicon carbide from by-product in silicon slice cutting process |
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| CN116288384A (en) * | 2023-01-06 | 2023-06-23 | 广东誉品实业有限公司 | Pickling solution for removing ash on surface of aluminum-based silicon carbide composite material |
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