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A kind of preparation method of defective fluorite phase gadolinium zirconate fiber

A technology of gadolinium zirconate and fiber, which is applied in the field of preparation of defective fluorite-phase gadolinium zirconate fiber, which can solve the problems of inability to form fibrous structure and high content of organic matter, achieve good fiber shape, simple preparation process, and uniform diameter Effect

Active Publication Date: 2021-04-23
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The content of organic matter in the spun preform is high, and the preform has a sheet-like structure after heat treatment, and cannot form a fibrous structure

Method used

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  • A kind of preparation method of defective fluorite phase gadolinium zirconate fiber
  • A kind of preparation method of defective fluorite phase gadolinium zirconate fiber
  • A kind of preparation method of defective fluorite phase gadolinium zirconate fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] A defect-type fluorite-phase gadolinium zirconate fiber and a preparation method thereof, comprising the following steps:

[0035] (1) According to the molar ratio of basic zirconium carbonate and gadolinium chloride hexahydrate as 1:0.4, weigh 20.0000g basic zirconium carbonate, 9.6642g gadolinium chloride hexahydrate and put in a beaker, then add 10.0000g glacial acetic acid and appropriate amount of Methanol was heated and stirred at 50°C until completely dissolved to form a clear gadolinium zirconate precursor solution.

[0036] (2) Add 0.02g polyethylene oxide (PEO) to the gadolinium zirconate precursor solution obtained in (1), stir at 25°C until dissolved, prepare 44.0000g of it with methanol, and continue stirring for 0.5h without heating, The spinning liquid of gadolinium zirconate precursor is prepared.

[0037] (3) Electrospinning the gadolinium zirconate precursor spinning solution obtained in (2) in an environment with a temperature of 25° C. and a humidit...

Embodiment 2

[0042] As described in Example 1, the difference is that in step (4), the obtained gadolinium zirconate precursor fiber is heated to 600°C at a heating rate of 1°C / min, and then to 600°C at a heating rate of 2°C / min. 1400°C, keep warm for 4 hours, and cool down naturally.

Embodiment 3

[0044] As described in Example 1, the difference is that in step (4), the obtained gadolinium zirconate precursor fiber is heated to 600°C at a heating rate of 1°C / min, and then to 600°C at a heating rate of 2°C / min. 1200°C, keep warm for 4 hours, and cool down naturally. Its Raman spectrum is as Figure 5 shown.

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Abstract

The invention relates to a preparation method of defective fluorite phase gadolinium zirconate fiber. The gadolinium zirconate fiber has a diameter of 1.5-2.5 μm, and is defect-type fluorite phase gadolinium zirconate. The preparation method includes: fully mixing basic zirconium carbonate, glacial acetic acid, gadolinium source, and solvent at 25-60°C in a certain proportion and stirring until the solution is clear to form a precursor solution; adding spinning aid to the precursor solution, The precursor solution is adjusted to a certain viscosity to obtain a precursor spinning solution; the precursor spinning solution is electrospun to obtain a precursor fiber, and high-temperature heat treatment is performed in air to obtain a gadolinium zirconate fiber. The preparation process of the invention is simple, the cost is low, and the prepared gadolinium zirconate fiber has a uniform diameter and no defects such as obvious pores and cracks, and can be used as a high-temperature refractory material, a thermal barrier coating material, and a curing material for high-radiation waste.

Description

technical field [0001] The invention relates to a preparation method of defective fluorite-phase gadolinium zirconate fiber, which belongs to the technical field of synthetic fibers. Background technique [0002] Rare earth zirconate materials (Re 2 Zr 2 o 7 , Re=rare earth elements) have been widely used in many fields because of their excellent properties such as low thermal conductivity, high melting point, high thermal expansion coefficient and high temperature phase stability. Among them, gadolinium zirconate (Gd 2 Zr 2 o 7 ) materials can form a defect-type fluorite structure, which can be regarded as derived from a fluorite structure lacking 1 / 8 lattice oxygen. It has more vacancies and a more complex unit cell structure. Compared with other rare earth zirconate materials, gadolinium zirconate material has lower thermal conductivity, higher thermal expansion coefficient and better thermal corrosion resistance. At the same time, gadolinium zirconate has excellen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F9/08D01F11/00D01D1/02D01D5/00
Inventor 王新强陈经纬谢永帅许东朱陆益张光辉刘雪松
Owner SHANDONG UNIV