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A kind of preparation method of high-purity polycrystalline yttrium aluminum garnet continuous fiber

A continuous fiber and high-purity technology, which is applied in the direction of spinning solution preparation, dry spinning method, fire-resistant and flame-retardant filament manufacturing, etc., can solve the problem of unwindable, two-dimensional and three-dimensional weaving, difficult to achieve continuous fiber preparation, Corrosion resistance is required to be high and other problems, to achieve the effect of grain refinement, compact structure, and low equipment requirements

Active Publication Date: 2021-09-17
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent document CN105002601A describes a method for preparing YAG fibers by a sol-gel method. The sol reaction formation process requires heating, reflux, and filtration, and the process is complicated. The length of the prepared YAG fibers is short, and it cannot be wound, two-dimensional and three-dimensional weaving.
[0006] The preparation of YAG fibers by the above sol-gel method either requires the addition of spinning aids or the use of strong acids, and the length of the prepared fibers is limited, so it is difficult to achieve continuous fiber preparation of several meters or even tens of meters.
[0007] Hyun Jun Kim et al. (Kim H J, Fair G E, Hart AM, et al. Development of polycrystalline yttrium aluminum garnet (YAG) fibers [J]. Journal of the European Ceramic Society, 2015, 35(15): 4251-4258.) adopted YAG Powder is used as raw material, methyl cellulose is used as binder, glycerin is used as plasticizer, and deionized water is used as solvent. After mixing evenly in a planetary vacuum mixer, it is fiberized by a high-pressure injector, and then vacuumized at 1700-1800 ° C. The YAG continuous fiber is prepared by sintering, the fiber diameter is less than 30μm, uniform and transparent, and the tensile strength reaches 0.91GPa, but the method is complicated and requires high equipment
[0008] Chinese patent document CN106927808 A has prepared a kind of YAG continuous fiber with aluminum sol and γ-AlOOH dispersion liquid as aluminum source, yttrium sol as yttrium source, and PVP as spinning aid. The fiber diameter is relatively uniform and the tensile strength reaches 1GPa, but During the preparation process, nitric acid needs to be used to adjust the pH to about 2.0, which requires high corrosion resistance of the equipment

Method used

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  • A kind of preparation method of high-purity polycrystalline yttrium aluminum garnet continuous fiber
  • A kind of preparation method of high-purity polycrystalline yttrium aluminum garnet continuous fiber
  • A kind of preparation method of high-purity polycrystalline yttrium aluminum garnet continuous fiber

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] A preparation method of high-purity polycrystalline YAG continuous fiber, comprising the steps of:

[0042] (1) Add 10.98g of crystalline aluminum chloride into a beaker containing 60g of deionized water, stir at room temperature until completely dissolved, then add 5.53g of aluminum powder (n(Al):n(AlCl 3 ·6H 2 (0)=4.5:1), heated and stirred at 85°C for about 2.5 hours to completely react the aluminum powder to obtain a PAC solution.

[0043] Add yttrium acetate to the PAC solution at a molar ratio of Y:Al=3:5, and add 120 g of deionized water, stir at room temperature until the yttrium acetate is completely dissolved, and filter to obtain a clear and transparent YAG precursor solution.

[0044] The YAG precursor solution was concentrated at 65 °C by evaporating the solvent until the viscosity of the sol was 350 Pa·S at 20 °C, and a transparent, uniform and stable YAG spinnable sol was obtained.

[0045] (2) Transfer YAG spinnable sol into the liquid material tank of...

Embodiment 2

[0050] As described in Example 1, the difference is: as described in step (2), the YAG spinnable sol is transferred to the liquid material tank of the spinning device, vacuum degassed for 10min, at a pressure of 2MPa, at an ambient temperature of 50°C, relatively Under the condition of 30% humidity, it is sprayed from a niobium-tantalum alloy spinneret with 50 holes and a diameter of 40 μm, and a transparent and orderly YAG precursor continuous fiber with a diameter of 35 μm is obtained through drawing and winding.

[0051] The photo of the YAG precursor continuous fiber obtained in the present embodiment step (2) is as follows figure 1 shown. Depend on figure 1 It can be seen that the continuous fiber of YAG precursor has uniform diameter, high strength, good flexibility, can be wound and crimped.

Embodiment 3

[0053] As described in Example 1, the difference is: as described in step (2), the YAG spinnable sol is transferred to the liquid feed tank of the spinning device, vacuum degassed for 10min, and after aging for one week at room temperature, the Under the condition of 2MPa, ambient temperature 60℃ and relative humidity 10%, it is sprayed from a niobium-tantalum alloy spinneret with 20 holes and a diameter of 250μm, and the diameter is 240μm after drawing and winding to obtain a transparent and orderly YAG precursor continuous fiber.

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Abstract

The invention relates to a preparation method of high-purity polycrystalline yttrium aluminum garnet continuous fiber, comprising the following steps: (1) adding crystalline aluminum chloride and aluminum powder into water and stirring to react to obtain polyaluminum chloride (PAC) solution, Add the yttrium source and stir to dissolve completely to obtain a precursor solution; concentrate the precursor solution to obtain a precursor spinning sol; (2) perform dry spinning on the precursor spinning sol to obtain a precursor continuous gel fiber; (3) The precursor continuous gel fiber is dried at 40-70°C, and then heat-treated in the range of 750-1200°C. During the heat treatment, water vapor is introduced when the temperature rises to 250-300°C. After the heat treatment is completed, high-purity polycrystalline YAG is obtained. continuous fiber. The YAG continuous fiber prepared by the invention can be used as refractory material and heat insulation material in the fields of aerospace, automobile, high-speed rail and the like. The invention has the characteristics of simple method, low cost, no pollution, stable fiber quality and the like.

Description

technical field [0001] The invention relates to a preparation process of yttrium aluminum garnet continuous fiber that can be used as winding or other two-dimensional and three-dimensional weaving, and belongs to the field of inorganic non-metallic materials. Background technique [0002] Yttrium aluminum garnet (YAG) is an Al 2 o 3 and Y 2 o 3 The composite oxide belongs to the cubic crystal system, has a garnet crystal structure, a melting point of 1970°C, and a density of 4.55g / cm 3 , chemically stable, insoluble in H 2 SO 4 , HNO 3 , HF and other strong acids, in addition to the high strength, high modulus, high temperature resistance, oxidation resistance, corrosion resistance and other excellent properties of alumina, YAG also has excellent high temperature creep resistance, thermal shock resistance and excellent optical properties. performance. [0003] Due to the unique structure and excellent performance of YAG, YAG is prepared into fibers so that it has the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F9/08D01F1/07D01D1/02D01D5/04
CPCD01D1/02D01D5/04D01F1/07D01F9/08
Inventor 朱陆益谢永帅汪林王新强张光辉许东
Owner SHANDONG UNIV