Surface modification process of aluminum silicon carbide
Through the hydroxylation of silicon carbide particles and the treatment of silane coupling agent, combined with the modification process of polyphenol compounds and magnesium ion complexes, the problem of Al4C3 brittle compounds in aluminum silicon carbide composites is solved, and the material performance is improved and process simplified is achieved.
Patent Information
- Application Number
- CN202510719915.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-30
- Publication Date
- 2025-08-29
- Estimated Expiration
- 2045-05-30
AI Technical Summary
In the prior art, the interfacial reaction of the aluminum silicon carbide composite material generates the brittle compound Al4C3, resulting in a degradation of material performance, and the existing surface modification process equipment has high requirements or complex processes.
The silicon carbide particles were modified with hydroxylation treatment and silane coupling agent, and then complexed with polyphenol compounds and magnesium ions were formed, and the SiC surface modification was prepared by heating and calcination.
The preparation of aluminum silicon carbide with low equipment requirements, simple process and uniform surface modification is achieved, which improves interface combination and improves the performance of the material.
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Abstract
Description
Technical Field
[0001] The present disclosure relates to the technical field of inorganic material preparation, and in particular to a surface modification process of aluminum silicon carbide. Background Art
[0002] Aluminum silicon carbide composite materials prepared by pressureless / pressure infiltration and powder metallurgy technology have been widely used in many fields including the packaging of electronic components. However, there is a silicon carbide / aluminum interface in the aluminum silicon carbide composite material. The most common interfacial reaction product of the silicon carbide / aluminum interface is the brittle compound Al4C3 phase; Al4C3 is formed on the surface of SiC in the form of discontinuous sheets or disks. Al4C3 has strong water absorption and is easily hydrolyzed. This reaction will significantly reduce the various properties of the composite material. The reaction of SiC with aluminum melt to form Al4C3 is often affected by two aspects: 1) When SiC comes into contact with Al alloy melt, slight thermal corrosion will occur on the surface, and Si and C atoms will diffuse into the metal melt. The reaction is as follows: SiC (s) Generates Si+C; 4Al+3C generates Al4C 3(s) ; 2) Al alloy melt reacts directly with SiC at high temperature to form Al4C3, the reaction is as follows: 4Al+3SiC to form Al4C 3 (s) . The measures to solve this problem mainly include surface modification of SiC particles, alloying of aluminum alloy matrix and optimization of preparation process. Among them, surface modification of SiC particles is considered to be the most effective method to regulate interface structure and improve interface bonding. After surface treatment, SiC particles can effectively form an intermediate layer between SiC and Al matrix. On the one hand, it can improve the wettability of aluminum melt on the SiC surface and promote the dispersion of reinforcement particles in the alloy melt; it can also form a protective layer between SiC particles and the melt to prevent direct contact between aluminum alloy melt and SiC, thereby inhibiting the occurrence of harmful interfacial chemical reactions between the two.
[0003] In the current existing technology, SiC is usually treated by chemical plating or high-energy beam irradiation, but it has high requirements on equipment, and the vapor deposition method is complicated. Therefore, there is an urgent need for a surface modification process that has high requirements on equipment, simple process, and uniform coating. Summary of the Invention
[0004] The present disclosure provides a surface modification process for aluminum silicon carbide to address the deficiencies in the related art.
[0005] According to a first aspect of an embodiment of the present disclosure, a surface modification process for aluminum silicon carbide is provided, wherein the surface modification process includes a process of surface modification of silicon carbide, and the process of surface modification of silicon carbide includes the following steps: Step 1: providing silicon carbide particles; performing surface hydroxylation treatment on the silicon carbide particles to obtain hydroxylated silicon carbide particles.
[0006] Step 2: using a silane coupling agent to perform surface modification treatment on the hydroxylated silicon carbide particles to obtain amino-modified silicon carbide particles.
[0007] Step 3: Prepare a solution containing the first complex.
[0008] Step 4: adding the amino-modified silicon carbide particles to the organic solution, maintaining stirring, adding the solution containing the first complex dropwise to the solution, adding an inorganic acid dropwise after the addition is complete, then heating to 80°C-100°C, stirring for 3-8 hours, and then standing for 8-20 hours; obtaining the product of step 4.
[0009] Step 5: The product obtained in step 4 is subjected to heat treatment to obtain surface-modified silicon carbide.
[0010] In one aspect of the embodiments of the present disclosure, the surface modification process also includes the step of preparing aluminum silicon carbide through surface-modified silicon carbide: Step 6: Dispersing the surface-modified silicon carbide in the aluminum alloy powder, and then preparing the aluminum silicon carbide by semi-solid sintering, heating and static pressing.
[0011] In one aspect of an embodiment of the present disclosure, specifically, step 1 includes: Step 1-1: providing silicon carbide particles, and washing and drying the silicon carbide particles to obtain cleaned silicon carbide particles.
[0012] Step 1-2: Mix hydrogen peroxide solution and ethanol to obtain a mixed solution; add the cleaned silicon carbide particles to the mixed solution, heat to 55°C-65°C, react for 2-6 hours, and after the reaction is completed, filter, wash, and dry to obtain the hydroxylated silicon carbide particles.
[0013] In one aspect of the embodiments of the present disclosure, more specifically, step 1 includes: Step 1-1: providing silicon carbide particles, washing and drying the silicon carbide particles to obtain cleaned silicon carbide particles.
[0014] Step 1-2: Mix hydrogen peroxide solution and ethanol to obtain a mixed solution with a hydrogen peroxide concentration of 15%; add the cleaned silicon carbide particles to the mixed solution, heat to 60° C., react for 3.5 hours, and after the reaction is completed, filter, wash, and dry to obtain the hydroxylated silicon carbide particles.
[0015] In one aspect of the embodiments of the present disclosure, step 2 includes: step 2-1: mixing the silane coupling agent with an ethanol solution, and stirring for 10-30 minutes to obtain a mixed solution.
[0016] Step 2-2: Add the hydroxylated silicon carbide particles to the mixed solution obtained in step 2-1, stir for 10-30 minutes, then let it stand for 1-3 hours, then place it in a reactor and react at 110°C-150°C for 3-6 hours; then filter, wash and dry to obtain the amino-modified silicon carbide particles.
[0017] In one aspect of an embodiment of the present disclosure, the silane coupling agent is selected from γ-aminopropyltriethoxysilane (silane coupling agent KH-550), 3-aminopropyltrimethoxysilane (APTMS), N-(β-aminoethyl)-γ-aminopropyltriethoxysilane (AEAPTS) or 3-[2-(2-aminoethylamino)ethylamino]propyltrimethoxysilane.
[0018] In one aspect of the embodiments of the present disclosure, in step 3, the first complex is a complex formed by a polyphenol compound and magnesium ions.
[0019] In one aspect of the embodiments of the present disclosure, specifically, step 3 includes: step 3-1: providing a polyphenol compound, dissolving the polyphenol compound in ethanol, and then adding a magnesium salt; then adding a boric acid-sodium hydroxide buffer solution to adjust the pH value of the solution to 8.5-9.0, and then reacting for 2-6 hours; obtaining a solution containing a first complex.
[0020] In one aspect of the embodiments of the present disclosure, further specifically, step 3 includes: step 3-1: providing a polyphenol compound, dissolving the polyphenol compound in ethanol, and then adding a magnesium salt; then adding a boric acid-sodium hydroxide buffer with a pH of 10.0 to adjust the pH to 8.8, and then reacting for 4 hours; obtaining a solution containing a first complex.
[0021] In one aspect of the embodiments of the present disclosure, the polyphenol compound is selected from chlorogenic acid, proanthocyanidins, epigallocatechin gallate, epicatechin gallate, 2,3-dihydroxybenzoic acid, luteolin or kaempferol.
[0022] In one aspect of the embodiments of the present disclosure, specifically, step 4 includes: step 4-1: adding the amino-modified silicon carbide particles to N,N-dimethylformamide or N,N-dimethylacetamide, maintaining a stirring state, adding a solution containing the first complex dropwise to the solution, adding sulfuric acid after the addition is complete, and then heating to 80°C-100°C, stirring for 4-6 hours, and then standing for 8-12 hours; obtaining the product of step 4.
[0023] In one aspect of the embodiments of the present disclosure, further specifically, step 4 includes: step 4-1: adding the amino-modified silicon carbide particles to N,N-dimethylformamide, maintaining a stirring state, dropping a solution containing the first complex into the solution, and then adding sulfuric acid after the addition is complete, and then heating to 90°C, stirring for 4-6 hours, and then standing for 8-12 hours; obtaining the product of step 4.
[0024] In one aspect of the embodiments of the present disclosure, specifically, step 5 includes: step 5-1: calcining the product of step 4 at 500°C-600°C in argon for 2-4 hours, then cooling to 420°C-450°C, introducing air, calcining for 2-3 hours, and finally heating to 480°C-520°C, first calcining in argon for 1-2 hours, then calcining in a hydrogen / argon mixture for 2-3 hours, and cooling to room temperature to obtain the surface-modified silicon carbide.
[0025] In one aspect of the embodiments of the present disclosure, further specifically, step 5 includes: step 5-1: calcining the product of step 4 at 550°C in argon for 3 hours, then cooling to 435°C, introducing air, calcining for 2.5 hours, and finally heating to 500°C, first calcining in argon for 1.5 hours, then calcining in a hydrogen / argon mixture for 2.5 hours, and cooling to room temperature to obtain the surface-modified silicon carbide.
[0026] According to a second aspect of an embodiment of the present disclosure, there is provided aluminum silicon carbide, which is prepared by a method comprising the aforementioned surface modification process.
[0027] According to a third aspect of the embodiments of the present disclosure, there is provided an application of the aforementioned surface modification process in the preparation of aluminum silicon carbide.
[0028] The technical solutions provided by the embodiments of the present disclosure may include the following beneficial effects: As can be seen from the above embodiments, the present disclosure has prepared a silicon carbide surface modification process for preparing aluminum silicon carbide, which has no special requirements for equipment, a simple process flow, and uniform surface modification.
[0029] It is to be understood that the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the disclosure. DETAILED DESCRIPTION
[0030] The embodiments described in the following exemplary embodiments do not represent all embodiments consistent with the present disclosure. Instead, they are merely examples of devices and methods consistent with some aspects of the present disclosure as detailed in the appended claims.
[0031] To make the purpose, technical solutions, and advantages of this application more clear, the technical solutions of this application will be clearly and completely described below in conjunction with the embodiments. Obviously, the described embodiments are part of the embodiments of this application, rather than all the embodiments. The relevant embodiments described herein are illustrative and are used to provide a basic understanding of this application. The embodiments of this application should not be interpreted as limiting this application.
[0032] For the sake of clarity, only some numerical ranges are specifically disclosed herein. However, any lower limit may be combined with any upper limit to form an unspecified range; and any lower limit may be combined with other lower limits to form an unspecified range, and similarly, any upper limit may be combined with any other upper limit to form an unspecified range. In addition, each individually disclosed point or single value may itself serve as a lower limit or upper limit and be combined with any other point or single value, or with other lower limits or upper limits, to form an unspecified range.
[0033] As used herein, the terms "comprises," "comprising," or any other variations thereof are intended to encompass non-exclusive inclusion, such that a process, method, article, or apparatus that includes a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such process, method, article, or apparatus. In the absence of further limitations, an element defined by the phrase "comprising a ..." does not preclude the presence of additional identical elements in the process, method, article, or apparatus that includes the element.
[0034] In the description herein, unless otherwise specified, “above” and “below” include the number itself.
[0035] Unless otherwise specified, the terms used in this disclosure have the commonly understood meanings commonly understood by those skilled in the art. Unless otherwise specified, the numerical values of the various parameters mentioned in this disclosure can be measured using various measurement methods commonly used in the art (for example, they can be tested according to the methods given in the examples of this disclosure).
[0036] The term "about" is used to describe and illustrate small changes. When used in conjunction with an event or situation, the term may refer to an example in which the event or situation occurs precisely and an example in which the event or situation occurs very approximately. For example, when used in conjunction with a numerical value, the term may refer to a variation range of less than or equal to ±10% of the numerical value, such as less than or equal to ±5%, less than or equal to ±4%, less than or equal to ±3%, less than or equal to ±2%, less than or equal to ±1%, less than or equal to ±0.5%, less than or equal to ±0.1%, or less than or equal to ±0.05%. In addition, amounts, ratios, and other numerical values are sometimes presented in this article in a range format. It should be understood that such range formats are for convenience and brevity, and should be flexibly understood to include not only numerical values explicitly designated as range limits, but also all individual numerical values or subranges encompassed within the range, as if each numerical value and subrange were explicitly designated.
[0037] A list of items connected by the terms "at least one of," "at least one of," "at least one of," or other similar terms can mean any combination of the listed items. For example, if items A and B are listed, the phrase "at least one of A and B" means only A; only B; or A and B. In another example, if items A, B, and C are listed, the phrase "at least one of A, B, and C" means only A; or only B; only C; A and B (excluding C); A and C (excluding B); B and C (excluding A); or all of A, B, and C. Item A can contain a single component or multiple components. Item B can contain a single component or multiple components. Item C can contain a single component or multiple components.
[0038] In the present disclosure, steps 1 and 2 first obtain hydroxyl groups on SiC particles, and then connect with a silane coupling agent containing an amino group through the hydroxyl group to obtain amino groups on the SiC particles. The reaction equation is shown below (taking KH550 as a silane coupling agent as an example):
[0039] In the present disclosure, because the polyphenol compound used herein has multiple phenolic hydroxyl groups, in addition to the phenolic hydroxyl groups complexed with magnesium ions, the magnesium-polyphenol complex also has unused phenolic hydroxyl groups that can form bonds with amino groups on SiC or bind via van der Waals forces, thereby uniformly introducing magnesium onto the SiC surface. The method used in the present disclosure prevents magnesium agglomeration, thereby preventing the formation of a bulky MgAlO4 phase, which can affect performance.
[0040] In the present disclosure, in an atmosphere of high temperature and oxygen, the surface of the silicon carbide material will react with the oxygen surface to form a SiO2 film, and when the Mg element is present, the following reaction occurs: SiO2+1 / 2Mg+Al generates 1 / 2MgAlO4+Si; therefore, when the surface-modified silicon carbide obtained in the present disclosure is prepared into aluminum silicon carbide by solid-state sintering, heating and static pressing, a MgAlO4 phase will be formed at the silicon carbide / aluminum interface, thereby avoiding the formation of a brittle Al4C3 phase, thereby improving the aluminum silicon carbide material.
[0041] The present disclosure is further described below with reference to the following examples. It should be understood that these examples are only used to illustrate the present disclosure and are not intended to limit the scope of the present disclosure.
[0042] Examples and Comparative Examples: Example 1: Example 1 includes the following steps: providing 50 g of silicon carbide particles (20 μm, commercially available), washing the silicon carbide particles with ethanol and deionized water, and drying at 60° C. to obtain cleaned silicon carbide particles.
[0043] A 30% hydrogen peroxide solution and 95% ethanol were mixed to obtain 300 mL of a mixed solution with a hydrogen peroxide concentration of 15%. The cleaned silicon carbide particles were added to the mixed solution, heated to 60°C, and reacted for 3.5 hours. After the reaction, the mixture was filtered, washed with ethanol and deionized water, and dried at 60°C to obtain hydroxylated silicon carbide particles.
[0044] 15 g of silane coupling agent γ-aminopropyltriethoxysilane was mixed with 150 mL of ethanol solution and stirred for 20 minutes to obtain a mixed solution; the hydroxylated silicon carbide particles were added to the mixed solution, stirred for 30 minutes, and then allowed to stand for 2 hours, and then placed in a reactor and reacted at 135° C. for 4 hours; then filtered, washed, and dried to obtain the amino-modified silicon carbide particles.
[0045] 500 mg of the polyphenol compound chlorogenic acid was provided and dissolved in 100 mL of ethanol, and then magnesium chloride was added (the molar amount of magnesium chloride added was 1 / 2 of the molar amount of the polyphenol compound); then, a boric acid-sodium hydroxide buffer solution with a pH of 10.0 was added to adjust the pH to 8.8, and then the mixture was reacted for 4 hours to obtain a solution containing a first complex.
[0046] The amino-modified silicon carbide particles were added to 120 mL of N,N-dimethylformamide and stirred. The solution containing the first complex prepared above was added dropwise to the above solution. After the addition was completed, 2 mL of concentrated sulfuric acid was added dropwise. The mixture was then heated to 90°C, stirred for 5 hours, and then allowed to stand for 10 hours to obtain the product of step 4.
[0047] The product of step 4 was calcined at 550°C in argon for 3 h, then cooled to 435°C, introduced into air, and calcined for 2.5 h. Finally, the temperature was raised to 500°C, first calcined in argon for 1.5 h, then calcined in a hydrogen / argon mixture for 2.5 h, and cooled to room temperature to obtain the surface-modified silicon carbide of Example 1; wherein the mass of the silicon carbide did not change significantly and remained about 50 g.
[0048] 50g of surface-modified silicon carbide, 50g of Al2014 alloy powder, and 0.2g of stearic acid were added to a mixing tank made of zirconium oxide, with a ball-to-material ratio of 5:1, a rotation speed set to 250rpm, and a mixing time of 4 hours. Then, the evenly mixed powder was passed through a hydraulic press to prepare a preform with a diameter of 45mm and a height of 32mm; finally, the preform was placed in a HVHP-II vacuum hot pressing molding equipment for hot pressing and sintering. Under a vacuum atmosphere, the temperature was raised to 610°C at a rate of 10°C / min. After the blank was raised to the same temperature, it was kept warm for 120min, then hot isostatically pressed for 15min and cooled with the furnace to obtain the aluminum silicon carbide of Example 1.
[0049] Example 2: The steps of Example 2 are the same as those of Example 1, except that 3-aminopropyltrimethoxysilane is used instead of γ-aminopropyltriethoxysilane used in Example 1.
[0050] Example 3: The steps of Example 3 are the same as those of Example 1, except that N-(β-aminoethyl)-γ-aminopropyltriethoxysilane is used instead of the γ-aminopropyltriethoxysilane used in Example 1.
[0051] Example 4: The steps of Example 4 are the same as those of Example 1, except that 3-[2-(2-aminoethylamino)ethylamino]propyltrimethoxysilane is used instead of the γ-aminopropyltriethoxysilane used in Example 1.
[0052] Characterization test: The surface-modified silicon carbide prepared in Examples 1-4 was tested using X-ray energy dispersive spectrometry (EDS). The surface Mg content of Example 1 was 4.2%, the surface Mg content of Example 2 was 3.9%, the surface Mg content of Example 3 was 5.7%, and the surface Mg content of Example 4 was 6.8%.
[0053] Example 5: The steps of Example 5 are the same as those of Example 4, except that an equimolar amount of proanthocyanidins is used instead of the chlorogenic acid used in Example 1.
[0054] Example 6: The steps of Example 6 are the same as those of Example 4, except that an equimolar amount of epigallocatechin gallate (CAS No.: 989-51-5) is used instead of the chlorogenic acid used in Example 1.
[0055] Example 7: The steps of Example 7 are the same as those of Example 4, except that an equimolar amount of epicatechin gallate (CAS No.: 1257-08-5) is used instead of the chlorogenic acid used in Example 1.
[0056] Example 8: The steps of Example 8 are the same as those of Example 4, except that an equal molar amount of luteolin (CAS No.: 491-70-3) is used instead of the chlorogenic acid used in Example 1.
[0057] Characterization test: The surface-modified silicon carbide prepared in Examples 5-8 was tested using X-ray energy dispersive spectrometry (EDS). The surface Mg content of Example 5 was 8.9%, the surface Mg content of Example 6 was 5.1%, the surface Mg content of Example 7 was 5.3%, and the surface Mg content of Example 8 was 7.4%.
[0058] Comparative Example 1: Comparative Example 1 includes the following steps: providing 50 g of silicon carbide particles (20 μm, commercially available), washing the silicon carbide particles with ethanol and deionized water, and drying at 60° C. to obtain cleaned silicon carbide particles.
[0059] A 30% hydrogen peroxide solution and 95% ethanol were mixed to obtain 300 mL of a mixed solution with a hydrogen peroxide concentration of 15%. The cleaned silicon carbide particles were added to the mixed solution, heated to 60°C, and reacted for 3.5 hours. After the reaction, the mixture was filtered, washed with ethanol and deionized water, and dried at 60°C to obtain hydroxylated silicon carbide particles.
[0060] 15 g of silane coupling agent 3-[2-(2-aminoethylamino)ethylamino]propyltrimethoxysilane was mixed with 150 mL of ethanol solution and stirred for 20 minutes to obtain a mixed solution; hydroxylated silicon carbide particles were added to the mixed solution, stirred for 30 minutes, and then allowed to stand for 2 hours, and then placed in a reactor and reacted at 135° C. for 4 hours; then filtered, washed, and dried to obtain the amino-modified silicon carbide particles.
[0061] Add the amino-modified silicon carbide particles to 120 mL of N,N-dimethylformamide and keep stirring. Add 1 g of magnesium chloride in 95% ethanol solution dropwise to the above solution. After the addition is complete, add 2 mL of concentrated sulfuric acid dropwise. Then heat to 90°C, stir for 5 hours, and then let stand for 10 hours to obtain the product of step 4.
[0062] The product of step 4 was calcined at 550°C in argon for 3 hours, then cooled to 435°C, introduced into air, and calcined for 2.5 hours. Finally, the temperature was raised to 500°C, first calcined in argon for 1.5 hours, then calcined in a hydrogen / argon mixture for 2.5 hours, and cooled to room temperature to obtain the surface-modified silicon carbide of Comparative Example 1.
[0063] 50g of surface-modified silicon carbide, 50g of Al2014 alloy powder, and 0.2g of stearic acid were added to a mixing tank made of zirconium oxide. The ball-to-material ratio was 5:1, the rotation speed was set to 250rpm, and the mixing time was 4 hours. Then, the evenly mixed powder was passed through a hydraulic press to prepare a preform with a diameter of 45mm and a height of 32mm; finally, the preform was placed in an HVHP-II vacuum hot pressing molding equipment for hot pressing and sintering. Under a vacuum atmosphere, the temperature was raised to 610℃ at a rate of 10℃ / min. After the blank was raised to the same temperature, it was kept warm for 120min, then hot isostatically pressed for 15min and cooled with the furnace to obtain the aluminum silicon carbide of Comparative Example 1.
[0064] The difference between Comparative Example 1 and Example 4 is that, in Comparative Example 1, magnesium chloride is used instead of the complex solution prepared in Example 4.
[0065] The surface-modified silicon carbide prepared in Comparative Example 1 was tested using X-ray energy dispersive spectroscopy (EDS). The surface Mg content of Comparative Example 1 was 2.7%.
[0066] Comparative Example 2: Comparative Example 2 includes the following steps: providing 50 g of silicon carbide particles (20 μm, commercially available), washing the silicon carbide particles with ethanol and deionized water, and drying at 60° C. to obtain cleaned silicon carbide particles.
[0067] A 30% hydrogen peroxide solution and 95% ethanol were mixed to obtain 300 mL of a mixed solution with a hydrogen peroxide concentration of 15%. The cleaned silicon carbide particles were added to the mixed solution, heated to 60°C, and reacted for 3.5 hours. After the reaction, the mixture was filtered, washed with ethanol and deionized water, and dried at 60°C to obtain hydroxylated silicon carbide particles.
[0068] The hydroxylated silicon carbide particles were mixed with a 95% ethanol solution containing 0.25 g of magnesium chloride, and then subjected to a hydrothermal reaction at 160° C. to obtain surface-modified silicon carbide of Comparative Example 2. 50g of surface-modified silicon carbide, 50g of Al2014 alloy powder, and 0.2g of stearic acid were added to a mixing tank made of zirconium oxide. The ball-to-material ratio was 5:1, the rotation speed was set to 250rpm, and the mixing time was 4 hours. Then, the evenly mixed powder was passed through a hydraulic press to prepare a preform with a diameter of 45mm and a height of 32mm; finally, the preform was placed in an HVHP-II vacuum hot pressing molding equipment for hot pressing and sintering. Under a vacuum atmosphere, the temperature was raised to 610℃ at a rate of 10℃ / min. After the blank was raised to the same temperature, it was kept warm for 120min, then hot isostatically pressed for 15min and cooled with the furnace to obtain the aluminum silicon carbide of Comparative Example 2.
[0069] Elastic modulus test: The elastic modulus of Examples 1-8 and Comparative Examples 1-2 was tested using a 38DLP-XT ultrasonic thickness gauge produced by Olympus; the elastic modulus of Example 1 was 86.2 GPa, the elastic modulus of Example 2 was 85.5 GPa, the elastic modulus of Example 3 was 97.4 GPa, the elastic modulus of Example 4 was 105.7 GPa, the elastic modulus of Example 5 was 100.3 GPa, the elastic modulus of Example 6 was 96.5 GPa, the elastic modulus of Example 7 was 96.0 GPa, and the elastic modulus of Example 8 was 112.2 GPa. The elastic modulus of Comparative Example 1 was 80.4 GPa, and the elastic modulus of Comparative Example 2 was 71.4 GPa.
[0070] It can be seen that when the surface density of magnesium does not exceed a certain range, the greater the surface density of magnesium, the better the elastic modulus of the prepared aluminum silicon carbide. However, when the surface density of magnesium exceeds a certain range, the elastic modulus of the prepared aluminum silicon carbide actually decreases. This is because the MgAlO4 phase can prevent the formation of the brittle Al4C3 phase. However, when the surface density of magnesium is too high, the existence of the MgAlO4 phase itself will affect performance. Therefore, the performance of Example 5 using proanthocyanidins is weaker than that of Example 8 using luteolin. Comparative Example 1, which does not use a polyphenol compound, has difficulty increasing its surface magnesium density (even with the use of an excess of magnesium salt). And Comparative Example 2, prepared by a hydrothermal method, inevitably forms magnesium-containing nanoparticles on the SiC surface, resulting in a significant decline in performance.
[0071] Those skilled in the art will readily appreciate other embodiments of the present disclosure after considering the specification and practicing the disclosure disclosed herein. This disclosure is intended to cover any variations, uses, or adaptations of the present disclosure that follow the general principles of the present disclosure and include common knowledge or customary techniques in the art not disclosed herein.
Claims
1. A surface modification process for aluminum silicon carbide, comprising a process for surface modification of silicon carbide, characterized in that: The process of surface modification of silicon carbide includes the following steps: step 1: providing silicon carbide particles; performing surface hydroxylation treatment on the silicon carbide particles to obtain hydroxylated silicon carbide particles; step 2: using a silane coupling agent to perform surface modification treatment on the hydroxylated silicon carbide particles to obtain amino-modified silicon carbide particles; step 3: preparing a solution containing a first complex; step 4: adding the amino-modified silicon carbide particles to an organic solution, maintaining a stirring state, and dropwise adding the solution containing the first complex to the solution, and then dropwise adding an inorganic acid after the dropwise addition is completed, and then heating to 80°C-100°C, stirring for 3-8 hours, and then standing for 8-20 hours to obtain the product of step 4; step 5: heat-treating the product obtained in step 4 to obtain surface-modified silicon carbide.
2. The surface modification process of aluminum silicon carbide according to claim 1, characterized in that: The surface modification process also includes the step of preparing aluminum silicon carbide using the surface-modified silicon carbide: Step 6: dispersing the surface-modified silicon carbide in the aluminum alloy powder, and then preparing the aluminum silicon carbide by semi-solid sintering, heating and static pressing.
3. The surface modification process of aluminum silicon carbide according to claim 1, characterized in that: Step 1 includes: step 1-1: providing silicon carbide particles, washing and drying the silicon carbide particles to obtain cleaned silicon carbide particles; step 1-2: mixing a hydrogen peroxide solution and ethanol to obtain a mixed solution; adding the cleaned silicon carbide particles to the mixed solution, heating to 55° C.-65° C., reacting for 2-6 hours, and filtering, washing, and drying after the reaction to obtain the hydroxylated silicon carbide particles.
4. The surface modification process of aluminum silicon carbide according to claim 1, characterized in that: Step 2 includes: step 2-1: mixing the silane coupling agent with an ethanol solution, stirring for 10-30 minutes, and obtaining a mixed solution; step 2-2: adding the hydroxylated silicon carbide particles to the mixed solution obtained in step 2-1, stirring for 10-30 minutes, and then standing for 1-3 hours, and then placing in a reactor, and reacting at 110° C.-150° C. for 3-6 hours; and then filtering, washing, and drying to obtain the amino-modified silicon carbide particles.
5. The surface modification process of aluminum silicon carbide according to claim 1, characterized in that: In step 3, the first complex is a complex formed by a polyphenol compound and magnesium ions.
6. The surface modification process of aluminum silicon carbide according to claim 1 or 5, characterized in that: Step 3 includes: Step 3-1: providing a polyphenol compound, dissolving the polyphenol compound in ethanol, and then adding a magnesium salt; then adding a boric acid-sodium hydroxide buffer solution to adjust the pH value of the solution to 8.5-9.0, and then reacting for 2-6 hours; obtaining a solution containing a first complex.
7. The surface modification process of aluminum silicon carbide according to claim 5, characterized in that: The polyphenol compound is selected from chlorogenic acid, proanthocyanidin, epigallocatechin gallate, epicatechin gallate, 2,3-dihydroxybenzoic acid, luteolin or kaempferol.
8. The surface modification process of aluminum silicon carbide according to claim 1, characterized in that: Step 4 includes: step 4-1: adding the amino-modified silicon carbide particles to N,N-dimethylformamide or N,N-dimethylacetamide, maintaining a stirring state, adding a solution containing the first complex dropwise to the solution, adding sulfuric acid dropwise after the addition is complete, and then heating to 80°C-100°C, stirring for 4-6 hours, and then standing for 8-12 hours; obtaining the product of step 4.
9. The surface modification process of aluminum silicon carbide according to claim 1, characterized in that: Step 5 includes: Step 5-1: calcining the product of step 4 at 500°C-600°C in argon for 2-4 hours, then cooling to 420°C-450°C, introducing air, calcining for 2-3 hours, and finally heating to 480°C-520°C, first calcining in argon for 1-2 hours, then calcining in a hydrogen / argon mixture for 2-3 hours, and cooling to room temperature to obtain the surface-modified silicon carbide.
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