WO2018188280A1 - 一种钇铝石榴石连续纤维的制备方法 - Google Patents

一种钇铝石榴石连续纤维的制备方法 Download PDF

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WO2018188280A1
WO2018188280A1 PCT/CN2017/104314 CN2017104314W WO2018188280A1 WO 2018188280 A1 WO2018188280 A1 WO 2018188280A1 CN 2017104314 W CN2017104314 W CN 2017104314W WO 2018188280 A1 WO2018188280 A1 WO 2018188280A1
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aluminum garnet
yttrium aluminum
sol
fiber
continuous fiber
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French (fr)
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陈代荣
孟强
贾玉娜
焦秀玲
朱超
柴鲁宁
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Shandong University
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Definitions

  • the invention relates to a preparation method of yttrium aluminum garnet (YAG) continuous fiber, belonging to the field of inorganic non-metal materials.
  • YAG yttrium aluminum garnet
  • Alumina fiber is a kind of high-performance inorganic ceramic fiber, and its main component is alumina, and some are also added with non-metal oxides such as silicon oxide, boron oxide, zirconium oxide and metal oxide components. According to the form, it can be divided into short fiber, continuous fiber, whisker and the like, wherein the diameter of the continuous fiber is generally about 10 ⁇ m and the length can be several kilometers.
  • Yttrium aluminum garnet continuous fiber is one of alumina fibers and is a composite oxide of Al 2 O 3 and Y 2 O 3 , which has a melting point of up to 1970 ° C and is chemically stable.
  • Yttrium aluminum garnet fiber not only has excellent properties such as high strength, high modulus and high temperature resistance, but also has excellent high temperature creep resistance, and can be widely used as an insulating refractory material and a structural reinforcing material.
  • the method for preparing yttrium aluminum garnet fiber is a melting method and a chemical method.
  • the melting method generally uses aluminum and lanthanum oxide as main raw materials, and the molten liquid is obtained by heating at a high temperature, and then the melt is spun into fibers (see: silicic acid). Salt Bulletin 2009, 28, 132); Mileiko et al. mixed the Al 2 O 3 and Y 2 O 3 melts in a stoichiometric ratio, infiltrating the melt into a molybdenum-based mold having a continuous cylindrical passage, and the melt was cooled and crystallized in the passage. The fiber is formed, and the yttrium aluminum garnet fiber is obtained by separating the fiber and the mold.
  • the fiber has a bending strength of up to 1 GPa and a creep strength of 169 MPa at 1100 ° C (see: J. Eur. Ceram. Soc. 2002). , 22, 1831); Maston et al. melted Al 2 O 3 and Y 2 O 3 in proportion, then directly drawn Al 2 O 3 /YAG eutectic fibers from special equipment (see: J.Eur.Ceram .Soc. 1999, 19, 2487).
  • the preparation of YAG fiber by melt method requires high temperature resistant equipment, and the production process is difficult and costly, which limits the development and application of YAG fiber.
  • the chemical method mainly adopts the sol-gel method, and the sol-gel method is a method for solidifying a compound containing a high chemically active component by a solution, a sol or a gel, and then heat-treating the oxide or other compound solid.
  • Towata et al. used aluminum isopropoxide and cesium isopropoxide as precursor materials, and added YAG spinning dope by adding water, hydrochloric acid, nano-alumina powder and viscosity modifier.
  • the gel fiber was sintered at high temperature to obtain yttrium aluminum garnet crystal fiber.
  • YAG/Al 2 O 3 eutectic fibers see: Composites Part A2001, 32, 1127
  • the price of metal alkoxide is relatively expensive, the cost is too high, limiting the development of YAG materials using metal alkoxide
  • Al(NO 3 ) 3 , YCl 3 or Y(NO 3 ) 3 is the main raw material
  • ammonia water is a precipitant
  • nitric acid is a peptizer
  • YAG fiber is prepared by a sol-gel method. The method adopts a blow spinning technique. Short fibers are obtained (see: Mater. Lett.
  • Shojaie-Bahaabad uses aluminum powder, aluminum chloride, hydrochloric acid and cerium oxide as raw materials to prepare YAG/Al 2 O 3 by sol-gel method.
  • the composite fiber has a grain size of 100-200 nm after heat treatment at 1400 °C.
  • CN102011215A discloses a method for preparing yttrium aluminum garnet continuous fiber by sol-gel method, which uses inorganic aluminum salt, metal aluminum, cerium oxide and acetic acid as raw materials, and adds a certain amount of spinning aid, and after concentrated spinning, A yttrium aluminum garnet-based fiber strand is obtained, and the gel fiber is dried and sintered to obtain a yttrium aluminum garnet-based continuous fiber.
  • this method does not discuss the fiber length, and it takes too much time in the preparation process of the spinning dope, and if industrial production is performed, the production efficiency is low.
  • the present invention provides a method for preparing a yttrium aluminum garnet continuous fiber which is simple and controllable in operation, short in production cycle, low in cost, and easy to realize industrialization.
  • the invention uses an alumina sol containing Al 13 colloidal particles, a ⁇ -AlOOH (hydrated alumina) nano dispersion liquid and a cerium oxide sol as raw materials, and adds glacial acetic acid and dilute nitric acid in proportion, and is spun with polyvinylpyrrolidone (PVP).
  • Silk auxiliaries, yttrium aluminum garnet gel fibers are obtained by sol-gel combined with dry spinning, and calcined to form YAG continuous fibers.
  • a method for preparing yttrium aluminum garnet continuous fiber comprises the following steps:
  • the alumina sol containing Al 13 colloidal particles and the ⁇ -AlOOH nanodispersion liquid are mixed and added to the cerium oxide sol, stirred in a water bath at 30-40 ° C, glacial acetic acid is added during the stirring, and then the pH is adjusted to 1-3 by adding dilute nitric acid.
  • the alumina sol containing Al 13 colloidal particles has an alumina content of 15 to 35 wt%, the cerium oxide sol has a solid content of 10 to 30 wt%, and the ⁇ -AlOOH nanodispersion has a solid content of 8.5 to 15 wt%, and cerium oxide.
  • the molar ratio to glacial acetic acid is 1: (1-2), the amount of PVP added is 0.5-5 wt% of the total solid content; the main component of the alumina sol and ⁇ -AlOOH nanodispersion containing Al 13 colloidal particles is alumina.
  • the molar ratio of cerium oxide to aluminum oxide is 1: (1-2);
  • the precursor spinnable sol prepared in the step (1) is dry-spun to obtain YAG gel fiber, and the dry spinning process conditions are as follows: the number of holes of the spinneret is 15-800, and the diameter of the spinneret is 0.06- 0.15mm, the wire take-up speed is 60-180m/min, the air temperature is 18-40°C, and the air humidity is 20-70%;
  • the YAG gel fiber obtained in the step (2) is ceramized, heated to 450-600 ° C at a rate of 0.5-3 ° C / min, kept at this temperature for 0.5-2 h, and then heated at a rate of 3-10 ° C / min. To 900-1400 ° C, at this temperature for 0.5-2 h, the yttrium aluminum garnet continuous fiber is obtained.
  • the step (1) contains colloidal alumina sol of 13 Al of Al content of 13 mass rubber is 20-25wt%, a solids content of ⁇ -AlOOH nano dispersion is 10-15wt%, The cerium oxide sol solid content is 15% by weight, and the spinning aid PVP is added in an amount of 1% by weight of the total solid content;
  • the mass ratio of the alumina content in the alumina sol and the ⁇ -AlOOH nanodispersion containing the Al 13 colloidal particles is (3-9):1.
  • the aging temperature in the step (1) is 35 to 50 ° C, and the aging is performed at a viscosity of 450 to 550 Pa ⁇ s.
  • the aging process in the step (1) is carried out under the condition that the degree of vacuum is 0.095 MPa.
  • the molar ratio of cerium oxide to glacial acetic acid in the step (1) is 1: (1.1 - 1.5).
  • dilute nitric acid it is preferred to add dilute nitric acid to adjust the pH to 1.5-2.5.
  • the alumina sol containing Al 13 colloidal particles described in the step (1) is prepared as follows:
  • the aluminum powder and the aluminum salt solution are used as raw materials, and the molar ratio of the aluminum salt to the aluminum powder is 1: (1-5), and the reaction is heated and refluxed until the aluminum powder is completely reacted, cooled, and filtered to obtain an alumina containing Al 13 colloidal particles.
  • the aluminum salt is aluminum chloride, aluminum nitrate or aluminum sulfate.
  • the spinneret has a pore size of 0.06-0.10 mm and a take-up speed of 80-140 m/min in the step (2).
  • the air temperature in the step (2) is 25 to 35 ° C, and the air humidity is 30 to 45%.
  • the YAG gel fiber in step (3) is heated to a temperature of 450-600 ° C at a rate of 0.8-1 ° C / min, at this temperature for 1-2 h; and then at a rate of 3-5 ° C / min Warm up to 900-1400 ° C, and keep at this temperature for 1-2 h.
  • the yttrium aluminum garnet continuous fiber prepared by the method of the invention belongs to a cubic crystal system and has a garnet crystal structure; the fiber diameter is 6-12 ⁇ m, no slag ball, the fiber length can reach several kilometers; the fiber surface is smooth and the internal structure is dense, Very flexible, high strength.
  • the preparation process of the spinnable precursor sol of the invention is a mixture of several metal inorganic salt sols, which can well control the uniformity of the precursor sol, and the reaction raw materials can easily obtain linear particles by hydrolysis and polycondensation, thereby facilitating less branching.
  • the production of high poly chain colloidal particles; the addition of glacial acetic acid to the precursor sol is beneficial to improve the spinning performance of the sol. This may be due to the fact that the acetate ion produced by the hydrolysis of acetic acid combines with the metal ion to form a complex, thereby forming a chain or network structure between the molecules, which is favorable for the spinning performance of the sol.
  • the invention adopts the dry spinning technology to prepare YAG continuous fiber, wherein the spinneret has a hole number of 15-800 and a pore diameter of 0.06-0.15 mm, which is made of special alloy steel.
  • the spinning dope is extruded from the orifice of the spinneret into the spinning tunnel to exchange heat with the flow of hot air flowing into the ramp, and the solvent in the trickle stream is rapidly volatilized and carried away by the hot air stream.
  • the fine stream of the raw liquid is solidified, and is elongated and thinned by the winding force of the wire take-up machine to form nascent fibers, which are wound around the take-up rolls.
  • the spinning speed depends mainly on the nature of the sol and the rate of volatilization of the solvent. This method makes it easier to produce continuous fibers than other methods.
  • the yttrium aluminum garnet continuous fiber prepared by the invention has uniform diameter, no slag ball, fiber length of several kilometers, smooth fiber surface and tight internal structure, is not easy to break, and has good flexibility.
  • the fiber has good thermal stability and stable mechanical properties.
  • the tensile strength of the fiber monofilament after heat treatment of 1200 can reach 1GPa on average, and has good resistance to high temperature creep.
  • the preparation process of the precursor of the invention is simple in operation, can greatly reduce the preparation time of the spinnable precursor sol, has a short production cycle, and is easy to realize industrialization.
  • the YAG continuous fiber is prepared by the sol-gel method, and the prepared precursor sol is stable in nature and can be stored for a long time.
  • the aging process of the invention is carried out under the condition of a vacuum degree of 0.095 MPa, which greatly reduces the sol aging time and can be industrially produced.
  • the invention adopts dry spinning, the spinning speed is high and the structure of the obtained fiber is relatively dense, and the continuous fiber is more easily produced compared with other methods, and the YAG continuous fiber obtained by the invention can be several kilometers in length.
  • the fiber is wound around a take-up roll using a wire take-up device.
  • Fig. 1 is an XRD chart of YAG continuous fibers obtained by sintering at different temperatures in Example 1 of the present invention.
  • Figure 2 is an optical photograph of a YAG continuous gel fiber obtained in Example 1 of the present invention.
  • Figure 3 is a SEM photograph of a YAG continuous fiber obtained in Example 1 of the present invention.
  • Figure 4 is a SEM photograph of a high magnification of YAG continuous fiber obtained in Example 1 of the present invention.
  • Fig. 5 is a SEM photograph showing a high magnification of a cross section of a YAG continuous fiber obtained in Example 1 of the present invention.
  • the alumina sol containing Al 13 colloidal particles described in the examples was prepared as follows:
  • the aluminum powder and the aluminum salt solution are used as raw materials, and the molar ratio of the aluminum salt to the aluminum powder is 1: (1-5), and the reaction is heated and refluxed until the aluminum powder is completely reacted, cooled, and filtered to obtain an alumina containing Al 13 colloidal particles.
  • the sol, the Al 13 colloidal particles have a mass content of 20-25% by weight, the colloidal particle diameter is ⁇ 5 nm, and the aluminum salt is aluminum chloride, aluminum nitrate or aluminum sulfate.
  • a method for preparing yttrium aluminum garnet continuous fiber comprises the following steps:
  • the aging temperature was set to 40 ° C, the aging process was carried out under the condition of a vacuum degree of 0.095 MPa, and the mixed sol was aged to a viscosity of 500 Pa ⁇ s to obtain a precursor spinnable sol.
  • the precursor sol prepared in the step (1) is dry-spun to obtain a YAG gel fiber.
  • the process conditions are as follows: the spinneret has a pore diameter of 0.06 mm, the wire take-up speed is 100 m/min, and the air temperature is 25-30 ° C, air. The humidity is 30-40%, as shown in Figure 2, the fiber length can reach several kilometers.
  • the YAG gel fiber prepared in the step (2) is ceramized, and the process conditions are as follows: the temperature is raised to 500 ° C at a rate of 1 ° C / min, the temperature is kept at this temperature for 1 h, and then the temperature is raised to 1200 ° C at a rate of 5 ° C / min. The temperature was kept for 2 hours to obtain YAG continuous fibers.
  • the obtained yttrium aluminum garnet continuous fiber has a diameter of 7.7-8.5 ⁇ m and a fiber shrinkage of about 30%.
  • the fiber surface is smooth and the internal structure is dense.
  • the XRD test fiber phase is a yttrium aluminum garnet crystal phase, and the fiber monofilament tensile strength is average. It is 932 MPa.
  • the final sintering temperature is selected as 700 ° C, 800 ° C, 900 ° C, 1000 ° C, and the XRD spectrum of the obtained yttrium aluminum garnet continuous fiber is shown in FIG. 1 .
  • the YAG fiber obtained at a sintering temperature of 800 ° C starts pomegranate, and when the sintering temperature is 1000 ° C, it is completely converted into yttrium aluminum garnet. Crystal phase.
  • the SEM photograph of the yttrium aluminum garnet continuous fiber obtained in this example is shown in Fig. 3.
  • the high-magnification SEM photograph is shown in Fig. 4, and the SEM photograph of the fiber cross-section magnification is shown in Fig. 5. It can be seen from Figures 3, 4 and 5 that the fiber has a uniform diameter, no slag ball and a smooth surface; the internal structure of the fiber is tight, and the number of pores between the grains is small, which is favorable for the mechanical strength of the fiber.
  • a method for preparing yttrium aluminum garnet continuous fiber comprises the following steps:
  • n(Al 2 O 3 ):n(Y 2 O 3 ) 5:3, 1156.5 g of an alumina sol containing Al 13 colloidal particles (solid content: 22.04% by weight) and 2258.1 g of cerium oxide sol ( The solid content is 15wt%) mixed, stirred in a 35°C water bath, and 450g of glacial acetic acid is added during the stirring process, wherein the molar ratio of cerium oxide to glacial acetic acid is 1:1.25, then 138g of dilute nitric acid is added to adjust the pH to 2.0, and 98.9g PVP is added. The solution was stirred and mixed well.
  • the aging temperature was set to 40 ° C, the aging process was carried out under the condition of a vacuum degree of 0.095 MPa, and the mixed sol was aged to a viscosity of 513 Pa ⁇ s to obtain a precursor spinnable sol.
  • the precursor sol prepared in the step (1) is dry-spun to obtain a YAG gel fiber.
  • the process conditions are as follows: the spinneret has a pore diameter of 0.06 mm, the wire take-up speed is 80 m/min, and the air temperature is 25-30 ° C, air. The humidity is 30-40%.
  • Step (3) is the same as in Embodiment 1.
  • the obtained yttrium aluminum garnet continuous fiber has a diameter of 9.5-10.2 ⁇ m.
  • the gel fiber is easy to break and the diameter is coarse during the spinning process, and the fiber shrinkage rate is about 33%; the fiber surface has slag balls and the internal structure is not dense, XRD test fiber
  • the crystal phase is a yttrium aluminum garnet crystal phase, and the tensile strength of the fiber monofilament is 494 MPa on average. It can be seen that the alumina sol containing Al 13 colloidal particles alone is used as the alumina source, which seriously affects the tensile strength of the monofilament of the yttrium aluminum garnet continuous fiber.
  • a method for preparing yttrium aluminum garnet continuous fiber comprises the following steps:
  • the aging temperature is set to 40 ° C
  • the aging process is carried out under the condition of a vacuum degree of 0.095 MPa
  • the aging process is carried out under the condition of a vacuum degree of 0.095 MPa
  • the mixed sol is aged to a viscosity of 496 Pa ⁇ s to obtain a precursor spinnable sol. .
  • Step (2) is the same as in Embodiment 1.
  • Step (3) is the same as in Embodiment 1.
  • the obtained yttrium aluminum garnet continuous fiber has a diameter of 7.8-9.0 ⁇ m; the fiber shrinkage rate is about 32%, the fiber surface is smooth, but the number of pores between the grains is large, and the XRD test fiber phase is a yttrium aluminum garnet crystal phase, and the fiber single
  • the tensile strength of the yarn was 583 MPa on average.
  • a method for preparing yttrium aluminum garnet continuous fiber comprises the following steps:
  • the aging temperature was set to 40 ° C, the aging process was carried out under the condition of a vacuum degree of 0.095 MPa, and the mixed sol was aged to a viscosity of 520 Pa ⁇ s to obtain a precursor spinnable sol.
  • Step (2) is the same as in Embodiment 1.
  • Step (3) is the same as in Embodiment 1.
  • the obtained yttrium aluminum garnet continuous fiber has a diameter of 7.8-9.0 ⁇ m; the fiber shrinkage rate is about 32%, the fiber surface is smooth, the internal structure is dense, and the XRD test fiber phase is a yttrium aluminum garnet crystal phase, and the fiber monofilament tensile strength is average It is 913 MPa.
  • a method for preparing yttrium aluminum garnet continuous fiber comprises the following steps:
  • the aging temperature was set to 40 ° C, the aging process was carried out under the condition of a vacuum degree of 0.095 MPa, and the mixed sol was aged to a viscosity of 515 Pa ⁇ s to obtain a precursor spinnable sol.
  • the precursor sol prepared in the step (1) is dry-spun to obtain a YAG gel fiber.
  • the process conditions are as follows: the spinneret has a pore diameter of 0.06 mm, the wire take-up speed is 80 m/min, and the air temperature is 25-30 ° C, air. The humidity is 30-40%, as shown in Figure 2, the fiber length can reach several kilometers.
  • Step (3) is the same as in Embodiment 1.
  • the obtained yttrium aluminum garnet continuous fiber has a diameter of 8.5-9.5 ⁇ m, and the gel fiber is easy to break and has a relatively large diameter during spinning; the fiber shrinkage rate is about 34%, the fiber surface is smooth, and the number of pores between the grains is large, XRD
  • the fiber phase of the test fiber was a yttrium aluminum garnet crystal phase, and the tensile strength of the fiber monofilament was 700 MPa on average.
  • a method for preparing yttrium aluminum garnet continuous fiber comprises the following steps:
  • Step (1) is the same as in Example 1.
  • the precursor sol prepared in the step (1) is dry-spun to obtain a YAG gel fiber.
  • the process conditions are as follows: the spinneret has a pore diameter of 0.1 mm, the wire take-up speed is 120 m/min, and the air temperature is 30-35 ° C, air. The humidity is 30-40%.
  • the YAG gel fiber prepared in the step (2) is ceramized, and the process conditions are as follows: the temperature is raised to 500 ° C at a rate of 0.8 ° C / min, the temperature is kept at this temperature for 1 h, and then the temperature is raised to 1200 ° C at a rate of 4 ° C / min. The temperature was kept for 2 hours to obtain YAG continuous fibers.
  • the obtained yttrium aluminum garnet continuous fiber has a diameter of 8.5-9.8 ⁇ m and a fiber shrinkage of about 30%.
  • the fiber surface is smooth and the internal structure is dense.
  • the XRD test fiber phase is a yttrium aluminum garnet crystal phase, and the fiber monofilament tensile strength is average. It is 826 MPa.
  • a method for preparing yttrium aluminum garnet continuous fiber comprises the following steps:
  • the aging temperature was set to 40 ° C, the aging process was carried out under the condition of a vacuum degree of 0.095 MPa, and the spinning solution was aged to a viscosity of 485 Pa ⁇ s to obtain a precursor spinnable sol.
  • Step (2) is the same as in Embodiment 1.
  • Step (3) is the same as in Embodiment 1.
  • the obtained yttrium aluminum garnet continuous fiber has a diameter of 7.1-8.5 ⁇ m and a fiber shrinkage of about 30%.
  • the fiber surface is smooth and the internal structure is dense.
  • the XRD test fiber phase is a yttrium aluminum garnet crystal phase, and the tensile strength of the fiber monofilament is on average. 809 MPa.
  • a method for preparing yttrium aluminum garnet continuous fiber comprises the following steps:
  • the aging temperature was set to 40 ° C, the aging process was carried out under the condition of a vacuum degree of 0.095 MPa, and the spinning solution was aged to a viscosity of 500 Pa ⁇ s to obtain a precursor spinnable sol.
  • Step (2) is the same as in Embodiment 1.
  • Step (3) is the same as in Embodiment 1.
  • the obtained yttrium aluminum garnet continuous fiber has a diameter of 6.7-8.5 ⁇ m and a fiber shrinkage of about 29%.
  • the fiber surface is smooth and the internal structure is dense.
  • the main crystal phase of the XRD test fiber is a yttrium aluminum garnet crystal phase, and the fiber monofilament tensile strength is obtained.
  • the average is 950 MPa.
  • a method for preparing yttrium aluminum garnet continuous fiber comprises the following steps:
  • the aging temperature was set to 40 ° C, the aging process was carried out under the condition of a vacuum degree of 0.095 MPa, and the spinning solution was aged to a viscosity of 515 Pa ⁇ s to obtain a precursor spinnable sol.
  • the precursor sol prepared in the step (1) is dry-spun to obtain a YAG gel fiber.
  • the process conditions are as follows: the spinneret has a pore diameter of 0.06 mm, the wire take-up speed is 100 m/min, and the air temperature is 25-30 ° C, air. The humidity is 25-35%.
  • the YAG gel fiber prepared in the step (2) is ceramized, and the process conditions are as follows: the temperature is raised to 450 ° C at a rate of 1 ° C / min, the temperature is kept at this temperature for 1 h, and then the temperature is raised to 1200 ° C at a rate of 5 ° C / min. The temperature was kept for 2 hours to obtain YAG continuous fibers.
  • the obtained yttrium aluminum garnet continuous fiber has a diameter of about 7.5-8.4 ⁇ m, a fiber shrinkage rate of about 33%, a smooth fiber surface, and a dense internal structure.
  • the main crystal phase of the XRD test fiber is a yttrium aluminum garnet crystal phase, and the fiber monofilament is stretched.
  • the average strength is 1077 MPa.

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Abstract

一种钇铝石榴石连续纤维的制备方法，该方法利用含Al 13胶粒的氧化铝溶胶、γ-AlOOH纳米分散液、氧化钇溶胶、冰醋酸和聚乙烯吡咯烷酮制备可纺性前驱体溶胶，采用干法纺丝技术制备凝胶连续纤维，再经过热处理得到钇铝石榴石连续纤维。

Description

一种钇铝石榴石连续纤维的制备方法 技术领域
本发明涉及一种钇铝石榴石(YAG)连续纤维的制备方法，属于无机非金属材料领域。
背景技术
氧化铝纤维是高性能无机陶瓷纤维的一种，其主要成分为氧化铝，有的还添加有氧化硅、氧化硼、氧化锆等非金属氧化物和金属氧化物组分。按形态可分为短纤维、连续纤维、晶须等不同类型，其中连续纤维的直径一般在10μm左右，长度可达几千米。钇铝石榴石连续纤维属于氧化铝纤维中的一种，是Al2O3和Y2O3的复合氧化物，其熔点高达1970℃，化学性质稳定。钇铝石榴石纤维不仅具有高强度、高模量、耐高温等优良性能，还具有优异的抗高温蠕变性能，可广泛用作绝热耐火材料和结构增强材料。
目前制备钇铝石榴石纤维的方法有熔融法和化学法，熔融法一般采用铝和钇的氧化物为主要原料，通过高温加热获取熔融液，再将熔融液纺丝成纤(参见：硅酸盐通报2009,28,132)；Mileiko等按化学计量比混合Al2O3和Y2O3熔融液，将熔融液浸润到具有连续圆柱状通道的钼基模具中，熔融液在通道内冷却结晶后形成纤维，将纤维和模具分离后即可获得钇铝石榴石纤维，该纤维的弯曲强度最高可达1GPa，在1100℃下抗蠕变强度为169MPa(参见：J.Eur.Ceram.Soc.2002,22,1831)；Maston等按比例混合Al2O3和Y2O3后熔融，然后从特制的设备中直接拉制出Al2O3/YAG共晶纤维(参见：J.Eur.Ceram.Soc.1999,19,2487)。然而，由于YAG熔点较高，采用熔融法制备YAG纤维需要耐高温设备，且生产工艺难度大，成本高，这限制了YAG纤维的发展和应用。
化学法主要是采用溶胶-凝胶法，溶胶-凝胶法就是将含高化学活性组分的化合物经过溶液、溶胶、凝胶而固化，再经热处理而成的氧化物或其它化合物固体的方法。Towata等以异丙醇铝和异丙醇钇为前驱体原料，辅助加入水、盐酸、纳米氧化铝粉、粘度调节剂合成了YAG纺丝原液，凝胶纤维高温烧结获得钇铝石榴石晶体纤维和YAG/Al2O3共晶纤维(参见：Composites Part A2001,32,1127)，由于金属醇盐的价格比较昂贵，成本太高，限制了利用金属醇盐制备YAG材料的发展；Pullar等采用Al(NO3)3、YCl3或Y(NO3)3为主要原料，氨水为沉淀剂，硝酸为胶溶剂，通过溶胶-凝胶法制备出YAG纤维，该方法采用喷吹纺丝技术，得到的是短纤维(参见：Mater.Lett.1999,39,173)；Shojaie-Bahaabad等采用铝粉、氯化铝、盐酸和氧化钇为原料，通过溶胶-凝胶法制备了YAG/Al2O3复合纤维，经1400℃热处理后纤维的晶粒尺 寸在100-200nm，该方法只对前驱体凝胶的流变性能和纺丝性能进行了详细的分析，但没有探讨纤维的强度等其它性能(参见：Ceram.Int.2007,7,32)；US005217933A公开了一种钇铝石榴石纤维的制备方法，采用氯化铝、铝粉、甲酸、乙酸、乳酸，硝酸等原料，按氧化钇和与氧化铝不同的摩尔比例制备出钇铝石榴石陶瓷纤维，该方法加入了大量有机酸，导致溶胶合成反应较为复杂。
李呈顺等以廉价的铝粉、工业盐酸和醋酸钇为主要原料，制备了高性能的多晶钇铝石榴石纤维，纤维经热处理到900℃时可获得纯相的钇铝石榴石晶体。经1550℃热处理后，所得到的多晶钇铝石榴石纤维的平均粒径约200nm，拉伸强度为485MPa(参见：硅酸盐学报2009,37,1165)；CN105002601A公开了一种多晶Al2O3-YAG复相纤维或纯YAG纤维的制备方法，采用氯化铝、铝微粉、硝酸钇、醋酸钇、醋酸为原料制备前驱体溶胶，经离心纺丝后制得钇铝石榴石凝胶纤维，干燥、热处理后得到多晶Al2O3-YAG复相纤维或纯YAG纤维，但是，上述文献描述的纤维是采用离心甩丝技术制得的短纤维，不可进行2维或3维编织。CN102011215A公开了一种溶胶-凝胶法制备钇铝石榴石连续纤维的方法，采用无机铝盐、金属铝、氧化钇、醋酸为原料，加入一定量的纺丝助剂，浓缩纺丝后即可得到钇铝石榴石基纤维原丝，将凝胶纤维干燥、烧结后得到钇铝石榴石基连续纤维。但是，此方法没有对纤维长度进行探讨，且在纺丝原液制备过程中耗时太大，若进行工业化生产，则生产效率较低。
发明内容
针对现有技术的不足，本发明提供了一种操作工艺简单可控，生产周期短，成本低，易于实现工业化的钇铝石榴石连续纤维的制备方法。
本发明以含有Al13胶粒的氧化铝溶胶、γ-AlOOH(水合氧化铝)纳米分散液和氧化钇溶胶为原料，按比例加入冰醋酸和稀硝酸，并以聚乙烯吡咯烷酮(PVP)做纺丝助剂，通过溶胶-凝胶结合干法纺丝制得钇铝石榴石凝胶纤维，经煅烧后形成YAG连续纤维。
本发明的技术方案如下：
一种钇铝石榴石连续纤维的制备方法，包括步骤如下：
(1)可纺性前驱体溶胶的制备
将含有Al13胶粒的氧化铝溶胶和γ-AlOOH纳米分散液混合并加入氧化钇溶胶，30-40℃水浴搅拌，搅拌过程中加入冰醋酸，然后加入稀硝酸调节pH值至1-3，加入纺丝助剂PVP，搅拌混合均匀，设定老化温度为25-80℃，将纺丝液老化至黏度为400-600Pa·s，得到前驱体可纺性溶胶；
所述含有Al13胶粒的氧化铝溶胶中氧化铝含量为15-35wt％，氧化钇溶胶的固含量为 10-30wt％，γ-AlOOH纳米分散液的固含量为8.5-15wt％，氧化钇与冰醋酸的摩尔比为1:(1-2)，PVP加入量为总固含量的0.5-5wt％；含有Al13胶粒的氧化铝溶胶和γ-AlOOH纳米分散液的主要成分以氧化铝计，氧化钇和氧化铝的摩尔比为1:(1-2)；
(2)干法纺丝制备YAG凝胶纤维
将步骤(1)制备的前驱体可纺性溶胶进行干法纺丝，得到YAG凝胶纤维，干法纺丝工艺条件：喷丝板孔数为15-800个，喷丝板孔径为0.06-0.15mm，收丝速度为60-180m/min，空气温度为18-40℃，空气湿度为20-70％；
(3)YAG凝胶纤维陶瓷化
将步骤(2)制得的YAG凝胶纤维陶瓷化，以0.5-3℃/min的速度升温至450-600℃，在此温度保温0.5-2h，再以3-10℃/min的速度升温至900-1400℃，在此温度保温0.5-2h，即得钇铝石榴石连续纤维。
根据本发明，优选的，步骤(1)中含有Al13胶粒的氧化铝溶胶中Al13胶粒的质量含量为20-25wt％，γ-AlOOH纳米分散液的固含量为10-15wt％，氧化钇溶胶固含量为15wt％，纺丝助剂PVP的加入量为总固含量的1wt％；
根据本发明，优选的，含有Al13胶粒的氧化铝溶胶和γ-AlOOH纳米分散液中氧化铝含量的质量比为(3-9)：1。
根据本发明，优选的，步骤(1)中老化温度为35-50℃，老化至黏度为450-550Pa·s。
根据本发明，优选的，步骤(1)中老化过程在真空度为0.095MPa条件下进行。
根据本发明，优选的，步骤(1)中氧化钇与冰醋酸的摩尔比为1:(1.1-1.5)。
根据本发明，优选的，加入稀硝酸调节pH值至1.5-2.5。
根据本发明，优选的，步骤(1)中所述的含Al13胶粒的氧化铝溶胶按以下方法制备：
以铝粉和铝盐溶液为原料，铝盐和铝粉的摩尔比为1:(1-5)，加热回流反应至铝粉完全反应，冷却、过滤，即得到含Al13胶粒的氧化铝溶胶，胶粒粒径≤5nm。优选的，所述的铝盐为氯化铝、硝酸铝或硫酸铝。
根据本发明，优选的，步骤(2)中喷丝板孔径为0.06-0.10mm，收丝速度为80-140m/min。
根据本发明，优选的，步骤(2)中空气温度为25-35℃，空气湿度为30-45％。
根据本发明，优选的，步骤(3)中YAG凝胶纤维以0.8-1℃/min的速度升温至450-600℃，在此温度保温1-2h；再以3-5℃/min的速度升温至900-1400℃，在此温度保温1-2h。
本发明方法制备的钇铝石榴石连续纤维属于立方晶系，具有石榴石晶体结构；纤维直径为6-12μm，无渣球，纤维长度可达数千米；纤维表面光滑且内部结构致密，有很好的柔韧性， 强度高。
本发明的原理：
本发明可纺性前驱体溶胶制备过程是几种金属无机盐溶胶的混合，可以很好的控制前驱体溶胶的均匀性，且反应原料通过水解、缩聚容易得到线性粒子，从而有利于少支链高聚链状胶粒的产生；前驱体溶胶中加入冰醋酸，有利于提高溶胶的纺丝性能。这可能是由于：醋酸水解产生的醋酸根离子与金属离子结合，形成络合物，从而分子之间形成链状或网状结构，有利于溶胶的纺丝性能。
本发明采用干法纺丝技术制备YAG连续纤维，其中喷丝板孔数在15-800之间，孔径为0.06-0.15mm，由特种合金钢制成。纺丝原液从喷丝板孔眼中被压出进入纺丝甬道，与通入甬道中的热空气流进行换热，原液细流中的溶剂快速挥发并被热空气流带走。在逐步脱去溶剂的同时，原液细流发生固化，并在收丝机卷绕拉力的作用下伸长变细而形成初生纤维，缠绕于收丝辊上。纺丝速度主要取决于溶胶的性质和溶剂的挥发速度。与其它方法相比，此方法更易制得连续纤维。
本发明的技术特点及优良效果如下：
1)本发明制备的钇铝石榴石连续纤维直径均匀，无渣球，纤维长度可达数千米，纤维表面光滑且内部结构紧密，不易断裂，有很好的柔韧性。此外，纤维的热稳定性好，力学性质稳定，经1200热处理后的纤维单丝拉伸强度平均可达1GPa，具有良好的抗高温蠕变性。
2)本发明前驱体制备过程操作简单，可大大减少可纺性前驱体溶胶的制备时间，生产周期短，易于实现工业化。
3)本发明采用溶胶-凝胶方法制备YAG连续纤维，所制备的前驱体溶胶性质稳定，可长时间存放。
4)本发明老化过程在真空度0.095MPa条件下进行，大大减少了溶胶老化时间，可进行工业化生产。
5)本发明采用干法纺丝，纺丝速度较高且所得纤维的结构较致密，与其它方法比较更易制得连续纤维，本发明所制得的YAG连续纤维长度可达数千米，可利用收丝设备将纤维缠绕于收丝辊上。
附图说明：
图1是本发明实施例1不同温度烧结所得YAG连续纤维的XRD谱图。
图2是本发明实施例1所得的YAG连续凝胶纤维的光学照片。
图3是本发明实施例1所得YAG连续纤维的SEM照片。
图4是本发明实施例1所得YAG连续纤维高倍放大的SEM照片。
图5是本发明实施例1所得YAG连续纤维截面高倍放大的SEM照片。
具体实施方式：
下面结合实施例对本发明做进一步说明，但不限于此。
实施例中所述的含Al13胶粒的氧化铝溶胶按以下方法制备得到：
以铝粉和铝盐溶液为原料，铝盐和铝粉的摩尔比为1:(1-5)，加热回流反应至铝粉完全反应，冷却、过滤，即得到含Al13胶粒的氧化铝溶胶，Al13胶粒的质量含量为20-25wt％，胶粒粒径≤5nm，所述的铝盐为氯化铝、硝酸铝、硫酸铝。
实施例1
一种钇铝石榴石连续纤维的制备方法，包括步骤如下：
(1)可纺性前驱体溶胶的制备
将925.2g含有Al13胶粒的氧化铝溶胶(固含量为22.04wt％)和419.6gγ-AlOOH纳米分散液(固含量为12.15wt％)混合，利用分散机搅拌至均匀，按n(Al2O3):n(Y2O3)＝5:3的计量组成加入2258.1g氧化钇溶胶(固含量为15wt％)，35℃水浴搅拌，搅拌过程中加入450g冰醋酸，其中氧化钇与冰醋酸的摩尔比为1:1.25，然后加入173g稀硝酸调节pH值至2.0，加入39.6g PVP溶液，搅拌混合均匀。
设定老化温度为40℃，老化过程在真空度为0.095MPa条件下进行，将混合溶胶老化至黏度为500Pa·s，得到前驱体可纺性溶胶。
(2)干法纺丝制备凝胶纤维
将步骤(1)制备的前驱体溶胶进行干法纺丝，得到YAG凝胶纤维，工艺条件：喷丝板孔径为0.06mm，收丝速度为100m/min，空气温度为25-30℃，空气湿度为30-40％，如图2所示，纤维长度可达数千米。
(3)YAG凝胶纤维陶瓷化
将步骤(2)制备的YAG凝胶纤维陶瓷化，工艺条件：以1℃/min的速度升温至500℃，在此温度保温1h，再以5℃/min的速度升温至1200℃，在此温度保温2h，得到YAG连续纤维。所得钇铝石榴石连续纤维直径为7.7-8.5μm，纤维收缩率约为30％，纤维表面光滑，内部结构致密，XRD测试纤维晶相为钇铝石榴石晶相，纤维单丝拉伸强度平均为932MPa。
本实施例步骤(3)YAG凝胶纤维陶瓷化过程中，选择最终的烧结温度分别为700℃、800℃、900℃、1000℃，得到的钇铝石榴石连续纤维的XRD谱图如图1所示，烧结温度为800℃时得到的YAG纤维开始石榴石化，当烧结温度为1000℃时，已全部转化为钇铝石榴石 晶相。
本实施例制得的钇铝石榴石连续纤维的SEM照片如图3所示，高倍放大的SEM照片如图4所示，纤维截面高倍放大的SEM照片如图5所示。由图3、4、5可知，纤维直径均匀，无渣球且表面光滑；纤维内部结构紧密，晶粒间气孔数量少，有利于纤维机械强度的提高。
对比例1
一种钇铝石榴石连续纤维的制备方法，包括步骤如下：
(1)可纺性前驱体溶胶的制备
按n(Al2O3):n(Y2O3)＝5:3的计量比将1156.5g含有Al13胶粒的氧化铝溶胶(固含量为22.04wt％)和2258.1g氧化钇溶胶(固含量为15wt％)混合，35℃水浴搅拌，搅拌过程中加入450g冰醋酸，其中氧化钇与冰醋酸的摩尔比为1:1.25，然后加入138g稀硝酸调节pH值至2.0，加入98.9g PVP溶液，搅拌混合均匀。
设定老化温度为40℃，老化过程在真空度为0.095MPa条件下进行，将混合溶胶老化至黏度为513Pa·s，得到前驱体可纺性溶胶。
(2)干法纺丝制备凝胶纤维
将步骤(1)制备的前驱体溶胶进行干法纺丝，得到YAG凝胶纤维，工艺条件：喷丝板孔径为0.06mm，收丝速度为80m/min，空气温度为25-30℃，空气湿度为30-40％。
步骤(3)同实施例1。
所得钇铝石榴石连续纤维直径为9.5-10.2μm，纺丝过程中凝胶纤维易断且直径较粗，纤维收缩率约为33％；纤维表面有渣球且内部结构不致密，XRD测试纤维晶相为钇铝石榴石晶相，纤维单丝拉伸强度平均为494MPa。可见单独采用含有Al13胶粒的氧化铝溶胶作为氧化铝源，严重影响钇铝石榴石连续纤维的单丝拉伸强度。
实施例2
一种钇铝石榴石连续纤维的制备方法，包括步骤如下：
(1)可纺性前驱体溶胶的制备
将925.2g含有Al13胶粒的氧化铝溶胶(固含量为22.04wt％)和419.6gγ-AlOOH纳米分散液(固含量为12.15wt％)混合，利用分散机搅拌至均匀，按n(Al2O3):n(Y2O3)＝5:3的计量组成加入2258.1g氧化钇溶胶(固含量为15wt％)，35℃水浴搅拌，搅拌过程中加入450g冰醋酸，其中氧化钇与冰醋酸的摩尔比为1:1.25，此时pH值为3.8，加入98.9g PVP溶液，搅拌混合均匀。
设定老化温度为40℃，老化过程在真空度为0.095MPa条件下进行，老化过程在真空度为0.095MPa条件下进行，将混合溶胶老化至黏度为496Pa·s，得到前驱体可纺性溶胶。
步骤(2)同实施例1。
步骤(3)同实施例1。
所得钇铝石榴石连续纤维直径为7.8-9.0μm；纤维收缩率约为32％，纤维表面较光滑但晶粒间气孔数量较多，XRD测试纤维晶相为钇铝石榴石晶相，纤维单丝拉伸强度平均为583MPa。
实施例3
一种钇铝石榴石连续纤维的制备方法，包括步骤如下：
(1)可纺性前驱体溶胶的制备
将925.2g含有Al13胶粒的氧化铝溶胶(固含量为22.04wt％)和419.6gγ-AlOOH纳米分散液(固含量为12.15wt％)混合，利用分散机搅拌至均匀，按n(Al2O3):n(Y2O3)＝5:3的计量组成加入2258.1g氧化钇溶胶(固含量为15wt％)，35℃水浴搅拌，搅拌过程中加入486g冰醋酸，其中氧化钇与冰醋酸的摩尔比为1:1.35，然后加入195g稀硝酸调节pH值至1.8，加入98.9g PVP溶液，搅拌混合均匀。
设定老化温度为40℃，老化过程在真空度为0.095MPa条件下进行，将混合溶胶老化至黏度为520Pa·s，得到前驱体可纺性溶胶。
步骤(2)同实施例1。
步骤(3)同实施例1。
所得钇铝石榴石连续纤维直径为7.8-9.0μm；纤维收缩率约为32％，纤维表面光滑，内部结构致密，XRD测试纤维晶相为钇铝石榴石晶相，纤维单丝拉伸强度平均为913MPa。
实施例4
一种钇铝石榴石连续纤维的制备方法，包括步骤如下：
(1)可纺性前驱体溶胶的制备
将925.2g含有Al13胶粒的氧化铝溶胶(固含量为22.04wt％)和419.6gγ-AlOOH纳米分散液(固含量为12.15wt％)混合，利用分散机搅拌至均匀，按n(Al2O3):n(Y2O3)＝5:3的计量组成加入2258.1g氧化钇溶胶(固含量为15wt％)，35℃水浴搅拌，搅拌过程中加入720g冰醋酸，其中氧化钇与冰醋酸的摩尔比为1:2，然后加入159g稀硝酸调节pH值至1.8，加入98.9g PVP溶液，搅拌混合均匀。
设定老化温度为40℃，老化过程在真空度为0.095MPa条件下进行，将混合溶胶老化至黏度为515Pa·s，得到前驱体可纺性溶胶。
(2)干法纺丝制备凝胶纤维
将步骤(1)制备的前驱体溶胶进行干法纺丝，得到YAG凝胶纤维，工艺条件：喷丝板孔径为0.06mm，收丝速度为80m/min，空气温度为25-30℃，空气湿度为30-40％，如图2所示，纤维长度可达数千米。
步骤(3)同实施例1。
所得钇铝石榴石连续纤维直径为8.5-9.5μm，纺丝过程中凝胶纤维易断且直径较粗；纤维收缩率约为34％，纤维表面较光滑，晶粒间气孔数量较多，XRD测试纤维晶相为钇铝石榴石晶相，纤维单丝拉伸强度平均为700MPa。
实施例5
一种钇铝石榴石连续纤维的制备方法，包括步骤如下：
步骤(1)同实施例1。
(2)干法纺丝制备凝胶纤维
将步骤(1)制备的前驱体溶胶进行干法纺丝，得到YAG凝胶纤维，工艺条件：喷丝板孔径为0.1mm，收丝速度为120m/min，空气温度为30-35℃，空气湿度为30-40％。
(3)YAG凝胶纤维陶瓷化
将步骤(2)制备的YAG凝胶纤维陶瓷化，工艺条件：以0.8℃/min的速度升温至500℃，在此温度保温1h，再以4℃/min的速度升温至1200℃，在此温度保温2h，得到YAG连续纤维。
所得钇铝石榴石连续纤维直径为8.5-9.8μm，纤维收缩率约为30％，纤维表面光滑，内部结构致密，XRD测试纤维晶相为钇铝石榴石晶相，纤维单丝拉伸强度平均为826MPa。
实施例6
一种钇铝石榴石连续纤维的制备方法，包括步骤如下：
(1)可纺性前驱体溶胶的制备
将809.6g含有Al13胶粒的氧化铝溶胶(固含量为22.04wt％)和629.4gγ-AlOOH纳米分散液(固含量为12.15wt％)混合，利用分散机搅拌至均匀，按n(Al2O3):n(Y2O3)＝5:3的计量组成加入2258.1g氧化钇溶胶(固含量为15wt％)，35℃水浴搅拌，搅拌过程中加入450g冰醋酸，其中氧化钇与冰醋酸的摩尔比为1:1.25，然后加入173g稀硝酸调节pH值至2.0，加入39.6g PVP溶液，搅拌混合均匀。
设定老化温度为40℃，老化过程在真空度为0.095MPa条件下进行，将纺丝液老化至黏度为485Pa·s，得到前驱体可纺性溶胶。
步骤(2)同实施例1。
步骤(3)同实施例1。
所得钇铝石榴石连续纤维直径为7.1-8.5μm，纤维收缩率约30％，纤维表面光滑，内部结构致密，XRD测试纤维晶相为钇铝石榴石晶相，纤维单丝拉伸强度平均为809MPa。
实施例7
一种钇铝石榴石连续纤维的制备方法，包括步骤如下：
(1)可纺性前驱体溶胶的制备
将925.2g含有Al13胶粒的氧化铝溶胶(固含量为22.04wt％)和419.6gγ-AlOOH纳米分散液(固含量为12.15wt％)混合，利用分散机搅拌至均匀，按n(Al2O3):n(Y2O3)＝5:3的计量组成加入2258.1g氧化钇溶胶(固含量为15wt％)，然后加入固含量为22％的醋酸锆54.9g，35℃水浴搅拌，搅拌过程中加入450g冰醋酸，其中氧化钇与冰醋酸的摩尔比为1:1.25，最后加入173g稀硝酸调节pH值至2.0，加入40.4g PVP溶液，搅拌混合均匀。
设定老化温度为40℃，老化过程在真空度为0.095MPa条件下进行，将纺丝液老化至黏度为500Pa·s，得到前驱体可纺性溶胶。
步骤(2)同实施例1。
步骤(3)同实施例1。
所得钇铝石榴石连续纤维直径为6.7-8.5μm，纤维收缩率约为29％，纤维表面光滑，内部结构致密，XRD测试纤维主晶相为钇铝石榴石晶相，纤维单丝拉伸强度平均为950MPa。
实施例8
一种钇铝石榴石连续纤维的制备方法，包括步骤如下：
(1)可纺性前驱体溶胶的制备
将1184.3g含有Al13胶粒的氧化铝溶胶(固含量为22.04wt％)和537.1gγ-AlOOH纳米分散液(固含量为12.15wt％)混合，利用分散机搅拌至均匀，按n(Al2O3):n(Y2O3)＝2:1的计量组成加入2408.6g氧化钇溶胶(固含量为15wt％)，35℃水浴搅拌，搅拌过程中加入450g冰醋酸，其中氧化钇与冰醋酸的摩尔比为1:1.25，然后加入206g稀硝酸调节pH值至2.0，加入45.8g PVP溶液，搅拌混合均匀。
设定老化温度为40℃，老化过程在真空度为0.095MPa条件下进行，将纺丝液老化至黏度为515Pa·s，得到前驱体可纺性溶胶。
(2)干法纺丝制备凝胶纤维
将步骤(1)制备的前驱体溶胶进行干法纺丝，得到YAG凝胶纤维，工艺条件：喷丝板孔径为0.06mm，收丝速度为100m/min，空气温度为25-30℃，空气湿度为25-35％。
(3)YAG凝胶纤维陶瓷化
将步骤(2)制备的YAG凝胶纤维陶瓷化，工艺条件：以1℃/min的速度升温至450℃，在此温度保温1h，再以5℃/min的速度升温至1200℃，在此温度保温2h，得到YAG连续纤维。
所得钇铝石榴石连续纤维直径约为7.5-8.4μm，纤维收缩率约为33％，纤维表面光滑，内部结构致密，XRD测试纤维主晶相为钇铝石榴石晶相，纤维单丝拉伸强度平均为1077MPa。

Claims (10)

  1. 一种钇铝石榴石连续纤维的制备方法，包括步骤如下：
    (1)可纺性前驱体溶胶的制备
    将含有Al13胶粒的氧化铝溶胶和γ-AlOOH纳米分散液混合并加入氧化钇溶胶，30-40℃水浴搅拌，搅拌过程中加入冰醋酸，然后加入稀硝酸调节pH值至1-3，加入纺丝助剂PVP，搅拌混合均匀，设定老化温度为25-80℃，将纺丝液老化至黏度为400-600Pa·s，得到前驱体可纺性溶胶；
    所述含有Al13胶粒的氧化铝溶胶中氧化铝含量为15-35wt％，氧化钇溶胶的固含量为10-30wt％，γ-AlOOH纳米分散液的固含量为8.5-15wt％，氧化钇与冰醋酸的摩尔比为1:(1-2)，PVP加入量为总固含量的0.5-5wt％；含有Al13胶粒的氧化铝溶胶和γ-AlOOH纳米分散液的主要成分以氧化铝计，氧化钇和氧化铝的摩尔比为1:(1-2)；
    (2)干法纺丝制备YAG凝胶纤维
    将步骤(1)制备的前驱体可纺性溶胶进行干法纺丝，得到YAG凝胶纤维，干法纺丝工艺条件：喷丝板孔数为15-800个，喷丝板孔径为0.06-0.15mm，收丝速度为60-180m/min，空气温度为18-40℃，空气湿度为20-70％；
    (3)YAG凝胶纤维陶瓷化
    将步骤(2)制得的YAG凝胶纤维陶瓷化，以0.5-3℃/min的速度升温至450-600℃，在此温度保温0.5-2h，再以3-10℃/min的速度升温至900-1400℃，在此温度保温0.5-2h，即得钇铝石榴石连续纤维。
  2. 根据权利要求1所述的钇铝石榴石连续纤维的制备方法，其特征在于，步骤(1)中含有Al13胶粒的氧化铝溶胶中Al13胶粒的质量含量为20-25wt％，γ-AlOOH纳米分散液的固含量为10-15wt％，氧化钇溶胶固含量为15wt％，纺丝助剂PVP的加入量为总固含量的1wt％。
  3. 根据权利要求1所述的钇铝石榴石连续纤维的制备方法，其特征在于，含有Al13胶粒的氧化铝溶胶和γ-AlOOH纳米分散液中氧化铝含量的质量比为(3-9)：1。
  4. 根据权利要求1所述的钇铝石榴石连续纤维的制备方法，其特征在于，步骤(1)中老化温度为35-50℃，老化至黏度为450-550Pa·s。
  5. 根据权利要求1所述的钇铝石榴石连续纤维的制备方法，其特征在于，步骤(1)中老化过程在真空度为0.095MPa条件下进行。
  6. 根据权利要求1所述的钇铝石榴石连续纤维的制备方法，其特征在于，步骤(1)中氧化钇与冰醋酸的摩尔比为1:(1.1-1.5)。
  7. 根据权利要求1所述的钇铝石榴石连续纤维的制备方法，其特征在于，加入稀硝酸调节pH值至1.5-2.5。
  8. 根据权利要求1所述的钇铝石榴石连续纤维的制备方法，其特征在于，步骤(2)中喷丝板孔径为0.06-0.10mm，收丝速度为80-140m/min。
  9. 根据权利要求1所述的钇铝石榴石连续纤维的制备方法，其特征在于，步骤(2)中空气温度为25-35℃，空气湿度为30-45％。
  10. 根据权利要求1所述的钇铝石榴石连续纤维的制备方法，其特征在于，步骤(3)中YAG凝胶纤维以0.8-1℃/min的速度升温至450-600℃，在此温度保温1-2h；再以3-5℃/min的速度升温至900-1400℃，在此温度保温1-2h。
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