A method for producing a low-shrinkage ceramic fiber blanket
By using Al2O3-SiC composite phase and yttrium-azidiac composite powder, combined with specific processes and adhesives, the problem of poor stability and mechanical properties of ceramic fiber blankets at high temperatures is solved, and a ceramic fiber blanket with low shrinkage and high strength is achieved.
Patent Information
- Application Number
- CN202510704833.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-29
- Publication Date
- 2025-08-29
- Estimated Expiration
- 2045-05-29
AI Technical Summary
Traditional ceramic fiber blankets are prone to binding agent failure and fiber creep under high temperature conditions, resulting in high high-temperature shrinkage, structural collapse, poor stability, and poor mechanical properties and high-temperature stability.
Al2O3-SiC composite phase and yttrium oxide-blueite composite powder are used as the main raw materials. Through wire-blowing, cold air quenching, cotton collection, needle-punching and high-temperature setting processes, combined with phenylboric acid modified kaolin, nano silica sol and aluminum phosphate sol as binders, a stable structural network is formed to improve the tensile strength and high-temperature stability of the fiber blanket.
It significantly improves the tensile strength and high temperature stability of ceramic fiber blankets, reduces shrinkage, maintains dimensional stability, excellent thermal insulation and low thermal conductivity, and improves mechanical properties.
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Abstract
Description
Technical Field
[0001] The invention relates to the technical field of ceramic fibers, in particular to a method for manufacturing a low-shrinkage ceramic fiber blanket. Background Art
[0002] Ceramic fiber blankets are fibrous, high-temperature thermal insulation materials characterized by high-temperature resistance, excellent thermal stability, and lightweight construction. They are widely used in metallurgy, chemical engineering, aerospace, and other fields. Traditional ceramic fiber blankets, also known as aluminum silicate fiber blankets, are typically made primarily of aluminum silicate or alumina fibers through wet molding or dry needling. These blankets are susceptible to binder failure and fiber creep at high temperatures. They also experience high shrinkage, leading to localized stress concentration and structural collapse. High-temperature sintering also causes fiber embrittlement, resulting in poor blanket stability.
[0003] Chinese patent application CN117822201A discloses a method for preparing a high-temperature-resistant ceramic fiber blanket. The method comprises the following steps: selecting 35-43% alumina and 50-55% silica, stirring and blending them, and then high-temperature melting. The method then centrifugally spins the fibers, adding 1-5 parts of a binder and 1-4 parts of an additive, collecting the fibers, needling, heat shrinking, and winding them to produce a high-temperature-resistant ceramic fiber blanket. The addition of the binder and additives improves the toughness and strength of the ceramic fiber blanket. However, the fiber structure is susceptible to crystallization under long-term high-temperature conditions, resulting in average stability. Chinese patent application CN102605553A discloses a method for producing a 1500°C chromium-free aluminum silicate fiber blanket. The method comprises the following steps: raw material mixing (alumina, silica, and zirconium oxide particles are mixed in a specific ratio), resistance furnace melting, blow-forming, mixing mullite fibers, airflow mixing, collecting the fibers, needling, and heat treatment for crystal transformation to produce the fiber blanket. The blanket is clean and environmentally friendly, with a low shrinkage rate, but it is expensive and has 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] In view of the shortcomings of the existing technology, the present invention provides a method for preparing a low-shrinkage ceramic fiber blanket, prepares a low-shrinkage ceramic fiber blanket, and solves the problems of poor mechanical properties and high-temperature stability of the ceramic fiber blanket.
[0006] In order to achieve the above object, the present invention discloses a method for manufacturing a low-shrinkage ceramic fiber blanket, comprising the following steps:
[0007] Step 1: Evenly mix the Al2O3-SiC composite phase and the yttrium oxide-kyanite composite powder, pass through a 200-mesh sieve, place in a resistance furnace, heat and melt to obtain a slurry;
[0008] Step 2: The slurry in step 1 is centrifugally spun through a spinning machine to form a cotton-like fiber, and then rapidly cooled with cold air to obtain a composite fiber;
[0009] Step 3: Mix the composite fiber and the adhesive, suck them into the cotton collector through negative pressure for cotton collection, transfer them to the needling machine for needling treatment, and then perform high-temperature shaping and cooling to obtain a low-shrinkage ceramic fiber blanket.
[0010] Preferably, the preparation method of the Al2O3-SiC composite phase in step 1 includes the following steps: mixing polyvinyl alcohol, deionized water, tetraethyl orthosilicate, and ethanol solution uniformly to obtain a mixed solution A; mixing aluminum nitrate nonahydrate, citric acid, sucrose, and deionized water, adjusting the pH to 4-5 with ammonia water, and mixing uniformly to obtain a mixed solution B; mixing the mixed solution A and the mixed solution B, stirring uniformly, drying, and sintering to obtain the Al2O3-SiC composite phase.
[0011] Preferably, the specific preparation method of the Al2O3-SiC composite phase is as follows: polyvinyl alcohol is added to deionized water, the mass ratio of polyvinyl alcohol to deionized water is 4-6:100, the temperature is raised, and the mixture is mixed uniformly at 80°C to obtain a polyvinyl alcohol aqueous solution, and ethyl orthosilicate and ethanol solution are mixed uniformly at a mass ratio of 10-15:100, wherein the ethanol solution is composed of deionized water and anhydrous ethanol in a volume ratio of 1:1, dilute hydrochloric acid is added dropwise to adjust the pH to 2, and the mixture is stirred for 2 hours to obtain a ethyl orthosilicate solution, and polyvinyl alcohol and ethanol solution are added in a volume ratio of 1:1. The enol aqueous solution and the ethyl orthosilicate solution are mixed and stirred for 3 hours to obtain a mixed solution A. Aluminum nitrate nonahydrate, citric acid, sucrose, and deionized water in a mass ratio of 100:70-75:12-15:950-1050 are mixed, and the pH is adjusted to 4-5 with ammonia water. The mixture is stirred for 2 hours and mixed evenly to obtain a mixed solution B. The mixed solution A and the mixed solution B are mixed in a volume ratio of 1:1, stirred for 4-6 hours, dried at 60°C for 6 hours, and placed in a sintering furnace for sintering. After sintering, an Al2O3-SiC composite phase is obtained.
[0012] Preferably, during the preparation of the Al2O3-SiC composite phase, the ammonia water is 25 wt% ammonia water.
[0013] Preferably, during the preparation of the Al2O3-SiC composite phase, the sintering process is carried out in argon, and a staged sintering method is adopted. The sintering temperature of the first stage is 550-600°C, the heating rate is 3°C / min, and the sintering time is 1h. The sintering temperature of the second stage is 1600-1650°C, the heating rate is 3°C / min, and the sintering time is 2-3h.
[0014] Preferably, the preparation method of the yttrium oxide-kyanite composite powder comprises the following steps: mixing nano yttrium oxide, kyanite and anhydrous ethanol in a mass ratio of 100:60-80:450-600, ball milling, the ball milling time is 12-15h, the ball milling speed is 400-500r / min, after the ball milling is completed, ultrasonication, the ultrasonic power is 400-500W, the ultrasonic time is 40-60min, filtering, and drying at 60°C for 24h to obtain yttrium oxide-kyanite composite powder.
[0015] Preferably, in step 1, the mass ratio of the Al2O3-SiC composite phase and 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 3-4h.
[0016] Preferably, the centrifugal spinning rate during the spinning process in step 2 is 1000-1300 r / min, the roller head diameter is 254 mL, and the roller head aperture is set to 0.5-0.8 mm.
[0017] Furthermore, in the step 2, the temperature of the cold air quenching is 10-15° C., the wind speed is 12-15 m / s, and the fiber diameter is controlled to be 15-25 μm.
[0018] Preferably, the specific preparation method of the low shrinkage ceramic fiber blanket in step 3 comprises the following steps: mixing the composite fiber and the adhesive in a mass ratio of 100:1-3, sucking the composite fiber into a cotton collector by negative pressure for cotton collection, and transferring the cotton to a needle loom for needle punching at a needle frequency of 8000 needles / m 2 The needle depth is 10-12mm, 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 stages of temperature control. The heating rate of the first stage of temperature control is 1℃ / min. When the temperature reaches 600℃, it is kept warm for 1h, and then in a nitrogen atmosphere, the temperature is raised to 1000℃ at a heating rate of 3℃ / min and kept warm for 1h. The high-temperature shaping time is 1h, and rapid air cooling is performed to obtain a low-shrinkage ceramic fiber blanket.
[0019] Preferably, the binder in step three is composed of phenylboric acid modified kaolin, nano-silica sol and aluminum phosphate sol in a mass ratio of 2:1:0.5.
[0020] Preferably, the preparation method of phenylboronic acid modified kaolin in the step three comprises the following steps: ultrasonically dispersing activated kaolin in toluene, and after uniform dispersion, adding 4-carboxyphenylboronic acid pinacol ester, dicyclohexylcarbodiimide and 4-dimethylaminopyridine in a nitrogen atmosphere, wherein the mass ratio of activated kaolin, toluene, 4-carboxyphenylboronic acid pinacol ester, dicyclohexylcarbodiimide and 4-dimethylaminopyridine is 100:1500-1800:105-120:5-8:0.8-1, stirring and mixing, reacting, centrifuging after the reaction, washing with anhydrous ethanol, and vacuum drying at 60°C for 24 hours to obtain phenylboronic acid modified kaolin.
[0021] Preferably, the reaction temperature during the preparation of the phenylboric acid-modified kaolin is 70-80° C., and the reaction time is 12-15 h.
[0022] Furthermore, the preparation method of the activated kaolin is as follows: kaolin, sodium hydroxide and deionized water in a mass ratio of 8:0.5:100 are stirred and mixed, heated, and an activation reaction occurs at 85°C for 8 hours. After the reaction is completed, centrifugation is performed at a rate of 6000 r / min for 8 minutes, washed with deionized water, and vacuum dried at 80°C for 24 hours to obtain activated kaolin.
[0023] Compared with the prior art, the present invention has the following beneficial effects:
[0024] (1) In the present invention, tetraethyl orthosilicate is used as a silicon source, aluminum nitrate nonahydrate as an aluminum source, citric acid as a chelating agent, and sucrose as a carbon source. After mixed reaction and sintering, a skeleton structure of silicate and alumina is formed. Sucrose is pyrolyzed to produce carbon, and an Al2O3-SiC composite phase is obtained. The composite combines the excellent properties of alumina and silicon carbide, and 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 to form 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 evenly coated on the surface of the kyanite, thereby reducing the sintering temperature. Kyanite can play a micro-expansion role. During the combustion process of the matrix, it can reduce the shrinkage ratio of the ceramic during sintering, help 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 creep resistance and stability.
[0025] (2) In the present invention, sodium hydroxide is used to activate kaolin, and the hydroxyl groups on the activated kaolin react with the carboxyl groups on 4-carboxylphenylboronic acid pinacol ester to undergo esterification reaction, thereby obtaining phenylboric acid-modified kaolin, and introducing phenylboric acid into the kaolin. The adhesive is composed of phenylboric acid-modified kaolin, nano-silica sol, and aluminum phosphate sol. The phenylboric acid-modified kaolin further enhances the bonding properties of the kaolin, and can better penetrate and interweave with the fibers of the ceramic fiber blanket, thereby improving the overall bonding strength, helping to form a stable structural network in the ceramic fiber blanket, and improving its overall strength and stability. In addition, the phenylboric acid-modified kaolin has a high specific surface area and porosity, and can adsorb tiny particles and impurities on the surface of the ceramic fiber blanket. The boron heterocycle can form a stronger bond with the ceramic fiber, forming a stable compound, improving the mechanical properties of the matrix, and effectively preventing oxidation. The nano-silica sol can fill the gaps between the fibers, forming a silica glass phase at high temperature, and improving the density of the matrix. Aluminum phosphate sol can generate AlPO4 ceramic phase under high temperature conditions and form a three-dimensional network structure.
[0026] (3) In the present invention, composite fibers are obtained through spinning and cold air quenching. The obtained fibers are finer and more uniform, providing a good foundation for subsequent production processes. Then, cotton gathering, needle punching, and high-temperature shaping are used to tightly interweave the fiber layers, significantly improving the tensile strength of the fiber blanket to obtain a ceramic fiber blanket. The ceramic fiber blanket uses Al2O3-SiC composite phase and yttrium oxide-kyanite composite powder as the main raw materials. It can maintain dimensional stability in high temperature environments, has a low shrinkage rate, and has excellent thermal insulation performance, a low thermal conductivity coefficient, and can isolate heat transfer, achieving energy saving and consumption reduction effects, and greatly improving mechanical properties. DETAILED DESCRIPTION
[0027] The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all 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. Example 1
[0028] A method for manufacturing a low-shrinkage ceramic fiber blanket comprises the following steps:
[0029] (1) Al2O3-SiC composite phase and yttrium oxide-kyanite composite powder with a mass ratio of 100:35 were mixed evenly, passed through a 200-mesh sieve, placed in a resistance furnace, and heated and melted. The heating and melting process was carried out in an argon atmosphere at a heating and melting temperature of 1900°C and a heating and melting time of 4 hours to obtain a slurry;
[0030] (2) The slurry was centrifugally spun through a spinning machine at a centrifugal spinning rate of 1000 r / min, a roller head diameter of 254 mL, a roller head aperture of 0.5 mm, and spun into a cotton-like state. The slurry was then rapidly cooled by cold air at a temperature of 10°C and a wind speed of 12 m / s. The fiber diameter was controlled to be 15 μm to obtain a composite fiber.
[0031] (3) The composite fiber and the adhesive with a mass ratio of 100:1 were mixed, wherein the adhesive consisted of phenylboric acid modified kaolin, nano-silica sol, and aluminum phosphate sol with a mass ratio of 2:1:0.5, and the mixture was sucked into the cotton collector by negative pressure for collection, and then transferred to the needle loom for needle punching at a needle frequency of 8000 needles / m 2 The needle depth is 10mm, 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 stages of temperature control. The heating rate of the first stage is 1℃ / min. When the temperature reaches 600℃, it is kept warm for 1h. Then, in a nitrogen atmosphere, the temperature is raised to 1000℃ at a heating rate of 3℃ / min and kept warm for 1h. The high-temperature shaping time is 1h, and rapid air cooling is performed to obtain a low-shrinkage ceramic fiber blanket.
[0032] The preparation method of the Al2O3-SiC composite phase includes the following steps: adding polyvinyl alcohol to deionized water, wherein the mass ratio of polyvinyl alcohol to deionized water is 4:100, heating, and mixing uniformly at 80°C to obtain a polyvinyl alcohol aqueous solution, uniformly mixing tetraethyl orthosilicate and ethanol solution with a mass ratio of 10:100, wherein the ethanol solution is composed of deionized water and anhydrous ethanol with a volume ratio of 1:1, adding dilute hydrochloric acid dropwise to adjust the pH to 2, stirring and mixing for 2 hours to obtain a tetraethyl orthosilicate solution, mixing the polyvinyl alcohol aqueous solution and the tetraethyl orthosilicate solution with a volume ratio of 1:1, stirring for 3 hours to obtain a mixed solution A, and adding tetraethyl orthosilicate with a mass ratio of 100:70:12:950. Aluminum nitrate nonahydrate, citric acid, sucrose, and deionized water are mixed, and the pH is adjusted to 4 with ammonia water (25 wt% ammonia water). The mixture is stirred for 2 hours. After uniform mixing, a mixed solution B is obtained. The mixed solution A and the mixed solution B are mixed in a volume ratio of 1:1, stirred for 4 hours, dried at 60°C for 6 hours, and placed in a sintering furnace for sintering. The sintering process is carried out in argon gas. A staged sintering method is adopted. The sintering temperature of the first stage is 550°C, the heating rate is 3°C / min, and the sintering time is 1 hour. The sintering temperature of the second stage is 1600°C, the heating rate is 3°C / min, and the sintering time is 3 hours. After the sintering is completed, an Al2O3-SiC composite phase is obtained.
[0033] The preparation method of the yttrium oxide-kyanite composite powder includes the following steps: uniformly mixing nano-yttrium oxide, kyanite, and anhydrous ethanol in a mass ratio of 100:60:450, ball milling for 12 hours at a speed of 400 r / min, ultrasonicating after the ball milling, with an ultrasonic power of 400 W and a ultrasonic time of 40 minutes, filtering, and drying at 60° C. for 24 hours to obtain the yttrium oxide-kyanite composite powder.
[0034] The preparation method of phenylboronic acid modified kaolin includes the following steps: ultrasonically dispersing activated kaolin in toluene, and after uniform dispersion, adding 4-carboxyphenylboronic acid pinacol ester, dicyclohexylcarbodiimide and 4-dimethylaminopyridine in a nitrogen atmosphere, wherein the mass ratio of activated kaolin, toluene, 4-carboxyphenylboronic acid pinacol ester, dicyclohexylcarbodiimide and 4-dimethylaminopyridine is 100:1500:105:5:0.8, stirring and mixing, reacting, the reaction temperature is 70°C, the reaction time is 15 hours, and after the reaction is completed, centrifuging, washing with anhydrous ethanol, and vacuum drying at 60°C for 24 hours to obtain phenylboronic acid modified kaolin. Example 2
[0035] A method for manufacturing a low-shrinkage ceramic fiber blanket comprises the following steps:
[0036] (1) Al2O3-SiC composite phase and yttrium oxide-kyanite composite powder with a mass ratio of 100:40 were mixed evenly, passed through a 200-mesh sieve, placed in a resistance furnace, and heated and melted. The heating and melting process was carried out in an argon atmosphere at a heating and melting temperature of 1920°C and a heating and melting time of 3.5 hours to obtain a slurry;
[0037] (2) The slurry was centrifugally spun through a spinning machine at a centrifugal spinning rate of 1100 r / min, a roller head diameter of 254 mL, a roller head aperture of 0.6 mm, and spun into a cotton-like state. The slurry was then rapidly cooled by cold air at a temperature of 12°C and a wind speed of 14 m / s. The fiber diameter was controlled to be 18 μm to obtain a composite fiber.
[0038] (3) The composite fiber and the adhesive with a mass ratio of 100:1.5 were mixed, wherein the adhesive consisted of phenylboric acid modified kaolin, nano-silica sol, and aluminum phosphate sol with a mass ratio of 2:1:0.5, and the mixture was sucked into the cotton collector by negative pressure for collection, and then transferred to the needle loom for needle punching at a needle frequency of 8000 needles / m 2The needle depth is 11mm, 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 stages of temperature control. The heating rate of the first stage is 1℃ / min. When the temperature reaches 600℃, it is kept warm for 1h. Then, in a nitrogen atmosphere, the temperature is raised to 1000℃ at a heating rate of 3℃ / min and kept warm for 1h. The high-temperature shaping time is 1h, and rapid air cooling is performed to obtain a low-shrinkage ceramic fiber blanket.
[0039] The preparation method of the Al2O3-SiC composite phase includes the following steps: adding polyvinyl alcohol to deionized water, wherein the mass ratio of polyvinyl alcohol to deionized water is 5:100, heating, and mixing uniformly at 80°C to obtain a polyvinyl alcohol aqueous solution; uniformly mixing tetraethyl orthosilicate and ethanol solution with a mass ratio of 12:100, wherein the ethanol solution is composed of deionized water and anhydrous ethanol with a volume ratio of 1:1; adding dilute hydrochloric acid to adjust the pH to 2, stirring and mixing for 2 hours to obtain a tetraethyl orthosilicate solution; mixing the polyvinyl alcohol aqueous solution and the tetraethyl orthosilicate solution with a volume ratio of 1:1, stirring for 3 hours to obtain a mixed solution A; and adding nitric acid with a mass ratio of 100:72:14:980. Aluminum nonahydrate, citric acid, sucrose, and deionized water were mixed, and the pH was adjusted to 4.5 with ammonia water (25 wt% ammonia water). The mixture was stirred for 2 hours. After uniform mixing, a mixed solution B was obtained. The mixed solution A and the mixed solution B were mixed in a volume ratio of 1:1, stirred for 5 hours, dried at 60°C for 6 hours, and placed in a sintering furnace for sintering. The sintering process was carried out in argon gas. A staged sintering method was adopted. The sintering temperature of the first stage was 560°C, the heating rate was 3°C / min, and the sintering time was 1 hour. The sintering temperature of the second stage was 1620°C, the heating rate was 3°C / min, and the sintering time was 2.5 hours. After the sintering was completed, an Al2O3-SiC composite phase was obtained.
[0040] The preparation method of the yttrium oxide-kyanite composite powder includes the following steps: uniformly mixing nano-yttrium oxide, kyanite, and anhydrous ethanol in a mass ratio of 100:68:500, ball milling for 14 hours at a rotation speed of 450 r / min, ultrasonicating after the ball milling, with an ultrasonic power of 450 W and a ultrasonic time of 50 minutes, filtering, and drying at 60° C. for 24 hours to obtain the yttrium oxide-kyanite composite powder.
[0041] The preparation method of phenylboronic acid modified kaolin includes the following steps: ultrasonically dispersing activated kaolin in toluene, and after uniform dispersion, adding 4-carboxyphenylboronic acid pinacol ester, dicyclohexylcarbodiimide and 4-dimethylaminopyridine in a nitrogen atmosphere, wherein the mass ratio of activated kaolin, toluene, 4-carboxyphenylboronic acid pinacol ester, dicyclohexylcarbodiimide and 4-dimethylaminopyridine is 100:1600:110:6:0.9, stirring and mixing, reacting, the reaction temperature is 75°C, the reaction time is 14 hours, and after the reaction is completed, centrifuging, washing with anhydrous ethanol, and vacuum drying at 60°C for 24 hours to obtain phenylboronic acid modified kaolin. Example 3
[0042] A method for manufacturing a low-shrinkage ceramic fiber blanket comprises the following steps:
[0043] (1) Al2O3-SiC composite phase and yttrium oxide-kyanite composite powder with a mass ratio of 100:40 were mixed evenly, passed through a 200-mesh sieve, placed in a resistance furnace, and heated and melted. The heating and melting process was carried out in an argon atmosphere at a heating and melting temperature of 1920°C and a heating and melting time of 3.5 hours to obtain a slurry;
[0044] (2) The slurry was centrifugally spun through a spinning machine at a centrifugal spinning rate of 1100 r / min, a roller head diameter of 254 mL, a roller head aperture of 0.6 mm, and spun into a cotton-like state. The slurry was then rapidly cooled by cold air at a temperature of 12°C and a wind speed of 14 m / s. The fiber diameter was controlled to be 18 μm to obtain a composite fiber.
[0045] (3) The composite fiber and the adhesive with a mass ratio of 100:1.5 were mixed, wherein the adhesive consisted of phenylboric acid modified kaolin, nano-silica sol, and aluminum phosphate sol with a mass ratio of 2:1:0.5, and the mixture was sucked into the cotton collector by negative pressure for collection, and then transferred to the needle loom for needle punching at a needle frequency of 8000 needles / m 2 The needle depth is 11mm, 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 stages of temperature control. The heating rate of the first stage is 1℃ / min. When the temperature reaches 600℃, it is kept warm for 1h. Then, in a nitrogen atmosphere, the temperature is raised to 1000℃ at a heating rate of 3℃ / min and kept warm for 1h. The high-temperature shaping time is 1h, and rapid air cooling is performed to obtain a low-shrinkage ceramic fiber blanket.
[0046] The preparation method of the Al2O3-SiC composite phase includes the following steps: adding polyvinyl alcohol to deionized water, wherein the mass ratio of polyvinyl alcohol to deionized water is 5.5:100, heating, and mixing uniformly at 80°C to obtain a polyvinyl alcohol aqueous solution, uniformly mixing tetraethyl orthosilicate and ethanol solution with a mass ratio of 14:100, wherein the ethanol solution is composed of deionized water and anhydrous ethanol with a volume ratio of 1:1, adding dilute hydrochloric acid to adjust the pH to 2, stirring and mixing for 2 hours to obtain a tetraethyl orthosilicate solution, mixing the polyvinyl alcohol aqueous solution and the tetraethyl orthosilicate solution with a volume ratio of 1:1, stirring for 3 hours to obtain a mixed solution A, and adding tetraethyl orthosilicate with a mass ratio of 100:74:14:1000. Aluminum nitrate nonahydrate, citric acid, sucrose, and deionized water are mixed, and the pH is adjusted to 4.5 with ammonia water, the ammonia water is 25wt% ammonia water, and the mixture is stirred for 2 hours. After mixing evenly, a mixed solution B is obtained. The mixed solution A and the mixed solution B are mixed in a volume ratio of 1:1, stirred for 5 hours, dried at 60°C for 6 hours, and placed in a sintering furnace for sintering. The sintering process is carried out in argon gas and a staged sintering method is adopted. The sintering temperature of the first stage is 580°C, the heating rate is 3°C / min, and the sintering time is 1 hour. The sintering temperature of the second stage is 1640°C, the heating rate is 3°C / min, and the sintering time is 2.5 hours. After the sintering is completed, an Al2O3-SiC composite phase is obtained.
[0047] The preparation method of the yttrium oxide-kyanite composite powder includes the following steps: uniformly mixing nano-yttrium oxide, kyanite, and anhydrous ethanol in a mass ratio of 100:75:550, ball milling for 14 hours at a rotation speed of 480 r / min, ultrasonicating after the ball milling, with an ultrasonic power of 480 W and a ultrasonic time of 55 minutes, filtering, and drying at 60° C. for 24 hours to obtain the yttrium oxide-kyanite composite powder.
[0048] The preparation method of phenylboronic acid modified kaolin includes the following steps: ultrasonically dispersing activated kaolin in toluene, and after uniform dispersion, adding 4-carboxyphenylboronic acid pinacol ester, dicyclohexylcarbodiimide and 4-dimethylaminopyridine in a nitrogen atmosphere, wherein the mass ratio of activated kaolin, toluene, 4-carboxyphenylboronic acid pinacol ester, dicyclohexylcarbodiimide and 4-dimethylaminopyridine is 100:1700:115:7:0.9, stirring and mixing, reacting, the reaction temperature is 75°C, the reaction time is 14 hours, and after the reaction is completed, centrifuging, washing with anhydrous ethanol, and vacuum drying at 60°C for 24 hours to obtain phenylboronic acid modified kaolin. Example 4
[0049] A method for manufacturing a low-shrinkage ceramic fiber blanket comprises the following steps:
[0050] (1) Al2O3-SiC composite phase and yttrium oxide-kyanite composite powders with a mass ratio of 100:42 were mixed evenly, passed through a 200-mesh sieve, placed in a resistance furnace, and heated and melted. The heating and melting process was carried out in an argon atmosphere at a heating and melting temperature of 1940°C and a heating and melting time of 3.5 hours to obtain a slurry;
[0051] (2) The slurry was centrifugally spun through a spinning machine at a rate of 1200 r / min, a roller head diameter of 254 mL, a roller head aperture of 0.7 mm, and spun into a cotton-like state. The slurry was then rapidly cooled by cold air at a temperature of 12°C and a wind speed of 13 m / s. The fiber diameter was controlled to be 20 μm to obtain a composite fiber.
[0052] (3) The composite fiber and the adhesive with a mass ratio of 100:2 were mixed, wherein the adhesive consisted of phenylboric acid modified kaolin, nano-silica sol, and aluminum phosphate sol with a mass ratio of 2:1:0.5, and the mixture was sucked into a cotton collector by negative pressure for collection, and then transferred to a needle loom for needle punching at a needle frequency of 8000 needles / m 2 The needle depth is 11mm, 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 stages of temperature control. The heating rate of the first stage is 1℃ / min. When the temperature reaches 600℃, it is kept warm for 1h. Then, in a nitrogen atmosphere, the temperature is raised to 1000℃ at a heating rate of 3℃ / min and kept warm for 1h. The high-temperature shaping time is 1h, and rapid air cooling is performed to obtain a low-shrinkage ceramic fiber blanket.
[0053] The preparation methods of the Al2O3-SiC composite phase, yttrium oxide-kyanite composite powder, and phenylboric acid-modified kaolin are the same as those of the Al2O3-SiC composite phase, yttrium oxide-kyanite composite powder, and phenylboric acid-modified kaolin in Example 3. Example 5
[0054] A method for manufacturing a low-shrinkage ceramic fiber blanket comprises the following steps:
[0055] (1) Al2O3-SiC composite phase and yttrium oxide-kyanite composite powder with a mass ratio of 100:45 were mixed evenly, passed through a 200-mesh sieve, placed in a resistance furnace, and heated and melted. The heating and melting process was carried out in an argon atmosphere at a heating and melting temperature of 1950°C and a heating and melting time of 3 hours to obtain a slurry;
[0056] (2) The slurry was centrifugally spun through a spinning machine at a centrifugal spinning rate of 1300 r / min, a roller head diameter of 254 mL, and a roller head aperture of 0.8 mm. The slurry was spun into a cotton-like state, and then rapidly cooled by cold air at a temperature of 15°C and a wind speed of 15 m / s. The fiber diameter was controlled to be 25 μm to obtain a composite fiber.
[0057] (3) The composite fiber and the adhesive with a mass ratio of 100:3 were mixed, wherein the adhesive consisted of phenylboric acid modified kaolin, nano-silica sol, and aluminum phosphate sol with a mass ratio of 2:1:0.5, and the mixture was sucked into the cotton collector by negative pressure for collection, and then transferred to the needle loom for needle punching at a needle frequency of 8000 needles / m 2 The needle depth is 12mm, 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 stages of temperature control. The heating rate of the first stage is 1℃ / min. When the temperature reaches 600℃, it is kept warm for 1h. Then, in a nitrogen atmosphere, the temperature is raised to 1000℃ at a heating rate of 3℃ / min and kept warm for 1h. The high-temperature shaping time is 1h, and rapid air cooling is performed to obtain a low-shrinkage ceramic fiber blanket.
[0058] The preparation method of the Al2O3-SiC composite phase includes the following steps: adding polyvinyl alcohol to deionized water, wherein the mass ratio of polyvinyl alcohol to deionized water is 6:100, heating, and mixing uniformly at 80°C to obtain a polyvinyl alcohol aqueous solution; uniformly mixing tetraethyl orthosilicate and ethanol solution at a mass ratio of 15:100, wherein the ethanol solution consists of deionized water and anhydrous ethanol at a volume ratio of 1:1; adding dilute hydrochloric acid dropwise to adjust the pH to 2, stirring and mixing for 2 hours to obtain a tetraethyl orthosilicate solution; mixing the polyvinyl alcohol aqueous solution and the tetraethyl orthosilicate solution at a volume ratio of 1:1, stirring for 3 hours to obtain a mixed solution A; and mixing tetraethyl orthosilicate with a mass ratio of 100:75:15:1050. Aluminum nitrate nonahydrate, citric acid, sucrose and deionized water are mixed, and the pH is adjusted to 5 with ammonia water, the ammonia water is 25wt% ammonia water, and the mixture is stirred for 2 hours. After mixing evenly, a mixed solution B is obtained, and the mixed solution A and the mixed solution B are mixed in a volume ratio of 1:1, stirred for 6 hours, dried at 60°C for 6 hours, and placed in a sintering furnace for sintering. The sintering process is carried out in argon gas and a staged sintering method is adopted. The sintering temperature of the first stage is 600°C, the heating rate is 3°C / min, and the sintering time is 1 hour. The sintering temperature of the second stage is 1650°C, the heating rate is 3°C / min, and the sintering time is 2 hours. After the sintering is completed, an Al2O3-SiC composite phase is obtained.
[0059] The preparation method of the yttrium oxide-kyanite composite powder includes the following steps: uniformly mixing nano-yttrium oxide, kyanite, and anhydrous ethanol in a mass ratio of 100:80:600, ball milling for 15 hours at a rotation speed of 500 r / min, ultrasonicating after the ball milling, with an ultrasonic power of 500 W and a ultrasonic time of 60 minutes, filtering, and drying at 60° C. for 24 hours to obtain the yttrium oxide-kyanite composite powder.
[0060] The preparation method of phenylboronic acid modified kaolin includes the following steps: ultrasonically dispersing activated kaolin in toluene, and after uniform dispersion, adding 4-carboxyphenylboronic acid pinacol ester, dicyclohexylcarbodiimide and 4-dimethylaminopyridine in a nitrogen atmosphere, wherein the mass ratio of activated kaolin, toluene, 4-carboxyphenylboronic acid pinacol ester, dicyclohexylcarbodiimide and 4-dimethylaminopyridine is 100:1800:120:8:1, stirring and mixing, reacting, the reaction temperature is 80°C, the reaction time is 15 hours, and after the reaction is completed, centrifuging, washing with anhydrous ethanol, and vacuum drying at 60°C for 24 hours to obtain phenylboronic acid modified kaolin.
[0061] Comparative Example 1
[0062] A method for manufacturing a ceramic fiber blanket comprises the following steps:
[0063] (1) Al2O3, SiC, and yttrium oxide-kyanite composite powders with a mass ratio of 100:42 were mixed evenly, passed through a 200-mesh sieve, placed in a resistance furnace, and heated and melted. The heating and melting process was carried out in an argon atmosphere at a heating and melting temperature of 1940°C and a heating and melting time of 3.5 hours to obtain a slurry;
[0064] (2) The slurry was centrifugally spun through a spinning machine at a rate of 1200 r / min, a roller head diameter of 254 mL, a roller head aperture of 0.7 mm, and spun into a cotton-like state. The slurry was then rapidly cooled by cold air at a temperature of 12°C and a wind speed of 13 m / s. The fiber diameter was controlled to be 20 μm to obtain a composite fiber.
[0065] (3) The composite fiber and the adhesive with a mass ratio of 100:2 were mixed, wherein the adhesive consisted of phenylboric acid modified kaolin, nano-silica sol, and aluminum phosphate sol with a mass ratio of 2:1:0.5, and the mixture was sucked into a cotton collector by negative pressure for collection, and then transferred to a needle loom for needle punching at a needle frequency of 8000 needles / m 2 The needle depth is 11mm, 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 stages of temperature control. The heating rate of the first stage of temperature control is 1℃ / min. When the temperature reaches 600℃, it is kept warm for 1h, and then in a nitrogen atmosphere, the temperature is raised to 1000℃ at a heating rate of 3℃ / min and kept warm for 1h. The high-temperature shaping time is 1h, and it is rapidly cooled by air to obtain a ceramic fiber blanket.
[0066] The preparation method of the yttrium oxide-kyanite composite powder includes the following steps: uniformly mixing nano-yttrium oxide, kyanite, and anhydrous ethanol in a mass ratio of 100:75:550, ball milling for 14 hours at a rotation speed of 480 r / min, ultrasonicating after the ball milling, with an ultrasonic power of 480 W and a ultrasonic time of 55 minutes, filtering, and drying at 60° C. for 24 hours to obtain the yttrium oxide-kyanite composite powder.
[0067] The preparation method of phenylboronic acid modified kaolin includes the following steps: ultrasonically dispersing activated kaolin in toluene, and after uniform dispersion, adding 4-carboxyphenylboronic acid pinacol ester, dicyclohexylcarbodiimide and 4-dimethylaminopyridine in a nitrogen atmosphere, wherein the mass ratio of activated kaolin, toluene, 4-carboxyphenylboronic acid pinacol ester, dicyclohexylcarbodiimide and 4-dimethylaminopyridine is 100:1700:115:7:0.9, stirring and mixing, reacting, the reaction temperature is 75°C, the reaction time is 14 hours, and after the reaction is completed, centrifuging, washing with anhydrous ethanol, and vacuum drying at 60°C for 24 hours to obtain phenylboronic acid modified kaolin.
[0068] Comparative Example 2
[0069] A method for manufacturing a ceramic fiber blanket comprises the following steps:
[0070] (1) Al2O3-SiC composite phase, yttrium oxide, and kyanite with a mass ratio of 100:42 were mixed evenly, passed through a 200-mesh sieve, placed in a resistance furnace, and heated to melt. The heating and melting process was carried out in an argon atmosphere at a heating and melting temperature of 1940°C and a heating and melting time of 3.5 hours to obtain a slurry;
[0071] (2) The slurry was centrifugally spun through a spinning machine at a rate of 1200 r / min, a roller head diameter of 254 mL, a roller head aperture of 0.7 mm, and spun into a cotton-like state. The slurry was then rapidly cooled by cold air at a temperature of 12°C and a wind speed of 13 m / s. The fiber diameter was controlled to be 20 μm to obtain a composite fiber.
[0072] (3) The composite fiber and the adhesive with a mass ratio of 100:2 were mixed, wherein the adhesive consisted of phenylboric acid modified kaolin, nano-silica sol, and aluminum phosphate sol with a mass ratio of 2:1:0.5, and the mixture was sucked into a cotton collector by negative pressure for collection, and then transferred to a needle loom for needle punching at a needle frequency of 8000 needles / m 2The needle depth is 11mm, 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 stages of temperature control. The heating rate of the first stage of temperature control is 1℃ / min. When the temperature reaches 600℃, it is kept warm for 1h, and then in a nitrogen atmosphere, the temperature is raised to 1000℃ at a heating rate of 3℃ / min and kept warm for 1h. The high-temperature shaping time is 1h, and it is rapidly cooled by air to obtain a ceramic fiber blanket.
[0073] The preparation method of the Al2O3-SiC composite phase includes the following steps: adding polyvinyl alcohol to deionized water, wherein the mass ratio of polyvinyl alcohol to deionized water is 5.5:100, heating, and mixing uniformly at 80°C to obtain a polyvinyl alcohol aqueous solution, uniformly mixing tetraethyl orthosilicate and ethanol solution with a mass ratio of 14:100, wherein the ethanol solution is composed of deionized water and anhydrous ethanol with a volume ratio of 1:1, adding dilute hydrochloric acid to adjust the pH to 2, stirring and mixing for 2 hours to obtain a tetraethyl orthosilicate solution, mixing the polyvinyl alcohol aqueous solution and the tetraethyl orthosilicate solution with a volume ratio of 1:1, stirring for 3 hours to obtain a mixed solution A, and adding tetraethyl orthosilicate with a mass ratio of 100:74:14:1000. Aluminum nitrate nonahydrate, citric acid, sucrose, and deionized water are mixed, and the pH is adjusted to 4.5 with ammonia water, the ammonia water is 25wt% ammonia water, and the mixture is stirred for 2 hours. After mixing evenly, a mixed solution B is obtained. The mixed solution A and the mixed solution B are mixed in a volume ratio of 1:1, stirred for 5 hours, dried at 60°C for 6 hours, and placed in a sintering furnace for sintering. The sintering process is carried out in argon gas and a staged sintering method is adopted. The sintering temperature of the first stage is 580°C, the heating rate is 3°C / min, and the sintering time is 1 hour. The sintering temperature of the second stage is 1640°C, the heating rate is 3°C / min, and the sintering time is 2.5 hours. After the sintering is completed, an Al2O3-SiC composite phase is obtained.
[0074] The preparation method of phenylboronic acid modified kaolin includes the following steps: ultrasonically dispersing activated kaolin in toluene, and after uniform dispersion, adding 4-carboxyphenylboronic acid pinacol ester, dicyclohexylcarbodiimide and 4-dimethylaminopyridine in a nitrogen atmosphere, wherein the mass ratio of activated kaolin, toluene, 4-carboxyphenylboronic acid pinacol ester, dicyclohexylcarbodiimide and 4-dimethylaminopyridine is 100:1700:115:7:0.9, stirring and mixing, reacting, the reaction temperature is 75°C, the reaction time is 14 hours, and after the reaction is completed, centrifuging, washing with anhydrous ethanol, and vacuum drying at 60°C for 24 hours to obtain phenylboronic acid modified kaolin.
[0075] Comparative Example 3
[0076] A method for manufacturing a ceramic fiber blanket comprises the following steps:
[0077] (1) Al2O3-SiC composite phase and yttrium oxide-kyanite composite powders with a mass ratio of 100:42 were mixed evenly, passed through a 200-mesh sieve, placed in a resistance furnace, and heated and melted. The heating and melting process was carried out in an argon atmosphere at a heating and melting temperature of 1940°C and a heating and melting time of 3.5 hours to obtain a slurry;
[0078] (2) The slurry was centrifugally spun through a spinning machine at a rate of 1200 r / min, a roller head diameter of 254 mL, a roller head aperture of 0.7 mm, and spun into a cotton-like state. The slurry was then rapidly cooled by cold air at a temperature of 12°C and a wind speed of 13 m / s. The fiber diameter was controlled to be 20 μm to obtain a composite fiber.
[0079] (3) The composite fiber and the adhesive with a mass ratio of 100:2 were mixed, wherein the adhesive consisted of kaolin, nano-silica sol, and aluminum phosphate sol with a mass ratio of 2:1:0.5, and the mixture was sucked into a cotton collector by negative pressure for collection, and then transferred to a needle loom for needle punching at a needle frequency of 8000 needles / m 2 The needle depth is 11mm, 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 stages of temperature control. The heating rate of the first stage of temperature control is 1℃ / min. When the temperature reaches 600℃, it is kept warm for 1h, and then in a nitrogen atmosphere, the temperature is raised to 1000℃ at a heating rate of 3℃ / min and kept warm for 1h. The high-temperature shaping time is 1h, and it is rapidly cooled by air to obtain a ceramic fiber blanket.
[0080] The preparation method of the Al2O3-SiC composite phase includes the following steps: adding polyvinyl alcohol to deionized water, wherein the mass ratio of polyvinyl alcohol to deionized water is 5.5:100, heating, and mixing uniformly at 80°C to obtain a polyvinyl alcohol aqueous solution, uniformly mixing tetraethyl orthosilicate and ethanol solution with a mass ratio of 14:100, wherein the ethanol solution is composed of deionized water and anhydrous ethanol with a volume ratio of 1:1, adding dilute hydrochloric acid to adjust the pH to 2, stirring and mixing for 2 hours to obtain a tetraethyl orthosilicate solution, mixing the polyvinyl alcohol aqueous solution and the tetraethyl orthosilicate solution with a volume ratio of 1:1, stirring for 3 hours to obtain a mixed solution A, and adding tetraethyl orthosilicate with a mass ratio of 100:74:14:1000. Aluminum nitrate nonahydrate, citric acid, sucrose, and deionized water are mixed, and the pH is adjusted to 4.5 with ammonia water, the ammonia water is 25wt% ammonia water, and the mixture is stirred for 2 hours. After mixing evenly, a mixed solution B is obtained. The mixed solution A and the mixed solution B are mixed in a volume ratio of 1:1, stirred for 5 hours, dried at 60°C for 6 hours, and placed in a sintering furnace for sintering. The sintering process is carried out in argon gas and a staged sintering method is adopted. The sintering temperature of the first stage is 580°C, the heating rate is 3°C / min, and the sintering time is 1 hour. The sintering temperature of the second stage is 1640°C, the heating rate is 3°C / min, and the sintering time is 2.5 hours. After the sintering is completed, an Al2O3-SiC composite phase is obtained.
[0081] The preparation method of the yttrium oxide-kyanite composite powder includes the following steps: uniformly mixing nano-yttrium oxide, kyanite, and anhydrous ethanol in a mass ratio of 100:75:550, ball milling for 14 hours at a rotation speed of 480 r / min, ultrasonicating after the ball milling, with an ultrasonic power of 480 W and a ultrasonic time of 55 minutes, filtering, and drying at 60° C. for 24 hours to obtain the yttrium oxide-kyanite composite powder.
[0082] The preparation method of activated kaolin in the examples and comparative examples of the present invention is as follows: kaolin, sodium hydroxide and deionized water in a mass ratio of 8:0.5:100 are stirred and mixed, heated, and an activation reaction is carried out at 85°C for 8 hours. After the reaction is completed, centrifugation is performed at a rate of 6000 r / min for 8 minutes, washed with deionized water, and vacuum dried at 80°C for 24 hours to obtain activated kaolin.
[0083] The raw materials used in the examples and comparative examples of the present invention are all common raw materials in the industry and can be purchased through commercial channels; kaolin was purchased from Shenzhen Haiyang Powder Technology Co., Ltd.; and other reagents are all commercially available.
[0084] The performance tests of the ceramic fiber blankets prepared in Examples 1-5 and Comparative Examples 1-3 were conducted as follows:
[0085] (1) Shrinkage test: The prepared ceramic fiber blanket was used as a sample. The sample was cut into a size of 100 mm × 100 mm × 10 mm and dried in an oven at 105 °C for 2 h. After cooling to room temperature, the initial size L0 was measured. The sample was placed on a quartz pad and placed in a high-temperature box furnace for performance testing. During the test, the heating rate was 5 °C / min, and the temperature was raised to 1300 °C. The temperature was kept at this temperature for 1 h. After naturally cooling to room temperature, the size L1 of the sample after heat treatment was measured. The shrinkage rate = (L0-L1) / L0×100%. Each group was tested three times and the average value was taken.
[0086] (2) Thermal conductivity test: The thermal conductivity of the samples was tested according to the test standard YB / T 4130-2005. The average thermal conductivity at 500°C was recorded. Each group was tested three times and the average value was taken.
[0087] (3) Mechanical properties test: The sample was cut into a dumbbell shape with a cutter. The total length of the sample was 75 cm, the length of the test part was 40 mm, and the width was 10 mm. The upper and lower ends of the sample were clamped on a tensile testing machine and stretched at a tensile speed of 100 mm / min. The tensile strength and elongation at break were measured. Each sample was tested three times and the average value was taken.
[0088] The test results are shown in Table 1:
[0089] Table 1
[0090]
[0091] The test results in Table 1 show that the ceramic fiber blankets corresponding to Examples 1-5 exhibit low shrinkage, low thermal conductivity, excellent high-temperature stability, and good mechanical properties. In Comparative Example 1, Al2O3 and SiC were directly added to replace the Al2O3-SiC composite phase, significantly reducing overall performance, increasing shrinkage and thermal conductivity, and reducing mechanical properties. In Comparative Example 2, yttrium oxide and kyanite were not treated, resulting in poor overall performance. In Comparative Example 3, kaolin was not modified and was directly added to the matrix as a binder, resulting in poor dispersibility, reduced shrinkage and thermal conductivity, and reduced tensile strength.
[0092] Although the embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and variations may be made to these embodiments without departing from the principles and spirit of the present invention, and that all equivalent changes and improvements made within the scope of the present invention should still fall within the scope of the present invention.
Claims
1. A method for producing a low-shrinkage ceramic fiber blanket, characterized by: The steps include: Step 1: uniformly mix the Al2O3-SiC composite phase and the yttrium oxide-kyanite composite powder, sieve, place in a resistance furnace, heat and melt to obtain slurry; The specific preparation method of the Al2O3-SiC composite phase is as follows: adding polyvinyl alcohol to deionized water, wherein the mass ratio of polyvinyl alcohol to deionized water is 4-6:100, heating, and mixing at 80°C to obtain a polyvinyl alcohol aqueous solution, uniformly mixing tetraethyl orthosilicate and an ethanol solution at a mass ratio of 10-15:100, wherein the ethanol solution is composed of deionized water and anhydrous ethanol at a volume ratio of 1:1, dropping dilute hydrochloric acid to adjust the pH to 2, stirring and mixing for 2 hours to obtain a tetraethyl orthosilicate solution, and adding polyvinyl alcohol at a volume ratio of 1:
1. The aqueous solution and the ethyl orthosilicate solution are mixed and stirred for 3 hours to obtain a mixed solution A. Aluminum nitrate nonahydrate, citric acid, sucrose, and deionized water are mixed in a mass ratio of 100:70-75:12-15:950-1050, the pH is adjusted to 4-5 with ammonia water, and the mixture is stirred for 2 hours. After mixing evenly, a mixed solution B is obtained. The mixed solution A and the mixed solution B are mixed in a volume ratio of 1:1, stirred for 4-6 hours, dried at 60°C for 6 hours, and placed in a sintering furnace for sintering. After the sintering is completed, an Al2O3-SiC composite phase is obtained; In the step 1, 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 3-4h; Step 2: The slurry in step 1 is centrifugally spun through a spinning machine to form a cotton-like fiber, and then cooled to obtain a composite fiber; Step 3: Mix the composite fiber and the adhesive, perform cotton collection and needle punching, then perform high-temperature shaping and cooling to obtain a low-shrinkage ceramic fiber blanket.
2. The method for producing a low-shrinkage ceramic fiber blanket according to claim 1, wherein: The sintering process is carried out in argon gas and adopts a staged sintering method. The sintering temperature of the first stage is 550-600℃, the heating rate is 3℃ / min, and the sintering time is 1h. The sintering temperature of the second stage is 1600-1650℃, the heating rate is 3℃ / min, and the sintering time is 2-3h.
3. The method for manufacturing 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: uniformly mixing nano-yttrium oxide, kyanite, and anhydrous ethanol in a mass ratio of 100:60-80:450-600, ball milling for 12-15 hours at a rotation speed of 400-500 r / min, ultrasonicating after the ball milling, with an ultrasonic power of 400-500 W and an ultrasonic time of 40-60 minutes, filtering, and drying at 60° C. for 24 hours to obtain the yttrium oxide-kyanite composite powder.
4. The method for producing a low-shrinkage ceramic fiber blanket according to claim 1, wherein: In the spinning process in step 2, the speed of centrifugal spinning is 1000-1300 r / min, the diameter of the roller head is 254 mL, and the hole diameter of the roller head is set to 0.5-0.8 mm.
5. The method for manufacturing 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 step 3 comprises the following steps: mixing the composite fiber and the adhesive in a mass ratio of 100:1-3, sucking the composite fiber into a cotton collector by negative pressure for collecting the cotton, and transferring the cotton to a needle loom for needle punching at a needle frequency of 8000 needles / m 2 , the needle depth is 10-12mm, the needle density is 20 needles / cm 2 , and then high-temperature shaping is carried out. During the high-temperature shaping process, it is divided into two stages of temperature control. The heating rate of the first stage of temperature control is 1℃ / min. When the temperature reaches 600℃, it is kept warm for 1h. Then, in a nitrogen atmosphere, the temperature is raised to 1000℃ at a heating rate of 3℃ / min and kept warm for 1h. The high-temperature shaping time is 1h, and it is rapidly cooled by air to obtain a low-shrinkage ceramic fiber blanket.
6. The method for manufacturing a low-shrinkage ceramic fiber blanket according to claim 1, characterized in that: In the step 3, the adhesive is composed of phenylboric acid-modified kaolin, nano-silica sol, and aluminum phosphate sol in a mass ratio of 2:1:0.
5.
7. The method for producing a low-shrinkage ceramic fiber blanket according to claim 6, wherein: The preparation method of phenylboronic acid modified kaolin in step 3 includes the following steps: ultrasonically dispersing activated kaolin in toluene, and after uniform dispersion, adding 4-carboxyphenylboronic acid pinacol ester, dicyclohexylcarbodiimide and 4-dimethylaminopyridine in a nitrogen atmosphere, wherein the mass ratio of activated kaolin, toluene, 4-carboxyphenylboronic acid pinacol ester, dicyclohexylcarbodiimide and 4-dimethylaminopyridine is 100:1500-1800:105-120:5-8:0.8-1, stirring and mixing, reacting, centrifuging after the reaction, washing with anhydrous ethanol, and vacuum drying at 60°C for 24 hours to obtain phenylboronic acid modified kaolin.
Citation Information
Patent Citations
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CN102605553A
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CN117822201A
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JP6355790B1