Semiconductor anticorrosion ceramic disc body material and preparation method thereof

Abstract

The application relates to the technical field of ceramic disc bodies, in particular to a semiconductor anticorrosion ceramic disc body material and a preparation method thereof, which comprises the following raw materials in parts by weight: 45-50 parts of silicon carbide, 15-20 parts of aluminum oxide, 10-15 parts of an improved body with incorporated hexagonal boron nitride, 3-5 parts of a sintering aid, and 2-4 parts of a bonding agent. The ceramic disc body material is prepared by matching and blending silicon carbide, aluminum oxide, the improved body with incorporated hexagonal boron nitride, the sintering aid, the bonding agent and a rare earth functional agent; the improved body with incorporated hexagonal boron nitride and the rare earth functional agent are added to the basic framework of silicon carbide and aluminum oxide to achieve mutual cooperation and synergistic effect; the obtained product has improved balance of crack resistance, bending resistance, insulation and Vickers hardness, and has remarkable anticorrosion and high-temperature stability.

Description

Technical Field

[0001] This invention relates to the field of ceramic disc technology, specifically to a semiconductor corrosion-resistant ceramic disc material and its preparation method. Background Technology

[0002] Ceramic disks can serve as core carrier components in the manufacture of semiconductor chips. Processes such as wafer etching, thin film deposition, and ion implantation must be completed in a sealed vacuum chamber. The ceramic disks are exposed to plasma, highly corrosive process gases, and high-temperature environments, ensuring the stability of equipment operation. However, existing conventional semiconductor ceramic disks have poor crack and bending resistance, and it is difficult to balance and improve their insulation and Vickers hardness. Furthermore, they suffer from poor corrosion resistance and high-temperature stability. Therefore, this invention provides further optimization and improvement. Summary of the Invention

[0003] In view of the deficiencies of the prior art, the purpose of this invention is to provide a semiconductor corrosion-resistant ceramic disk material and its preparation method, so as to solve the problems mentioned in the background art.

[0004] The present invention solves the technical problem by adopting the following technical solution: This invention provides a semiconductor corrosion-resistant ceramic disk material, comprising the following raw materials in parts by weight: 45-50 parts silicon carbide, 15-20 parts alumina, 10-15 parts modified by incorporating hexagonal boron nitride, 3-5 parts sintering aid, and 2-4 parts binder.

[0005] Preferably, the silicon carbide has a particle size of 80-150 nm; the alumina is α-alumina, and the specific surface area of ​​α-alumina is 8-12 m². / g; the sintering aid is magnesium oxide; the binder is polyvinyl alcohol.

[0006] Preferably, the method for preparing the modified body doped with hexagonal boron nitride is as follows: S01: Mix 5-8 parts by weight of hexagonal boron nitride, 25-30 parts by weight of water, and 2-5 parts by weight of polyethylene glycol evenly. Then add 2-4 parts by weight of pyromellitic anhydride and 1-2 parts by weight of pyridine and react for 2-3 hours at a reaction temperature of 45-50℃. After the reaction is completed, dry to obtain pretreated hexagonal boron nitride. S02: Dissolve dopamine hydrochloride in water to obtain a dopamine hydrochloride buffer solution with a mass concentration of 0.5-0.8 g / mL. Then, mix 4-7 parts by weight of carbon nanotubes and 8-12 parts by weight of the dopamine hydrochloride buffer solution thoroughly to obtain a carbon nanotube solution. S03: The pretreated hexagonal boron nitride and carbon nanotube liquid is ultrasonically treated at a weight ratio of 3:(5-7), with an ultrasonic power of 350-400W, for 1-2 hours. After ultrasonic treatment, the liquid is filtered and dried to obtain the ultrasonic agent of hexagonal boron nitride-carbon nanotube. S04: Hexagonal boron nitride-carbon nanotube ultrasonic agent and zirconium oxide-titanium dioxide combined liquid were mixed and ball-milled at a weight ratio of (8-11):5. The ball milling speed was 1000-1200 r / min and the ball milling time was 2 h. After the ball milling was completed, the mixture was filtered and dried to obtain the improved body doped with hexagonal boron nitride.

[0007] Preferably, the hexagonal boron nitride is hexagonal boron nitride nanosheets, the nanosheets having a sheet thickness of 5–20 nm, a lateral dimension of 0.5–3 μm, and a specific surface area of ​​100–200 m². / g; The carbon nanotubes are multi-walled carbon nanotubes with a diameter of 10–50 nm and a length of 5–20 μm.

[0008] Preferably, the zirconium oxide-titanium dioxide combined solution comprises the following raw materials in parts by weight: The mixture consists of 5-8 parts zirconium oxide, 3-5 parts sodium silicate aqueous solution, 2-4 parts titanium dioxide, 1-3 parts yttrium nitrate solution, and 0.5-0.6 parts nano-niobium silicide.

[0009] The improved boron nitride-incorporated compound is made by modifying boron nitride with polyethylene glycol, pyromellitic anhydride, and pyridine raw materials, and then blending it with carbon nanotubes treated with dopamine hydrochloride buffer solution. The resulting boron nitride-carbon nanotube ultrasonic agent optimizes the product's functionality in the system. Using boron nitride and carbon nanotubes as carrier media, the performance coordination of the product system is enhanced. At the same time, the zirconia-titanium dioxide co-solution uses zirconia and titanium dioxide as the matrix, combined with nano-niobium silicide, sodium silicate aqueous solution, and yttrium nitrate solution. Through the co-combination improvement of the raw materials, mutual optimization and coordination are achieved. The resulting zirconia-titanium dioxide co-solution further synergizes with the boron nitride-carbon nanotube ultrasonic agent, thereby further enhancing the product's functional coordination, corrosion resistance, and high-temperature stability.

[0010] Preferably, the sodium silicate aqueous solution has a mass fraction of 2-5%; and the yttrium nitrate solution has a mass fraction of 2-3%.

[0011] Preferably, the ceramic disc material further includes 6-10 parts of rare earth functional agents; The preparation method of the rare earth functional agent is as follows: S11, trifluoropropyl dimethoxysilazane, ethanol solvent, acetic acid and deionized water are mixed and reacted in a weight ratio of (2-4):(55-58):2:(3-5), the reaction temperature is 30-40℃, the reaction is carried out for 1-2 hours, and the reaction is completed to obtain silanol solution. Silicon nitride nanofibers, nano-tantalum carbide and silanol solution were thoroughly mixed in a weight ratio of (4-7):2:(8-11) to obtain a silanol solution based on silicon nitride nanofibers. S12, add 3-6 parts of sodium alginate powder and 1-2 parts of β-cyclodextrin to 10-15 parts of N,N dimethylformamide, then add 3-5 parts of rare earth lanthanum oxide and 1-2 parts of rare earth cerium oxide and mix thoroughly. After mixing, filter and dry to obtain rare earth compound agent. S13, based on silicon nitride nanofibers, silanol liquid and rare earth compounding agent are mixed and ball-milled at a weight ratio of (8-11):5. After ball milling, the mixture is filtered and dried to obtain rare earth functional agent.

[0012] Preferably, the silicon nitride nanofibers have a diameter of 80-100 nm, a length of 5-20 μm, and an aspect ratio of (80-100):1.

[0013] The rare earth functional agent uses silicon nitride nanofibers as the matrix and as the fiber structure, which are interwoven and reinforced in the system. It is then blended with nano-tantalum carbide and silanol solution. Through the co-regulation improvement between raw materials, the performance coordination of the product is further enhanced. Furthermore, after being co-regulated with rare earth compounding agent, the rare earth functional agent has a better synergistic effect with the modified body doped with hexagonal boron nitride, thereby further improving the performance of the product. The rare earth compounding agent uses sodium alginate powder and β-cyclodextrin for joint blending, and then combines rare earth lanthanum oxide and rare earth cerium oxide. Through the co-regulation improvement between raw materials, the performance of the product is further coordinated and improved.

[0014] The present invention also provides a method for preparing a semiconductor anti-corrosion ceramic disk material, comprising the following steps: weighing raw materials according to the weight parts, wet ball milling the raw materials thoroughly, then pressing them into shape, with a molding pressure of 80-120MPa and molding time of 8-10min to obtain a green body, and then sintering the green body to obtain the ceramic disk material.

[0015] Preferably, the specific operation steps for sintering improvement are as follows: Step 1: First, raise the temperature to 570-590℃ at a rate of 3-5℃ / min and hold for 1-2 hours; Step 2: Increase the temperature to 1050-1100℃ at a rate of 5-8℃ / min and hold for 2-3 hours. Then increase the temperature to 1550-1580℃ at a rate of 1-3℃ / min and hold for 1-2 hours. Step three: Finally, cool down to 750-760℃ at a rate of 7-9℃ / min, hold for 15-20 minutes, and then cool down to room temperature at a rate of 2-4℃ / min. By using gradient heating sintering followed by gradual cooling, and by optimizing homogeneous and refined sintering, the resulting ceramic material exhibits stronger density, and the product's performance is further optimized.

[0016] Compared with the prior art, the present invention has the following beneficial effects: The ceramic disc material of this invention is made by combining silicon carbide, alumina, a modified body doped with hexagonal boron nitride, sintering aid, binder and rare earth functional agent. With silicon carbide and alumina as the basic skeleton, the modified body doped with hexagonal boron nitride and rare earth functional agent work together synergistically to obtain a product with improved crack resistance, bending resistance, insulation and Vickers hardness, as well as significant anti-corrosion and high-temperature stability. Detailed Implementation

[0017] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to specific examples. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0018] Example 1.

[0019] This embodiment of a semiconductor corrosion-resistant ceramic disk material comprises the following raw materials in parts by weight: 45 parts silicon carbide, 15 parts alumina, 10 parts modified by incorporating hexagonal boron nitride, 3 parts sintering aid, and 2 parts binder.

[0020] In this embodiment, the silicon carbide has a particle size of 80 nm; the alumina is α-alumina, and the specific surface area of ​​α-alumina is 8 m². / g; the sintering aid is magnesium oxide; the binder is polyvinyl alcohol.

[0021] The preparation method of the modified hexagonal boron nitride doped in this embodiment is as follows: S01: Mix 5 parts by weight of hexagonal boron nitride, 25 parts by weight of water and 2 parts by weight of polyethylene glycol evenly, then add 2 parts by weight of pyromellitic anhydride and 1 part by weight of pyridine and mix for 2 hours at a reaction temperature of 45°C. After the reaction is completed, dry to obtain pretreated hexagonal boron nitride. S02: Dissolve dopamine hydrochloride in water to obtain a dopamine hydrochloride buffer solution with a mass concentration of 0.5 g / mL. Then, mix 4 parts by weight of carbon nanotubes and 8 parts by weight of the dopamine hydrochloride buffer solution thoroughly to obtain a carbon nanotube solution. S03: The pretreated hexagonal boron nitride and carbon nanotube liquid was ultrasonically treated at a weight ratio of 3:5, with an ultrasonic power of 350W for 1 hour. After ultrasonication, the liquid was filtered and dried to obtain the ultrasonic agent of hexagonal boron nitride-carbon nanotube. S04: The ultrasonic agent of hexagonal boron nitride-carbon nanotubes and the combined solution of zirconium oxide-titanium dioxide were mixed and ball-milled at a weight ratio of 8:5 for 2 hours at a speed of 1000 r / min. After ball milling, the mixture was filtered and dried to obtain the improved body doped with hexagonal boron nitride.

[0022] In this embodiment, hexagonal boron nitride is presented as hexagonal boron nitride nanosheets. The nanosheets have a thickness of 5 nm, a lateral dimension of 0.5 μm, and a specific surface area of ​​100 m². / g; The carbon nanotubes are multi-walled carbon nanotubes with a diameter of 10 nm and a length of 5 μm.

[0023] The zirconium oxide-titanium dioxide combined solution of this embodiment comprises the following raw materials in parts by weight: Five parts zirconium oxide, three parts sodium silicate aqueous solution, two parts titanium dioxide, one part yttrium nitrate solution, and 0.5 parts nano-niobium silicide.

[0024] In this embodiment, the sodium silicate aqueous solution has a mass fraction of 2%; the yttrium nitrate solution has a mass fraction of 2%.

[0025] The ceramic disc material in this embodiment also includes 6 parts of rare earth functional agents; The preparation method of the rare earth functional agent is as follows: S11, trifluoropropyldimethoxysilazane, ethanol solvent, acetic acid and deionized water are mixed in a weight ratio of 2:55:2:3 and reacted at 30℃ for 1 h. After the reaction is completed, a silanol solution is obtained. Silicon nitride nanofibers, nano-tantalum carbide and silanol solution were thoroughly mixed at a weight ratio of 4:2:8 to obtain a silanol solution based on silicon nitride nanofibers. S12, add 3 parts sodium alginate powder and 1 part β-cyclodextrin to 10 parts N,N dimethylformamide, then add 3 parts rare earth lanthanum oxide and 1 part rare earth cerium oxide and mix thoroughly. After mixing, filter and dry to obtain rare earth compound agent. S13, based on silicon nitride nanofibers, silanol liquid and rare earth compounding agent are mixed and ball-milled at a weight ratio of 8:5. After ball milling, the mixture is filtered and dried to obtain rare earth functional agent.

[0026] The silicon nitride nanofibers in this embodiment have a diameter of 80 nm, a length of 5 μm, and an aspect ratio of 80:1.

[0027] The preparation method of a semiconductor anti-corrosion ceramic disk material in this embodiment includes the following steps: weighing the raw materials according to the weight parts, wet ball milling the raw materials thoroughly, then pressing and molding them at a molding pressure of 80MPa for 8min to obtain a green body, and then sintering and improving the green body to obtain the ceramic disk material.

[0028] The specific operation steps of the sintering improvement in this embodiment are as follows: Step 1: First, raise the temperature to 570℃ at a rate of 3℃ / min and hold for 1 hour; Step 2: Increase the temperature to 1050℃ at a rate of 5℃ / min and hold for 2 hours, then increase the temperature to 1550℃ at a rate of 1℃ / min and hold for 1 hour. Step 3: Finally, cool down to 750℃ at a rate of 7℃ / min, hold for 15 minutes, and then cool down to room temperature at a rate of 2℃ / min.

[0029] Example 2.

[0030] This embodiment of a semiconductor corrosion-resistant ceramic disk material comprises the following raw materials in parts by weight: 50 parts silicon carbide, 20 parts alumina, 15 parts modified by incorporating hexagonal boron nitride, 5 parts sintering aid, and 4 parts binder.

[0031] In this embodiment, the silicon carbide has a particle size of 150 nm; the alumina is α-alumina, and the specific surface area of ​​α-alumina is 12 m². / g; the sintering aid is magnesium oxide; the binder is polyvinyl alcohol.

[0032] The preparation method of the modified hexagonal boron nitride doped in this embodiment is as follows: S01: Mix 8 parts by weight of hexagonal boron nitride, 30 parts by weight of water and 5 parts by weight of polyethylene glycol evenly, then add 4 parts by weight of pyromellitic anhydride and 2 parts by weight of pyridine and mix for 3 hours at a reaction temperature of 50°C. After the reaction is completed, dry to obtain pretreated hexagonal boron nitride. S02: Dissolve dopamine hydrochloride in water to obtain a dopamine hydrochloride buffer solution with a mass concentration of 0.8 g / mL. Then, mix 7 parts by weight of carbon nanotubes and 12 parts by weight of the dopamine hydrochloride buffer solution thoroughly to obtain a carbon nanotube solution. S03: The pretreated hexagonal boron nitride and carbon nanotube liquid was ultrasonically treated at a weight ratio of 3:7, with an ultrasonic power of 400W for 2 hours. After ultrasonication, the liquid was filtered and dried to obtain the ultrasonic agent of hexagonal boron nitride-carbon nanotube. S04: Hexagonal boron nitride-carbon nanotube ultrasonic agent and zirconium oxide-titanium dioxide combined liquid were mixed and ball-milled at a weight ratio of 11:5 for 2 hours at a ball milling speed of 1200 r / min. After ball milling, the mixture was filtered and dried to obtain the improved body doped with hexagonal boron nitride.

[0033] In this embodiment, hexagonal boron nitride is presented as hexagonal boron nitride nanosheets. The nanosheets have a thickness of 20 nm, a lateral dimension of 3 μm, and a specific surface area of ​​200 m². / g; The carbon nanotubes are multi-walled carbon nanotubes with a diameter of 50 nm and a length of 20 μm.

[0034] The zirconium oxide-titanium dioxide combined solution of this embodiment comprises the following raw materials in parts by weight: The mixture consisted of 8 parts zirconium oxide, 5 parts sodium silicate aqueous solution, 4 parts titanium dioxide, 3 parts yttrium nitrate solution, and 0.6 parts nano-niobium silicide.

[0035] In this embodiment, the sodium silicate aqueous solution has a mass fraction of 5%; the yttrium nitrate solution has a mass fraction of 3%.

[0036] The ceramic disc material in this embodiment also includes 10 parts of rare earth functional agents; The preparation method of the rare earth functional agent is as follows: S11, trifluoropropyldimethoxysilazane, ethanol solvent, acetic acid and deionized water are mixed in a weight ratio of 4:58:2:5 and reacted at 40℃ for 2 hours. After the reaction is completed, a silanol solution is obtained. Silicon nitride nanofibers, nano-tantalum carbide and silanol solution were thoroughly mixed at a weight ratio of 7:2:11 to obtain a silanol solution based on silicon nitride nanofibers. S12, add 6 parts sodium alginate powder and 2 parts β-cyclodextrin to 15 parts N,N dimethylformamide, then add 5 parts rare earth lanthanum oxide and 2 parts rare earth cerium oxide and mix thoroughly. After mixing, filter and dry to obtain rare earth compound agent. S13, based on silicon nitride nanofibers, silanol liquid and rare earth compounding agent are mixed and ball-milled at a weight ratio of 11:5. After ball milling, the mixture is filtered and dried to obtain rare earth functional agent.

[0037] The silicon nitride nanofibers in this embodiment have a diameter of 100 nm, a length of 20 μm, and an aspect ratio of 100:1.

[0038] The preparation method of a semiconductor anti-corrosion ceramic disk material in this embodiment includes the following steps: weighing raw materials according to the weight parts, wet ball milling the raw materials thoroughly, then pressing and molding them at a molding pressure of 120MPa for 10 minutes to obtain a green body, and then sintering and improving the green body to obtain the ceramic disk material.

[0039] The specific operation steps of the sintering improvement in this embodiment are as follows: Step 1: First, raise the temperature to 590℃ at a rate of 5℃ / min and hold for 2 hours; Step 2: Increase the temperature to 1100℃ at a rate of 8℃ / min and hold for 3 hours, then increase the temperature to 1580℃ at a rate of 3℃ / min and hold for 2 hours. Step 3: Finally, cool down to 760℃ at a rate of 9℃ / min, hold for 20 minutes, and then cool down to room temperature at a rate of 4℃ / min.

[0040] Example 3.

[0041] This embodiment of a semiconductor corrosion-resistant ceramic disk material comprises the following raw materials in parts by weight: 47.5 parts silicon carbide, 17.5 parts alumina, 12.5 parts modified by incorporating hexagonal boron nitride, 4 parts sintering aid, and 3 parts binder.

[0042] In this embodiment, the silicon carbide has a particle size of 110 nm; the alumina is α-alumina, and the specific surface area of ​​α-alumina is 10 m². / g; the sintering aid is magnesium oxide; the binder is polyvinyl alcohol.

[0043] The preparation method of the modified hexagonal boron nitride doped in this embodiment is as follows: S01: 6.5 parts by weight of hexagonal boron nitride, 27.5 parts by weight of water, and 3.5 parts by weight of polyethylene glycol are mixed evenly, and then 3 parts by weight of pyromellitic anhydride and 1.5 parts by weight of pyridine are added and the mixture is reacted for 2.5 h at a reaction temperature of 47 °C. After the reaction is completed, the mixture is dried to obtain pretreated hexagonal boron nitride. S02: Dissolve dopamine hydrochloride in water to obtain a dopamine hydrochloride buffer solution with a mass concentration of 0.6 g / mL. Then, mix 5.5 parts by weight of carbon nanotubes and 10 parts by weight of the dopamine hydrochloride buffer solution thoroughly to obtain a carbon nanotube solution. S03: The pretreated hexagonal boron nitride and carbon nanotube liquid was ultrasonically treated at a weight ratio of 3:6, with an ultrasonic power of 375W for 1.5 hours. After ultrasonication, the mixture was filtered and dried to obtain the ultrasonic agent of hexagonal boron nitride-carbon nanotube. S04: Hexagonal boron nitride-carbon nanotube ultrasonic agent and zirconium oxide-titanium dioxide combined liquid were mixed and ball-milled at a weight ratio of 9:5 for 2 hours at a speed of 1100 r / min. After ball milling, the mixture was filtered and dried to obtain the improved product doped with hexagonal boron nitride.

[0044] In this embodiment, hexagonal boron nitride is presented as hexagonal boron nitride nanosheets. The thickness of the hexagonal boron nitride nanosheets is 10 nm, the lateral dimension is 1 μm, and the specific surface area is 150 m². / g; The carbon nanotubes are multi-walled carbon nanotubes with a diameter of 30 nm and a length of 10 μm.

[0045] The zirconium oxide-titanium dioxide combined solution of this embodiment comprises the following raw materials in parts by weight: 6.5 parts zirconium oxide, 4 parts sodium silicate aqueous solution, 3 parts titanium dioxide, 2 parts yttrium nitrate solution and 0.55 parts nano-niobium silicide.

[0046] In this embodiment, the sodium silicate aqueous solution has a mass fraction of 3.5%; the yttrium nitrate solution has a mass fraction of 2.5%.

[0047] The ceramic disc material in this embodiment also includes 8 parts of rare earth functional agents; The preparation method of the rare earth functional agent is as follows: S11, trifluoropropyl dimethoxysilazane, ethanol solvent, acetic acid and deionized water are mixed in a weight ratio of 3:56:2:4 and reacted at 35℃ for 1.5 h. After the reaction is completed, a silanol solution is obtained. Silicon nitride nanofibers, nano-tantalum carbide and silanol solution were thoroughly mixed at a weight ratio of 5.5:2:9 to obtain a silanol solution based on silicon nitride nanofibers. S12, add 4.5 parts sodium alginate powder and 1.5 parts β-cyclodextrin to 12.5 parts N,N dimethylformamide, then add 4 parts rare earth lanthanum oxide and 1.5 parts rare earth cerium oxide and mix thoroughly. After mixing, filter and dry to obtain rare earth compound agent. S13, based on silicon nitride nanofibers, silanol liquid and rare earth compounding agent are mixed and ball-milled at a weight ratio of 9:5. After ball milling, the mixture is filtered and dried to obtain rare earth functional agent.

[0048] The silicon nitride nanofibers in this embodiment have a diameter of 90 nm, a length of 10 μm, and an aspect ratio of 90:1.

[0049] The preparation method of a semiconductor anti-corrosion ceramic disk material in this embodiment includes the following steps: weighing raw materials according to the weight parts, wet ball milling the raw materials thoroughly, then pressing and molding them at a molding pressure of 100MPa for 9 minutes to obtain a green body, and then sintering and improving the green body to obtain the ceramic disk material.

[0050] The specific operation steps of the sintering improvement in this embodiment are as follows: Step 1: First, raise the temperature to 580℃ at a rate of 4℃ / min and hold for 1.5 hours; Step 2: Increase the temperature to 1075℃ at a rate of 6.5℃ / min and hold for 2.5h, then increase the temperature to 1570℃ at a rate of 2℃ / min and hold for 1.5h. Step 3: Finally, cool down to 755℃ at a rate of 8℃ / min, hold for 18 minutes, and then cool down to room temperature at a rate of 3℃ / min.

[0051] Comparative Example 1. Unlike Example 3, this is an improved version without the addition of hexagonal boron nitride dopant.

[0052] Comparative Example 2. Unlike Example 3, the preparation of the improved version doped with hexagonal boron nitride did not include the ultrasonic agent of hexagonal boron nitride-carbon nanotubes.

[0053] Comparative Example 3. Unlike Example 3, carbon nanotube liquid treatment was not used in the preparation of the hexagonal boron nitride-carbon nanotube ultrasonic agent.

[0054] Comparative Example 4. Unlike Example 3, in the preparation of the ultrasonic agent for hexagonal boron nitride-carbon nanotubes, the pretreated hexagonal boron nitride was directly replaced by hexagonal boron nitride raw material.

[0055] Comparative Example 5. Unlike Example 3, the zirconium oxide-titanium dioxide combined solution was not added in the preparation of the improved body doped with hexagonal boron nitride.

[0056] Comparative Example 6. Unlike Example 3, neither zirconium oxide nor titanium dioxide was added in the preparation of the zirconium oxide-titanium dioxide combined solution.

[0057] Comparative Example 7. Unlike Example 3, yttrium nitrate solution and nano-niobium silicide were not added in the preparation of the zirconium oxide-titanium dioxide combined solution.

[0058] Comparative Example 8. Unlike Example 3, no rare earth functional agents were added.

[0059] Comparative Example 9. Unlike Example 3, no rare earth compounding agent was added in the preparation of the rare earth functional agent.

[0060] Comparative Example 10. Unlike Example 3, sodium alginate powder and β-cyclodextrin were not added in the preparation of the rare earth compound.

[0061] Comparative Example 11. Unlike Example 3, lanthanum oxide and cerium oxide were not added in the preparation of the rare earth compound.

[0062] Comparative Example 12. Unlike Example 3, silicon nitride nanofibers and nano-tantalum carbide were not added in the preparation of the silanol liquid based on silicon nitride nanofibers.

[0063] Comparative Example 13. The difference from Example 3 is that the specific conditions of the sintering process are different. In step one, the temperature is first raised to 580°C at a rate of 4°C / min and held for 1.5 hours; then the temperature is raised to 1570°C at a rate of 2°C / min and held for 1.5 hours; finally, the temperature is lowered to room temperature at a rate of 3°C / min.

[0064] The products of Examples 1-3 and Comparative Examples 1-13 were subjected to routine performance tests. The tests included the crack resistance, bending resistance, insulation, and Vickers hardness of the semiconductor ceramic disks, as well as the corrosion resistance and high-temperature stability (placed in 5% hydrochloric acid mist for 12 hours, then placed at 75°C for 12 hours; this constituted one cycle, repeated 10 times). The test results are as follows. As can be seen from Comparative Examples 1-13 and Examples 1-3, the product of Example 3 has excellent crack resistance, bending resistance, insulation and Vickers hardness, excellent overall coordination, and significant anti-corrosion and high-temperature stability. The performance of the product is significantly worse and its corrosion resistance and high-temperature stability are significantly reduced when neither the improved hexagonal boron nitride nor the rare earth functional agent is added. By using the two in combination, the product's performance is significantly improved. At the same time, the performance of the product also tends to deteriorate depending on the specific conditions of the sintering process. By using the specific process and specific raw materials of this invention, the performance of the product is significantly improved. In the preparation of the improved hexagonal boron nitride-doped body, no hexagonal boron nitride-carbon nanotube ultrasonic agent was added; in the preparation of the hexagonal boron nitride-carbon nanotube ultrasonic agent, no carbon nanotube liquid treatment was used; in the preparation of the hexagonal boron nitride-carbon nanotube ultrasonic agent, the pretreated hexagonal boron nitride was directly replaced by hexagonal boron nitride raw material; in the preparation of the improved hexagonal boron nitride-doped body, no zirconium oxide-titanium dioxide combined liquid was added; in the preparation of the zirconium oxide-titanium dioxide combined liquid, no zirconium oxide and titanium dioxide were added; in the preparation of the zirconium oxide-titanium dioxide combined liquid, no yttrium nitrate solution and nano-niobium silicide were added; the performance of the products all showed a trend of deterioration to varying degrees. The ultrasonic agent of hexagonal boron nitride-carbon nanotubes obtained by the specific method of this invention is coordinated and optimized with the zirconium oxide-titanium dioxide combined liquid. The modified body doped with hexagonal boron nitride has a significant effect on improving the functionality of the product. The preparation of the zirconium oxide-titanium dioxide combined liquid and the ultrasonic agent of hexagonal boron nitride-carbon nanotubes are both unique. The technical solution of this invention has the best effect. In the preparation of rare earth functional agents, no rare earth compounding agent was added; in the preparation of rare earth compounding agent, no sodium alginate powder or β-cyclodextrin was added; in the preparation of rare earth compounding agent, no rare earth lanthanum oxide or rare earth cerium oxide was added; and in the preparation of silanol liquid based on silicon nitride nanofibers, no silicon nitride nanofibers or nano tantalum carbide were added. The performance of the products all tended to deteriorate. Only the rare earth compounding agent prepared by the method of this invention, combined with the silanol liquid based on silicon nitride nanofibers, showed the most significant performance effect. Meanwhile, the inventors of this invention also discovered that when silicon nitride nanofibers and tantalum carbide nanofibers were not added during the preparation of silanol liquid based on silicon nitride nanofibers, the performance of the product tended to deteriorate significantly. Silicon nitride nanofibers and tantalum carbide nanofibers significantly promoted the performance of the product.

[0065] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the invention can be implemented in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, it is intended that all variations falling within the meaning and scope of equivalents of the claims be included within the present invention.

[0066] Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. A semiconductor corrosion-resistant ceramic disk material, characterized in that, Including the following parts by weight of raw materials: 45-50 parts silicon carbide, 15-20 parts alumina, 10-15 parts modified by incorporating hexagonal boron nitride, 3-5 parts sintering aid, and 2-4 parts binder.

2. The semiconductor corrosion-resistant ceramic disk material according to claim 1, characterized in that, The silicon carbide has a particle size of 80-150 nm; the alumina is α-alumina with a specific surface area of ​​8-12 m². / g; the sintering aid is magnesium oxide; the binder is polyvinyl alcohol.

3. The semiconductor corrosion-resistant ceramic disk material according to claim 1, characterized in that, The preparation method of the modified hexagonal boron nitride-doped body is as follows: S01: Mix 5-8 parts by weight of hexagonal boron nitride, 25-30 parts by weight of water, and 2-5 parts by weight of polyethylene glycol evenly. Then add 2-4 parts by weight of pyromellitic anhydride and 1-2 parts by weight of pyridine and react for 2-3 hours at a reaction temperature of 45-50℃. After the reaction is completed, dry to obtain pretreated hexagonal boron nitride. S02: Dissolve dopamine hydrochloride in water to obtain a dopamine hydrochloride buffer solution with a mass concentration of 0.5-0.8 g / mL. Then, mix 4-7 parts by weight of carbon nanotubes and 8-12 parts by weight of the dopamine hydrochloride buffer solution thoroughly to obtain a carbon nanotube solution. S03: The pretreated hexagonal boron nitride and carbon nanotube liquid is ultrasonically treated at a weight ratio of 3:(5-7), with an ultrasonic power of 350-400W, for 1-2 hours. After ultrasonic treatment, the liquid is filtered and dried to obtain the ultrasonic agent of hexagonal boron nitride-carbon nanotube. S04: Hexagonal boron nitride-carbon nanotube ultrasonic agent and zirconium oxide-titanium dioxide combined liquid were mixed and ball-milled at a weight ratio of (8-11):

5. The ball milling speed was 1000-1200 r / min and the ball milling time was 2 h. After the ball milling was completed, the mixture was filtered and dried to obtain the improved body doped with hexagonal boron nitride.

4. The semiconductor corrosion-resistant ceramic disk material according to claim 3, characterized in that, The hexagonal boron nitride is in the form of hexagonal boron nitride nanosheets, with a sheet thickness of 5–20 nm, a lateral dimension of 0.5–3 μm, and a specific surface area of ​​100–200 m². / g; The carbon nanotubes are multi-walled carbon nanotubes with a diameter of 10–50 nm and a length of 5–20 μm.

5. The semiconductor corrosion-resistant ceramic disk material according to claim 3, characterized in that, The zirconium oxide-titanium dioxide combined solution comprises the following raw materials in parts by weight: The mixture consists of 5-8 parts zirconium oxide, 3-5 parts sodium silicate aqueous solution, 2-4 parts titanium dioxide, 1-3 parts yttrium nitrate solution, and 0.5-0.6 parts nano-niobium silicide.

6. The semiconductor corrosion-resistant ceramic disk material according to claim 5, characterized in that, The sodium silicate aqueous solution has a mass fraction of 2-5%; the yttrium nitrate solution has a mass fraction of 2-3%.

7. The semiconductor corrosion-resistant ceramic disk material according to claim 1, characterized in that, The ceramic disc material also includes 6-10 parts of rare earth functional agents; The preparation method of the rare earth functional agent is as follows: S11, trifluoropropyl dimethoxysilazane, ethanol solvent, acetic acid and deionized water are mixed and reacted in a weight ratio of (2-4):(55-58):2:(3-5), the reaction temperature is 30-40℃, the reaction is carried out for 1-2 hours, and the reaction is completed to obtain silanol solution. Silicon nitride nanofibers, nano-tantalum carbide and silanol solution were thoroughly mixed in a weight ratio of (4-7):2:(8-11) to obtain a silanol solution based on silicon nitride nanofibers. S12, add 3-6 parts of sodium alginate powder and 1-2 parts of β-cyclodextrin to 10-15 parts of N,N dimethylformamide, then add 3-5 parts of rare earth lanthanum oxide and 1-2 parts of rare earth cerium oxide and mix thoroughly. After mixing, filter and dry to obtain rare earth compound agent. S13, based on silicon nitride nanofibers, silanol liquid and rare earth compounding agent are mixed and ball-milled at a weight ratio of (8-11):

5. After ball milling, the mixture is filtered and dried to obtain rare earth functional agent.

8. The semiconductor corrosion-resistant ceramic disk material according to claim 7, characterized in that, The silicon nitride nanofibers have a diameter of 80-100 nm, a length of 5-20 μm, and an aspect ratio of (80-100):

1.

9. The method for preparing a semiconductor corrosion-resistant ceramic disk material according to any one of claims 1 to 8, characterized in that, The process includes the following steps: weighing the raw materials according to their weight proportions, wet ball milling the raw materials thoroughly, then pressing them into shape at a pressure of 80-120 MPa for 8-10 minutes to obtain a green body, which is then sintered and improved to obtain the ceramic disc material.

10. A semiconductor corrosion-resistant ceramic disk material according to claim 9, characterized in that, The specific operational steps for the sintering improvement are as follows: Step 1: First, raise the temperature to 570-590℃ at a rate of 3-5℃ / min and hold for 1-2 hours; Step 2: Increase the temperature to 1050-1100℃ at a rate of 5-8℃ / min and hold for 2-3 hours. Then increase the temperature to 1550-1580℃ at a rate of 1-3℃ / min and hold for 1-2 hours. Step 3: Finally, cool down to 750-760℃ at a rate of 7-9℃ / min, hold for 15-20 minutes, and then cool down to room temperature at a rate of 2-4℃ / min.

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