Silicon carbide ceramic reaction connection method and silicon carbide ceramic connection structure
By forming a silicon carbide and silicon nitride bonding layer on the surface of silicon carbide ceramics, the problems of acid and alkali resistance and brittleness of silicon carbide ceramic connectors are solved, achieving a stable connection effect at high temperatures, which is suitable for photovoltaic material processing equipment.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-12
- Publication Date
- 2026-03-13
AI Technical Summary
Existing silicon carbide ceramic bonding methods suffer from problems such as poor acid and alkali resistance of the connectors, harsh reaction conditions, and high brittleness of the bonding layer, making it difficult to meet the high-temperature environment requirements of photovoltaic material processing equipment.
An adhesive slurry is formed by mixing a resin solution containing silicon and nitrogen elements, silicon carbide powder, and carbon powder. This slurry is then coated onto the surface of a silicon carbide ceramic part. After curing, it reacts and sintersects with a silicon source to form a silicon carbide and silicon nitride bonding layer, thereby improving the bonding strength and toughness.
This invention achieves high connection strength, acid and alkali resistance, and bending strength of silicon carbide ceramic connection structure at high temperatures, while reducing the brittleness of the connection layer, making it suitable for photovoltaic material processing equipment.
Smart Images

Figure CN121651972A_ABST
Abstract
Description
Technical Field
[0001] This application relates to the field of ceramic materials technology, and in particular to a method for reactive bonding of silicon carbide ceramics and a silicon carbide ceramic bonding structure. Background Technology
[0002] Silicon carbide ceramics are a promising high-temperature structural material. Besides excellent high-temperature mechanical properties (such as strength), silicon carbide ceramics also possess high flexural strength, oxidation resistance, and resistance to acid and alkali corrosion. In the field of photovoltaic material processing, silicon carbide boats are widely used in photovoltaic material processing equipment.
[0003] Currently, silicon carbide ceramics can be joined using methods such as mechanical bonding, adhesive bonding, diffusion welding, and brazing. However, due to the hardness and brittleness of silicon carbide ceramics, their high melting point, small coefficient of linear expansion, and covalent bonding, problems often arise regarding incompatibility with the physical properties and metallurgical properties of the welding materials. Therefore, using the above-mentioned traditional joining methods to join silicon carbide ceramics has the following drawbacks: the joined parts are not resistant to acids and alkalis, the reaction conditions are harsh, and the high-temperature resistance after resin curing is poor. In addition, the joined silicon carbide ceramics also suffer from the problem of high brittleness of the joining layer. Summary of the Invention
[0004] In view of this, in order to solve at least one of the above defects, it is necessary to propose a silicon carbide ceramic reactive bonding method that can improve the acid and alkali resistance of silicon carbide ceramic bonding structures and improve the toughness of the bonding layer.
[0005] In addition, this application also provides a silicon carbide ceramic connection structure prepared using the aforementioned silicon carbide ceramic reactive bonding method.
[0006] This application provides a method for reactive bonding of silicon carbide ceramics, the method comprising:
[0007] A resin solution containing silicon and nitrogen, silicon carbide powder, and carbon powder are mixed to form an adhesive slurry;
[0008] An adhesive slurry is applied to the surfaces of silicon carbide ceramic parts to be joined to obtain an intermediate connector.
[0009] After the two intermediate connectors to be joined are aligned, they are cured to obtain a cured connector; and
[0010] The solidified connector is reacted and sintered together with the silicon source to obtain a silicon carbide ceramic connector structure.
[0011] In some possible embodiments, the resin solution includes at least one of a silica-containing phthalonitrile resin, a silica-containing polytriazole resin, and a silica-containing polyimide resin.
[0012] In some possible embodiments, the adhesive slurry comprises, by weight percentage: the silicon carbide powder: 30% to 50%; the carbon powder: 10% to 20%; the resin solution: 30% to 50%; and the balance being a dispersant.
[0013] In some possible embodiments, the resin solution comprises, by weight percentage, the following components: a resin containing silicon and nitrogen: 30% to 50%; and a solvent: 50% to 70%, wherein the solvent includes at least one selected from tetrahydrofuran, acetonitrile, N,N-dimethylacetamide, N,N-dimethylformamide, and acetone.
[0014] In some possible embodiments, the particle size of silicon carbide powder is 1 μm to 50 μm; the particle size of carbon powder is 0.5 μm to 50 μm.
[0015] In some possible embodiments, in the step of mixing the resin solution containing silicon and nitrogen, silicon carbide powder and carbon powder to form an adhesive slurry, ball milling is used for mixing. The ball milling speed is 100 rpm to 1000 rpm, the ball milling time is 2 h to 25 h, and the mass ratio of ball to material is 1:1 to 3:1.
[0016] In some possible embodiments, the step of bonding the two intermediate connectors face to face to obtain a cured connector includes:
[0017] Align the two intermediate connectors face to face, slide and press them together to expel air bubbles; and
[0018] The two intermediate connectors after docking are cured at 100-350℃ to obtain a cured connector.
[0019] In some possible embodiments, during the reaction sintering step, the sintering temperature is 1300–1800°C and the sintering time is 1–4 h.
[0020] In some possible embodiments, during the reaction sintering step, the mass ratio of silicon source to adhesive slurry is 0.5:1 to 2.5:1.
[0021] This application embodiment also provides a silicon carbide ceramic connection structure, which is prepared by the silicon carbide ceramic reaction connection method described above. The silicon carbide ceramic connection structure includes two silicon carbide ceramic parts and a connection layer located between the connection surfaces of the two silicon carbide ceramic parts. The connection layer contains silicon carbide and silicon nitride, and the connection layer and the silicon carbide ceramic parts form an integral connection interface.
[0022] The silicon carbide ceramic reactive bonding method provided in this application uses a high-temperature resistant adhesive after curing. After the silicon carbide ceramic parts are bonded and cured with the adhesive, they maintain high bonding strength at high temperatures, allowing for stress resistance and facilitating high-temperature handling. Furthermore, the silicon and nitrogen-containing resin in the adhesive undergoes pyrolysis during sintering to form silicon carbide and silicon nitride, which can essentially form an integral structure with the silicon carbide ceramic connector, improving bonding strength and acid and alkali resistance at the joint. Simultaneously, the formation of silicon nitride effectively improves the toughness of the bonding layer, reduces its brittleness, and increases the flexural strength of the silicon carbide ceramic connector. Additionally, by performing silicon infiltration during sintering, the remaining carbon and nitrogen from the pyrolysis components of the silicon and nitrogen-containing resin can further form silicon carbide and silicon nitride, further improving bonding strength, acid and alkali resistance, and toughness. The silicon carbide ceramic reactive bonding method provided in this application is simple, easy to operate, and the reaction conditions are easily achieved. Attached Figure Description
[0023] Figure 1 A flowchart of a silicon carbide ceramic reactive bonding method provided in one embodiment of this application.
[0024] Figure 2 This is a schematic diagram of a silicon carbide ceramic connection structure provided in one embodiment of this application.
[0025] Figure 3 This is a SEM image of the silicon carbide ceramic connection structure of Embodiment 1 of this application.
[0026] Figure 4 This is a SEM image of the silicon carbide ceramic connection structure of Embodiment 4 of this application.
[0027] Figure 5 This is a SEM image of the silicon carbide ceramic connection structure of Embodiment 7 of this application.
[0028] Explanation of main component symbols
[0029] Silicon carbide ceramic connection structure: 100, silicon carbide ceramic component: 10, connection layer: 20.
[0030] The following detailed description, in conjunction with the accompanying drawings, further illustrates the embodiments of this application. Detailed Implementation
[0031] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which the embodiments of this application pertain. The terminology used herein is for the purpose of describing particular implementations only and is not intended to limit the embodiments of this application. Where specific conditions are not specified in the embodiments, conventional conditions or conditions recommended by the manufacturer shall apply. Raw materials, reagents, or instruments whose manufacturers are not specified are all conventional products that can be purchased commercially.
[0032] It should be noted that all directional indicators (such as up, down, left, right, front, back, etc.) in the embodiments of this application are only used to explain the relative positional relationship and movement of each component in a certain specific posture (as shown in the figure). If the specific posture changes, the directional indicator will also change accordingly.
[0033] It will be understood that when a layer is referred to as "on" another layer, it can be directly on that other layer or there can be an intermediate layer in between. Conversely, when a layer is referred to as "directly on" another layer, there is no intermediate layer. When a component is referred to as "fixed to," "mounted to," or "set on" another component, it can be directly on that other component or there can be an intermediate component.
[0034] Embodiments of this application are described herein with reference to cross-sectional views, which are schematic diagrams of idealized embodiments (and intermediate configurations) of this application. Therefore, variations in the shapes illustrated due to manufacturing processes and / or tolerances are foreseeable. Consequently, embodiments of this application should not be construed as limited to the specific shapes of the areas illustrated herein, but should include, for example, deviations in shape due to manufacturing processes. The areas shown in the figures are merely illustrative, and their shapes are not intended to represent the actual shapes of the illustrated devices, nor are they intended to limit the scope of this application.
[0035] The following detailed description of some embodiments of this application is provided in conjunction with the accompanying drawings. Unless otherwise specified, the following embodiments and features can be combined with each other.
[0036] Please see Figure 1 This application provides a method for reactive bonding of silicon carbide ceramics, specifically including the following steps:
[0037] Step S1: Mix the resin solution containing silicon and nitrogen, silicon carbide powder and carbon powder to form an adhesive slurry.
[0038] In some embodiments, the adhesive slurry comprises, by weight percentage: silicon carbide powder: 30% to 50%; carbon powder: 10% to 20%; the resin solution (i.e., a resin solution containing silicon and nitrogen): 30% to 50%; and the balance being a dispersant.
[0039] In some embodiments, the silicon- and nitrogen-containing resin solution comprises, by mass percentage, 30% to 50% of silicon- and nitrogen-containing resin and 50% to 70% of solvent, wherein the solvent may include at least one of tetrahydrofuran, acetonitrile, N,N-dimethylacetamide, N,N-dimethylformamide, and acetone.
[0040] Specifically, the resin containing silicon and nitrogen can include at least one of the following: silicon-containing phthalonitrile resin, silicon-containing polytriazole resin, and silicon-containing polyimide resin.
[0041] Among them, the silicon-containing phthalonitrile resin has the general formula structure shown in formula (1):
[0042]
[0043] Wherein, n is an integer greater than or equal to 1; R can be selected from at least one of alkyl and its derivatives, aryl and its derivatives, for example, R can be an alkyl or benzene ring with 1-4 carbon atoms.
[0044] In some embodiments, the silicone-containing phthalonitrile resin may specifically have the structure shown in formula (2):
[0045]
[0046] Silicon-containing polytriazole resins have the general formula structure shown in formula (3):
[0047]
[0048] Wherein, n is an integer greater than or equal to 1; R' and R” can be selected from at least one of alkyl and its derivatives, aryl and its derivatives, for example, R' and R” can be alkyl or benzene rings with 1-4 carbon atoms, and R' and R” can be the same or different.
[0049] In some embodiments, the silicone-containing polytriazole resin may specifically have the structure shown in formula (4):
[0050]
[0051] Silicone-containing polyimide resins have the general formula structure shown in formula (5):
[0052]
[0053] Where n is an integer greater than or equal to 1; R can be selected from Si4O6 or (H3CO)3Si, etc.
[0054] In some embodiments, the silicone-containing polyimide resin may specifically have the structure shown in formula (6):
[0055]
[0056] Resins such as silicon-containing phthalonitrile resin, silicon-containing polytriazole resin, and silicon-containing polyimide resin, used as the main adhesive components in adhesives, exhibit high-temperature resistance after curing. This allows silicon carbide ceramic parts to maintain high bond strength and withstand stress even after being bonded and cured with adhesives, facilitating high-temperature handling. The introduction of silicon and nitrogen elements into these resins allows silicon and carbon to form silicon carbide ceramics during sintering, improving the acid and alkali resistance of the bond structure. Simultaneously, the nitrogen formed from the cracking process forms silicon nitride ceramics, which toughens the silicon carbide and improves the toughness of the bond layer. Furthermore, the introduction of silicon and nitrogen elements into the resin molecular chain improves the resin's solubility, facilitating the formation of adhesive slurries and application. Moreover, the introduction of silicon into the resin results in a higher degree of compatibility with silicon carbide ceramics, enhancing the bonding strength of the silicon carbide ceramic parts.
[0057] In some embodiments, the dispersant may be a copolymer of polystyrene and maleic anhydride (referred to as polymeric dispersant 2013), which can improve the dispersibility of silicon carbide powder and carbon powder in resin solutions containing silicon and nitrogen.
[0058] In some embodiments, the particle size of the silicon carbide powder ranges from 1 μm to 50 μm, more specifically from 1 μm to 30 μm, and even more specifically from 1 μm to 10 μm. The silicon carbide powder is a micron-sized powder. By controlling the particle size of the silicon carbide powder within the above range, the dispersion uniformity of the silicon carbide powder in the resin solution containing silicon and nitrogen elements can be improved. Furthermore, the micron-sized silicon carbide powder can more effectively repair defects on the bonding surface of silicon carbide ceramic parts during subsequent sintering, improving bonding strength and the consistency of the bonding interface.
[0059] In some embodiments, the particle size of the carbon powder ranges from 0.5 μm to 50 μm, more specifically from 0.5 μm to 30 μm, more specifically from 1 μm to 15 μm, more specifically from 1 μm to 10 μm, and more specifically from 1 μm to 5 μm. By adding micron-sized carbon powder, the dispersibility of the carbon powder can be improved, thereby increasing the contact opportunity between the carbon powder and silicon, which facilitates the formation of silicon carbide ceramics during subsequent sintering.
[0060] In some embodiments, a weighed resin solution containing silicon and nitrogen, silicon carbide powder, and carbon powder are mixed by ball milling. The ball milling speed can be 100 rpm to 1000 rpm, more specifically 100 rpm to 900 rpm, or more specifically 300 rpm to 900 rpm. The ball milling time can be 2 hours to 25 hours, more specifically 5 hours to 24 hours, more specifically 5 hours to 20 hours, or more specifically 10 hours to 20 hours. The mass ratio of grinding balls to material (i.e., the ball-to-material mass ratio) can be 1:1 to 3:1, more specifically 1:1 to 2:1. Ball milling improves the dispersibility of silicon carbide powder and carbon powder in the silicon and nitrogen-containing resin solution, resulting in a uniformly dispersed adhesive slurry.
[0061] For example, when the silicon and nitrogen-containing resin is a silicon-containing polyimide resin, the ball milling speed can be 300 rpm to 900 rpm, the milling time can be 10 h to 24 h, and the ball-to-material mass ratio can be 1:1 to 3:1. When the silicon and nitrogen-containing resin is a silicon-containing phthalonitrile resin, the ball milling speed can be 100 rpm to 900 rpm, the milling time can be 5 h to 20 h, and the ball-to-material mass ratio can be 1:1 to 3:1. When the silicon and nitrogen-containing resin is a silicon-containing polytriazole resin, the ball milling speed can be 100 rpm to 1000 rpm, the milling time can be 2 h to 25 h, and the ball-to-material mass ratio can be 1:1 to 2:1.
[0062] Step S2: Apply adhesive slurry to the surface of the silicon carbide ceramic part to be joined to obtain the intermediate connector.
[0063] In some embodiments, the silicon carbide ceramic parts need to be pretreated before applying the adhesive slurry. The pretreatment process includes: first, ultrasonically cleaning the silicon carbide ceramic parts with anhydrous ethanol for 5-15 minutes, followed by drying; then, smoothing the surfaces of the cleaned silicon carbide ceramic parts to be joined; finally, ultrasonically cleaning the smoothed silicon carbide ceramic parts with acetone for 5-15 minutes, and drying them. Pretreatment of the silicon carbide ceramic parts removes impurities from the surfaces to be joined, which improves the joining effect.
[0064] Step S3: After the two intermediate connectors are joined together, they are cured to obtain a cured connector.
[0065] Specifically, the two intermediate connectors are joined face-to-face, slid together, and pressed tightly to remove air bubbles. Then, the joined intermediate connectors are cured at 60–350°C to obtain a cured connector. It is understandable that adhesive slurry can be applied to both connectors simultaneously, or only to one connector, depending on actual needs. It is also understandable that more than one connector can be joined, depending on actual needs.
[0066] The curing temperature can be adjusted appropriately according to different resin types. For example, when the resin containing silicon and nitrogen is a silicon-containing polyimide resin, the curing temperature can be 100-300℃; when the resin containing silicon and nitrogen is a silicon-containing phthalonitrile resin, the curing temperature can be 100-350℃; and when the resin containing silicon and nitrogen is a silicon-containing polytriazole resin, the curing temperature can be 60-250℃.
[0067] After the adhesive slurry cures, the connection between the two components can be initially secured, maintaining the connection under stress without being damaged. This is mainly because the silicon- and nitrogen-containing resin adhesive used has excellent high-temperature resistance. The cured adhesive maintains good bonding even at high temperatures, ensuring that the cured components can withstand stress at high temperatures and can be freely transported.
[0068] Step S4 involves reacting and sintering the cured connector together with the silicon source to obtain a silicon carbide ceramic connection structure. Specifically, the sintering temperature can be 1300–1800℃, and the sintering time can be 1–4 hours.
[0069] In some embodiments, the silicon source can be a solid phase, such as elemental silicon powder or silicon particles. During the silicon infiltration process, the silicon source can contact the connection point of the solidified connector to form silicon carbide in the connection layer. At the same time, the silicon source can also repair defects in other parts of the connection surface of the silicon carbide ceramic component.
[0070] In some embodiments, the mass ratio of silicon source to adhesive slurry can be 0.5:1 to 2.5:1. By adjusting the mass ratio of silicon source to adhesive slurry, the carbon and nitrogen elements formed in the adhesive slurry during the pyrolysis process can be fully reacted and sintered to form silicon carbide and silicon nitride, respectively.
[0071] During high-temperature sintering, the molecular chains of the resin containing silicon and nitrogen elements undergo pyrolysis. The carbon and silicon in the pyrolysis components can form silicon carbide ceramics, and the nitrogen and silicon can form silicon nitride ceramics. At the same time, through further silicon infiltration treatment, the unreacted carbon and nitrogen in the pyrolysis components can react more fully to form silicon carbide and silicon nitride, thereby repairing defects on the joint surface of silicon carbide ceramic parts. The generated silicon carbide can effectively improve the bonding strength and acid and alkali resistance of the silicon carbide ceramic joint structure, while the generated silicon nitride can impart toughness to the joint layer.
[0072] Please see Figure 2 This application also provides a silicon carbide ceramic connection structure 100 prepared by the silicon carbide ceramic reaction bonding method described above. The silicon carbide ceramic connection structure 100 includes two silicon carbide ceramic parts 10 and a connection layer 20 located between the connection surfaces of the two silicon carbide ceramic parts 10. The connection layer 20 and the silicon carbide ceramic parts 10 form an integral connection interface, that is, the adhesive slurry forms silicon carbide ceramic during the high-temperature sintering process, forming an integral structure with the original silicon carbide ceramic parts 10. At the same time, silicon nitride ceramic is also formed in the connection layer, which can improve the toughness of silicon carbide and reduce the brittleness of the connection layer.
[0073] The silicon carbide ceramic reactive bonding method provided in this application is mainly used to achieve reliable bonding of silicon carbide components in the field of photovoltaic material processing. A high-temperature resistant adhesive is designed and prepared, enabling silicon carbide ceramic parts to be bonded and cured using the adhesive, achieving high-temperature transportability. Furthermore, the silicon and nitrogen-containing resin in the adhesive undergoes pyrolysis during sintering, forming silicon carbide and silicon nitride. The silicon carbide and silicon carbide ceramic connector essentially form an integral whole, improving bonding strength and acid / alkali resistance. Silicon nitride ceramics improve the toughness of silicon carbide, reduce the brittleness of the bonding layer, and increase the flexural strength of the silicon carbide ceramic connector. Additionally, by performing silicon infiltration during sintering, the pyrolysis components that did not form silicon carbide and silicon nitride can further form silicon carbide and silicon nitride, further improving bonding strength, acid / alkali resistance, and toughness. The silicon carbide ceramic reactive bonding method provided in this application is simple in process, easy to operate, and the reaction conditions are easy to achieve.
[0074] Specifically, by introducing silicon-containing phthalonitrile resin into the adhesive, the resin undergoes pyrolysis during sintering and, combined with silicon infiltration, generates silicon carbide and silicon nitride. The silicon carbide and silicon nitride bonding layer achieves strong acid and alkali resistance, high bonding strength, and high flexural strength. Tests show that using silicon-containing phthalonitrile resin adhesive for bonding silicon carbide ceramics ensures a cured strength of 23 MPa, maintaining bond strength even at 400°C, enabling high-temperature handling. After silicon infiltration and sintering, the minimum bond strength of the silicon carbide ceramic connectors reaches 275 MPa. Even after treatment with 5% HF and 10% NaOH solutions, the bond strength remains at 267 MPa.
[0075] By incorporating silicon-containing polytriazole resin into the adhesive, the resin undergoes pyrolysis during sintering and, combined with silicon infiltration, generates silicon carbide and silicon nitride. The silicon carbide and silicon nitride bonding layer achieves strong acid and alkali resistance, high bond strength, and high flexural strength. Testing showed that using silicon-containing polytriazole resin adhesive for bonding silicon carbide ceramics ensures a cured strength of 11 MPa, maintaining bond strength even at 300°C, enabling high-temperature handling. After silicon infiltration and sintering, the minimum bond strength of the silicon carbide ceramic connectors reaches 275 MPa. Even after treatment with 5% HF and 10% NaOH solutions, a bond strength of 264 MPa is maintained.
[0076] By incorporating silicon-containing polyimide resin into the adhesive, the resin undergoes pyrolysis during sintering and, combined with silicon infiltration, generates silicon carbide and silicon nitride. The silicon carbide and silicon nitride bonding layer achieves strong acid and alkali resistance, high bond strength, and high flexural strength. Testing shows that using silicon-containing polyimide adhesives for bonding silicon carbide ceramics ensures a cured strength of 10 MPa, maintaining bond strength even at 500°C, enabling high-temperature handling. After silicon infiltration and sintering, the bond strength of the silicon carbide ceramic connectors reaches a minimum of 284 MPa. Even after treatment with 5% HF and 10% NaOH solutions, the bond strength remains at 271 MPa.
[0077] The embodiments of this application will be further described below through specific examples.
[0078] Synthesis of silicone-containing phthalonitrile resins
[0079] The structural formulas of the silicon-containing phthalonitrile resins used in Examples 1 to 3 of this application are all as shown in the aforementioned formula (2). For the preparation method of the silicon-containing phthalonitrile resin, please refer to the literature: "Jiang Xinxin, Zhao Xingnuo, Zhang Yulin, et al. Preparation and properties of polysiloxane-containing phthalonitrile resins [J]. Polymer Materials Science and Engineering, 2024(2)."
[0080] Synthesis of silicone-containing polytriazole resin
[0081] The structural formulas of the silicon-containing polytriazole yne resins used in Examples 4 to 6 of this application are all as shown in the aforementioned formula (4). For the preparation method of the silicon-containing polytriazole resin, please refer to the literature: "Li Yuanmeng, Wan Liqiang, Shu Da, et al. Preparation and properties of all-endoyne type silicon-containing polytriazole resin [J]. Journal of Functional Polymers, 2019, 032(003):360-366,388."
[0082] Synthesis of silicone-containing polyimide resin
[0083] The structural formulas of the silicon-containing polyimide resins used in Examples 7 to 9 of this application are all as shown in the aforementioned formula (6). For the preparation method of this silicon-containing polyimide resin, please refer to the literature: "Liu Yi, Mo Song, Pan Lingying, et al. High-temperature resistant organic-inorganic hybrid polyimide resins and their composites [J]. Aerospace Materials and Processes, 2018, 048(003):1-5."
[0084] Example 1
[0085] (1) Preparation of silicon-containing phthalonitrile resin adhesive
[0086] Step 1: According to the mass fraction, weigh 50% silicon-containing phthalonitrile resin and 50% tetrahydrofuran to prepare a silicon-containing phthalonitrile resin solution.
[0087] Step 2: According to the mass fraction, weigh 40% SiC, 12% C, 30% silica-containing phthalonitrile resin solution and the balance polymeric dispersant 2013, and ball mill them at 300 rpm for 15 hours to obtain silica-containing phthalonitrile resin adhesive slurry.
[0088] (2) Sample preparation steps
[0089] Step 1: Use an internal circular slicer to cut the silicon carbide ceramic into 3mm×4mm×40mm pieces to be connected.
[0090] Step 2: The parts to be connected are first ultrasonically cleaned with anhydrous ethanol for 10 minutes, then dried, and then polished with a sanding disc until the surface is smooth. After that, they are ultrasonically cleaned with acetone for 10 minutes and finally dried to obtain the pretreated silicon carbide ceramic parts.
[0091] (3) Preparation of silicon carbide ceramic connection structure
[0092] Step 1: Apply the silicon-containing phthalonitrile resin adhesive slurry between the pretreated surfaces of the two silicon carbide ceramic parts to be joined, and gently slide and press them together.
[0093] Step 2: Cur the connector to be cured at 300℃ for 3 hours to obtain the cured connector.
[0094] Step 3: The cured connector and the silicon source are reacted and sintered together at 1500℃ to obtain silicon carbide ceramic connector structure 1. The mass ratio of silicon source to adhesive slurry is 1:1.
[0095] like Figure 3 The image shows the microstructure of the silicon carbide ceramic connection structure 1 in Example 1, which is composed of... Figure 3 It can be seen that the substrate (silicon carbide ceramic part) and the connecting layer (of the silicon carbide ceramic connection structure 1) Figure 3 The interface between the two dotted lines is seamlessly integrated and virtually indistinguishable, demonstrating excellent connection. A three-point bending test was conducted at the connection point of the silicon carbide ceramic connection structure 1, and the average bending strength of the connected silicon carbide ceramic connection structure 1 was measured to be 281 MPa.
[0096] Example 2
[0097] (1) Preparation of silicon-containing phthalonitrile resin adhesive
[0098] Step 1: According to the mass fraction, weigh 45% silicon-containing phthalonitrile resin and 55% tetrahydrofuran to prepare a silicon-containing phthalonitrile resin solution.
[0099] Step 2: According to the mass fraction, weigh 45% SiC, 12% C, 35% silica-containing phthalonitrile resin solution and the balance of polymeric dispersant 2013, and ball mill them at 500 rpm for 10 hours to obtain silica-containing phthalonitrile resin adhesive slurry.
[0100] (2) Sample preparation steps
[0101] Step 1: Use an internal circular slicer to cut the silicon carbide ceramic into 3mm×4mm×40mm pieces to be connected.
[0102] Step 2: The parts to be connected are first ultrasonically cleaned with anhydrous ethanol for 10 minutes, then dried, and then polished with a sanding disc until the surface is smooth. After that, they are ultrasonically cleaned with acetone for 10 minutes and finally dried to obtain the pretreated silicon carbide ceramic parts.
[0103] (3) Preparation of silicon carbide ceramic connection structure
[0104] Step 1: Apply the silicon-containing phthalonitrile resin adhesive slurry between the pretreated surfaces of the two silicon carbide ceramic parts to be joined, and gently slide and press them together.
[0105] Step 2: Cur the connector to be cured at 250℃ for 4 hours to obtain the cured connector.
[0106] Step 3: The cured connector and the silicon source are reacted and sintered together at 1650℃ to obtain silicon carbide ceramic connector structure 2. The mass ratio of silicon source to adhesive slurry is 0.5:1.
[0107] Three-point bending tests were conducted at the connection point of silicon carbide ceramic connection structure 2, and the average bending strength of the connected silicon carbide ceramic connection structure 2 was measured to be 275 MPa.
[0108] Example 3
[0109] (1) Preparation of silicon-containing phthalonitrile resin adhesive
[0110] Step 1: According to the mass fraction, weigh 50% silicon-containing phthalonitrile resin and 50% tetrahydrofuran to prepare a silicon-containing phthalonitrile resin solution.
[0111] Step 2: According to the mass fraction, weigh 55% SiC, 12% C, 35% silica-containing phthalonitrile resin solution and the balance of polymeric dispersant 2013, and ball mill them at 700 rpm for 8 hours to obtain silica-containing phthalonitrile resin adhesive slurry.
[0112] (2) Sample preparation steps
[0113] Step 1: Use an internal circular slicer to cut the silicon carbide ceramic into 3mm×4mm×40mm pieces to be connected.
[0114] Step 2: The parts to be connected are first ultrasonically cleaned with anhydrous ethanol for 10 minutes, then dried, and then polished with a sanding disc until the surface is smooth. After that, they are ultrasonically cleaned with acetone for 10 minutes and finally dried to obtain the pretreated silicon carbide ceramic parts.
[0115] (3) Preparation of silicon carbide ceramic connection structure
[0116] Step 1: Apply the silicon-containing phthalonitrile resin adhesive slurry between the pretreated surfaces of the two silicon carbide ceramic parts to be joined, and gently slide and press them together.
[0117] Step 2: Cur the connector to be cured at 260℃ for 3.5 hours to obtain the cured connector.
[0118] Step 3: The cured connector and silicon are reacted and sintered together at 1750℃ to obtain silicon carbide ceramic connection structure 3. The mass ratio of silicon source to adhesive slurry is 2:1.
[0119] Three-point bending tests were conducted at the connection points of silicon carbide ceramic connection structure 3, and the average bending strength of the connected silicon carbide ceramic connection structure 3 was measured to be 297 MPa.
[0120] Example 4
[0121] (1) Preparation of silicone-containing polytriazole resin adhesive
[0122] Step 1: Weigh 50% of the silicone polytriazole resin and 50% of the tetrahydrofuran according to the mass fraction to prepare a silicone polytriazole resin solution.
[0123] Step 2: According to the mass fraction, weigh 50% SiC, 12% C, 35% silicon-containing polytriazole resin solution and the balance polymeric dispersant 2013, and ball mill them at 900 rpm for 15 hours to obtain the silicone-containing polytriazole resin adhesive slurry.
[0124] (2) Sample preparation steps
[0125] Step 1: Use an internal circular slicer to cut the silicon carbide ceramic into 3mm×4mm×40mm pieces to be connected.
[0126] Step 2: The parts to be connected are first ultrasonically cleaned with anhydrous ethanol for 10 minutes, then dried, and then polished with a sanding disc until the surface is smooth. After that, they are ultrasonically cleaned with acetone for 10 minutes and finally dried to obtain the pretreated silicon carbide ceramic parts.
[0127] (3) Preparation of silicon carbide ceramic connection structure
[0128] Step 1: Apply the silicone-containing polytriazole resin adhesive slurry between the pretreated surfaces of the two silicon carbide ceramic parts to be joined, and gently slide and press them together.
[0129] Step 2: Cur the connector to be cured at 120℃ for 5 hours to obtain the cured connector.
[0130] Step 3: The cured connector and the silicon source are reacted and sintered together at 1500℃ to obtain the silicon carbide ceramic connection structure 4. The mass ratio of silicon source to adhesive slurry is 1.2:1.
[0131] like Figure 4 The image shows the microstructure of the silicon carbide ceramic connection structure 4 in Example 4, which is composed of... Figure 4 It can be seen that the substrate (silicon carbide ceramic part) and the connecting layer (of the silicon carbide ceramic connection structure 4) are... Figure 4The interface between the two dotted lines is seamlessly integrated and virtually indistinguishable, demonstrating excellent connection. A three-point bending test was conducted at the connection point of the silicon carbide ceramic connection structure 4, and the average bending strength of the connected silicon carbide ceramic connection structure 4 was measured to be 283 MPa.
[0132] Example 5
[0133] (1) Preparation of silicone-containing polytriazole resin adhesive
[0134] Step 1: Weigh 40% silicone polytriazole resin and 60% tetrahydrofuran according to the mass fraction to prepare a silicone polytriazole resin solution.
[0135] Step 2: According to the mass fraction, weigh 45% SiC, 16% C, 35% silicon-containing polytriazole resin solution and the balance polymeric dispersant 2013, and ball mill them at 400 rpm for 12 hours to obtain the adhesive slurry containing silicon-containing polytriazole yttrium resin.
[0136] (2) Sample preparation steps
[0137] Step 1: Use an internal circular slicer to cut the silicon carbide ceramic into 3mm×4mm×40mm pieces to be connected.
[0138] Step 2: The parts to be connected are first ultrasonically cleaned with anhydrous ethanol for 10 minutes, then dried, and then polished with a sanding disc until the surface is smooth. After that, they are ultrasonically cleaned with acetone for 10 minutes and finally dried to obtain the pretreated silicon carbide ceramic parts.
[0139] (3) Preparation of silicon carbide ceramic connection structure
[0140] Step 1: Apply the silicone-containing polytriazole resin adhesive slurry between the pretreated surfaces of the two silicon carbide ceramic parts to be joined, and gently slide and press them together.
[0141] Step 2: Cur the connector to be cured at 140℃ for 4 hours to obtain the cured connector.
[0142] Step 3: The cured connector and the silicon source are reacted and sintered together at 1550℃ to obtain the silicon carbide ceramic connector structure 5. The mass ratio of silicon source to adhesive slurry is 2.5:1.
[0143] Three-point bending tests were conducted at the connection points of silicon carbide ceramic connection structure 5, and the average bending strength of the connected silicon carbide ceramic connection structure 5 was measured to be 275 MPa.
[0144] Example 6
[0145] (1) Preparation of silicone-containing polytriazole resin adhesive
[0146] Step 1: Weigh 45% silicone polytriazole resin and 55% tetrahydrofuran according to the mass fraction to prepare a silicone polytriazole resin solution.
[0147] Step 2: According to the mass fraction, weigh 55% SiC, 12% C, 35% silicon-containing polytriazole resin solution and the balance of polymeric dispersant 2013, and ball mill them at 600 rpm for 14 hours to obtain the adhesive slurry containing silicon-containing polytriazole resin.
[0148] (2) Sample preparation steps
[0149] Step 1: Use an internal circular slicer to cut the silicon carbide ceramic into 3mm×4mm×40mm pieces to be connected.
[0150] Step 2: The parts to be connected are first ultrasonically cleaned with anhydrous ethanol for 10 minutes, then dried, and then polished with a sanding disc until the surface is smooth. After that, they are ultrasonically cleaned with acetone for 10 minutes and finally dried to obtain the pretreated silicon carbide ceramic parts.
[0151] (3) Preparation of silicon carbide ceramic connection structure
[0152] Step 1: Apply the silicone-containing polytriazole resin adhesive slurry between the pretreated surfaces of the two silicon carbide ceramic parts to be joined, and gently slide and press them together.
[0153] Step 2: Cur the connector to be cured at 200℃ for 1 hour to obtain the cured connector.
[0154] Step 3: The cured connector and silicon are reacted and sintered together at 1750℃ to obtain silicon carbide ceramic connector structure 6. The mass ratio of silicon source to adhesive slurry is 0.8:1.
[0155] Three-point bending tests were conducted at the connection points of the silicon carbide ceramic connection structure 6, and the average bending strength of the connected silicon carbide ceramic connection structure 6 was measured to be 276 MPa.
[0156] Example 7
[0157] (1) Preparation of silicone-containing polyimide resin adhesive
[0158] Step 1: Weigh 50% silicone polyimide resin and 50% tetrahydrofuran according to the mass fraction to prepare a silicone polyimide resin solution.
[0159] Step 2: According to the mass fraction, weigh 40% SiC, 12% C, 30% silicone polyimide resin solution and the balance polymer dispersant 2013, and ball mill them at 800 rpm for 12 hours to obtain silicone polyimide resin adhesive slurry.
[0160] (2) Sample preparation steps
[0161] Step 1: Use an internal circular slicer to cut the silicon carbide ceramic into 3mm×4mm×40mm pieces to be connected.
[0162] Step 2: The parts to be connected are first ultrasonically cleaned with anhydrous ethanol for 10 minutes, then dried, and then polished with a sanding disc until the surface is smooth. After that, they are ultrasonically cleaned with acetone for 10 minutes and finally dried to obtain the pretreated silicon carbide ceramic parts.
[0163] (3) Preparation of silicon carbide ceramic connection structure
[0164] Step 1: Apply the silicone polyimide resin adhesive slurry between the pretreated surfaces of the two silicon carbide ceramic parts to be joined, and gently slide and press them together.
[0165] Step 2: Cur the connector to be cured at 235℃ for 3 hours to obtain the cured connector.
[0166] Step 3: The cured connector and the silicon source are reacted and sintered together at 1500℃ to obtain the silicon carbide ceramic connection structure 7. The mass ratio of silicon source to adhesive slurry is 2.1:1.
[0167] like Figure 5 The image shows the microstructure of the silicon carbide ceramic connection structure 7 in Example 7, which is composed of... Figure 5 It can be seen that the substrate (silicon carbide ceramic part) and the connecting layer (of the silicon carbide ceramic connecting structure 7) are... Figure 5 The interface between the two dotted lines is seamlessly integrated and virtually indistinguishable, demonstrating excellent connection. A three-point bending test was conducted at the connection point of the silicon carbide ceramic connection structure 7, and the average bending strength of the connected silicon carbide ceramic connection structure 7 was measured to be 287 MPa.
[0168] Example 8
[0169] (1) Preparation of silicone-containing polyimide resin adhesive
[0170] Step 1: Weigh 45% silicone polyimide resin and 55% tetrahydrofuran according to the mass fraction to prepare a silicone polyimide resin solution.
[0171] Step 2: According to the mass fraction, weigh 45% SiC, 12% C, 35% silicone polyimide resin solution and the balance polymer dispersant 2013, and ball mill them at 500 rpm for 12 hours to obtain silicone polyimide resin adhesive slurry.
[0172] (2) Sample preparation steps
[0173] Step 1: Use an internal circular slicer to cut the silicon carbide ceramic into 3mm×4mm×40mm pieces to be connected.
[0174] Step 2: The parts to be connected are first ultrasonically cleaned with anhydrous ethanol for 10 minutes, then dried, and then polished with a sanding disc until the surface is smooth. After that, they are ultrasonically cleaned with acetone for 10 minutes and finally dried to obtain the pretreated silicon carbide ceramic parts.
[0175] (3) Preparation of silicon carbide ceramic connection structure
[0176] Step 1: Apply the silicone polyimide resin adhesive slurry between the pretreated surfaces of the two silicon carbide ceramic parts to be joined, and gently slide and press them together.
[0177] Step 2: Cur the connector to be cured at 250℃ for 2.5 hours to obtain the cured connector.
[0178] Step 3: The cured connector and the silicon source are reacted and sintered together at 1550℃ to obtain the silicon carbide ceramic connector structure 8. The mass ratio of silicon source to adhesive slurry is 0.7:1.
[0179] Three-point bending tests were conducted at the connection points of the silicon carbide ceramic connection structure 8, and the average bending strength of the connected silicon carbide ceramic connection structure 8 was measured to be 284 MPa.
[0180] Example 9
[0181] (1) Preparation of silicone-containing polyimide resin adhesive
[0182] Step 1: Weigh 50% silicone polyimide resin and 50% tetrahydrofuran according to the mass fraction to prepare a silicone polyimide resin solution.
[0183] Step 2: According to the mass fraction, weigh 55% SiC, 12% C, 35% silicone polyimide resin solution and the balance polymer dispersant 2013, and ball mill them at 600 rpm for 14 hours to obtain silicone polyimide resin adhesive slurry.
[0184] (2) Sample preparation steps
[0185] Step 1: Use an internal circular slicer to cut the silicon carbide ceramic into 3mm×4mm×40mm pieces to be connected.
[0186] Step 2: The parts to be connected are first ultrasonically cleaned with anhydrous ethanol for 10 minutes, then dried, and then polished with a sanding disc until the surface is smooth. After that, they are ultrasonically cleaned with acetone for 10 minutes and finally dried to obtain the pretreated silicon carbide ceramic parts.
[0187] (3) Preparation of silicon carbide ceramic connection structure
[0188] Step 1: Apply the silicone polyimide resin adhesive slurry between the pretreated surfaces of the two silicon carbide ceramic parts to be joined, and gently slide and press them together.
[0189] Step 2: Cur the connector to be cured at 300℃ for 1 hour to obtain the cured connector.
[0190] Step 3: The cured connector and silicon are reacted and sintered together at 1650℃ to obtain silicon carbide ceramic connection structure 9. The mass ratio of silicon source to adhesive slurry is 1.4:1.
[0191] Three-point bending tests were conducted at the connection points of the silicon carbide ceramic connection structure 9, and the average bending strength of the connected silicon carbide ceramic connection structure 9 was measured to be 298 MPa.
[0192] Comparative Example 1
[0193] Step 1: Weigh out Al2O3, SiO2 and CaO according to their mass fractions of 14.7% Al2O3, 62% SiO2 and 23.3% CaO.
[0194] Step 2: The weighed oxides are mixed and mechanically ball-milled at 550 rpm for 10 hours using anhydrous ethanol as the medium. After treatment, the mixture is dried in a muffle furnace at 120°C for 1 hour. Then, it is melted in an alumina crucible at 1600°C for 2 hours. The crucible is removed using crucible tongs, and the molten glass is quenched in water to obtain glass fragments. These fragments are then wet-ground and passed through a 325-mesh sieve to obtain glass powder with a particle size less than 47 μm. Finally, the powder is dried at 120°C for 1 hour to obtain microcrystalline glass solder.
[0195] Step 3: The silicon carbide ceramic to be brazed is cut into shape using a diamond incision circle cutter. It is first ultrasonically cleaned with anhydrous ethanol for 10 minutes. After ultrasonic cleaning, it is placed in a muffle furnace and kept at 120°C for 1 hour for drying. Then, it is polished with a 400# sanding disc to remove surface stains and ensure the consistency of surface condition. It is then ultrasonically cleaned with acetone for 10 minutes. Finally, it is kept at 120°C for 1 hour for drying to obtain the pretreated silicon carbide ceramic.
[0196] Step 4: Mix the microcrystalline glass solder with terpineol to form a solder paste, and then coat it evenly between the upper and lower silicon carbide ceramic specimens to obtain the silicon carbide ceramic connector to be soldered.
[0197] Step 5: Place the components to be welded in a muffle furnace and heat them to 300°C at a heating rate of 10°C / min, and hold for 1 hour. Then heat them to 1000°C at a heating rate of 10°C / min, and then heat them to 1500°C at a heating rate of 5°C / min, and hold at 1500°C for 10 minutes. Finally, cool them with the furnace to obtain the brazed silicon carbide ceramic.
[0198] Comparative Example 2
[0199] (1) Preparation of raw blank adhesive
[0200] Step 11: 18% silicon carbide micro powder of the same particle size as the preform; 2% carbon black with a particle size of 0.5 μm; 30% thermoplastic resin; 2% acrylamide; 1% silica powder; 30% ethanol; 5% polyethylene glycol 200 (PEG 200); 5% dibutyl phthalate (DBP); 4% hexamethylenetetramine; 3% polyvinyl butyral; the above proportions are by volume, and the total percentage content is 100%.
[0201] Step 12: After mixing silicon carbide micro powder with carbon black, the mixture is calcined at 1600℃ to completely dissolve polyvinyl butyral in 10% ethanol for later use.
[0202] Step 13: Add thermoplastic resin, acrylamide, silicon powder, ethanol, polyethylene glycol 200, dibutyl phthalate, hexamethylenetetramine, and high-temperature treated silicon carbide and carbon black mixed micro powder in sequence to prepare a slurry. Then, use silicon carbide grinding balls to ball mill the mixture for 3 hours.
[0203] Step 14: Add the prepared polyvinyl butyral ethanol solution and continue ball mixing for 20 hours to obtain the adhesive.
[0204] (2) Connection of blanks
[0205] Step 21: Apply adhesive to the two surfaces to be joined, align the two surfaces, gently slide them together, and then press them firmly. Place the joined blanks in an environment of 160℃ for curing for 4 hours. Pressure can also be applied to the joined blanks during the curing process. The resulting green blank is now joined.
[0206] Step 22: Place the joined green blank into a vacuum reaction sintering furnace and sinter it together with silicon. The sintering process involves holding at 1550℃ for 1 hour to obtain a joined silicon carbide green blank.
[0207] like Figures 3 to 5 The figures shown are the microstructures of the silicon carbide ceramic connection structures in Examples 1, 4, and 7, respectively. Figures 3 to 5 It can be seen that the interface between the substrate (silicon carbide ceramic part) and the connecting layer (the part between the two dotted lines in the figure) of the silicon carbide ceramic connecting structure is integrated and basically indistinguishable, indicating a good connection effect.
[0208] As can be seen from Examples 1-3, when silicon carbide ceramics are bonded using silicon-containing phthalonitrile resin adhesives, the bonding strength of the connectors is above 275 MPa, reaching 297 MPa. As can be seen from Examples 4-6, when silicon carbide ceramics are bonded using silicon-containing polytriazole resin adhesives, the bonding strength of the connectors is above 275 MPa, reaching 283 MPa. As can be seen from Examples 7-9, when silicon carbide ceramics are bonded using silicon-containing polyimide resin adhesives, the bonding strength of the connectors is above 284 MPa, reaching 298 MPa. Therefore, the bonding method of this application allows the silicon and nitrogen-containing resin adhesive slurry to decompose during sintering, forming silicon carbide ceramics and silicon nitride, thereby fusing the bonding layer and the substrate together, resulting in good bonding efficiency. Moreover, the silicon carbide ceramic bonding structures of Examples 1-9 all exhibit high bonding strength. Furthermore, the formation of silicon nitride in the bonding layer effectively improves the toughness of the bonding layer.
[0209] The silicon carbide ceramic bonding structures of Examples 1, 4, and 7, as well as Comparative Example 1, were subjected to acid and alkali resistance tests in 5% HF and 10% NaOH solutions. The results showed that, since Al₂O₃, SiO₂, and CaO in Comparative Example 1 can all react with NaOH solution (response equations as follows: Al₂O₃ + 2NaOH = 2NaAlO₂ + H₂O; SiO₂ + 2NaOH = Na₂SiO₃ + H₂O; CaO + H₂O = Ca(OH)₂), and the products are all soluble in water, the silicon carbide ceramic bonding structure of Comparative Example 1 fractured at the joint after acid and alkali treatment, failing to meet the usage requirements. In contrast, the silicon carbide ceramic bonding structures of Examples 1, 4, and 7 maintained high bonding strength after acid and alkali treatment. Specifically, the silicon carbide ceramic bonding structure of Example 1 maintained a bonding strength of 267 MPa, the silicon carbide ceramic bonding structure of Example 4 maintained a bonding strength of 264 MPa, and the silicon carbide ceramic bonding structure of Example 7 maintained a bonding strength of 271 MPa.
[0210] High-temperature resistance tests were conducted on the cured connectors of Examples 2, 5, and 8, as well as Comparative Example 2. The test results showed that the silicon carbide ceramic connector of Example 2, after curing at 400°C, still possessed a flexural strength of 15 MPa; the silicon carbide ceramic connector of Example 5, after curing at 300°C, still possessed a flexural strength of 9 MPa; and the silicon carbide ceramic connector of Example 8, after curing at 400°C, still possessed a flexural strength of 19 MPa. Examples 2, 5, and 8 all ensured that the cured silicon carbide ceramic connectors could withstand stress at high temperatures without breaking, thus achieving the desired handling effect. However, the adhesive used in Comparative Example 2 was a thermoplastic resin, and the cured connectors struggled to maintain their bonding strength at high temperatures. This is because the molecular structure of thermoplastic resin oxidizes at high temperatures, causing the molecular chains to break down.
[0211] Therefore, the silicon carbide ceramic reactive bonding method provided in this application, by introducing silicon and nitrogen-containing resin into the adhesive slurry, enables the adhesive to maintain good bonding strength and withstand stress even at high temperatures after curing. Furthermore, the bonding layer generated through the pyrolysis and silicon infiltration treatment of the silicon and nitrogen-containing resin contains silicon carbide and silicon nitride, achieving strong acid and alkali resistance, high bonding strength, and good toughness.
[0212] The above description describes some specific embodiments of this application, but in actual applications, the application should not be limited to these embodiments. For those skilled in the art, other modifications and alterations made based on the technical concept of this application should fall within the protection scope of this application.
Claims
1. A method for reactive bonding of silicon carbide ceramics, characterized in that, include: A resin solution containing silicon and nitrogen, silicon carbide powder, and carbon powder are mixed to form an adhesive slurry; The adhesive slurry is applied to the surface of the silicon carbide ceramic part to be joined to obtain an intermediate connector; After the two intermediate connectors to be connected are joined together, they are cured to obtain a cured connector; as well as The cured connector is reacted and sintered together with a silicon source to obtain a silicon carbide ceramic connection structure.
2. The method for reactive bonding of silicon carbide ceramics according to claim 1, characterized in that, The resin solution includes at least one of silicon-containing phthalonitrile resin, silicon-containing polytriazole resin, and silicon-containing polyimide resin.
3. The method for reactive bonding of silicon carbide ceramics according to claim 1, characterized in that, The adhesive slurry comprises the following components by weight percentage: The silicon carbide powder: 30%–50%; The toner: 10%–20%; The resin solution: 30%–50%; and Dispersant: Balance.
4. The method for reactive bonding of silicon carbide ceramics according to claim 3, characterized in that, The resin solution comprises the following components by weight percentage: Resins containing silicon and nitrogen: 30%–50%; and Solvent: 50% to 70%, wherein the solvent includes at least one of tetrahydrofuran, acetonitrile, N,N-dimethylacetamide, N,N-dimethylformamide and acetone.
5. The method for reactive bonding of silicon carbide ceramics according to claim 1, characterized in that, The silicon carbide powder has a particle size of 1 μm to 50 μm; the carbon powder has a particle size of 0.5 μm to 50 μm.
6. The method for reactive bonding of silicon carbide ceramics according to claim 1, characterized in that, In the step of mixing a resin solution containing silicon and nitrogen, silicon carbide powder, and carbon powder to form an adhesive slurry, ball milling is used for mixing. The ball milling speed is 100 rpm to 1000 rpm, the ball milling time is 2 h to 25 h, and the mass ratio of ball to material is 1:1 to 3:
1.
7. The method for reactive bonding of silicon carbide ceramics according to claim 1, characterized in that, The step of bonding the two intermediate connectors face to face and then curing them to obtain a cured connector includes: The two intermediate connectors are brought together face to face, slid and pressed against each other to expel air bubbles; and The two intermediate connectors after docking are cured at 60–350°C to obtain the cured connector.
8. The method for reactive bonding of silicon carbide ceramics according to claim 1, characterized in that, In the reaction sintering step, the sintering temperature is 1300-1800℃ and the sintering time is 1h-4h.
9. The method for reactive bonding of silicon carbide ceramics according to claim 1, characterized in that, In the reaction sintering step, the mass ratio of the silicon source to the adhesive slurry is 0.5:1 to 2.5:
1.
10. A silicon carbide ceramic connection structure, characterized in that, The silicon carbide ceramic connection structure is prepared by the silicon carbide ceramic reaction connection method as described in any one of claims 1 to 9. The silicon carbide ceramic connection structure includes two silicon carbide ceramic parts and a connection layer located between the connection surfaces of the two silicon carbide ceramic parts. The connection layer contains silicon carbide and silicon nitride, and the connection layer forms an integral connection interface with the silicon carbide ceramic parts.
Citation Information
Patent Citations
Online reaction connection method of ceramic blanks
CN104496511A
Resin matrix sizing agent and SiC ceramic reaction connecting method
CN108218462A
Method for connecting polysilazane ceramic precursor with silicon carbide ceramic
CN111470878A
Silicon carbide ceramic connecting piece as well as preparation method and application thereof
CN115849933A
Silicon carbide ceramic joint as well as preparation method and application thereof
CN117125996A