A process for the preparation of aluminum silicon carbide from surface-modified silicon carbide
By hydroxylating and amylating silicon carbide particles, combined with surface modification using polyphenolic compounds and magnesium ion complexes, the problem of Al4C3 formation in aluminum silicon carbide composites was solved, enabling the preparation of aluminum silicon carbide with simple equipment and uniform process, thus improving material properties.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-30
- Publication Date
- 2026-03-31
AI Technical Summary
In existing technologies, brittle compounds Al4C3 are formed at the silicon carbide/aluminum interface in aluminum-silicon carbide composites, leading to a decline in material properties. Furthermore, existing surface modification processes require advanced equipment or involve complex processes.
Aluminum silicon carbide is prepared by hydroxylation and amination of silicon carbide particles, combined with surface modification of polyphenolic compounds and magnesium ion complexes to form a uniform protective layer, thus avoiding the formation of Al4C3.
This method enables the preparation of aluminum silicon carbide with low equipment requirements, simple process, and uniform surface modification, thereby improving the material's performance, especially its elastic modulus.
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Abstract
Description
Technical Field
[0001] This disclosure relates to the field of inorganic material preparation technology, and in particular to a preparation process for preparing aluminum silicon carbide by surface modification of silicon carbide. Background Technology
[0002] Aluminum-silicon carbide composites prepared by pressureless / pressure infiltration and powder metallurgy have been widely used in many fields, including the packaging of electronic components. However, an interface between silicon carbide and aluminum exists in aluminum-silicon carbide composites. The most common product of the interface reaction at the silicon carbide / aluminum interface is the brittle compound Al4C3 phase. Al4C3 forms on the surface of SiC in a discontinuous plate-like or disc-like form. Al4C3 has strong water absorption and is easily hydrolyzed. This reaction significantly reduces the various properties of the composite material. The formation of Al4C3 by the reaction of SiC with aluminum melt is often affected by two factors: 1) When SiC comes into contact with Al alloy melt, slight hot corrosion occurs on the surface, and Si and C atoms diffuse into the molten metal. The reaction is as follows: SiC (s) Si + C is formed; 4Al + 3C is formed to form Al4C. 3(s) 2) Al alloy melt reacts directly with SiC at high temperature to form Al4C3, as shown in the following reaction: 4Al + 3SiC to form Al4C3. 3 (s) The main solutions to this problem include surface modification of SiC particles, alloying of the aluminum alloy matrix, and optimization of the preparation process. Among these, surface modification of SiC particles is considered the most effective method for controlling the interfacial structure and improving interfacial bonding. After surface treatment, SiC particles can effectively form an intermediate layer between SiC and the Al matrix. On the one hand, this improves the wettability of the aluminum melt on the SiC surface and promotes the dispersion of reinforcing particles in the alloy melt; on the other hand, it creates a protective layer between the SiC particles and the melt, preventing direct contact between the aluminum alloy melt and SiC, thereby inhibiting harmful interfacial chemical reactions between the two.
[0003] Currently, SiC is typically modified using chemical plating or high-energy beam irradiation, but these methods require sophisticated equipment, while vapor deposition is a complex process. Therefore, there is an urgent need for a surface modification process that requires sophisticated equipment, is simple to implement, and provides uniform coating. Summary of the Invention
[0004] This disclosure provides a preparation process for preparing aluminum silicon carbide by surface modification of silicon carbide, thereby overcoming the shortcomings of related technologies.
[0005] According to a first aspect of the present disclosure, a process for preparing aluminum silicon carbide by surface modification of silicon carbide is provided. The process includes a process of surface modification of silicon carbide, the surface modification of silicon carbide comprising the following steps:
[0006] Step 1: Provide silicon carbide particles; perform surface hydroxylation treatment on the silicon carbide particles to obtain hydroxylated modified silicon carbide particles;
[0007] Step 2: The hydroxylated silicon carbide particles are surface modified using a silane coupling agent to obtain aminated silicon carbide particles.
[0008] Step 3: Prepare a solution containing the first complex;
[0009] Step 4: Add the aminated silicon carbide particles to the organic solution while stirring. Add the solution containing the first complex dropwise to the solution. After the addition is complete, add the inorganic acid dropwise. Then heat to 80℃-100℃ and stir for 3-8 hours. Then let stand for 8-20 hours to obtain the product of Step 4.
[0010] Step 5: The product obtained in Step 4 is subjected to heat treatment to obtain surface-modified silicon carbide.
[0011] In one aspect of this disclosure, the preparation process further includes the step of preparing aluminum silicon carbide using surface-modified silicon carbide:
[0012] Step 6: The surface-modified silicon carbide is dispersed in aluminum alloy powder, and then the aluminum silicon carbide is prepared by semi-solid sintering and hot static pressing.
[0013] In one aspect of this disclosure, specifically, step 1 includes:
[0014] Step 1-1: Provide silicon carbide particles, and after washing and drying, obtain clean silicon carbide particles;
[0015] Steps 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℃-65℃, and react for 2-6 hours. After the reaction is completed, filter, wash, and dry to obtain the hydroxylated modified silicon carbide particles.
[0016] In one aspect of the embodiments of this disclosure, more specifically, step 1 includes:
[0017] Step 1-1: Provide silicon carbide particles, and after washing and drying, obtain clean silicon carbide particles;
[0018] Steps 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, and react for 3.5 hours. After the reaction is completed, filter, wash, and dry to obtain the hydroxylated modified silicon carbide particles.
[0019] In one aspect of this disclosure, step 2 includes:
[0020] Step 2-1: Mix the silane coupling agent with an ethanol solution and stir for 10-30 minutes to obtain a mixed solution;
[0021] Step 2-2: Add the hydroxylated modified silicon carbide particles to the mixed solution obtained in step 2-1, stir for 10-30 min, then let stand for 1-3 h, then place in a reaction vessel and react at 110℃-150℃ for 3-6 h; then filter, wash and dry to obtain the amination modified silicon carbide particles.
[0022] In one aspect of the embodiments of this 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.
[0023] In one aspect of this disclosure, in step 3, the first complex is a complex formed by a polyphenolic compound and magnesium ions.
[0024] In one aspect of this disclosure, specifically, step 3 includes:
[0025] Step 3-1: Provide a polyphenolic compound, dissolve the polyphenolic compound in ethanol, then add a magnesium salt; then add borate-sodium hydroxide buffer to adjust the pH of the solution to 8.5-9.0, and then react for 2-6 hours to obtain a solution containing the first complex.
[0026] In one aspect of the embodiments of this disclosure, more specifically, step 3 includes:
[0027] Step 3-1: Provide a polyphenolic compound, dissolve the polyphenolic compound in ethanol, and then add a magnesium salt; then add a borate-sodium hydroxide buffer solution with a pH of 10.0 to adjust the pH to 8.8, and then react for 4 hours; to obtain a solution containing the first complex.
[0028] In one aspect of the embodiments of this disclosure, the polyphenolic compound is selected from chlorogenic acid, proanthocyanidins, epigallocatechin gallate, epicatechin gallate, 2,3-dihydroxybenzoic acid, luteolin, or kaempferol.
[0029] In one aspect of this disclosure, specifically, step 4 includes:
[0030] Step 4-1: Add the aminated silicon carbide particles to N,N-dimethylformamide or N,N-dimethylacetamide while stirring. Add the solution containing the first complex dropwise to the solution. After the addition is complete, add sulfuric acid dropwise. Then heat to 80℃-100℃ and stir for 4-6 hours. Then let stand for 8-12 hours to obtain the product of step 4.
[0031] In one aspect of this disclosure, more specifically, step 4 includes:
[0032] Step 4-1: Add the aminated silicon carbide particles to N,N-dimethylformamide while stirring. Add the solution containing the first complex dropwise to the solution. After the addition is complete, add sulfuric acid dropwise. Then heat to 90°C and stir for 4-6 hours. Then let stand for 8-12 hours to obtain the product of step 4.
[0033] In one aspect of this disclosure, specifically, step 5 includes:
[0034] Step 5-1: The product from step 4 is calcined in argon at 500℃-600℃ for 2-4 hours, then cooled to 420℃-450℃, air is introduced, and calcined for 2-3 hours. Finally, the temperature is raised to 480℃-520℃, calcined in argon for 1-2 hours, and then calcined in a hydrogen / argon mixture for 2-3 hours. The product is then cooled to room temperature to obtain the surface-modified silicon carbide.
[0035] In one aspect of the embodiments of this disclosure, more specifically, step 5 includes:
[0036] Step 5-1: The product from step 4 is calcined in argon at 550°C for 3 hours, then cooled to 435°C, air is introduced, and calcined for 2.5 hours. Finally, the temperature is raised to 500°C, calcined in argon for 1.5 hours, and then calcined in a hydrogen / argon mixture for 2.5 hours. The product is then cooled to room temperature to obtain the surface-modified silicon carbide.
[0037] According to a second aspect of the present disclosure, aluminum silicon carbide is provided, which is prepared by a method comprising the aforementioned preparation process.
[0038] According to a third aspect of the present disclosure, the aforementioned preparation process is provided for use in the preparation of aluminum silicon carbide.
[0039] The technical solutions provided by the embodiments of this disclosure may include the following beneficial effects:
[0040] As can be seen from the above embodiments, this disclosure provides a silicon carbide preparation process for preparing aluminum silicon carbide that has no special requirements for equipment, a simple process flow, and uniform surface modification.
[0041] It should be understood that the above general description and the following detailed description are exemplary and explanatory only, and are not intended to limit this disclosure. Detailed Implementation
[0042] The embodiments described in the following exemplary embodiments do not represent all embodiments consistent with this disclosure. Rather, they are merely examples of apparatuses and methods consistent with some aspects of this disclosure as detailed in the appended claims.
[0043] To make the objectives, technical solutions, and advantages of this application clearer, the technical solutions of this application will be clearly and completely described below in conjunction with embodiments. Obviously, the described embodiments are only some embodiments of this application, not all embodiments. The embodiments described herein are illustrative in nature and are used to provide a basic understanding of this application. The embodiments of this application should not be construed as limiting this application.
[0044] For the sake of brevity, this article only discloses a few specific numerical ranges. However, any lower limit can be combined with any upper limit to form an unspecified range; and any lower limit can be combined with other lower limits to form an unspecified range, just as any upper limit can be combined with any other upper limit to form an unspecified range. Furthermore, each individually disclosed point or single value can itself serve as a lower or upper limit and be combined with any other point or single value or with other lower or upper limits to form an unspecified range.
[0045] In this document, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one..." does not exclude the presence of other identical elements in the process, method, article, or apparatus that includes said element.
[0046] In this description, unless otherwise stated, "above" and "below" include the stated number.
[0047] Unless otherwise stated, the terms used in this disclosure have their common meanings as commonly understood by those skilled in the art. Unless otherwise stated, the values of the parameters mentioned in this disclosure can be measured using various measurement methods commonly used in the art (e.g., they can be tested according to the methods given in the embodiments of this disclosure).
[0048] The term "about" is used to describe and indicate small variations. When used in conjunction with an event or situation, the term may refer to examples in which the event or situation occurred precisely or in examples in which the event or situation occurred very approximately. For example, when used in conjunction with numerical values, the term may refer to a range of variation 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%. Additionally, quantities, ratios, and other numerical values are sometimes presented in range format herein. It should be understood that such range format is for convenience and brevity and should be interpreted flexibly to include not only numerical values explicitly specified as range limits but also all individual numerical values or subranges covered within the range, as if each numerical value and subrange were explicitly specified.
[0049] The 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, then the phrase "at least one of A and B" means only A; only B; or A and B. In another instance, if items A, B, and C are listed, then 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 may contain a single component or multiple components. Item B may contain a single component or multiple components. Item C may contain a single component or multiple components.
[0050] In this disclosure, steps 1 and 2 first involve obtaining hydroxyl groups on SiC particles, and then connecting the hydroxyl groups with an amino-containing silane coupling agent to obtain amino groups on the SiC particles. The reaction equation is shown below (taking KH550 as the silane coupling agent as an example):
[0051]
[0052] In this disclosure, because the polyphenolic compounds used have multiple phenolic hydroxyl groups, in addition to the phenolic hydroxyl groups complexed with magnesium ions, the magnesium-polyphenolic compound complex also has vacant phenolic hydroxyl groups that can bond with amino groups on SiC or bind through van der Waals forces, thereby uniformly introducing magnesium elements into the SiC surface. The method used in this disclosure avoids magnesium element agglomeration, thereby avoiding the formation of a large MgAlO4 phase, which would affect performance.
[0053] In this disclosure, in an atmosphere of high temperature and oxygen, the surface of silicon carbide reacts with oxygen to form a SiO2 film. When Mg is present, the following reaction occurs: SiO2 + 1 / 2Mg + Al to form 1 / 2MgAlO4 + Si. Therefore, when the surface-modified silicon carbide obtained in this disclosure is used to prepare aluminum silicon carbide by solid-state sintering and hot pressing, a MgAlO4 phase will form at the silicon carbide / aluminum interface, thereby avoiding the formation of the brittle Al4C3 phase and thus improving the aluminum silicon carbide material.
[0054] The present disclosure is further illustrated below with reference to embodiments. It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of the disclosure.
[0055] Examples and comparative examples:
[0056] Example 1:
[0057] Example 1 includes the following steps:
[0058] 50g of silicon carbide particles (20μm, commercially available) are provided. The silicon carbide particles are washed with ethanol and deionized water and dried at 60°C to obtain clean silicon carbide particles.
[0059] A 30% hydrogen peroxide solution and 95% ethanol were mixed to obtain 300 mL of a 15% hydrogen peroxide solution. Cleaned silicon carbide particles were added to the solution and heated to 60°C for 3.5 h. After the reaction was completed, the particles were filtered, washed with ethanol and deionized water, and dried at 60°C to obtain hydroxylated silicon carbide particles.
[0060] 15g of silane coupling agent γ-aminopropyltriethoxysilane was mixed with 150mL of ethanol solution and stirred for 20min to obtain a mixed solution. The hydroxylated modified silicon carbide particles were added to the mixed solution and stirred for 30min. Then, the mixture was allowed to stand for 2h and then placed in a reaction vessel and reacted at 135℃ for 4h. The mixture was then filtered, washed, and dried to obtain the aminated modified silicon carbide particles.
[0061] 500 mg of the polyphenol compound chlorogenic acid was 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 borate-sodium hydroxide buffer solution with pH 10.0 was added to adjust the pH to 8.8, and the reaction was carried out for 4 h; a solution containing the first complex was obtained.
[0062] Aminated silicon carbide particles were added to 120 mL of N,N-dimethylformamide while stirring. The solution containing the first complex prepared above was added dropwise to the solution above. After the addition was complete, 2 mL of concentrated sulfuric acid was added dropwise. The mixture was then heated to 90 °C and stirred for 5 h, and then allowed to stand for 10 h to obtain the product of step 4.
[0063] The product from step 4 was calcined in argon at 550°C for 3 hours, then cooled to 435°C, calcined in air for 2.5 hours, and finally heated to 500°C, calcined in argon for 1.5 hours, and then calcined in a hydrogen / argon mixture for 2.5 hours. After cooling to room temperature, the surface-modified silicon carbide of Example 1 was obtained; the mass of silicon carbide did not change significantly and remained at approximately 50 g.
[0064] 50g of surface-modified silicon carbide, 50g of Al2O14 alloy powder, and 0.2g of stearic acid were added to a zirconium oxide mixing tank at a ball-to-powder ratio of 5:1, a rotation speed of 250 rpm, and a mixing time of 4 hours. The uniformly mixed powder was then used to prepare a preform with a diameter of 45mm and a height of 32mm using a hydraulic press. Finally, the preform was placed in an HVHP-II type vacuum hot pressing forming equipment for hot pressing sintering. Under a vacuum atmosphere, the temperature was increased to 610℃ at a rate of 10℃ / min. After the preform reached the same temperature, it was held for 120min, followed by hot isostatic pressing for 15min and then furnace cooling to obtain the aluminum silicon carbide of Example 1.
[0065] Example 2:
[0066] The steps in Example 2 are the same as in Example 1, except that 3-aminopropyltrimethoxysilane is used instead of γ-aminopropyltriethoxysilane used in Example 1.
[0067] Example 3:
[0068] The steps in Example 3 are the same as in Example 1, except that N-(β-aminoethyl)-γ-aminopropyltriethoxysilane is used instead of γ-aminopropyltriethoxysilane used in Example 1.
[0069] Example 4:
[0070] The steps in Example 4 are the same as in Example 1, except that 3-[2-(2-aminoethylamino)ethylamino]propyltrimethoxysilane is used instead of γ-aminopropyltriethoxysilane used in Example 1.
[0071] Characterization tests:
[0072] The surface-modified silicon carbide prepared in Examples 1-4 was tested using X-ray energy dispersive spectroscopy (EDS). The surface Mg content of Example 1 was 4.2%, that of Example 2 was 3.9%, that of Example 3 was 5.7%, and that of Example 4 was 6.8%.
[0073] Example 5:
[0074] The steps in Example 5 are the same as those in Example 4, except that an equimolar amount of proanthocyanidins is used instead of chlorogenic acid used in Example 1.
[0075] Example 6:
[0076] The steps in Example 6 are the same as those in Example 4, except that an equimolar amount of epigallocatechin gallate (CAS No.: 989-51-5) is used instead of chlorogenic acid used in Example 1.
[0077] Example 7:
[0078] The steps in Example 7 are the same as those in Example 4, except that an equimolar amount of epicatechin gallate (CAS No.: 1257-08-5) is used instead of chlorogenic acid used in Example 1.
[0079] Example 8:
[0080] The steps in Example 8 are the same as those in Example 4, except that an equimolar amount of luteolin (CAS No.: 491-70-3) is used instead of chlorogenic acid used in Example 1.
[0081] Characterization tests:
[0082] The surface-modified silicon carbide prepared in Examples 5-8 was tested using X-ray energy dispersive spectroscopy (EDS). The surface Mg content of Example 5 was 8.9%, that of Example 6 was 5.1%, that of Example 7 was 5.3%, and that of Example 8 was 7.4%.
[0083] Comparative Example 1:
[0084] Comparative Example 1 includes the following steps:
[0085] 50g of silicon carbide particles (20μm, commercially available) are provided. The silicon carbide particles are washed with ethanol and deionized water and dried at 60°C to obtain clean silicon carbide particles.
[0086] A 30% hydrogen peroxide solution and 95% ethanol were mixed to obtain 300 mL of a 15% hydrogen peroxide solution. Cleaned silicon carbide particles were added to the solution and heated to 60°C for 3.5 h. After the reaction was completed, the particles were filtered, washed with ethanol and deionized water, and dried at 60°C to obtain hydroxylated silicon carbide particles.
[0087] 15g of silane coupling agent 3-[2-(2-aminoethylamino)ethylamino]propyltrimethoxysilane was mixed with 150mL of ethanol solution and stirred for 20min to obtain a mixed solution. Hydroxylated modified silicon carbide particles were added to the mixed solution and stirred for 30min. The mixture was then allowed to stand for 2h and then placed in a reaction vessel and reacted at 135℃ for 4h. The mixture was then filtered, washed, and dried to obtain the aminated modified silicon carbide particles.
[0088] Aminated silicon carbide particles were added to 120 mL of N,N-dimethylformamide while stirring. A 95% ethanol solution containing 1 g of magnesium chloride was added dropwise to the solution. After the addition was complete, 2 mL of concentrated sulfuric acid was added. The mixture was then heated to 90 °C and stirred for 5 h, followed by standing for 10 h to obtain the product from step 4.
[0089] The product from step 4 was calcined in argon at 550°C for 3 hours, then cooled to 435°C, air was introduced, and calcined for 2.5 hours. Finally, the temperature was raised to 500°C, calcined in argon for 1.5 hours, and then calcined in a hydrogen / argon mixture for 2.5 hours. The product was then cooled to room temperature to obtain the surface-modified silicon carbide of Comparative Example 1.
[0090] 50g of surface-modified silicon carbide, 50g of Al2O14 alloy powder, and 0.2g of stearic acid were added to a zirconium oxide mixing tank at a ball-to-powder ratio of 5:1, a rotation speed of 250 rpm, and a mixing time of 4 hours. The uniformly mixed powder was then used to prepare a preform with a diameter of 45mm and a height of 32mm using a hydraulic press. Finally, the preform was placed in an HVHP-II type vacuum hot pressing forming equipment for hot pressing sintering. Under a vacuum atmosphere, the temperature was increased to 610℃ at a rate of 10℃ / min. After the preform reached the same temperature, it was held for 120min, followed by hot isostatic pressing for 15min and then furnace cooling to obtain aluminum silicon carbide (Comparative Example 1).
[0091] The difference between Comparative Example 1 and Example 4 is that Comparative Example 1 used magnesium chloride instead of the complex solution prepared in Example 4.
[0092] The surface-modified silicon carbide prepared in Comparative Example 1 was tested using X-ray energy dispersive spectroscopy (EDS), and the surface Mg content of Comparative Example 1 was 2.7%.
[0093] Comparative Example 2:
[0094] Comparative Example 2 includes the following steps:
[0095] 50g of silicon carbide particles (20μm, commercially available) are provided. The silicon carbide particles are washed with ethanol and deionized water and dried at 60°C to obtain clean silicon carbide particles.
[0096] A 30% hydrogen peroxide solution and 95% ethanol were mixed to obtain 300 mL of a 15% hydrogen peroxide solution. Cleaned silicon carbide particles were added to the solution and heated to 60°C for 3.5 h. After the reaction was completed, the particles were filtered, washed with ethanol and deionized water, and dried at 60°C to obtain hydroxylated silicon carbide particles.
[0097] Hydroxylated silicon carbide particles were mixed with a 95% ethanol solution containing 0.25g magnesium chloride, and then subjected to a hydrothermal reaction at 160℃ to obtain surface-modified silicon carbide of Comparative Example 2.
[0098] 50g of surface-modified silicon carbide, 50g of Al2O14 alloy powder, and 0.2g of stearic acid were added to a zirconium oxide mixing tank at a ball-to-powder ratio of 5:1, a rotation speed of 250 rpm, and a mixing time of 4 hours. The uniformly mixed powder was then used to prepare a preform with a diameter of 45mm and a height of 32mm using a hydraulic press. Finally, the preform was placed in an HVHP-II type vacuum hot pressing forming equipment for hot pressing sintering. Under a vacuum atmosphere, the temperature was increased to 610℃ at a rate of 10℃ / min. After the preform reached the same temperature, it was held for 120min, followed by hot isostatic pressing for 15min and then furnace cooling to obtain aluminum silicon carbide (Comparative Example 2).
[0099] Elastic modulus test:
[0100] The elastic modulus of Examples 1-8 and Comparative Examples 1-2 were tested using an Olympus 38DLP-XT ultrasonic thickness gauge. The elastic modulus of Example 1 was 86.2 GPa, Example 2 was 85.5 GPa, Example 3 was 97.4 GPa, Example 4 was 105.7 GPa, Example 5 was 100.3 GPa, Example 6 was 96.5 GPa, Example 7 was 96.0 GPa, Example 8 was 112.2 GPa, Comparative Example 1 was 80.4 GPa, and Comparative Example 2 was 71.4 GPa.
[0101] As can be seen, when the surface density of magnesium does not exceed a certain range, the higher 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 decreases. This is because the MgAlO4 phase can prevent the formation of the brittle Al4C3 phase, but when the surface density of magnesium is too high, the presence of the MgAlO4 phase itself will affect the performance. Therefore, the performance of Example 5 using proanthocyanidins is weaker than that of Example 8 using luteolin. The surface magnesium density of Comparative Example 1, which does not use polyphenolic compounds, is difficult to increase (even though an excessive amount of magnesium salt has been used). And the performance of Comparative Example 2, prepared by hydrothermal method, will decrease significantly because magnesium-containing nanoparticles will inevitably form on the SiC surface.
[0102] Other embodiments of this disclosure will readily occur to those skilled in the art upon consideration of the specification and practice of the disclosure herein. This disclosure is intended to cover any variations, uses, or adaptations of this disclosure that follow the general principles of this disclosure and include common knowledge or customary techniques in the art not disclosed herein.
Claims
1. A production process for producing aluminum silicon carbide by surface-modified silicon carbide, the production process comprising a process of surface modification of silicon carbide, characterized by, The process for surface modification of silicon carbide comprises the following steps: Step 1: providing silicon carbide particles; surface hydroxylating the silicon carbide particles to obtain hydroxylated modified silicon carbide particles; Step 2: using a silane coupling agent to surface modify the hydroxylated modified silicon carbide particles to obtain aminated modified silicon carbide particles; Step 3: preparing a solution comprising a first complex; Step 4: adding the aminated modified silicon carbide particles to an organic solution, keeping stirring, adding the solution comprising the first complex to the solution, after the addition is completed, adding an inorganic acid dropwise, then heating to 80-100 DEG C, stirring for 3-8 h, then standing for 8-20 h; obtaining the product of step 4; Step 5: heat treating the product obtained in step 4 to obtain surface modified silicon carbide; The preparation process further comprises: Step 6: dispersing the surface modified silicon carbide in aluminum alloy powder, and then preparing the aluminum silicon carbide by semi-solid sintering and hot pressing; And In step 3, the first complex is a complex formed by a polyphenol compound and magnesium ions; Step 3 comprises: Step 3-1: providing a polyphenol compound, dissolving the polyphenol compound in ethanol, then adding a magnesium salt; then adding a borate-sodium hydroxide buffer solution with a pH of 10.0 to adjust the pH value to 8.8, then reacting for 4 h; obtaining a solution comprising a first complex; The polyphenol compound is selected from chlorogenic acid, procyanidin or luteolin; Step 4 comprises: Step 4-1: adding the aminated modified silicon carbide particles to N,N-dimethylformamide, keeping stirring, adding the solution comprising the first complex to the solution, after the addition is completed, adding sulfuric acid dropwise, then heating to 90 DEG C, stirring for 4-6 h, then standing for 8-12 h; obtaining the product of step 4.
2. The manufacturing process according to claim 1, characterized in that, Step 1 comprises: Step 1-1: providing silicon carbide particles, after washing and drying the silicon carbide particles, obtaining clean silicon carbide particles; Step 1-2: mixing hydrogen peroxide solution and ethanol to obtain a mixed solution; adding the clean silicon carbide particles to the mixed solution, heating to 55-65 DEG C, reacting for 2-6 h, after the reaction is completed, filtering, washing and drying to obtain the hydroxylated modified silicon carbide particles.
3. The manufacturing process of claim 1, wherein, Step 2 comprises: Step 2-1: mixing the silane coupling agent with the ethanol solution, stirring for 10-30 min to obtain a mixed solution; Step 2-2: adding the hydroxylated modified silicon carbide particles to the mixed solution obtained in step 2-1, stirring for 10-30 min, then standing for 1-3 h, then placing in a reaction kettle and reacting at 110-150 DEG C for 3-6 h; then filtering, washing and drying to obtain the aminated modified silicon carbide particles.
4. The manufacturing process of claim 1, wherein, Step 5 comprises: Step 5-1 : The product of Step 4 is calcined under argon at 500-600°C for 2-4 h, then cooled to 420-450°C, air is introduced and calcined for 2-3 h, finally the temperature is raised to 480-520°C, calcined under argon for 1-2 h, then under hydrogen / argon mixture for 2-3 h, cooled to room temperature to obtain the surface-modified silicon carbide.
Citation Information
Patent Citations
A process for electroless nickel-phosphorus alloy plating on the surface of aluminum-silicon carbide composite materials
CN102277564A
High-strength and high-toughness aluminum-based silicon carbide composite material and preparation process thereof
CN118086800A