Manufacturing method of low-shrinkage ceramic fiber blanket

Abstract

The invention relates to the technical field of ceramic fibers, and particularly discloses a manufacturing method of a low-shrinkage ceramic fiber blanket, which comprises the following steps: step 1, uniformly mixing an Al2O3-SiC composite phase and yttrium oxide-kyanite composite powder, sieving, putting into a resistance furnace, and heating and melting to obtain molten slurry; step 2, performing centrifugal thread throwing on the molten slurry in the step 1 through a thread throwing machine to form a cotton wool shape, and cooling to obtain composite fibers; step 3, mixing the composite fiber with an adhesive, carrying out cotton collection and needling treatment, and then carrying out high-temperature setting and cooling to obtain a low-shrinkage ceramic fiber blanket; according to the ceramic fiber blanket, the Al2O3-SiC composite phase and the yttrium oxide-kyanite composite powder are adopted as main raw materials, the size stability can be kept in a high-temperature environment, the shrinkage rate is low, the heat preservation and insulation performance is excellent, the heat conductivity coefficient is small, heat transfer can be isolated, the energy-saving and consumption-reducing effects are achieved, and the mechanical property is greatly improved.

Description

Technical Field

[0001] The present invention relates to the technical field of ceramic fibers, and specifically to a manufacturing method of a ceramic fiber blanket with a low shrinkage rate. Background Art

[0002] Ceramic fiber blankets are fibrous high-temperature thermal insulation materials, which have the characteristics of high temperature resistance, good thermal stability, and light weight, and are widely used in the fields of metallurgy, chemical industry, aerospace, etc. Traditional ceramic fiber blankets, also known as aluminosilicate fiber blankets, usually have aluminosilicate or alumina fibers as the main body, and are prepared by wet forming or dry needling processes. The fiber blankets made are prone to problems such as binder failure and fiber creep under high-temperature conditions, with a high high-temperature shrinkage rate, resulting in local stress concentration and structural collapse. High-temperature sintering will also cause fiber embrittlement, leading to poor stability of the fiber blankets.

[0003] Chinese Patent Application CN117822201A discloses a preparation method of a high-temperature resistant ceramic fiber blanket, including the following steps: selecting 35 - 43% of alumina and 50 - 55% of silica, stirring and fusing them and performing high-temperature melting, centrifugal spinning, then adding 1 - 5 parts of binder and 1 - 4 parts of additive, cotton collecting, needling, heat shrinking and winding to obtain a high-temperature resistant ceramic fiber blanket. This ceramic fiber blanket improves the toughness and strength of the fiber blanket by adding a binder and an additive, but the fiber structure of this ceramic fiber blanket is prone to crystallization under high temperature for a long time, and the stability is average. Chinese Patent Application CN102605553A discloses a production method of a 1500°C chrome-free aluminosilicate fiber blanket, including the following steps: raw material mixing (mixing alumina, silica and zirconia particles in a certain proportion), resistance furnace melting, fiber blowing, mullite fiber mixing, air flow mixing, cotton collecting, needling, heat treatment for crystal form transformation to obtain a fiber blanket; this fiber blanket is clean and environmentally friendly, with a lower shrinkage rate, but has a high cost and poor mechanical properties.

[0004] Therefore, it is of great significance to provide a ceramic fiber blanket with excellent comprehensive performance. Summary of the Invention

[0005] Aiming at the deficiencies of the prior art, the present invention provides a manufacturing method of a ceramic fiber blanket with a low shrinkage rate, prepares a ceramic fiber blanket with a low shrinkage rate, and solves the problems of poor mechanical properties and high-temperature stability of the ceramic fiber blanket.

[0006] To achieve the above object, the present invention discloses a manufacturing method of a ceramic fiber blanket with a low shrinkage rate, including the following steps: Step 1: Mix the Al2O3 - SiC composite phase and the yttrium oxide - kyanite composite powder evenly, pass through a 200 - mesh sieve, place it in a resistance furnace, heat and melt it to obtain a molten slurry; Step 2: Centrifugally spin the molten slurry in Step 1 with a spinning machine to form cotton-like filaments, and rapidly cool them with cold air to obtain composite fibers. Step 3: Mix the composite fibers and an adhesive, suck them into a cotton collector under negative pressure for cotton collection, transfer them to a needle punching machine for needle punching treatment, and then perform high-temperature shaping and cooling to obtain a ceramic fiber blanket with a low shrinkage rate.

[0007] Preferably, the preparation method of the Al2O3-SiC composite phase in Step 1 includes the following steps: Mix polyvinyl alcohol, deionized water, tetraethyl orthosilicate, and an ethanol solution evenly to obtain a mixed solution A. Mix aluminum nitrate nonahydrate, citric acid, sucrose, and deionized water, adjust the pH to 4-5 with ammonia water, and after mixing evenly, obtain a mixed solution B. Mix the mixed solution A and the mixed solution B, stir evenly, dry, and sinter to obtain the Al2O3-SiC composite phase.

[0008] Preferably, the specific preparation method of the Al2O3-SiC composite phase is as follows: Add polyvinyl alcohol to deionized water, with the mass ratio of polyvinyl alcohol to deionized water being 4-6:100. Heat up and mix evenly at 80°C to obtain an aqueous polyvinyl alcohol solution. Mix tetraethyl orthosilicate and an ethanol solution with a mass ratio of 10-15:100, where the ethanol solution consists of deionized water and absolute ethanol with a volume ratio of 1:1. Dropwise add dilute hydrochloric acid to adjust the pH to 2, and stir and mix for 2 h to obtain a tetraethyl orthosilicate solution. Mix the aqueous polyvinyl alcohol solution and the tetraethyl orthosilicate solution with a volume ratio of 1:1, and stir for 3 h to obtain a mixed solution A. Mix aluminum nitrate nonahydrate, citric acid, sucrose, and deionized water with a mass ratio of 100:70-75:12-15:950-1050, adjust the pH to 4-5 with ammonia water, stir and mix for 2 h, and after mixing evenly, obtain a mixed solution B. Mix the mixed solution A and the mixed solution B in a volume ratio of 1:1, stir for 4-6 h, dry at 60°C for 6 h, place it in a sintering furnace for sintering, and after the sintering is completed, obtain the Al2O3-SiC composite phase.

[0009] Preferably, during the preparation of the Al2O3-SiC composite phase, the ammonia water is 25wt% ammonia water.

[0010] Preferably, during the preparation of the Al2O3-SiC composite phase, the sintering process is carried out in argon, and a segmented sintering method is adopted. The first-stage sintering temperature is 550-600°C, the heating rate is 3°C / min, and the sintering time is 1 h. The second-stage sintering temperature is 1600-1650°C, the heating rate is 3°C / min, and the sintering time is 2-3 h.

[0011] Preferably, the method for preparing the yttrium oxide - kyanite composite powder comprises the following steps: Mix nano - yttrium oxide, kyanite, and absolute ethanol with a mass ratio of 100:60 - 80:450 - 600 evenly, carry out ball milling. The ball milling time is 12 - 15 h, and the ball milling speed is 400 - 500 r / min. After ball milling, carry out ultrasonic treatment. The ultrasonic power is 400 - 500 W, and the ultrasonic time is 40 - 60 min. Then carry out suction filtration and dry at 60 °C for 24 h to obtain the yttrium oxide - kyanite composite powder.

[0012] Preferably, the mass ratio of the Al2O3 - SiC composite phase to the yttrium oxide - kyanite composite powder in step one is 100:35 - 45. The heating and melting process is carried out in an argon atmosphere. The heating and melting temperature is 1900 °C - 1950 °C, and the heating and melting time is 3 - 4 h.

[0013] Preferably, during the fiber spinning process in step two, the centrifugal spinning rate is 1000 - 1300 r / min, the diameter of the roller head is 254 mL, and the aperture of the roller head is set to 0.5 - 0.8 mm.

[0014] Further, the temperature of the rapid cooling with cold air in step two is 10 - 15 °C, the wind speed is 12 - 15 m / s, and the fiber diameter is controlled to be 15 - 25 μm.

[0015] Preferably, the specific method for preparing the low - shrinkage ceramic fiber blanket in step three comprises the following steps: Mix the composite fiber and the binder with a mass ratio of 100:1 - 3, suck them into the cotton collector through negative pressure for cotton collection, and then transfer them to the needling machine for needling. The needle frequency is 8000 needles / m 2 , the depth of the needle is 10 - 12 mm, the needle density is 20 needles / cm², and then carry out high - temperature setting. During the high - temperature setting process, it is divided into two - stage temperature control. The heating rate of the first - stage temperature control is 1 °C / min. When the temperature reaches 600 °C, keep it warm for 1 h. Then, in a nitrogen atmosphere, with a heating rate of 3 °C / min, heat up to 1000 °C and keep it warm for 1 h. The high - temperature setting time is 1 h, and then carry out rapid air cooling to obtain the low - shrinkage ceramic fiber blanket.

[0016] Preferably, the binder in step three is composed of phenylboric acid - modified kaolin, nano - silica sol, and aluminum phosphate sol with a mass ratio of 2:1:0.5.

[0017] Preferably, the preparation method of the phenylboronic acid modified kaolin in the step three comprises the following steps: ultrasonically disperse the activated kaolin in toluene, after uniform dispersion, in a nitrogen atmosphere, add 4-carboxyphenylboronic acid pinacol ester, dicyclohexylcarbodiimide and 4-dimethylaminopyridine, wherein the mass ratio of the activated kaolin, toluene, 4-carboxyphenylboronic acid pinacol ester, dicyclohexylcarbodiimide and 4-dimethylaminopyridine is 100:1500-1800:105-120:5-8:0.8-1, stir and mix to react, after the reaction is completed, centrifuge, wash with absolute ethanol, and vacuum dry at 60 °C for 24 h to obtain the phenylboronic acid modified kaolin.

[0018] Preferably, the reaction temperature in the preparation process of the phenylboronic acid modified kaolin is 70-80 °C, and the reaction time is 12-15 h.

[0019] Further, the preparation method of the activated kaolin is as follows: stir and mix kaolin, sodium hydroxide and deionized water with a mass ratio of 8:0.5:100, heat up, carry out an activation reaction at 85 °C, the reaction time is 8 h, after the reaction is completed, centrifuge, the centrifugation rate is 6000 r / min, the centrifugation time is 8 min, wash with deionized water, and vacuum dry at 80 °C for 24 h to obtain the activated kaolin.

[0020] Compared with the prior art, the beneficial effects of the present invention are as follows: (1) In the present invention, tetraethyl orthosilicate is used as the silicon source, aluminum nitrate nonahydrate is used as the aluminum source, citric acid is used as the complexing agent, and sucrose is used as the carbon source. After mixing and reacting, sintering is carried out to form a framework structure of silicate and alumina. Sucrose pyrolyzes to produce carbon, and an Al2O3-SiC composite phase is obtained. This composite combines the excellent properties of alumina and silicon carbide, has excellent high-temperature resistance, a high melting point, and good stability. Yttrium oxide has a high melting point and can form yttrium aluminum garnet with alumina, effectively inhibiting grain boundary migration. Kyanite decomposes into mullite under high-temperature conditions, which can improve the creep resistance of the matrix. Yttrium oxide and kyanite are ball-milled and ultrasonically treated, so that the yttrium oxide particles are uniformly coated on the surface of kyanite, reducing the sintering temperature. Kyanite can play a micro-expansion role, and during the combustion process of the matrix, it can reduce the shrinkage ratio during the ceramic sintering process, helping to reduce defects such as cracks and deformation caused by shrinkage during the firing process, and can effectively improve the overall strength. At the same time, it improves the compactness of the internal structure of the ceramic fiber blanket, reduces oxidation pores, and improves the creep resistance and stability.

[0021] (2) In the present invention, sodium hydroxide is used to activate kaolin. The hydroxyl groups on the activated kaolin react with the carboxyl groups on 4-carboxyphenylboronic acid pinacol ester to undergo an esterification reaction, resulting in phenylboronic acid-modified kaolin, and phenylboronic acid is introduced onto the kaolin. The binder is composed of phenylboronic acid-modified kaolin, nano-silica sol, and aluminum phosphate sol. Among them, the phenylboronic acid-modified kaolin further enhances the binding performance of kaolin, enabling it to better penetrate and interweave with the fibers of the ceramic fiber blanket, thereby improving the overall binding strength, contributing to the formation of a stable structural network in the ceramic fiber blanket, and enhancing its overall strength and stability. Moreover, the phenylboronic acid-modified kaolin has a very high specific surface area and porosity, and can adsorb fine particles and impurities on the surface of the ceramic fiber blanket. The boron heterocycle can form a stronger bond with the ceramic fiber, form a stable compound, improve the mechanical properties of the matrix, and can effectively prevent oxidation. The nano-silica sol can fill the fiber gaps and form a silica glass phase at high temperatures, improving the densification of the matrix. The aluminum phosphate sol can generate an AlPO4 ceramic phase under high-temperature conditions to form a three-dimensional network structure.

[0022] (3) In the present invention, composite fibers are obtained through a spinning process and rapid cooling with cold air. The obtained fibers are finer and more uniform, providing a good foundation for subsequent manufacturing processes. Then, cotton collection, needling, and high-temperature shaping are adopted to tightly interweave the fiber layer, significantly improving the tensile strength of the fiber blanket, and obtaining a ceramic fiber blanket. This ceramic fiber blanket uses an Al2O3-SiC composite phase and a yttrium oxide - kyanite composite powder as the main raw materials, can maintain dimensional stability in a high-temperature environment, has a low shrinkage rate, excellent heat insulation and heat preservation performance, a small thermal conductivity, can isolate the transfer of heat, achieve the effect of energy conservation and consumption reduction, and greatly improve the mechanical properties. Specific embodiments

[0023] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative efforts belong to the scope of protection of the present invention. Example 1

[0024] A method for manufacturing a low-shrinkage ceramic fiber blanket includes the following steps: (1) Mix the Al2O3-SiC composite phase and the yttrium oxide - kyanite composite powder with a mass ratio of 100:35 evenly, pass through a 200-mesh sieve, place them in a resistance furnace, heat and melt them. The heating and melting process is carried out in an argon atmosphere. The heating and melting temperature is 1900 °C, and the heating and melting time is 4 h to obtain a molten slurry. (2) Centrifugally spin the molten slurry using a centrifugal spinning machine at a spinning rate of 1000 r / min. The diameter of the spinning head is 254 mL, and the aperture of the spinning head is set to 0.5 mm. Spin it into a cotton-like shape and rapidly cool it with cold air. The temperature of the rapid cold air is 10 °C, and the wind speed is 12 m / s. Control the fiber diameter to be 15 μm to obtain composite fibers. (3) Mix the composite fibers and the binder at a mass ratio of 100:1. The binder consists of phenylboric acid-modified kaolin, nano-silica sol, and aluminum phosphate sol at a mass ratio of 2:1:0.5. Suction it into a cotton collector under negative pressure for cotton collection, and then transfer it to a needle punching machine for needle punching. The needle frequency is 8000 needles / m 2 , the depth of the punching needle is 10 mm, the needle density is 20 needles / cm², and then perform high-temperature shaping. During the high-temperature shaping process, it is divided into two-stage temperature control. The heating rate of the first-stage temperature control is 1 °C / min. When the temperature reaches 600 °C, keep it warm for 1 h. Then, in a nitrogen atmosphere, heat it up to 1000 °C at a heating rate of 3 °C / min and keep it warm for 1 h. The high-temperature shaping time is 1 h, and then rapidly air-cool to obtain a low shrinkage ceramic fiber blanket.

[0025] The preparation method of the Al2O3-SiC composite phase includes the following steps: Add polyvinyl alcohol to deionized water. The mass ratio of polyvinyl alcohol to deionized water is 4:100. Heat it up and mix evenly at 80 °C to obtain an aqueous polyvinyl alcohol solution. Mix evenly the tetraethyl orthosilicate and ethanol solution at a mass ratio of 10:100. The ethanol solution consists of deionized water and absolute ethanol at a volume ratio of 1:1. Dropwise add dilute hydrochloric acid to adjust the pH to 2 and stir and mix for 2 h to obtain a tetraethyl orthosilicate solution. Mix the aqueous polyvinyl alcohol solution and the tetraethyl orthosilicate solution at a volume ratio of 1:1 and stir for 3 h to obtain a mixture A. Mix aluminum nitrate nonahydrate, citric acid, sucrose, and deionized water at a mass ratio of 100:70:12:950, use ammonia water to adjust the pH to 4 (the ammonia water is 25 wt% ammonia water), stir and mix for 2 h, and after mixing evenly, obtain a mixture B. Mix the mixture A and the mixture B in a volume ratio of 1:1, stir for 4 h, dry at 60 °C for 6 h, and place it in a sintering furnace for sintering. The sintering process is carried out in argon, and a segmented sintering method is adopted. The first-stage sintering temperature is 550 °C, the heating rate is 3 °C / min, and the sintering time is 1 h. The second-stage sintering temperature is 1600 °C, the heating rate is 3 °C / min, and the sintering time is 3 h. After sintering, obtain the Al2O3-SiC composite phase.

[0026] The preparation method of the yttrium oxide - kyanite composite powder includes the following steps: Mix nano - yttrium oxide, kyanite, and absolute ethanol with a mass ratio of 100:60:450 evenly, carry out ball milling. The ball milling time is 12 h, and the ball milling speed is 400 r / min. After ball milling, carry out ultrasonic treatment. The ultrasonic power is 400 W, and the ultrasonic time is 40 min. Then carry out suction filtration and dry at 60 °C for 24 h to obtain the yttrium oxide - kyanite composite powder.

[0027] The preparation method of the phenylboronic acid - modified kaolin includes the following steps: Ultrasonically disperse activated kaolin in toluene. After uniform dispersion, in a nitrogen atmosphere, add 4 - carboxyphenylboronic acid pinacol ester, dicyclohexylcarbodiimide, and 4 - dimethylaminopyridine. The mass ratio of activated kaolin, toluene, 4 - carboxyphenylboronic acid pinacol ester, dicyclohexylcarbodiimide, and 4 - dimethylaminopyridine is 100:1500:105:5:0.8. Stir and mix to carry out the reaction. The reaction temperature is 70 °C, and the reaction time is 15 h. After the reaction ends, carry out centrifugation, wash with absolute ethanol, and vacuum - dry at 60 °C for 24 h to obtain the phenylboronic acid - modified kaolin. Example 2

[0028] A manufacturing method of a low - shrinkage ceramic fiber blanket includes the following steps: (1) Mix the Al2O3 - SiC composite phase and the yttrium oxide - kyanite composite powder with a mass ratio of 100:40 evenly, pass through a 200 - mesh sieve, place it in a resistance furnace, and heat and melt. The heating and melting process is carried out in an argon atmosphere. The heating and melting temperature is 1920 °C, and the heating and melting time is 3.5 h to obtain a molten slurry. (2) Centrifugally spin - draw the molten slurry with a spin - drawing machine at a rate of 1100 r / min. The diameter of the spinneret is 254 mL, the aperture of the spinneret is set to 0.6 mm, and it is spun into a cotton - like shape and rapidly cooled with cold air. The temperature of the rapid cold - air cooling is 12 °C, and the wind speed is 14 m / s. Control the fiber diameter to be 18 μm to obtain composite fibers. (3) Mix the composite fibers and the binder with a mass ratio of 100:1.5. The binder is composed of phenylboronic acid - modified kaolin, nano - silica sol, and aluminum phosphate sol with a mass ratio of 2:1:0.5. Through negative pressure, suck it into a cotton collector for cotton collection, and then transfer it to a needling machine for needling. The needle frequency is 8000 needles / m 2 , the depth of the barbed needle is 11 mm, the needle density is 20 needles / cm², and then carry out high - temperature shaping. During the high - temperature shaping process, it is divided into two - stage temperature control. The heating rate of the first - stage temperature control is 1 °C / min. When the temperature reaches 600 °C, keep it warm for 1 h. Then, in a nitrogen atmosphere, with a heating rate of 3 °C / min, raise the temperature to 1000 °C and keep it warm for 1 h. The high - temperature shaping time is 1 h, and then rapidly air - cool to obtain the low - shrinkage ceramic fiber blanket.

[0029] The preparation method of the Al2O3-SiC composite phase includes the following steps: Add polyvinyl alcohol to deionized water, with the mass ratio of polyvinyl alcohol to deionized water being 5:100. Heat up and mix evenly at 80 °C to obtain an aqueous polyvinyl alcohol solution. Mix tetraethyl orthosilicate and an ethanol solution with a mass ratio of 12:100 evenly. The ethanol solution consists of deionized water and absolute ethanol with a volume ratio of 1:1. Dropwise add dilute hydrochloric acid to adjust the pH to 2, and stir and mix for 2 h to obtain a tetraethyl orthosilicate solution. Mix the aqueous polyvinyl alcohol solution and the tetraethyl orthosilicate solution with a volume ratio of 1:1, and stir for 3 h to obtain a mixture A. Mix aluminum nitrate nonahydrate, citric acid, sucrose, and deionized water with a mass ratio of 100:72:14:980, use ammonia water to adjust the pH to 4.5 (the ammonia water is 25 wt% ammonia water), stir and mix for 2 h, and after mixing evenly, obtain a mixture B. Mix mixture A and mixture B in a volume ratio of 1:1, stir for 5 h, dry at 60 °C for 6 h, place it in a sintering furnace for sintering. The sintering process is carried out in argon, and a segmented sintering method is adopted. The first-stage sintering temperature is 560 °C, the heating rate is 3 °C / min, and the sintering time is 1 h. The second-stage sintering temperature is 1620 °C, the heating rate is 3 °C / min, and the sintering time is 2.5 h. After sintering, the Al2O3-SiC composite phase is obtained.

[0030] The preparation method of the yttrium oxide - kyanite composite powder includes the following steps: Mix nano yttrium oxide, kyanite, and absolute ethanol with a mass ratio of 100:68:500 evenly, carry out ball milling. The ball milling time is 14 h, and the ball milling speed is 450 r / min. After ball milling is completed, carry out ultrasonic treatment. The ultrasonic power is 450 W, and the ultrasonic time is 50 min. Carry out suction filtration and dry at 60 °C for 24 h to obtain the yttrium oxide - kyanite composite powder.

[0031] The preparation method of the phenylboronic acid modified kaolin includes the following steps: Ultrasonically disperse activated kaolin in toluene. After dispersing evenly, in a nitrogen atmosphere, add 4 - carboxyphenylboronic acid pinacol ester, dicyclohexylcarbodiimide, and 4 - dimethylaminopyridine. The mass ratio of activated kaolin, toluene, 4 - carboxyphenylboronic acid pinacol ester, dicyclohexylcarbodiimide, and 4 - dimethylaminopyridine is 100:1600:110:6:0.9. Stir and mix to carry out a reaction. The reaction temperature is 75 °C, and the reaction time is 14 h. After the reaction is completed, carry out centrifugation, wash with absolute ethanol, and vacuum dry at 60 °C for 24 h to obtain the phenylboronic acid modified kaolin. Example 3

[0032] A manufacturing method of a low shrinkage ceramic fiber blanket includes the following steps: (1) Mix the Al2O3-SiC composite phase and yttrium oxide-kyanite composite powder with a mass ratio of 100:40 evenly, pass through a 200-mesh sieve, place it in an electric resistance furnace, heat and melt it. The heating and melting process is carried out in an argon atmosphere. The heating and melting temperature is 1920 °C, and the heating and melting time is 3.5 h to obtain a molten slurry. (2) Centrifugally spin the molten slurry with a spinning machine. The centrifugal spinning speed is 1100 r / min, the diameter of the spinning head is 254 mL, the aperture of the spinning head is set to 0.6 mm, and it is spun into a cotton-like shape and rapidly cooled with cold air. The temperature of the rapid cold air cooling is 12 °C, and the wind speed is 14 m / s. Control the fiber diameter to be 18 μm to obtain composite fibers. (3) Mix the composite fibers and the binder with a mass ratio of 100:1.5. The binder consists of phenylboric acid-modified kaolin, nano-silica sol, and aluminum phosphate sol with a mass ratio of 2:1:0.5. Suction it into a cotton collector under negative pressure for cotton collection, and transfer it to a needling machine for needling. The needle frequency is 8000 needles / m 2 , the depth of the needle is 11 mm, the needle density is 20 needles / cm², and then carry out high-temperature setting. During the high-temperature setting process, it is divided into two-stage temperature control. The heating rate of the first-stage temperature control is 1 °C / min. When the temperature reaches 600 °C, keep it warm for 1 h. Then, in a nitrogen atmosphere, with a heating rate of 3 °C / min, heat up to 1000 °C and keep it warm for 1 h. The high-temperature setting time is 1 h, and it is rapidly air-cooled to obtain a low shrinkage ceramic fiber blanket.

[0033] The preparation method of the Al2O3-SiC composite phase includes the following steps: Add polyvinyl alcohol to deionized water. The mass ratio of polyvinyl alcohol to deionized water is 5.5:100. Heat up and mix evenly at 80 °C to obtain an aqueous polyvinyl alcohol solution. Mix the tetraethyl orthosilicate and ethanol solution with a mass ratio of 14:100 evenly. The ethanol solution consists of deionized water and absolute ethanol with a volume ratio of 1:1. Dropwise add dilute hydrochloric acid to adjust the pH to 2, and stir and mix for 2 h to obtain a tetraethyl orthosilicate solution. Mix the aqueous polyvinyl alcohol solution and the tetraethyl orthosilicate solution with a volume ratio of 1:1 and stir for 3 h to obtain a mixed solution A. Mix aluminum nitrate nonahydrate, citric acid, sucrose, and deionized water with a mass ratio of 100:74:14:1000, use ammonia water to adjust the pH to 4.5, and the ammonia water is 25 wt% ammonia water. Stir and mix for 2 h, and after mixing evenly, obtain a mixed solution B. Mix the mixed solution A and the mixed solution B according to a volume ratio of 1:1, stir for 5 h, dry at 60 °C for 6 h, and place it in a sintering furnace for sintering. The sintering process is carried out in argon, and a segmented sintering method is adopted. The first-stage sintering temperature is 580 °C, the heating rate is 3 °C / min, and the sintering time is 1 h. The second-stage sintering temperature is 1640 °C, the heating rate is 3 °C / min, and the sintering time is 2.5 h. After sintering, obtain the Al2O3-SiC composite phase.

[0034] The preparation method of the yttrium oxide - kyanite composite powder comprises the following steps: Mix nano - yttrium oxide, kyanite, and absolute ethanol with a mass ratio of 100:75:550 evenly, carry out ball milling. The ball milling time is 14 h, the ball milling speed is 480 r / min. After ball milling, carry out ultrasonic treatment. The ultrasonic power is 480 W, and the ultrasonic time is 55 min. Then carry out suction filtration and dry at 60 °C for 24 h to obtain the yttrium oxide - kyanite composite powder.

[0035] The preparation method of the phenylboronic acid - modified kaolin comprises the following steps: Ultrasonically disperse activated kaolin in toluene. After uniform dispersion, in a nitrogen atmosphere, add 4 - carboxyphenylboronic acid pinacol ester, dicyclohexylcarbodiimide, and 4 - dimethylaminopyridine. The mass ratio of activated kaolin, toluene, 4 - carboxyphenylboronic acid pinacol ester, dicyclohexylcarbodiimide, and 4 - dimethylaminopyridine is 100:1700:115:7:0.9. Stir and mix to carry out the reaction. The reaction temperature is 75 °C, and the reaction time is 14 h. After the reaction ends, carry out centrifugation, wash with absolute ethanol, and vacuum - dry at 60 °C for 24 h to obtain the phenylboronic acid - modified kaolin. Example 4

[0036] A manufacturing method of a low - shrinkage ceramic fiber blanket comprises the following steps: (1) Mix the Al2O3 - SiC composite phase and the yttrium oxide - kyanite composite powder with a mass ratio of 100:42 evenly, pass through a 200 - mesh sieve, place it in a resistance furnace, and heat - melt. The heat - melting process is carried out in an argon atmosphere. The heat - melting temperature is 1940 °C, and the heat - melting time is 3.5 h to obtain a molten slurry. (2) Centrifugally spin - draw the molten slurry with a centrifugal spin - drawing rate of 1200 r / min using a spinneret. The spinneret diameter is 254 mL, the spinneret hole diameter is set to 0.7 mm, and it is spun into a cotton - like shape, and then rapidly cooled with cold air. The temperature of the rapid cold air is 12 °C, the wind speed is 13 m / s, and the fiber diameter is controlled to be 20 μm to obtain composite fibers. (3) Mix the composite fibers and the binder with a mass ratio of 100:2. The binder is composed of phenylboronic acid - modified kaolin, nano - silica sol, and aluminum phosphate sol with a mass ratio of 2:1:0.5. Suction - inhale it into a cotton collector through negative pressure for cotton collection, and then transfer it to a needling machine for needling. The needle frequency is 8000 needles / m 2 , the depth of the barbed needle is 11 mm, the needle density is 20 needles / cm², and then carry out high - temperature shaping. During the high - temperature shaping process, it is divided into two - stage temperature control. The heating rate of the first - stage temperature control is 1 °C / min. When the temperature reaches 600 °C, keep it warm for 1 h. Then, in a nitrogen atmosphere, with a heating rate of 3 °C / min, raise the temperature to 1000 °C and keep it warm for 1 h. The high - temperature shaping time is 1 h, and then rapidly air - cool to obtain the low - shrinkage ceramic fiber blanket.

[0037] Among them, the preparation methods of the Al2O3-SiC composite phase, yttrium oxide - kyanite composite powder, and phenylboronic acid - modified kaolin are the same as those of the Al2O3-SiC composite phase, yttrium oxide - kyanite composite powder, and phenylboronic acid - modified kaolin in Example 3. Example 5

[0038] A method for manufacturing a low - shrinkage ceramic fiber blanket includes the following steps: (1) Mix the Al2O3 - SiC composite phase and yttrium oxide - kyanite composite powder with a mass ratio of 100:45 evenly, pass through a 200 - mesh sieve, place it in a resistance furnace, heat and melt it. The heating and melting process is carried out in an argon atmosphere. The heating and melting temperature is 1950 °C, and the heating and melting time is 3 h to obtain a molten slurry. (2) Centrifugally spin - draw the molten slurry with a centrifugal spin - drawing rate of 1300 r / min using a spin - drawing machine. The diameter of the spinning head is 254 mL, the aperture of the spinning head is set to 0.8 mm, and it is spun into a cotton - like shape and rapidly cooled with cold air. The temperature of the rapid cold air cooling is 15 °C, the wind speed is 15 m / s, and the fiber diameter is controlled to be 25 μm to obtain composite fibers. (3) Mix the composite fibers and the binder with a mass ratio of 100:3. The binder is composed of phenylboronic acid - modified kaolin, nano - silica sol, and aluminum phosphate sol with a mass ratio of 2:1:0.5. It is sucked into a cotton collector under negative pressure for cotton collection and then transferred to a needling machine for needling. The needle frequency is 8000 needles / m 2 , the depth of the needle penetration is 12 mm, the needle density is 20 needles / cm², and then high - temperature shaping is carried out. During the high - temperature shaping process, it is divided into two - stage temperature control. The heating rate of the first - stage temperature control is 1 °C / min. When the temperature reaches 600 °C, it is kept warm for 1 h. Then, in a nitrogen atmosphere, it is heated to 1000 °C at a heating rate of 3 °C / min and kept warm for 1 h. The high - temperature shaping time is 1 h, and it is rapidly air - cooled to obtain a low - shrinkage ceramic fiber blanket.

[0039] The preparation method of the Al2O3-SiC composite phase includes the following steps: Add polyvinyl alcohol to deionized water, with the mass ratio of polyvinyl alcohol to deionized water being 6:100. Heat up and mix evenly at 80 °C to obtain an aqueous polyvinyl alcohol solution. Mix tetraethyl orthosilicate and an ethanol solution with a mass ratio of 15:100 evenly, where the ethanol solution consists of deionized water and absolute ethanol with a volume ratio of 1:1. Dropwise add dilute hydrochloric acid to adjust the pH to 2, and stir and mix for 2 h to obtain a tetraethyl orthosilicate solution. Mix the aqueous polyvinyl alcohol solution and the tetraethyl orthosilicate solution with a volume ratio of 1:1, and stir for 3 h to obtain mixture A. Mix aluminum nitrate nonahydrate, citric acid, sucrose, and deionized water with a mass ratio of 100:75:15:1050, use ammonia water to adjust the pH to 5 (the ammonia water is 25 wt% ammonia water), stir and mix for 2 h, and after mixing evenly, obtain mixture B. Mix mixture A and mixture B in a volume ratio of 1:1, stir for 6 h, dry at 60 °C for 6 h, place it in a sintering furnace for sintering. The sintering process is carried out in argon, and a segmented sintering method is adopted. The first-stage sintering temperature is 600 °C, the heating rate is 3 °C / min, and the sintering time is 1 h. The second-stage sintering temperature is 1650 °C, the heating rate is 3 °C / min, and the sintering time is 2 h. After sintering is completed, the Al2O3-SiC composite phase is obtained.

[0040] The preparation method of the yttrium oxide - kyanite composite powder includes the following steps: Mix nano yttrium oxide, kyanite, and absolute ethanol with a mass ratio of 100:80:600 evenly, carry out ball milling. The ball milling time is 15 h, and the ball milling speed is 500 r / min. After ball milling is completed, carry out ultrasonic treatment. The ultrasonic power is 500 W, and the ultrasonic time is 60 min. Carry out suction filtration and dry at 60 °C for 24 h to obtain the yttrium oxide - kyanite composite powder.

[0041] The preparation method of the phenylboronic acid - modified kaolin includes the following steps: Ultrasonically disperse activated kaolin in toluene. After dispersing evenly, in a nitrogen atmosphere, add 4 - carboxyphenylboronic acid pinacol ester, dicyclohexylcarbodiimide, and 4 - dimethylaminopyridine. The mass ratio of activated kaolin, toluene, 4 - carboxyphenylboronic acid pinacol ester, dicyclohexylcarbodiimide, and 4 - dimethylaminopyridine is 100:1800:120:8:1. Stir and mix to carry out a reaction. The reaction temperature is 80 °C, and the reaction time is 15 h. After the reaction is completed, carry out centrifugation, wash with absolute ethanol, and vacuum dry at 60 °C for 24 h to obtain the phenylboronic acid - modified kaolin.

[0042] Comparative Example 1 A manufacturing method of a ceramic fiber blanket includes the following steps: (1)Mix the Al2O3, SiC, yttrium oxide - kyanite composite powder with a mass ratio of 100:42 evenly, pass through a 200 - mesh sieve, place it in a resistance furnace, heat and melt it. The heating and melting process is carried out in an argon atmosphere. The heating and melting temperature is 1940 °C, and the heating and melting time is 3.5 h to obtain a molten slurry; (2)Centrifugally spin - draw the molten slurry with a centrifugal spinning machine at a speed of 1200 r / min. The diameter of the spinning head is 254 mL, the aperture of the spinning head is set to 0.7 mm, and it is spun into a cotton - like shape and rapidly cooled with cold air. The temperature of the rapid cold air is 12 °C, and the wind speed is 13 m / s. Control the fiber diameter to be 20 μm to obtain composite fibers; (3)Mix the composite fibers and the binder with a mass ratio of 100:2. The binder consists of phenylboronic acid - modified kaolin, nano - silica sol, and aluminum phosphate sol with a mass ratio of 2:1:0.5. Suck it into a cotton collector under negative pressure for cotton collection, and then transfer it to a needle - punching machine for needle - punching. The needle frequency is 8000 needles / m 2 The depth of the punching needle is 11 mm, the needle density is 20 needles / cm², and then high - temperature setting is carried out. During the high - temperature setting process, it is divided into two - stage temperature control. The heating rate of the first - stage temperature control is 1 °C / min. When the temperature reaches 600 °C, keep it warm for 1 h. Then, in a nitrogen atmosphere, with a heating rate of 3 °C / min, raise the temperature to 1000 °C and keep it warm for 1 h. The high - temperature setting time is 1 h, and then rapidly air - cool to obtain a ceramic fiber blanket.

[0043] The preparation method of the yttrium oxide - kyanite composite powder includes the following steps: Mix the nano - yttrium oxide, kyanite, and absolute ethanol with a mass ratio of 100:75:550 evenly, carry out ball - milling. The ball - milling time is 14 h, the ball - milling speed is 480 r / min. After ball - milling, carry out ultrasonic treatment. The ultrasonic power is 480 W, and the ultrasonic time is 55 min. Then carry out suction filtration and dry it at 60 °C for 24 h to obtain the yttrium oxide - kyanite composite powder.

[0044] The preparation method of the phenylboronic acid - modified kaolin includes the following steps: Ultrasonically disperse the activated kaolin in toluene. After uniform dispersion, in a nitrogen atmosphere, add 4 - carboxyphenylboronic acid pinacol ester, dicyclohexylcarbodiimide, and 4 - dimethylaminopyridine. The mass ratio of the activated kaolin, toluene, 4 - carboxyphenylboronic acid pinacol ester, dicyclohexylcarbodiimide, and 4 - dimethylaminopyridine is 100:1700:115:7:0.9. Stir and mix them to react. The reaction temperature is 75 °C, and the reaction time is 14 h. After the reaction, carry out centrifugation, wash it with absolute ethanol, and vacuum - dry it at 60 °C for 24 h to obtain the phenylboronic acid - modified kaolin.

[0045] Comparative Example 2 A method for making a ceramic fiber blanket, including the following steps: (1) Mix the Al2O3-SiC composite phase, yttrium oxide, and cyanite with a mass ratio of 100:42 evenly, pass through a 200-mesh sieve, place them in a resistance furnace, heat and melt. The heating and melting process is carried out in an argon atmosphere. The heating and melting temperature is 1940 °C, and the heating and melting time is 3.5 h to obtain a molten slurry. (2) Centrifugally spin the molten slurry with a centrifugal spinning machine at a rate of 1200 r / min. The diameter of the roller head is 254 mL, the aperture of the roller head is set to 0.7 mm, and it is spun into a cotton-like shape and rapidly cooled with cold air. The temperature of the rapid cold air cooling is 12 °C, and the wind speed is 13 m / s. Control the fiber diameter to be 20 μm to obtain composite fibers. (3) Mix the composite fibers and the binder with a mass ratio of 100:2. The binder is composed of phenylboric acid-modified kaolin, nano-silica sol, and aluminum phosphate sol with a mass ratio of 2:1:0.5. Suction it into a cotton collector under negative pressure for cotton collection, and then transfer it to a needle punching machine for needle punching. The needle frequency is 8000 needles / m 2 , the depth of the needle is 11 mm, the needle density is 20 needles / cm², and then perform high-temperature shaping. During the high-temperature shaping process, it is divided into two-stage temperature control. The heating rate of the first-stage temperature control is 1 °C / min. When the temperature reaches 600 °C, keep it warm for 1 h. Then, in a nitrogen atmosphere, increase the temperature to 1000 °C at a heating rate of 3 °C / min and keep it warm for 1 h. The high-temperature shaping time is 1 h, and it is rapidly air-cooled to obtain a ceramic fiber blanket.

[0046] The preparation method of the Al2O3-SiC composite phase includes the following steps: Add polyvinyl alcohol to deionized water. The mass ratio of polyvinyl alcohol to deionized water is 5.5:100. Heat up and mix evenly at 80 °C to obtain an aqueous polyvinyl alcohol solution. Mix the tetraethyl orthosilicate and ethanol solution with a mass ratio of 14:100 evenly. The ethanol solution is composed of deionized water and absolute ethanol with a volume ratio of 1:1. Dropwise add dilute hydrochloric acid to adjust the pH to 2, and stir and mix for 2 h to obtain a tetraethyl orthosilicate solution. Mix the aqueous polyvinyl alcohol solution and the tetraethyl orthosilicate solution with a volume ratio of 1:1 and stir for 3 h to obtain a mixed solution A. Mix aluminum nitrate nonahydrate, citric acid, sucrose, and deionized water with a mass ratio of 100:74:14:1000, use ammonia water to adjust the pH to 4.5 (the ammonia water is 25 wt% ammonia water), stir and mix for 2 h, and after mixing evenly, obtain a mixed solution B. Mix the mixed solution A and the mixed solution B in a volume ratio of 1:1, stir for 5 h, dry at 60 °C for 6 h, and place it in a sintering furnace for sintering. The sintering process is carried out in argon, and a segmented sintering method is adopted. The first-stage sintering temperature is 580 °C, the heating rate is 3 °C / min, and the sintering time is 1 h. The second-stage sintering temperature is 1640 °C, the heating rate is 3 °C / min, and the sintering time is 2.5 h. After sintering, the Al2O3-SiC composite phase is obtained.

[0047] The preparation method of the phenylboronic acid modified kaolin comprises the following steps: Ultrasonically disperse the activated kaolin in toluene. After uniform dispersion, in a nitrogen atmosphere, add 4-carboxyphenylboronic acid pinacol ester, dicyclohexylcarbodiimide and 4-dimethylaminopyridine. The mass ratio of the activated kaolin, toluene, 4-carboxyphenylboronic acid pinacol ester, dicyclohexylcarbodiimide and 4-dimethylaminopyridine is 100:1700:115:7:0.9. Stir and mix to carry out the reaction. The reaction temperature is 75 °C and the reaction time is 14 h. After the reaction, centrifuge, wash with absolute ethanol, and vacuum dry at 60 °C for 24 h to obtain the phenylboronic acid modified kaolin.

[0048] Comparative Example 3 A manufacturing method of a ceramic fiber blanket comprises the following steps: (1) Mix the Al2O3-SiC composite phase and yttrium oxide-kyanite composite powder with a mass ratio of 100:42 evenly, pass through a 200-mesh sieve, place it in a resistance furnace, heat and melt. The heating and melting process is carried out in an argon atmosphere. The heating and melting temperature is 1940 °C and the heating and melting time is 3.5 h to obtain a molten slurry; (2) Centrifugally spin the molten slurry through a spinneret. The centrifugal spinning rate is 1200 r / min, the spinneret diameter is 254 mL, the spinneret pore diameter is set to 0.7 mm, spin it into a cotton-like shape, and rapidly cool with cold air. The temperature of the rapid cold air is 12 °C and the wind speed is 13 m / s. Control the fiber diameter to be 20 μm to obtain composite fibers; (3) Mix the composite fibers and the binder with a mass ratio of 100:2. The binder is composed of kaolin, nano-silica sol and aluminum phosphate sol with a mass ratio of 2:1:0.5. Suction it into a cotton collector under negative pressure for cotton collection, and transfer it to a needling machine for needling. The needle frequency is 8000 needles / m 2 , the depth of the stabbing needle is 11 mm, the needle density is 20 needles / cm², and then carry out high-temperature shaping. During the high-temperature shaping process, it is divided into two-stage temperature control. The heating rate of the first-stage temperature control is 1 °C / min. When the temperature reaches 600 °C, keep it warm for 1 h. Then, in a nitrogen atmosphere, heat it up to 1000 °C at a heating rate of 3 °C / min and keep it warm for 1 h. The high-temperature shaping time is 1 h, and rapidly air-cool to obtain the ceramic fiber blanket.

[0049] The preparation method of the Al2O3-SiC composite phase includes the following steps: Add polyvinyl alcohol to deionized water, with the mass ratio of polyvinyl alcohol to deionized water being 5.5:100. Heat up and mix evenly at 80 °C to obtain an aqueous polyvinyl alcohol solution. Mix tetraethyl orthosilicate and an ethanol solution with a mass ratio of 14:100 evenly. The ethanol solution consists of deionized water and absolute ethanol with a volume ratio of 1:1. Dropwise add dilute hydrochloric acid to adjust the pH to 2, and stir and mix for 2 h to obtain a tetraethyl orthosilicate solution. Mix the aqueous polyvinyl alcohol solution and the tetraethyl orthosilicate solution with a volume ratio of 1:1, and stir for 3 h to obtain mixture A. Mix aluminum nitrate nonahydrate, citric acid, sucrose, and deionized water with a mass ratio of 100:74:14:1000, use ammonia water to adjust the pH to 4.5 (the ammonia water is 25 wt% ammonia water), stir and mix for 2 h, and after mixing evenly, obtain mixture B. Mix mixture A and mixture B in a volume ratio of 1:1, stir for 5 h, dry at 60 °C for 6 h, place it in a sintering furnace for sintering. The sintering process is carried out in argon, and a segmented sintering method is adopted. The first-stage sintering temperature is 580 °C, the heating rate is 3 °C / min, and the sintering time is 1 h. The second-stage sintering temperature is 1640 °C, the heating rate is 3 °C / min, and the sintering time is 2.5 h. After sintering, the Al2O3-SiC composite phase is obtained.

[0050] The preparation method of the yttrium oxide - kyanite composite powder includes the following steps: Mix nano yttrium oxide, kyanite, and absolute ethanol with a mass ratio of 100:75:550 evenly, carry out ball milling. The ball milling time is 14 h, and the ball milling speed is 480 r / min. After ball milling, carry out ultrasonic treatment. The ultrasonic power is 480 W, and the ultrasonic time is 55 min. Then carry out suction filtration and dry at 60 °C for 24 h to obtain the yttrium oxide - kyanite composite powder.

[0051] In the present invention, the preparation method of the activated kaolin in the examples and comparative examples is as follows: Stir and mix kaolin, sodium hydroxide, and deionized water with a mass ratio of 8:0.5:100, heat up, and carry out an activation reaction at 85 °C. The reaction time is 8 h. After the reaction, carry out centrifugation. The centrifugation rate is 6000 r / min, and the centrifugation time is 8 min. Wash with deionized water and vacuum dry at 80 °C for 24 h to obtain the activated kaolin.

[0052] The raw materials used in the examples and comparative examples of the present invention are all general raw materials in the industry and can be purchased through commercial channels; the kaolin is purchased from Shenzhen Haiyang Powder Technology Co., Ltd.; other reagents are all commercially available.

[0053] Perform performance tests on the ceramic fiber blankets prepared in Examples 1 - 5 and Comparative Examples 1 - 3. The tests are as follows: (1)Shrinkage rate test: Use the prepared ceramic fiber blanket as a sample. The size of the cut sample is 100mm×100mm×10mm. Dry it in an oven at 105°C for 2h. After cooling to room temperature, measure the initial size L0. Place the sample on a quartz backing plate and put it in a high-temperature box furnace for performance testing. During the testing process, the heating rate is 5°C / min. Heat up to 1300°C and hold for 1h. After natural cooling to room temperature, measure the size L1 of the sample after heat treatment. Shrinkage rate = (L0 - L1) / L0×100%. Each group is tested three times and the average value is taken; (2)Thermal conductivity test: Conduct a thermal conductivity test on the sample. The test standard refers to YB / T 4130 - 2005. Record the thermal conductivity at an average of 500°C. Each group is tested three times and the average value is taken; (3)Mechanical property test: Cut the sample into a dumbbell shape with a total length of 75cm and a test part length of 40mm and a width of 10mm. Clamp the upper and lower ends of the specimen to a tensile testing machine and stretch it at a tensile speed of 100mm / min. Measure the tensile strength and elongation at break when it breaks. Each sample is tested three times and the average value is taken; The above test results are shown in Table 1 as follows: Table 1

[0054] It can be seen from the test results in Table 1 that the ceramic fiber blankets corresponding to Examples 1 - 5 have a low shrinkage rate, a low thermal conductivity, excellent high-temperature stability, and good mechanical properties. In Comparative Example 1, Al2O3 and SiC were directly added instead of the Al2O3 - SiC composite phase, and the comprehensive performance was greatly reduced, the shrinkage rate and thermal conductivity increased, and the mechanical properties decreased. In Comparative Example 2, yttrium oxide and kyanite were not treated, and the comprehensive performance deteriorated. In Comparative Example 3, kaolin was not modified and was directly added to the matrix as an adhesive, with poor dispersibility, affected shrinkage rate and thermal conductivity, and a decrease in tensile strength.

[0055] Although the embodiments of the present invention have been shown and described, for those of ordinary skill in the art, it can be understood that various changes, modifications, substitutions, and variations can be made to these embodiments without departing from the principles and spirit of the present invention. All equivalent changes and improvements made within the scope of the present invention application shall still fall within the scope covered by the present invention.

Claims

1. A manufacturing method of a ceramic fiber blanket with a low shrinkage rate, characterized in that: It includes the following steps: Step 1: Mix the Al2O3-SiC composite phase and yttrium oxide-kyanite composite powder evenly, sieve them, place them in a resistance furnace, heat and melt them to obtain a molten slurry; Step 2: Centrifugally spin the molten slurry in Step 1 with a spinning machine to make it cotton-like, and cool it to obtain composite fibers; Step 3: Mix the composite fibers and an adhesive, perform cotton collection and needling treatments, and then perform high-temperature shaping and cooling to obtain a ceramic fiber blanket with a low shrinkage rate.

2. The manufacturing method of a ceramic fiber blanket with low shrinkage rate according to claim 1, characterized in that: The preparation method of the Al2O3-SiC composite phase in Step 1 includes the following steps: Mix polyvinyl alcohol, deionized water, tetraethyl orthosilicate, and ethanol solution evenly to obtain a mixed solution A. Mix aluminum nitrate nonahydrate, citric acid, sucrose, and deionized water, adjust the pH to 4-5 with ammonia water, and after mixing evenly, obtain a mixed solution B. Mix the mixed solution A and the mixed solution B, stir evenly, dry, and sinter to obtain the Al2O3-SiC composite phase.

3. The manufacturing method of a low shrinkage ceramic fiber blanket according to claim 2, characterized in that: The specific preparation method of the Al2O3-SiC composite phase is as follows: Add polyvinyl alcohol to deionized water, and the mass ratio of polyvinyl alcohol to deionized water is 4-6:

100. Heat up and mix evenly at 80°C to obtain an aqueous polyvinyl alcohol solution. Mix tetraethyl orthosilicate and ethanol solution with a mass ratio of 10-15:100, where the ethanol solution is composed of deionized water and absolute ethanol with a volume ratio of 1:

1. Dropwise add dilute hydrochloric acid to adjust the pH to 2, and stir and mix for 2 h to obtain a tetraethyl orthosilicate solution. Mix the aqueous polyvinyl alcohol solution and the tetraethyl orthosilicate solution with a volume ratio of 1:1, and stir for 3 h to obtain a mixed solution A. Mix aluminum nitrate nonahydrate, citric acid, sucrose, and deionized water with a mass ratio of 100:70-75:12-15:950-1050, adjust the pH to 4-5 with ammonia water, stir and mix for 2 h, and after mixing evenly, obtain a mixed solution B. Mix the mixed solution A and the mixed solution B in a volume ratio of 1:1, stir for 4-6 h, dry at 60°C for 6 h, place it in a sintering furnace for sintering, and after the sintering is completed, obtain the Al2O3-SiC composite phase.

4. The manufacturing method of a low shrinkage ceramic fiber blanket according to claim 3, characterized in that: The sintering process is carried out in argon, and a segmented sintering method is adopted. The sintering temperature in the first stage is 550-600°C, the heating rate is 3°C / min, and the sintering time is 1 h. The sintering temperature in the second stage is 1600-1650°C, the heating rate is 3°C / min, and the sintering time is 2-3 h.

5. The manufacturing method of a low shrinkage ceramic fiber blanket according to claim 1, characterized in that: The preparation method of the yttrium oxide-kyanite composite powder includes the following steps: Mix nano yttrium oxide, kyanite, and absolute ethanol with a mass ratio of 100:60-80:450-600 evenly, perform ball milling for 12-15 h, and the ball milling speed is 400-500 r / min. After the ball milling is completed, perform ultrasonic treatment with a power of 400-500 W and an ultrasonic time of 40-60 min. Perform suction filtration and dry at 60°C for 24 h to obtain the yttrium oxide-kyanite composite powder.

6. The manufacturing method of a low shrinkage ceramic fiber blanket according to claim 1, characterized in that: In the first step, the mass ratio of the Al2O3-SiC composite phase to the yttrium oxide - kyanite composite powder is 100:35 - 45. The heating and melting process is carried out in an argon atmosphere. The heating and melting temperature is 1900°C - 1950°C, and the heating and melting time is 3 - 4 h.

7. The manufacturing method of a low shrinkage ceramic fiber blanket according to claim 1, characterized in that: In the second step, during the centrifugal spinning process, the centrifugal spinning rate is 1000 - 1300 r / min, the diameter of the spinning head is 254 mL, and the pore diameter of the spinning head is set to 0.5 - 0.8 mm.

8. The manufacturing method of a low shrinkage ceramic fiber blanket according to claim 1, characterized in that: The specific preparation method of the low shrinkage ceramic fiber blanket in the third step includes the following steps: mixing composite fibers and adhesives with a mass ratio of 100:1-3, sucking them into a cotton collector through negative pressure for cotton collection, and then transferring them to a needling machine for needling. The needle frequency is 8000 needles / m 2 , the depth of the barbed needle is 10-12 mm, the needle density is 20 needles / cm², and then high temperature setting is carried out. During the high temperature setting process, it is divided into two-stage temperature control. The heating rate of the first-stage temperature control is 1℃ / min. When the temperature reaches 600℃, it is kept warm for 1 h. Then, in a nitrogen atmosphere, it is heated to 1000℃ at a heating rate of 3℃ / min and kept warm for 1 h. The high temperature setting time is 1 h, and it is rapidly air-cooled to obtain the low shrinkage ceramic fiber blanket.

9. The manufacturing method of a low shrinkage ceramic fiber blanket according to claim 1, characterized in that: In the third step, the binder is composed of phenylboric acid - modified kaolin, nano - silica sol, and aluminum phosphate sol with a mass ratio of 2:1:0.

5.

10. The manufacturing method of a ceramic fiber blanket with a low shrinkage rate according to claim 9, characterized in that: The preparation method of the phenylboric acid - modified kaolin in the third step includes the following steps: Ultrasonically disperse the activated kaolin in toluene. After uniform dispersion, in a nitrogen atmosphere, add 4 - carboxyphenylboric acid pinacol ester, dicyclohexylcarbodiimide, and 4 - dimethylaminopyridine. The mass ratio of the activated kaolin, toluene, 4 - carboxyphenylboric acid pinacol ester, dicyclohexylcarbodiimide, and 4 - dimethylaminopyridine is 100:1500 - 1800:105 - 120:5 - 8:0.8 - 1. Stir and mix to react. After the reaction is completed, centrifuge, wash with absolute ethanol, and vacuum - dry at 60°C for 24 h to obtain the phenylboric acid - modified kaolin.

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