High-temperature-resistant composite ceramic material and preparation method thereof

Abstract

The invention discloses a high-temperature-resistant composite ceramic material and a preparation method thereof, and the high-temperature-resistant composite ceramic material is prepared from the following raw materials in parts by weight: 43-60 parts of aluminum oxide, 70-90 parts of silicon nitride, 30-45 parts of silicon carbide, 14-23 parts of mullite, 15-28 parts of aluminum silicate fiber, 15-28 parts of silicon powder, 16-23 parts of aluminosilicate clay, 8-10 parts of a binder and 8-10 parts of a pore forming agent. The pore-forming agent is one or more of silicon dioxide, silicon carbide and calcium oxide, and the binder comprises a high-molecular substance and a low-molecular substance. According to the high-temperature-resistant composite ceramic material and the preparation method thereof, through combination of ceramic matrix components and specific reinforced fibers in an accurate proportion, the material can keep stable physical and chemical properties in an extremely high-temperature environment, the service life under a high-temperature working condition is prolonged, and the high-temperature-resistant composite ceramic material is prepared according to the reasonable proportion of the ceramic matrix to the reinforced material. And the high-quality binder and the pore-forming agent are used, so that the compressive strength and the breaking strength of the material are remarkably improved.

Description

Technical Field

[0001] The present invention relates to the technical field of zirconia ceramic materials, and specifically to a high-temperature resistant composite ceramic material and a preparation method thereof. Background Art

[0002] High-temperature resistant composite ceramic materials are advanced materials with excellent properties. They are usually composed of multiple ceramic components and reinforcing materials. Such materials have extremely excellent high-temperature resistance and can maintain the stability of their physical and chemical properties in high-temperature environments. For example, at temperatures exceeding 1000 °C or even higher, they still have high strength, low creep, and good oxidation resistance. In terms of performance, high-temperature resistant composite ceramic materials have high strength and can withstand large loads; good thermal stability, low thermal expansion coefficient, and small dimensional changes during temperature changes; excellent chemical inertness and are not easily chemically reactive with other substances; excellent wear resistance and are suitable for high-wear environments. Due to these excellent properties, high-temperature resistant composite ceramic materials are widely used in the aerospace field, such as manufacturing engine components, thermal protection systems, etc.; in the industrial field, for the inner lining of high-temperature kilns and key components of metallurgical equipment; in the energy field, they can be used as heat-absorbing components of solar thermal power generation systems, structural materials of nuclear reactors, etc. Since ceramic materials are mostly used in extreme environments, there are relatively high requirements for the high-temperature resistance and self-strength of ceramic materials. Therefore, there is an urgent need for a high-temperature resistant composite ceramic material and a preparation method thereof that can meet the above requirements. Summary of the Invention

[0003] To achieve the above objectives, the present invention is realized through the following technical solutions: A high-temperature resistant composite ceramic material is composed of raw materials in the following weight components, including: 43 - 60 parts of alumina, 70 - 90 parts of silicon nitride, 30 - 45 parts of silicon carbide, 14 - 23 parts of mullite, 15 - 28 parts of aluminosilicate fiber, 15 - 28 parts of silicon powder, 16 - 23 parts of aluminosilicate clay, 8 - 10 parts of binder, 8 - 10 parts of pore former, and 10 - 15 parts of modified composite material.

[0004] Preferably, the pore former is one or more of silicon dioxide, silicon carbide, and calcium oxide.

[0005] Preferably, the binder includes high-molecular substances and low-molecular substances.

[0006] A preparation method of a high-temperature resistant composite ceramic material includes the following steps:

[0007] First step: Select a ceramic matrix material, where the ceramic matrix material includes 43 - 60 parts of alumina, 70 - 90 parts of silicon nitride, 30 - 45 parts of silicon carbide, and 14 - 23 parts of mullite. Put the above ceramic matrix materials into a mixing device and mix evenly;

[0008] Step 2: Prepare the reinforcing material. The reinforcing material includes 15 - 28 parts of aluminum silicate fiber, 15 - 28 parts of silicon powder, and 16 - 23 parts of aluminosilicate clay. Put the above-mentioned reinforcing material into a mixing device and mix evenly;

[0009] Step 3: Pretreat the ceramic matrix material and the reinforcing material, including cleaning, drying, and removing impurities;

[0010] Step 4: Put the ceramic matrix material and the reinforcing material after the pretreatment in Step 3 into a mixing device for uniform mixing. The mixing process is carried out in a vacuum environment or under the protection of an inert gas;

[0011] Step 5: Put the mixed material in Step 4 into a ball mill and perform ball milling on the mixed material until it becomes a powder with a particle size of 400 - 600 μm;

[0012] Step 6: Put the material after ball milling in Steps 4 and 5 into a drying device and dry the material after ball milling. The drying temperature is controlled at 130 °C and the drying time is 2 - 3 min;

[0013] Step 7: Treat the pore-forming agent. Put the pore-forming agent into a calcination furnace and calcine it at a temperature of 600 - 800 °C. After calcination, put the calcined pore-forming agent into a ball mill again for ball milling until it becomes a powder with a particle size of 200 - 400 μm, obtaining the treated pore-forming agent powder;

[0014] Step 8: Add 10 - 15 parts of modified composite material, 8 - 10 parts of binder, and 8 - 10 parts of pore-forming agent to the dried material, and then stir and mix;

[0015] Step 9: Put the mixed material into a mold and perform a hot pressing forming operation;

[0016] Step 10: Perform high-temperature sintering on the formed green body. The sintering temperature is 1550 °C - 1780 °C, the sintering time is 15 - 26 h, and an argon atmosphere is maintained during the sintering process;

[0017] Step 11: Perform post-treatment on the sintered material, including cutting, grinding, and polishing, to obtain a high-temperature resistant composite ceramic material.

[0018] Preferably, the mixing time in Step 1 is 1 - 2.5 h and the stirring speed is 50 r / min.

[0019] Preferably, the mixing time in Step 2 is 0.5 - 2 h and the stirring speed is 120 r / min.

[0020] Preferably, the pretreatment in Step 3 includes the following steps:

[0021] (1) Place the ceramic matrix material and the reinforcement material in an ultrasonic cleaner respectively, and clean them with deionized water and organic solvents. The cleaning time is 0.5 - 1 h;

[0022] (2) Place the cleaned materials in an oven and dry them at 130 °C for 2 - 3 h to remove surface moisture and impurities;

[0023] (3) Screen the dried materials to remove particles that are too large or too small and possible foreign objects.

[0024] Preferably, in the tenth step, the obtained green body is placed in a kiln and fired according to the following heating process: First, heat from room temperature to 400 °C at a heating rate of 10 °C / min and hold at this temperature for 30 min; then heat to 850 °C at a heating rate of 4 °C / min and hold for 60 min; finally, heat to a final temperature of 1550 °C - 1780 °C at a heating rate of 8 °C / min and fire at this final temperature for 15 - 26 h to obtain a high-temperature resistant ceramic.

[0025] Preferably, the preparation method of the modified composite material is as follows:

[0026] Step 1: Pretreat 8 parts of graphene nanosheets, 10 parts of boron carbide, and 8 parts of aluminum titanate respectively. Place the graphene nanosheets in a vacuum oven and dry at 100 °C for 2 h to remove moisture and impurities. Put boron carbide and aluminum titanate into a ball mill respectively and ball mill for 1 h at a ball mill speed of 80 r / min to make their particle size reach 300 μm;

[0027] Step 2: Put the pretreated graphene nanosheets, boron carbide, and aluminum titanate into a high-speed mixer according to the above ratio, add an appropriate amount of dispersant, with a weight of 10% of the total weight of the raw materials, and stir at a speed of 200 r / min for 2 h;

[0028] Step 3: Put the mixed powder of the modified composite material into a vacuum drying oven and dry at 80 °C for 3 h to remove the dispersant and obtain the final modified composite material.

[0029] The present invention provides a high-temperature resistant composite ceramic material and its preparation method. It has the following beneficial effects:

[0030] The high temperature resistant composite ceramic material and its preparation method, through the combination of precisely proportioned ceramic matrix components and specific reinforcing fibers, enable the material to maintain stable physical and chemical properties in an extremely high temperature environment, extend the service life under high temperature conditions, and significantly improve the compressive strength and flexural strength of the material by using a reasonable ratio of ceramic matrix to reinforcing materials, as well as high-quality binders and pore-forming agents, so that the material is not easy to break or fail when subjected to heavy loads and complex stresses. At the same time, the ratio of the ceramic matrix and each component is optimized, so that the material has a small size change when the temperature changes, ensuring the stability and reliability of the material during the thermal cycle. The graphene nanosheet has excellent mechanical properties and self-lubricating properties, and can form a lubricating film on the surface of the ceramic material to reduce the friction coefficient, thereby improving the wear resistance; the boron carbide has high hardness, which can enhance the overall hardness of the ceramic material and improve its wear resistance; aluminum titanate has good thermal stability and thermal shock resistance, which helps to maintain the structural stability of the ceramic material under high temperature environments, and also has a certain improvement effect on the wear resistance. The three work synergistically to effectively improve the wear resistance of the high temperature resistant composite ceramic material. DETAILED DESCRIPTION

[0031] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0032] In the first embodiment, the present invention provides a technical solution: a method for preparing a high temperature resistant composite ceramic material, comprising the following steps:

[0033] Step 1: Select a ceramic matrix material, which includes 43 parts of aluminum oxide, 70 parts of silicon nitride, 30 parts of silicon carbide, and 14 parts of mullite. Put the above ceramic matrix materials into a mixing device and mix them evenly. The mixing time is 1 hour and the stirring speed is 50r / min.

[0034] Step 2: prepare reinforcing materials, which include 15 parts of aluminum silicate fiber, 15 parts of silicon powder, and 16 parts of aluminosilicate clay. Put the above reinforcing materials into a mixing device and mix them evenly. The mixing time is 0.5h and the stirring speed is 120r / min.

[0035] Step 3: Pre-treat the ceramic matrix material and reinforcement material, including cleaning, drying, and removing impurities. The pre-treatment includes the following steps:

[0036] (1) Place the ceramic matrix material and the reinforcement material in an ultrasonic cleaning machine and clean them with deionized water and an organic solvent for 0.5 h.

[0037] (2) Place the cleaned material in a drying oven and dry it at 130 °C for 2 h to remove surface moisture and impurities;

[0038] (3) Screen the dried material to remove particles that are too large or too small and any foreign objects that may be present;

[0039] Step 4: Put the ceramic matrix material and reinforcing material after the pretreatment in the third step into a mixing device for uniform mixing. The mixing process is carried out under a vacuum environment or inert gas protection;

[0040] Step 5: Put the mixed material in the fourth step into a ball mill and carry out ball milling on the mixed material until it becomes a powder with a particle size of 400 μm;

[0041] Step 6: Put the material after ball milling in the fourth and fifth steps into a drying device and dry the material after ball milling. The drying temperature is controlled at 130 °C and the drying time is 2 min;

[0042] Step 7: Treat the pore-forming agent. Put the pore-forming agent into a calcination furnace and calcine it at a temperature of 600 °C. After calcination, put the calcined pore-forming agent into a ball mill and carry out ball milling until it becomes a powder with a particle size of 200 μm to obtain the treated pore-forming agent powder;

[0043] Step 8: Add 10 parts of the modified composite material, 8 parts of the binder, and 8 parts of the pore-forming agent to the dried material, and then stir and mix;

[0044] Step 9: Put the mixed material into a mold and carry out a hot pressing forming operation;

[0045] Step 10: Carry out high-temperature sintering on the formed green body. The sintering temperature is 1550 °C and the sintering time is 15 - 26 h. Keep an argon atmosphere during sintering. When sintering, put the obtained green body into a kiln and fire it according to the following heating process: First, heat from room temperature to 400 °C at a heating rate of 10 °C / min and hold at this temperature for 30 min; then heat to 850 °C at a heating rate of 4 °C / min and hold for 60 min; finally, heat to the final temperature of 1550 °C at a heating rate of 8 °C / min and fire at this final temperature for 15 hours - 26 hours to obtain the high-temperature resistant ceramic;

[0046] Step 11: Carry out post-treatment on the sintered material, including cutting, grinding, and polishing, to obtain the high-temperature resistant composite ceramic material.

[0047] Second Embodiment. The present invention provides a technical solution: A method for preparing a high-temperature resistant composite ceramic material, comprising the following steps:

[0048] Step 1: Select a ceramic matrix material, which includes 46 parts of alumina, 75 parts of silicon nitride, 34 parts of silicon carbide, and 16 parts of mullite. Put the above ceramic matrix material into a mixing device and mix evenly. The mixing time is 1 h, and the stirring speed is 50 r / min;

[0049] Step 2: Prepare a reinforcing material, which includes 18 parts of aluminum silicate fiber, 18 parts of silicon powder, and 17 parts of aluminosilicate clay. Put the above reinforcing material into a mixing device and mix evenly. The mixing time is 0.5 h, and the stirring speed is 120 r / min;

[0050] Step 3: Pretreat the ceramic matrix material and the reinforcing material, including cleaning and drying to remove impurities. The pretreatment includes the following steps:

[0051] (1) Place the ceramic matrix material and the reinforcing material in an ultrasonic cleaner respectively, and use deionized water and organic solvents for cleaning. The cleaning time is 0.5 h;

[0052] (2) Place the cleaned materials in a drying oven and dry them at 130 °C for 2 h to remove surface moisture and impurities;

[0053] (3) Screen the dried materials to remove particles that are too large or too small and possible foreign objects;

[0054] Step 4: Put the ceramic matrix material and the reinforcing material after the pretreatment in Step 3 into a mixing device and mix evenly. The mixing process is carried out in a vacuum environment or under the protection of an inert gas;

[0055] Step 5: Put the mixed material in Step 4 into a ball mill and carry out ball milling on the mixed material until it becomes a powder with a particle size of 400 μm;

[0056] Step 6: Put the ball-milled material in Steps 4 and 5 into a drying device and dry the ball-milled material. The drying temperature is controlled at 130 °C, and the drying time is 2 min;

[0057] Step 7: Process the pore-forming agent. Put the pore-forming agent into a calcination furnace and calcine it at a temperature of 600 °C. After calcination, put the calcined pore-forming agent into a ball mill again and ball mill it until it becomes a powder with a particle size of 200 μm to obtain the processed pore-forming agent powder;

[0058] Step 8: Add 12 parts of a modified composite material, 8 parts of a binder, and 8 parts of a pore-forming agent to the dried material, and then stir and mix;

[0059] Step 9: Put the mixed material into a mold and carry out a hot pressing forming operation;

[0060] Step 10: Subject the formed green body to high-temperature sintering. Maintain an argon atmosphere during the sintering process. Place the obtained green body into a kiln for firing according to the following heating process: First, heat from room temperature to 400 °C at a heating rate of 10 °C / min and hold at this temperature for 30 min; then heat to 850 °C at a heating rate of 4 °C / min and hold for another 60 min; finally, heat to the final temperature of 1550 °C at a heating rate of 8 °C / min and fire at this final temperature for 15 hours to obtain a high-temperature resistant ceramic.

[0061] Step 11: Conduct post-treatment on the sintered material, including cutting, grinding, and polishing, to obtain a high-temperature resistant composite ceramic material.

[0062] Third Embodiment. The present invention provides a technical solution: A method for preparing a high-temperature resistant composite ceramic material, comprising the following steps:

[0063] Step 1: Select a ceramic matrix material. The ceramic matrix material includes 50 parts of alumina, 79 parts of silicon nitride, 37 parts of silicon carbide, and 18 parts of mullite. Place the above ceramic matrix material into a mixing device and mix evenly. The mixing time is 1 h, and the stirring speed is 50 r / min.

[0064] Step 2: Prepare a reinforcing material. The reinforcing material includes 20 parts of aluminum silicate fiber, 20 parts of silicon powder, and 19 parts of aluminosilicate clay. Place the above reinforcing material into a mixing device and mix evenly. The mixing time is 0.5 h, and the stirring speed is 120 r / min.

[0065] Step 3: Pretreat the ceramic matrix material and the reinforcing material, including cleaning and drying to remove impurities. The pretreatment includes the following steps:

[0066] (1) Place the ceramic matrix material and the reinforcing material respectively in an ultrasonic cleaner and clean them with deionized water and organic solvents. The cleaning time is 0.5 h.

[0067] (2) Place the cleaned materials in a drying oven and dry them at 130 °C for 2 h to remove surface moisture and impurities.

[0068] (3) Screen the dried materials to remove particles that are too large or too small and possible foreign objects.

[0069] Step 4: Place the ceramic matrix material and the reinforcing material after the pretreatment in Step 3 into a mixing device and mix evenly. The mixing process is carried out in a vacuum environment or under inert gas protection.

[0070] Step 5: Put the mixed material in the fourth step into the ball mill, and conduct ball milling on the mixed material until the powder with a particle size of 400 μm is obtained;

[0071] Step 6: Put the ball-milled material in the fifth and sixth steps into the drying equipment, and dry the ball-milled material. The drying temperature is controlled at 130 °C, and the drying time is 2 min;

[0072] Step 7: Process the pore-forming agent. Put the pore-forming agent into the calcination furnace and conduct calcination at a temperature of 600 °C. After the calcination is completed, put the calcined pore-forming agent into the ball mill again for ball milling until the powder with a particle size of 200 μm is obtained, and the processed pore-forming agent powder is obtained;

[0073] Step 8: Add 14 parts of the modified composite material, 9 parts of the binder, and 9 parts of the pore-forming agent to the dried material, and then stir and mix;

[0074] Step 9: Put the mixed material into the mold and perform a molding operation using a hot pressing process;

[0075] Step 10: Conduct high-temperature sintering on the formed green body. Keep an argon atmosphere during the sintering process. When sintering, put the obtained green body into the kiln and conduct firing according to the following heating process: First, heat from room temperature to 400 °C at a heating rate of 10 °C / min and hold at this temperature for 30 min; then heat to 850 °C at a heating rate of 4 °C / min and hold for 60 min; finally, heat to the final temperature of 1550 °C at a heating rate of 8 °C / min and fire at this final temperature for 15 hours to obtain a high-temperature resistant ceramic;

[0076] Step 11: Conduct subsequent processing on the sintered material, including cutting, grinding, and polishing, to obtain a high-temperature resistant composite ceramic material.

[0077] Fourth Embodiment. The present invention provides a technical solution: A preparation method of a high-temperature resistant composite ceramic material, comprising the following steps:

[0078] Step 1: Select a ceramic matrix material. The ceramic matrix material includes 50 parts of alumina, 85 parts of silicon nitride, 40 parts of silicon carbide, and 20 parts of mullite. Put the above ceramic matrix materials into a mixing device and mix evenly. The mixing time is 1 h, and the stirring speed is 50 r / min;

[0079] Step 2: Prepare a reinforcing material. The reinforcing material includes 24 parts of aluminum silicate fiber, 24 parts of silicon powder, and 21 parts of aluminosilicate clay. Put the above reinforcing materials into a mixing device and mix evenly. The mixing time is 0.5 h, and the stirring speed is 120 r / min;

[0080] Step 3: Pretreat the ceramic matrix material and the reinforcing material, including cleaning, drying, and removing impurities. The pretreatment includes the following steps:

[0081] (1) Place the ceramic matrix material and the reinforcing material in an ultrasonic cleaner respectively, and clean them with deionized water and organic solvents for 0.5 h;

[0082] (2) Place the cleaned materials in a drying oven and dry them at 130 °C for 2 h to remove surface moisture and impurities;

[0083] (3) Screen the dried materials to remove particles that are too large or too small and possible foreign matters;

[0084] Step 4: Put the ceramic matrix material and the reinforcing material after the pretreatment in Step 3 into a mixing device for uniform mixing. The mixing process is carried out under a vacuum environment or inert gas protection;

[0085] Step 5: Put the mixed material in Step 4 into a ball mill and perform ball milling on the mixed material until it becomes a powder with a particle size of 400 μm;

[0086] Step 6: Put the material after ball milling in Steps 4 and 5 into a drying device and dry the material after ball milling. Control the drying temperature at 130 °C and the drying time at 2 min;

[0087] Step 7: Treat the pore former. Put the pore former into a calcination furnace and calcine it at a temperature of 600 °C. After calcination, put the calcined pore former into a ball mill again and perform ball milling until it becomes a powder with a particle size of 200 μm to obtain the treated pore former powder;

[0088] Step 8: Add 14 parts of the modified composite material, 9 parts of the binder, and 9 parts of the pore former to the dried material, and then stir and mix;

[0089] Step 9: Put the mixed material into a mold and perform a molding operation using a hot pressing process;

[0090] Step 10: Perform high-temperature sintering on the formed green body. Maintain an argon atmosphere during the sintering process. Place the obtained green body in a kiln during sintering and fire it according to the following heating process: First, heat from room temperature to 400 °C at a heating rate of 10 °C / min and hold at this temperature for 30 min; then heat to 850 °C at a heating rate of 4 °C / min and hold for 60 min; finally, heat to a final temperature of 1550 °C at a heating rate of 8 °C / min and fire at this final temperature for 15 hours to obtain a high-temperature resistant ceramic;

[0091] The eleventh step: perform subsequent processing on the sintered material, including cutting, grinding, and polishing, to obtain a high-temperature resistant composite ceramic material.

[0092] The fifth embodiment, the present invention provides a technical solution: a preparation method of a high-temperature resistant composite ceramic material, comprising the following steps:

[0093] The first step: select a ceramic matrix material, the ceramic matrix material includes 60 parts of alumina, 90 parts of silicon nitride, 45 parts of silicon carbide, and 23 parts of mullite. Put the above ceramic matrix materials into a mixing device and mix evenly. The mixing time is 1h, and the stirring speed is 50r / min;

[0094] The second step: prepare a reinforcing material, the reinforcing material includes 28 parts of aluminum silicate fiber, 28 parts of silicon powder, and 23 parts of aluminosilicate clay. Put the above reinforcing materials into a mixing device and mix evenly. The mixing time is 0.5h, and the stirring speed is 120r / min;

[0095] The third step: pre-treat the ceramic matrix material and the reinforcing material, including cleaning and drying to remove impurities. The pre-treatment includes the following steps:

[0096] (1) Respectively place the ceramic matrix material and the reinforcing material in an ultrasonic cleaner, and use deionized water and organic solvents for cleaning. The cleaning time is 0.5h;

[0097] (2) Place the cleaned materials in a drying oven and dry them at 130 degrees Celsius for 2h to remove surface moisture and impurities;

[0098] (3) Screen the dried materials to remove particles that are too large or too small and possible foreign objects;

[0099] The fourth step: put the ceramic matrix material and the reinforcing material after the pre-treatment in the third step into a mixing device for uniform mixing. The mixing process is carried out in a vacuum environment or under the protection of an inert gas;

[0100] The fifth step: put the mixed material in the fourth step into a ball mill and perform ball milling on the mixed material until it becomes a powder with a particle size of 400μm;

[0101] The sixth step: put the ball-milled material in the fourth and fifth steps into a drying device and dry the ball-milled material. The drying temperature is controlled at 130°C, and the drying time is 2min;

[0102] The seventh step: process the pore-forming agent. Put the pore-forming agent into a calcination furnace and calcine it at a temperature of 600°C. After calcination, put the calcined pore-forming agent into a ball mill and perform ball milling until it becomes a powder with a particle size of 200μm to obtain the processed pore-forming agent powder;

[0103] Step 8: Add 15 parts of modified composite material, 10 parts of binder, and 10 parts of pore former to the dried material, and then stir and mix them.

[0104] Step 9: Put the mixed material into a mold and perform a molding operation using a hot pressing process.

[0105] Step 10: Subject the formed green body to high-temperature sintering. The sintering temperature is 1550 °C, and the sintering time is 15 - 26 h. Maintain an argon atmosphere during the sintering process. Place the obtained green body in a kiln and fire it according to the following heating process: First, heat from room temperature to 400 °C at a heating rate of 10 °C / min and hold at this temperature for 30 min; then heat to 850 °C at a heating rate of 4 °C / min and hold for 60 min; finally, heat to the final temperature of 1550 °C at a heating rate of 8 °C / min and fire at this final temperature for 15 - 26 hours to obtain a high-temperature resistant ceramic.

[0106] Step 11: Perform post-treatment on the sintered material, including cutting, grinding, and polishing, to obtain a high-temperature resistant composite ceramic material.

[0107] The first comparative example. The present invention provides a technical solution: A preparation method of a high-temperature resistant composite ceramic material, comprising the following steps:

[0108] Step 1: Select a ceramic matrix material. The ceramic matrix material includes 43 parts of alumina, 70 parts of silicon nitride, 30 parts of silicon carbide, and 14 parts of mullite. Put the above ceramic matrix material into a mixing device and mix it evenly. The mixing time is 2.5 h, and the stirring speed is 50 r / min.

[0109] Step 2: Prepare a reinforcing material. The reinforcing material includes 15 parts of aluminum silicate fiber, 15 parts of silicon powder, and 16 parts of aluminosilicate clay. Put the above reinforcing material into a mixing device and mix it evenly. The mixing time is 2 h, and the stirring speed is 120 r / min.

[0110] Step 3: Pretreat the ceramic matrix material and the reinforcing material, including cleaning and drying to remove impurities. The pretreatment includes the following steps:

[0111] (1) Respectively place the ceramic matrix material and the reinforcing material in an ultrasonic cleaner and clean them with deionized water and organic solvents. The cleaning time is 1 h.

[0112] (2) Place the cleaned materials in a drying oven and dry them at 130 °C for 3 h to remove surface moisture and impurities.

[0113] (3) Screen the dried material to remove particles that are too large or too small in size and any possible foreign matter;

[0114] Fourth step: Put the ceramic matrix material and the reinforcing material after the pretreatment in the third step into a mixing device for uniform mixing. The mixing process is carried out in a vacuum environment or under the protection of an inert gas;

[0115] Fifth step: Put the mixed material in the fourth step into the interior of a ball mill and perform ball milling on the mixed material until a powder with a particle size of 600 μm is obtained;

[0116] Sixth step: Put the material after ball milling in the fourth and fifth steps into a drying device and dry the material after ball milling. The drying temperature is controlled at 130 °C and the drying time is 3 min;

[0117] Seventh step: Treat the pore-forming agent. Put the pore-forming agent into the interior of a calcination furnace and calcine it at a temperature of 800 °C. After calcination, put the calcined pore-forming agent into the ball mill again for ball milling until a powder with a particle size of 400 μm is obtained, obtaining the treated pore-forming agent powder;

[0118] Eighth step: Add 8 parts of binder and 8 parts of pore-forming agent to the dried material, and then stir and mix;

[0119] Ninth step: Put the mixed material into a mold and perform a hot pressing forming operation;

[0120] Tenth step: Perform high-temperature sintering on the formed green body. The sintering temperature is 1780 °C and the sintering time is 26 h. Keep an argon atmosphere during sintering. When sintering, put the obtained green body into a kiln and fire it according to the following heating process: First, heat from room temperature to 400 °C at a heating rate of 10 °C / min and hold at this temperature for 30 min; then heat to 850 °C at a heating rate of 4 °C / min and hold for 60 min; finally, heat to the final temperature of 1550 °C - 1780 °C at a heating rate of 8 °C / min and fire at this final temperature for 15 hours - 26 hours to obtain a high-temperature resistant ceramic;

[0121] Eleventh step: Perform post-treatment on the sintered material, including cutting, grinding, and polishing, to obtain a high-temperature resistant composite ceramic material.

[0122] Second comparative example, the present invention provides a technical solution: A preparation method of a high-temperature resistant composite ceramic material, comprising the following steps:

[0123] Step 1: Select a ceramic matrix material. The ceramic matrix material includes 60 parts of alumina, 90 parts of silicon nitride, 45 parts of silicon carbide, and 23 parts of mullite. Put the above ceramic matrix material into a mixing device and mix evenly. The mixing time is 2.5 h, and the stirring speed is 50 r / min;

[0124] Step 2: Prepare a reinforcing material. The reinforcing material includes 28 parts of aluminum silicate fiber, 28 parts of silicon powder, and 23 parts of aluminosilicate clay. Put the above reinforcing material into a mixing device and mix evenly. The mixing time is 2 h, and the stirring speed is 120 r / min;

[0125] Step 3: Pretreat the ceramic matrix material and the reinforcing material, including cleaning and drying to remove impurities. The pretreatment includes the following steps:

[0126] (1) Place the ceramic matrix material and the reinforcing material in an ultrasonic cleaner respectively, and use deionized water and organic solvents for cleaning. The cleaning time is 1 h;

[0127] (2) Place the cleaned materials in a drying oven and dry them at 130 °C for 3 h to remove surface moisture and impurities;

[0128] (3) Screen the dried materials to remove particles that are too large or too small and possible foreign objects;

[0129] Step 4: Put the ceramic matrix material and the reinforcing material after the pretreatment in Step 3 into a mixing device and mix evenly. The mixing process is carried out in a vacuum environment or under the protection of an inert gas;

[0130] Step 5: Put the mixed material in Step 4 into a ball mill and perform ball milling on the mixed material until it becomes a powder with a particle size of 600 μm;

[0131] Step 6: Put the ball-milled material in Steps 4 and 5 into a drying device and dry the ball-milled material. The drying temperature is controlled at 130 °C, and the drying time is 3 min;

[0132] Step 7: Treat the pore-forming agent. Put the pore-forming agent into a calcination furnace and calcine it at a temperature of 800 °C. After calcination, put the calcined pore-forming agent into a ball mill again and ball mill it until it becomes a powder with a particle size of 400 μm to obtain the treated pore-forming agent powder;

[0133] Step 8: Add 10 parts of binder and 10 parts of pore-forming agent to the dried material, and then stir and mix;

[0134] Step 9: Put the mixed material into a mold and perform a hot pressing forming operation;

[0135] Step 10: Subject the formed green body to high-temperature sintering at a sintering temperature of 1780 °C for 15 - 26 h. Maintain an argon atmosphere during the sintering process. Place the obtained green body in a kiln for firing according to the following heating process: First, heat from room temperature to 400 °C at a heating rate of 10 °C / min and hold at this temperature for 30 min; then heat to 850 °C at a heating rate of 4 °C / min and hold for 60 min; finally, heat to the final temperature of 1550 °C - 1780 °C at a heating rate of 8 °C / min and fire at this final temperature for 15 - 26 h to obtain a high-temperature resistant ceramic;

[0136] Step 11: Conduct post-treatment on the sintered material, including cutting, grinding, and polishing, to obtain a high-temperature resistant composite ceramic material.

[0137] Through the comparison of the finished product effects of the above embodiments and comparative examples, it is found that the finished product obtained in the fourth embodiment has the best effect;

[0138] The optimal ratio is: 50 parts of alumina, 85 parts of silicon nitride, 40 parts of silicon carbide, 20 parts of mullite, 24 parts of aluminosilicate fiber, 24 parts of silicon powder, 21 parts of aluminosilicate clay, 9 parts of binder, 9 parts of pore former, and 14 parts of modified composite material.

[0139] Obviously, the described embodiments are only a part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art and related fields without creative efforts shall fall within the protection scope of the present invention. The structures, devices, and operation methods not specifically described and explained in the present invention shall be implemented according to the conventional means in the art without special instructions and limitations..

Claims

1. A high-temperature resistant composite ceramic material, characterized in that, It is composed of raw materials with the following weight components, including: 43-60 parts of alumina, 70-90 parts of silicon nitride, 30-45 parts of silicon carbide, 14-23 parts of mullite, 15-28 parts of aluminosilicate fiber, 15-28 parts of silicon powder, 16-23 parts of aluminosilicate clay, 8-10 parts of binder, 8-10 parts of pore former, and 10-15 parts of modified composite material.

2. The high-temperature resistant composite ceramic material according to claim 1, wherein: The pore former is one or more of silica, silicon carbide, and calcium oxide.

3. The high-temperature resistant composite ceramic material according to claim 1, characterized in that: The binder includes high-molecular substances and low-molecular substances.

4. The preparation method of a high-temperature resistant composite ceramic material according to claim 1, characterized in that, It includes the following steps: The first step: Select a ceramic matrix material, which includes 43-60 parts of alumina, 70-90 parts of silicon nitride, 30-45 parts of silicon carbide, and 14-23 parts of mullite. Put the above ceramic matrix material into a mixing device and mix evenly. The second step: Prepare reinforcing materials, which include 15-28 parts of aluminosilicate fiber, 15-28 parts of silicon powder, and 16-23 parts of aluminosilicate clay. Put the above reinforcing materials into a mixing device and mix evenly. The third step: Pretreat the ceramic matrix material and the reinforcing materials, including cleaning and drying to remove impurities. The fourth step: Put the ceramic matrix material and the reinforcing materials after the pretreatment in the third step into a mixing device and mix evenly. The mixing process is carried out in a vacuum environment or under the protection of an inert gas. The fifth step: Put the mixed material in the fourth step into a ball mill and perform ball milling on the mixed material until it becomes a powder with a particle size of 400-600 μm. The sixth step: Put the ball-milled material in the fourth and fifth steps into a drying device and dry the ball-milled material. The drying temperature is controlled at 130 °C and the drying time is 2-3 min. The seventh step: Treat the pore former. Put the pore former into a calcining furnace and calcine it at a temperature of 600-800 °C. After calcination, put the calcined pore former into a ball mill and perform ball milling until it becomes a powder with a particle size of 200-400 μm to obtain the treated pore former powder. The eighth step: Add 10-15 parts of modified composite material, 8-10 parts of binder, and 8-10 parts of pore former to the dried material, and then stir and mix. The ninth step: Put the mixed material into a mold and perform a hot pressing forming process. The tenth step: Perform high-temperature sintering on the formed green body. The sintering temperature is 1550 °C - 1780 °C, and the sintering time is 15-26 h. Maintain an argon atmosphere during the sintering process. The eleventh step: Perform subsequent processing on the sintered material, including cutting, grinding, and polishing, to obtain a high-temperature resistant composite ceramic material.

5. The preparation method of a high-temperature resistant composite ceramic material according to claim 4, characterized in that: The mixing time in the first step is 1-2.5 h, and the stirring speed is 50 r / min.

6. The preparation method of a high-temperature resistant composite ceramic material according to claim 4, characterized in that: The mixing time in the second step is 0.5-2 h, and the stirring speed is 120 r / min.

7. The preparation method of a high-temperature resistant composite ceramic material according to claim 4, characterized in that, The pretreatment in the third step includes the following steps: (1). Respectively place the ceramic matrix material and the reinforcing materials in an ultrasonic cleaner and clean them with deionized water and organic solvents. The cleaning time is 0.5-1 h. (2) Place the cleaned material in a drying oven and dry it at 130 °C for 2 - 3 h to remove surface moisture and impurities; (3) Screen the dried material to remove particles that are too large or too small in size and any possible foreign matter.

8. The preparation method of a high-temperature resistant composite ceramic material according to claim 4, characterized in that: In the tenth step, place the obtained green body in a kiln and fire it according to the following heating process: First, heat it from room temperature to 400 °C at a heating rate of 10 °C / min and hold it at this temperature for 30 min; then heat it to 850 °C at a heating rate of 4 °C / min and hold it for 60 min; finally, heat it to a final temperature of 1550 °C - 1780 °C at a heating rate of 8 °C / min and fire it at this final temperature for 15 - 26 h to obtain a high-temperature resistant ceramic.

9. The preparation method of a high-temperature resistant composite ceramic material according to claim 4, wherein: The preparation method of the modified composite material is as follows: Step 1: Pretreat 8 parts of graphene nanosheets, 10 parts of boron carbide, and 8 parts of aluminum titanate respectively. Place the graphene nanosheets in a vacuum oven and dry them at 100 °C for 2 h to remove moisture and impurities. Put boron carbide and aluminum titanate into a ball mill respectively and ball mill them for 1 h at a ball mill speed of 80 r / min to make their particle size reach 300 μm; Step 2: Put the pretreated graphene nanosheets, boron carbide, and aluminum titanate into a high-speed mixer according to the above ratios, add an appropriate amount of dispersant, with a weight of 10% of the total weight of the raw materials, and stir at a speed of 200 r / min for 2 h; Step 3: Put the mixed powder of the modified composite material into a vacuum drying oven and dry it at 80 °C for 3 h to remove the dispersant and obtain the final modified composite material.