A method for manufacturing an inner flow channel silicon carbide vacuum chuck

Abstract

The application relates to the technical field of silicon carbide ceramic material processing, and particularly discloses a manufacturing method of a silicon carbide vacuum chuck with an inner flow channel, which comprises the following steps: dispersing functionalized nanometer silicon carbide in a mixed solution of acrylamide and N-hydroxyethyl acrylamide aqueous solution to obtain a premixed slurry; adding an initiator solution and an accelerator into the premixed slurry, stirring and reacting for 2.6-3.4 hours to obtain modified ceramic slurry; coating a release agent on the inner side wall of a mold, injecting the modified ceramic slurry, standing for forming, demolding and drying to obtain a green body, and then performing reaction sintering, fine grinding and polishing to obtain the silicon carbide vacuum chuck with the inner flow channel; in the application, the functionalized nanometer silicon carbide is prepared through chemical bonding of epoxy-based nanometer silicon carbide and reinforcing components, so that the compactness and mechanical properties of the silicon carbide vacuum chuck are improved.

Description

Technical Field

[0001] This application relates to the field of silicon carbide ceramic material processing technology, and more specifically, it relates to a method for manufacturing a silicon carbide vacuum chuck with an internal flow channel. Background Technology

[0002] Silicon carbide vacuum chucks are key components in semiconductor manufacturing used to stabilize and hold wafers, especially suitable for the high-temperature, high-speed processing environments of third-generation semiconductor materials such as silicon carbide wafers. Because they directly affect wafer processing accuracy, yield, and production efficiency, they have received widespread attention from industry and academia in recent years.

[0003] In existing technologies, when preparing silicon carbide vacuum chucks with complex internal flow channels, paraffin wax is often used to fill the flow channels, combined with lamination or cold isostatic pressing. However, at complex structures such as the flow channel tips, stress concentration occurs due to the contact and extrusion of silicon carbide micropowder with the mold, leading to cracks on the surface of the green blank and the formation of silicon line defects after reaction sintering. In addition, the BN barrier agent pre-added into the flow channels may not be applied evenly or effectively, failing to prevent the silicon melt from penetrating. As a result, the flow channels are blocked by the penetrating silicon beads after sintering, resulting in low green blank strength, easy deformation, and affecting the final accuracy of the vacuum chuck.

[0004] Therefore, there is an urgent need to develop a silicon carbide vacuum chuck with high mechanical strength and excellent dimensional stability to break through the bottlenecks of existing technologies in terms of materials, processes and performance, and meet the stringent requirements of high-end equipment for core components. Summary of the Invention

[0005] To address the problems mentioned in the background section, this application provides a method for manufacturing a silicon carbide vacuum chuck with an internal flow channel.

[0006] A method for manufacturing a silicon carbide vacuum chuck with an internal flow channel includes the following steps:

[0007] Step S1: Disperse functionalized nano-silicon carbide ultrasonically in a mixed solution of acrylamide and N-hydroxyethylacrylamide aqueous solution to obtain a premixed slurry, wherein the mass ratio of functionalized nano-silicon carbide to the mixed solution is 0.8-1.2:20-30, and the mass ratio of acrylamide to N-hydroxyethylacrylamide aqueous solution in the mixed solution is 1:10-12.

[0008] Step S2: Add the initiator solution and accelerator to the premixed slurry prepared in step S1, stir evenly, heat to 72-76℃, stir and react for 2.6-3.4h, degas, and obtain modified ceramic slurry. The mass ratio of initiator solution, accelerator and premixed slurry is 0.4-0.6:0.02-0.04:40-50.

[0009] Step S3: Coat the inner wall of the mold with a release agent, inject the modified ceramic slurry from step S2 into the mold, let it stand to form, demold and dry to obtain a green body, sinter it by reaction, and then perform fine grinding and polishing to obtain a silicon carbide vacuum chuck with an internal flow channel.

[0010] Preferably, in step S1, the mass fraction of the N-hydroxyethylacrylamide aqueous solution is 0.2-0.4%.

[0011] Preferably, in step S2, the initiator solution is an aqueous solution of ammonium persulfate with a mass fraction of 12-16%.

[0012] Preferably, in step S2, the accelerator is tetramethylethylenediamine.

[0013] Preferably, in step S3, the mold is a stainless steel mold made of SUS304.

[0014] Preferably, in step S3, the static molding temperature is 42-46℃ and the static molding time is 3-5h.

[0015] Preferably, in step S3, the mass of the release agent is 0.24-0.28% of the mass of the modified ceramic slurry.

[0016] Preferably, in step S3, the release agent is dimethyl silicone oil.

[0017] Preferably, in step S3, the temperature for demolding and drying is 52-58℃, and the time is 22-24h.

[0018] Preferably, the reaction sintering process in step S3 specifically involves: placing the green blank into a high-temperature sintering furnace for silicon diffusion reaction sintering, controlling the mass ratio of green blank to metallic silicon to be 1:0.66-0.74, heating to 1540-1600℃ at a heating rate of 10-20℃ / min, and holding at that temperature for 3.6-4.2h.

[0019] Preferably, the method for preparing the functionalized nano-silicon carbide includes the following steps:

[0020] Step A1: Mix coupling agent KH-560, anhydrous ethanol, and deionized water evenly, adjust the pH to 8-9, stir for 5-10 min, add nano-silicon carbide, heat to 60-66℃, stir and react for 4-5 h, filter, wash and dry to obtain epoxidized nano-silicon carbide. The mass ratio of coupling agent KH-560, anhydrous ethanol, deionized water, and nano-silicon carbide is 0.3-0.5:35-45:4-6:2.4-3. In the above reaction process, nano-silicon carbide is first treated with KH-560 to obtain epoxy-based nano-silicon carbide.

[0021] Step A2: Ultrasonically disperse epoxy-based nano-silicon carbide, reinforcing components, and anhydrous DMF until uniform. Add potassium hydroxide, heat to 82-86℃, stir and react for 3.6-4.8 hours, filter, wash, and dry to obtain functionalized nano-silicon carbide. The mass ratio of epoxy-based nano-silicon carbide, reinforcing components, anhydrous DMF, and potassium hydroxide is 2.4-2.8:0.6-0.8:40-50:1.2-1.6. Under alkaline conditions, the epoxy groups on the epoxy-based silicon carbide can undergo a ring-opening reaction with the reinforcing components to obtain functionalized nano-silicon carbide.

[0022] Preferably, the reinforcing component is prepared by the following steps:

[0023] Step B1: Place the carbon fiber in acetone and stir at 50-54℃ for 8-12 hours. Remove, wash, and then place in a 66-68% nitric acid solution. Stir at 82-86℃ for 2.6-3.2 hours. Filter and wash until the washing solution is neutral to obtain pretreated carbon fiber. The mass ratio of carbon fiber to acetone is 3-5:40, and the mass ratio of carbon fiber to nitric acid solution is 5:50-60. Use acetone to wash away impurities on the surface of the carbon fiber, and then oxidize it with nitric acid solution to increase the oxygen-containing groups on the surface of the carbon fiber.

[0024] Step B2: Add pretreated carbon fiber, α-acetaminocinnamic acid, and p-toluenesulfonic acid to anhydrous DMF, stir evenly, heat to 90-110℃ under nitrogen protection, stir and react for 18-20 hours, let stand for 4-6 hours, filter, wash, and dry to obtain the reinforcing component. The mass ratio of pretreated carbon fiber, α-acetaminocinnamic acid, p-toluenesulfonic acid, and anhydrous DMF is 1:0.3-0.5:0.02-0.04:80-100. In the above reaction process, p-toluenesulfonic acid is used as an accelerator and anhydrous DMF is used as a solvent. The hydroxyl groups on the surface of the pretreated carbon fiber undergo an esterification reaction with α-acetaminocinnamic acid, so that the surface of the pretreated carbon fiber is grafted with a reinforcing component containing ester groups and unsaturated double bonds.

[0025] Compared with the prior art, this application has the following beneficial effects:

[0026] (1) In the technical solution of the present invention, functionalized nano-silicon carbide, acrylamide, N-hydroxyethylacrylamide and initiator are mixed and reacted to form a modified ceramic slurry with a three-dimensional network structure. In the process of preparing silicon carbide vacuum chuck, the modified ceramic slurry with a three-dimensional network structure is carbonized to form a dense nano-carbon network. The nano-carbon network can not only absorb stress to avoid cracking, but also the functionalized nano-silicon carbide can form hydrogen bond with the active amide groups on acrylamide and N-hydroxyethylacrylamide, embedding into the three-dimensional network structure of the nano-carbon network, increasing the crosslinking density, improving the mechanical properties of the silicon carbide vacuum chuck, and increasing its density.

[0027] (2) In the technical solution of the present invention, functionalized nano-silicon carbide is added. The functionalized nano-silicon carbide is prepared by chemical bonding of epoxy-based nano-silicon carbide and reinforcing components. On the one hand, it can give full play to the excellent physical properties of nano-silicon carbide itself and thus improve the mechanical strength of silicon carbide vacuum chuck. On the other hand, the carbon fibers grafted on the surface of functionalized nano-silicon carbide can serve as a reinforcing phase. With its high tensile strength, it can inhibit the propagation and penetration of cracks and enhance its shrinkage resistance. At the same time, it can improve the mechanical strength of silicon carbide vacuum chuck. Moreover, functionalized nano-silicon carbide can also act as a carbon source during high-temperature sintering and react with molten silicon to form silicon carbide in situ, thereby improving the mechanical strength of silicon carbide vacuum chuck. α-acetaminocinnamic acid has a rigid benzene ring structure and amide group structure. When it is introduced into functionalized nano-silicon carbide, it can play a synergistic role with epoxy-based nano-silicon carbide to improve the mechanical properties and density of silicon carbide vacuum chuck. Detailed Implementation

[0028] To make the implementation methods of this application easier to understand, the application will be described in detail below with reference to specific embodiments. These embodiments are for illustrative purposes only and are not limited to the application scope of this application.

[0029] The specific parameters of the raw materials used in this invention are as follows:

[0030] Nano-silicon carbide, particle size / mesh: 3000 mesh, supplied by Qinghe County Chaotai Metal Materials Co., Ltd., grade SF93; acrylamide and N-hydroxyethyl acrylamide were purchased from Aladdin Reagent Network; carbon fiber, item number 10011, supplied by Toray New Materials (Guangdong) Co., Ltd.; dimethyl silicone oil, CAS number: 63148-62-9, product number: D817599, supplied by Shanghai Maclean Biochemical Technology Co., Ltd.

[0031] Preparation Examples 1-3 and Comparative Preparation Examples 1-3 provide an enhancing component.

[0032] Preparation Example 1

[0033] This preparation example provides a reinforcing component, which is prepared by the following steps:

[0034] Carbon fibers were placed in acetone and stirred at 50°C and 500 rpm for 12 hours. After stirring, the fibers were removed, washed with deionized water, and then placed in a 66% nitric acid solution and stirred at 80°C and 600 rpm for 3.2 hours. The mixture was then filtered and washed with deionized water until the washing solution was neutral to obtain pretreated carbon fibers. The mass ratio of carbon fibers to acetone was 3:40, and the mass ratio of carbon fibers to 66% nitric acid solution was 5:50.

[0035] Step B2: Add pretreated carbon fiber, α-acetaminocinnamic acid, and p-toluenesulfonic acid to anhydrous DMF. Stir at 650 rpm for 20 min until homogeneous. Under nitrogen protection, heat to 90°C, maintain constant stirring speed, and continue stirring for 20 h. Let stand for 4 h, filter, wash with deionized water until neutral, and dry at 65°C to constant weight to obtain the reinforcing component. The mass ratio of pretreated carbon fiber, α-acetaminocinnamic acid, p-toluenesulfonic acid, and anhydrous DMF is 1:0.3:0.02:80.

[0036] Preparation Example 2

[0037] This preparation example provides a reinforcing component, which is prepared by the following steps:

[0038] Step B1: Place the carbon fiber in acetone and stir at 52°C and 550 rpm for 10 hours. Remove the carbon fiber, wash it with deionized water, and then place it in a 67% nitric acid solution and stir at 84°C and 650 rpm for 2.9 hours. Filter the solution and wash it with deionized water until the washing solution is neutral to obtain pretreated carbon fiber. The mass ratio of carbon fiber to acetone is 4:40, and the mass ratio of carbon fiber to 67% nitric acid solution is 5:55.

[0039] Step B2: Add the pretreated carbon fiber, α-acetaminocinnamic acid, and p-toluenesulfonic acid to anhydrous DMF. Stir at 700 rpm for 16 min until homogeneous. Under nitrogen protection, heat to 100℃ and maintain the stirring speed for 19 h. Let stand for 5 h, filter, wash with deionized water until neutral, and dry at 70℃ to constant weight to obtain the reinforcing component. The mass ratio of pretreated carbon fiber, α-acetaminocinnamic acid, p-toluenesulfonic acid, and anhydrous DMF is 1:0.4:0.03:90.

[0040] Preparation Example 3

[0041] This preparation example provides a reinforcing component, which is prepared by the following steps:

[0042] Step B1: Place the carbon fiber in acetone and stir at 54°C and 6000 rpm for 8 hours. Remove the carbon fiber, wash it with deionized water, and then place it in 68% concentrated nitric acid and stir at 86°C and 700 rpm for 2.6 hours. Filter the mixture and wash it with deionized water until the washing solution is neutral to obtain pretreated carbon fiber. The mass ratio of carbon fiber to acetone is 5:40, and the mass ratio of carbon fiber to 68% concentrated nitric acid is 5:60.

[0043] Step B2: Add pretreated carbon fiber, α-acetaminocinnamic acid, and p-toluenesulfonic acid to anhydrous DMF. Stir at 750 rpm for 12 minutes until homogeneous. Under nitrogen protection, heat to 110°C and maintain the stirring speed for 18 hours. Let stand for 6 hours, filter, wash with deionized water until neutral, and dry at 75°C to constant weight to obtain the reinforcing component. The mass ratio of pretreated carbon fiber, α-acetaminocinnamic acid, p-toluenesulfonic acid, and anhydrous DMF is 1:0.5:0.04:100.

[0044] Comparative Preparation Example 1

[0045] This comparative preparation example provides a reinforcing component, which is prepared by the following steps:

[0046] Carbon fibers were placed in acetone and stirred at 50°C and 500 rpm for 12 hours. After stirring, the fibers were removed, washed with deionized water, and then placed in a 66% ethanol aqueous solution and stirred at 80°C and 600 rpm for 3.2 hours. The mixture was then filtered and washed with deionized water until the washing solution was neutral to obtain pretreated carbon fibers. The mass ratio of carbon fibers to acetone was 3:40, and the mass ratio of carbon fibers to 66% nitric acid solution was 5:50.

[0047] Step B2: Add pretreated carbon fiber, α-acetaminocinnamic acid, and p-toluenesulfonic acid to anhydrous DMF. Stir at 650 rpm for 20 min until homogeneous. Under nitrogen protection, heat to 90°C, maintain constant stirring speed, and continue stirring for 20 h. Let stand for 4 h, filter, wash with deionized water until neutral, and dry at 65°C to constant weight to obtain the reinforcing component. The mass ratio of pretreated carbon fiber, α-acetaminocinnamic acid, p-toluenesulfonic acid, and anhydrous DMF is 1:0.3:0.02:80.

[0048] Comparative Preparation Example 2

[0049] This comparative preparation example provides a reinforcing component, which is prepared by the following steps:

[0050] Carbon fibers were placed in acetone and stirred at 50°C and 500 rpm for 12 hours. After stirring, the fibers were removed, washed with deionized water, and then placed in a 66% nitric acid solution and stirred at 80°C and 600 rpm for 3.2 hours. The mixture was then filtered and washed with deionized water until the washing solution was neutral to obtain pretreated carbon fibers. The mass ratio of carbon fibers to acetone was 3:40, and the mass ratio of carbon fibers to 66% nitric acid solution was 5:50.

[0051] Step B2: Add the pretreated carbon fiber, α-methylcinnamic acid, and p-toluenesulfonic acid to anhydrous DMF, and stir at 650 rpm for 20 min until homogeneous. Under nitrogen protection, heat to 90°C, maintain the stirring speed, and continue stirring for 20 h. Let stand for 4 h, filter, wash with deionized water until neutral, and dry at 65°C to constant weight to obtain the reinforcing component. The mass ratio of pretreated carbon fiber, α-methylcinnamic acid, p-toluenesulfonic acid, and anhydrous DMF is 1:0.3:0.02:80.

[0052] Comparative preparation example 3

[0053] This comparative preparation example provides a reinforcing component, which is prepared by the following steps:

[0054] Carbon fibers were placed in acetone and stirred at 50°C and 500 rpm for 12 hours. After stirring, the fibers were removed, washed with deionized water, and then placed in a 66% nitric acid solution and stirred at 80°C and 600 rpm for 3.2 hours. The mixture was then filtered and washed with deionized water until the washing solution was neutral to obtain pretreated carbon fibers. The mass ratio of carbon fibers to acetone was 3:40, and the mass ratio of carbon fibers to 66% nitric acid solution was 5:50.

[0055] Step B2: Add the pretreated carbon fiber, 3-phenylpropionic acid, and p-toluenesulfonic acid to anhydrous DMF. Stir at 650 rpm for 20 minutes until homogeneous. Under nitrogen protection, heat to 90°C and maintain the stirring speed for 20 hours. Let stand for 4 hours, filter, wash with deionized water until neutral, and dry at 65°C to constant weight to obtain the reinforcing component. The mass ratio of pretreated carbon fiber, 3-phenylpropionic acid, p-toluenesulfonic acid, and anhydrous DMF is 1:0.3:0.02:80.

[0056] Preparation Examples 4-6 and Comparative Preparation Examples 4-6 provide a functionalized silicon carbide nanoparticle.

[0057] Preparation Example 4

[0058] This preparation example provides a functionalized silicon carbide nanoparticle, and the preparation method of the functionalized silicon carbide nanoparticle includes the following steps:

[0059] Step A1: Coupling agent KH-560, anhydrous ethanol, and deionized water are stirred at 500 rpm for 20 min until homogeneous. The pH is adjusted to 8 with a 0.2 M sodium carbonate aqueous solution. Stirring continues for 5 min. Nano-silicon carbide is added, and the temperature is raised to 60℃. The stirring speed is maintained and the reaction continues for 5 h. The mixture is filtered and washed three times each with anhydrous ethanol and deionized water. It is then dried at 55℃ to constant weight to obtain epoxidized nano-silicon carbide. The mass ratio of coupling agent KH-560, anhydrous ethanol, deionized water, and nano-silicon carbide is 0.3:35:4:2.4.

[0060] Step A2: The epoxy-based nano-silicon carbide, the reinforcing component prepared in Example 1, and anhydrous DMF were ultrasonically sonicated at a frequency of 30 kHz and a power of 400 W for 40 min until uniformly dispersed. Potassium hydroxide was added, the temperature was raised to 82 °C, the stirring speed was controlled at 550 rpm, and the reaction was stirred for 4.8 h. After filtration, the nano-silicon carbide was washed three times each with anhydrous ethanol and deionized water, and dried at 55 °C to constant weight to obtain functionalized nano-silicon carbide. The mass ratio of epoxy-based nano-silicon carbide, reinforcing component, anhydrous DMF, and potassium hydroxide was 2.4:0.6:40:1.2.

[0061] Preparation Example 5

[0062] This preparation example provides a functionalized silicon carbide nanoparticle, and the preparation method of the functionalized silicon carbide nanoparticle includes the following steps:

[0063] Step A1: Coupling agent KH-560, anhydrous ethanol, and deionized water are stirred at 600 rpm for 18 min until homogeneous. Then, 0.35 M sodium carbonate aqueous solution is added and stirring is continued for 7 min. Nano-silicon carbide is added, the temperature is raised to 63℃, and the stirring speed is maintained at a constant speed for 4.5 h. The mixture is then filtered and washed 4 times each with anhydrous ethanol and deionized water. Finally, it is dried at 60℃ to constant weight to obtain epoxidized nano-silicon carbide. The mass ratio of coupling agent KH-560, anhydrous ethanol, deionized water, and nano-silicon carbide is 0.4:40:5:2.7.

[0064] Step A2: The epoxy-based nano-silicon carbide, the reinforcing component prepared in Example 2, and anhydrous DMF were ultrasonically sonicated at a frequency of 35 kHz and a power of 450 W for 35 min until uniformly dispersed. Potassium hydroxide was added, the temperature was raised to 84 °C, the stirring speed was controlled at 600 rpm, and the reaction was stirred for 4.2 h. After filtration, the nano-silicon carbide was washed four times each with anhydrous ethanol and deionized water, and dried at 60 °C to constant weight to obtain functionalized nano-silicon carbide. The mass ratio of epoxy-based nano-silicon carbide, reinforcing component, anhydrous DMF, and potassium hydroxide was 2.6:0.7:45:1.4.

[0065] Preparation Example 6

[0066] This preparation example provides a functionalized silicon carbide nanoparticle, and the preparation method of the functionalized silicon carbide nanoparticle includes the following steps:

[0067] Step A1: Coupling agent KH-560, anhydrous ethanol, and deionized water are stirred at 650 rpm for 16 min until homogeneous. The pH is adjusted to 9 with a 0.5 M sodium carbonate aqueous solution. Stirring continues for 5 min. Nano-silicon carbide is added, and the temperature is raised to 66℃. The stirring speed is maintained and the reaction continues for 4 h. The mixture is filtered and washed 5 times each with anhydrous ethanol and deionized water. It is then dried at 65℃ to constant weight to obtain epoxidized nano-silicon carbide. The mass ratio of coupling agent KH-560, anhydrous ethanol, deionized water, and nano-silicon carbide is 0.5:45:6:3.

[0068] Step A2: The epoxy-based nano-silicon carbide, the reinforcing component prepared in Example 3, and anhydrous DMF were ultrasonically dispersed for 30 minutes at an ultrasonic frequency of 40 kHz and an ultrasonic power of 500 W. Potassium hydroxide was added, the temperature was raised to 86 °C, the stirring speed was controlled at 650 rpm, and the reaction was stirred for 3.6 h. The mixture was filtered, washed 5 times each with anhydrous ethanol and deionized water, and dried at 65 °C to constant weight to obtain functionalized nano-silicon carbide. The mass ratio of epoxy-based nano-silicon carbide, reinforcing component, anhydrous DMF, and potassium hydroxide was 2.8:0.8:50:1.6.

[0069] Comparative preparation example 4

[0070] This comparative preparation example provides a functionalized silicon carbide nanoparticle, the preparation method of which includes the following steps:

[0071] Step A1: The coupling agent KH-560, anhydrous ethanol, and deionized water were stirred at 500 rpm for 20 min until homogeneous. The pH was adjusted to 8 with a 0.2 M sodium carbonate aqueous solution. The stirring was continued for 5 min. Nano-silicon carbide was added, and the temperature was raised to 60 °C. The stirring speed was maintained and the reaction was continued for 5 h. The mixture was filtered, washed three times each with anhydrous ethanol and deionized water, and dried at 55 °C to constant weight to obtain epoxidized nano-silicon carbide. The mass ratio of coupling agent KH-560, anhydrous ethanol, deionized water, and nano-silicon carbide was 0.3:35:4:2.4.

[0072] Step A2: The epoxy-based nano-silicon carbide, the reinforcing component prepared in Comparative Preparation Example 1, and anhydrous DMF were ultrasonically sonicated at a frequency of 30 kHz and an ultrasonic power of 400 W for 40 min until uniformly dispersed. Potassium hydroxide was added, the temperature was raised to 82 °C, the stirring speed was controlled at 550 rpm, and the reaction was stirred for 4.8 h. After filtration, the nano-silicon carbide was washed three times each with anhydrous ethanol and deionized water, and dried at 55 °C to constant weight to obtain functionalized nano-silicon carbide. The mass ratio of epoxy-based nano-silicon carbide, reinforcing component, anhydrous DMF, and potassium hydroxide was 2.4:0.6:40:1.2.

[0073] Comparative preparation example 5

[0074] This comparative preparation example provides a functionalized silicon carbide nanoparticle, the preparation method of which includes the following steps:

[0075] Step A1: Coupling agent KH-560, anhydrous ethanol, and deionized water are stirred at 500 rpm for 20 min until homogeneous. The pH is adjusted to 8 with a 0.2 M sodium carbonate aqueous solution. Stirring continues for 5 min. Nano-silicon carbide is added, and the temperature is raised to 60℃. The stirring speed is maintained and the reaction continues for 5 h. The mixture is filtered and washed three times each with anhydrous ethanol and deionized water. It is then dried at 55℃ to constant weight to obtain epoxidized nano-silicon carbide. The mass ratio of coupling agent KH-560, anhydrous ethanol, deionized water, and nano-silicon carbide is 0.3:35:4:2.4.

[0076] Step A2: The epoxy-based nano-silicon carbide, the reinforcing component prepared in Comparative Preparation Example 2, and anhydrous DMF were ultrasonically sonicated at a frequency of 30 kHz and an ultrasonic power of 400 W for 40 min until uniformly dispersed. Potassium hydroxide was added, the temperature was raised to 82 °C, the stirring speed was controlled at 550 rpm, and the reaction was stirred for 4.8 h. After filtration, the nano-silicon carbide was washed three times each with anhydrous ethanol and deionized water, and dried at 55 °C to constant weight to obtain functionalized nano-silicon carbide. The mass ratio of epoxy-based nano-silicon carbide, reinforcing component, anhydrous DMF, and potassium hydroxide was 2.4:0.6:40:1.2.

[0077] Comparative preparation example 6

[0078] This comparative preparation example provides a functionalized silicon carbide nanoparticle, the preparation method of which includes the following steps:

[0079] Step A1: Coupling agent KH-560, anhydrous ethanol, and deionized water are stirred at 500 rpm for 20 min until homogeneous. The pH is adjusted to 8 with a 0.2 M sodium carbonate aqueous solution. Stirring continues for 5 min. Nano-silicon carbide is added, and the temperature is raised to 60℃. The stirring speed is maintained and the reaction continues for 5 h. The mixture is filtered and washed three times each with anhydrous ethanol and deionized water. It is then dried at 55℃ to constant weight to obtain epoxidized nano-silicon carbide. The mass ratio of coupling agent KH-560, anhydrous ethanol, deionized water, and nano-silicon carbide is 0.3:35:4:2.4.

[0080] Step A2: The epoxy-based nano-silicon carbide, the reinforcing component prepared in Comparative Preparation Example 3, and anhydrous DMF were ultrasonically dispersed for 40 min at an ultrasonic frequency of 30 kHz and an ultrasonic power of 400 W. Potassium hydroxide was added, the temperature was raised to 82 °C, the stirring speed was controlled at 550 rpm, and the reaction was stirred for 4.8 h. The mixture was filtered, washed three times each with anhydrous ethanol and deionized water, and dried at 55 °C to constant weight to obtain functionalized nano-silicon carbide. The mass ratio of epoxy-based nano-silicon carbide, reinforcing component, anhydrous DMF, and potassium hydroxide was 2.4:0.6:40:1.2.

[0081] Examples 1-3 and Comparative Examples 1-3 provide a method for manufacturing a silicon carbide vacuum chuck with an internal flow channel.

[0082] Example 1

[0083] This embodiment provides a method for manufacturing a silicon carbide vacuum chuck with an internal flow channel, including the following steps:

[0084] Step S1: Disperse the functionalized nano-silicon carbide prepared in Example 4 in a mixed solution of acrylamide and N-hydroxyethylacrylamide aqueous solution with a mass fraction of 0.2% to obtain a premixed slurry, wherein the mass ratio of functionalized nano-silicon carbide to the mixed solution is 0.8:20, and the mass ratio of acrylamide to N-hydroxyethylacrylamide aqueous solution in the mixed solution is 1:10;

[0085] Step S2: Add 12% ammonium persulfate aqueous solution and tetramethylethylenediamine to the premixed slurry prepared in step S1, control the rotation speed at 600 rpm, stir for 24 min until uniform, raise the temperature to 72℃, stir and react for 3.4 h, degas, and obtain modified ceramic slurry, wherein the mass ratio of ammonium persulfate aqueous solution, tetramethylethylenediamine and premixed slurry is 0.4:0.02:40;

[0086] Step S3: Coat the inner wall of the SUS304 stainless steel mold with dimethyl silicone oil, inject the modified ceramic slurry from step S2 into the mold, allow it to stand and form, control the standing forming temperature at 42°C for 5 hours, demold and dry, control the demolding and drying temperature at 52°C for 24 hours to obtain a green body, and then perform reaction sintering. The reaction sintering process is as follows: place the green body in a high-temperature sintering furnace for silicon diffusion reaction sintering, control the mass ratio of green body to metallic silicon at 1:0.66, raise the temperature to 1540°C at a heating rate of 10°C / min, and hold for 4.2 hours, then perform fine grinding and polishing to obtain a silicon carbide vacuum chuck with internal flow channels, wherein the mass of dimethyl silicone oil is 0.24% of the mass of the modified ceramic slurry.

[0087] Example 2

[0088] This embodiment provides a method for manufacturing a silicon carbide vacuum chuck with an internal flow channel, including the following steps:

[0089] Step S1: Disperse the functionalized nano-silicon carbide prepared in Example 5 in a mixed solution of acrylamide and N-hydroxyethylacrylamide aqueous solution with a mass fraction of 0.3% to obtain a premixed slurry, wherein the mass ratio of functionalized nano-silicon carbide to the mixed solution is 1:25, and the mass ratio of acrylamide to N-hydroxyethylacrylamide aqueous solution in the mixed solution is 1:11.

[0090] Step S2: Add 14% ammonium persulfate aqueous solution and tetramethylethylenediamine to the premixed slurry prepared in step S1, control the rotation speed at 650 rpm, stir for 20 min until uniform, raise the temperature to 74℃, stir and react for 3 h, degas, and obtain modified ceramic slurry. The mass ratio of ammonium persulfate aqueous solution, tetramethylethylenediamine and premixed slurry is 0.5:0.03:45.

[0091] Step S3: Coat the inner wall of the SUS304 stainless steel mold with dimethyl silicone oil, inject the modified ceramic slurry from step S2 into the mold, allow it to stand and form, control the standing forming temperature at 44℃ for 4 hours, demold and dry, control the demolding and drying temperature at 55℃ for 23 hours to obtain a green body, and then perform reaction sintering. The reaction sintering process is as follows: place the green body in a high-temperature sintering furnace for silicon infiltration reaction sintering, control the mass ratio of green body to metallic silicon at 1:0.7, heat to 1570℃ at a heating rate of 15℃ / min, hold for 3.9 hours, and then perform fine grinding and polishing to obtain a silicon carbide vacuum chuck with internal flow channels, wherein the mass of dimethyl silicone oil is 0.26% of the mass of the modified ceramic slurry.

[0092] Example 3

[0093] This embodiment provides a method for manufacturing a silicon carbide vacuum chuck with an internal flow channel, including the following steps:

[0094] Step S1: Disperse the functionalized nano-silicon carbide prepared in Example 6 in a mixed solution of acrylamide and N-hydroxyethylacrylamide aqueous solution with a mass fraction of 0.4% to obtain a premixed slurry, wherein the mass ratio of functionalized nano-silicon carbide to the mixed solution is 1.2:30, and the mass ratio of acrylamide to N-hydroxyethylacrylamide aqueous solution in the mixed solution is 1:12.

[0095] Step S2: Add 16% ammonium persulfate aqueous solution and tetramethylethylenediamine to the premixed slurry prepared in step S1, control the rotation speed at 700 rpm, stir for 16 min until uniform, raise the temperature to 76℃, stir and react for 2.6 h, degas, and obtain modified ceramic slurry, wherein the mass ratio of ammonium persulfate aqueous solution, tetramethylethylenediamine and premixed slurry is 0.6:0.04:50;

[0096] Step S3: Coat the inner wall of the SUS304 stainless steel mold with dimethyl silicone oil, inject the modified ceramic slurry from step S2 into the mold, allow it to stand and form, control the standing forming temperature at 46°C for 3 hours, demold and dry, control the demolding and drying temperature at 58°C for 22 hours to obtain a green body, and then perform reaction sintering. The reaction sintering process is as follows: place the green body in a high-temperature sintering furnace for silicon infiltration reaction sintering, control the mass ratio of green body to metallic silicon at 1:0.74, heat to 1600°C at a heating rate of 20°C / min, and hold for 3.6 hours, then perform fine grinding and polishing to obtain a silicon carbide vacuum chuck with internal flow channels, wherein the mass of dimethyl silicone oil is 0.28% of the mass of the modified ceramic slurry.

[0097] Comparative Example 1

[0098] Comparative Example 1 is the same as Example 1, except that the functionalized nano-silicon carbide in Example 1 is replaced with the functionalized nano-silicon carbide prepared in Comparative Preparation Example 4.

[0099] Comparative Example 2

[0100] Comparative Example 2 is the same as Example 1, except that the functionalized nano-silicon carbide in Example 1 is replaced with the functionalized nano-silicon carbide prepared in Comparative Preparation Example 5.

[0101] Comparative Example 3

[0102] Comparative Example 3 is the same as Example 1, except that the functionalized nano-silicon carbide in Example 1 is replaced with the functionalized nano-silicon carbide prepared in Comparative Preparation Example 6.

[0103] Performance testing

[0104] The silicon carbide vacuum chucks with internal flow channels prepared in Examples 1-3 and Comparative Examples 1-3 were subjected to density, hardness, and flexural strength tests. Density was tested using a density analyzer; hardness was tested using a Vickers hardness tester; and flexural strength was tested according to GB / T 6569-2006 standard. The test results are shown in Table 1 below.

[0105] Table 1 Performance parameters of the silicon carbide vacuum chucks prepared in Examples 1-3 and Comparative Examples 1-3

[0106]

[0107] As can be seen from Table 1, compared with Comparative Examples 1-3, the silicon carbide vacuum chucks with internal flow channels prepared by the method provided in Examples 1-3 have higher density and mechanical properties.

[0108] This specific embodiment is merely an explanation of this application and is not intended to limit it. After reading this specification, those skilled in the art can make modifications to this embodiment without contributing any inventive step, but such modifications are protected by patent law as long as they fall within the scope of the claims of this application.

Claims

1. A method of manufacturing a vacuum chuck having an inner flow channel of silicon carbide, characterized by, The method comprises the following steps: Step S1, dispersing functionalized nanometer silicon carbide in a mixed solution of acrylamide and N-hydroxyethyl acrylamide aqueous solution by ultrasonic, to obtain a premix slurry; Step S2, adding an initiator solution and an accelerator to the premix slurry prepared in step S1, stirring uniformly, heating to 72-76℃, stirring and reacting for 2.6-3.4h, degassing, to obtain a modified ceramic slurry; Step S3, coating a release agent on the inner side wall of a mold, injecting the modified ceramic slurry in step S2 into the mold, standing and forming, demolding and drying, to obtain a green body, and then performing reaction sintering, fine grinding and polishing, to obtain a vacuum chuck with inner runner silicon carbide; In step S2, the initiator solution is an ammonium persulfate aqueous solution with a mass fraction of 12-16%; In step S2, the accelerator is tetramethyl ethylenediamine; The functionalized nanometer silicon carbide is prepared by modifying nanometer silicon carbide by KH-560 to obtain epoxy nanometer silicon carbide, and then performing ring-opening reaction with a reinforcing component; The reinforcing component is prepared by oxidizing carbon fibers by nitric acid to obtain pretreated carbon fibers, and then performing esterification reaction with α-acetamidocinnamic acid; The preparation method of the functionalized nanometer silicon carbide comprises the following steps: Step A1, uniformly mixing coupling agent KH-560, anhydrous ethanol and deionized water, adjusting pH to 8-9, stirring for 5-10min, adding nanometer silicon carbide, heating to 60-66℃, stirring and reacting for 4-5h, filtering, washing and drying, to obtain epoxy nanometer silicon carbide; Step A2, uniformly ultrasonically dispersing epoxy nanometer silicon carbide, a reinforcing component and anhydrous DMF, adding potassium hydroxide, heating to 82-86℃, stirring and reacting for 3.6-4.8h, filtering, washing and drying, to obtain functionalized nanometer silicon carbide; The reinforcing component is prepared by the following steps: Step B1, placing carbon fibers in acetone, stirring at 50-54℃ for 8-12h, taking out, washing, and then placing in a nitric acid solution with a mass fraction of 66-68%, stirring at 82-86℃ for 2.6-3.2h, filtering, and washing until the washing liquid is neutral, to obtain pretreated carbon fibers; Step B2, adding pretreated carbon fibers, α-acetamidocinnamic acid and p-toluenesulfonic acid into anhydrous DMF, stirring uniformly, heating to 90-110℃ under nitrogen protection, stirring and reacting for 18-20h, standing for 4-6h, filtering, washing and drying, to obtain the reinforcing component.

2. The manufacturing method of a vacuum chuck with an inner flow channel of silicon carbide according to claim 1, wherein In step S1, the mass ratio of functionalized nanometer silicon carbide to the mixed solution is 0.8-1.2:20-30, and in the mixed solution, the mass ratio of acrylamide to N-hydroxyethyl acrylamide aqueous solution is 1:10-12.

3. The method of manufacturing a vacuum chuck having an inner flow channel of silicon carbide according to claim 1, wherein In step A1, the mass ratio of coupling agent KH-560, anhydrous ethanol, deionized water and nanometer silicon carbide is 0.3-0.5:35-45:4-6:2.4-3.

4. The method of manufacturing a vacuum chuck having an inner flow channel of silicon carbide according to claim 1, wherein In step A2, the mass ratio of epoxy nanometer silicon carbide, a reinforcing component, anhydrous DMF and potassium hydroxide is 2.4-2.8:0.6-0.8:40-50:1.2-1.

6.

5. The method of manufacturing a vacuum chuck having an inner flow channel of silicon carbide according to claim 1, wherein In the step B1, the mass ratio of carbon fiber and acetone is 3-5:40, and the mass ratio of carbon fiber and nitric acid solution is 5:50-60.

6. The method of manufacturing a vacuum chuck having an inner flow channel of silicon carbide according to claim 1, wherein In the step B2, the mass ratio of pretreated carbon fiber, α-acetamidocinnamic acid, p-toluenesulfonic acid and anhydrous DMF is 1:0.3-0.5:0.02-0.04:80-100.

7. The method of manufacturing a vacuum chuck having an inner flow channel of silicon carbide according to claim 1, wherein In the step S2, the mass ratio of initiator solution, accelerator and premixed slurry is 0.4-0.6:0.02-0.04:40-50.

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