Method for preparing zirconia crystal fiber from basic zirconium carbonate-methanol system

Abstract

The invention relates to a method for preparing a polyvinyl acetate zirconium oxygen precursor sol spinning solution and a zirconia crystal fiber based on a basic zirconium carbonate-methyl alcohol system. The method comprises the steps that the mixed solution of glacial acetic acid and methyl alcohol is added into a basic zirconium carbonate methanol solution to prepare the polyvinyl acetate zirconium oxygen precursor sol spinning solution; high-speed centrifugation spinning is carried out based on the centrifugal pan silk throwing method to prepare the poly-zirconium precursor fiber; the precursor fiber is placed into a pressure vessel, the pressure vessel is inflated with the air with the pressure being 2-20 atm and the temperature ranging from 120 DEG C to 210 DEG C, dissolving is carried out, and the ligand acetic acid in the precursor fiber is separated out; the fiber on which the ligand acetic acid is separated out is placed in a sintering furnace to be processed at the medium and high temperature. The prepared polyvinyl acetate zirconium oxygen precursor fibers are fluffy and freely stacked, zirconium oxide crystal fiber grains are arranged densely, the polyvinyl acetate zirconium oxygen precursor fiber has ultra-high temperature performance, the strength ranges from 0.6 GPa to 2.0 GPa, and the polyvinyl acetate zirconium oxygen precursor fiber can be used at the ultra-high temperature being 2,200 DEG C for a long time.

Description

technical field [0001] The invention relates to a method for preparing zirconia crystal fibers from a basic zirconium carbonate-methanol system, and belongs to the field of inorganic non-metal refractory materials. Background technique [0002] Zirconia crystal fibers have extremely high melting point (2715°C), extremely low thermal conductivity, extremely low high-temperature vapor pressure and excellent chemical stability, and have very broad application prospects in the fields of aviation, aerospace and ultra-high temperature electric furnaces. It is currently the top-grade high-grade refractory fiber material in the world. The large-scale preparation and application of high-tech materials will give full play to their performance advantages such as high temperature resistance, good heat insulation, good stability, and energy saving, greatly promote the development and technological progress of related fields, and further accelerate the formation of related industrial chai...

AI Technical Summary

Problems solved by technology

However, the existing high-performance zirconia crystal fiber preparation technology still has disadvantages such as complex precursor preparation process, long post-processing time, and harsh conditions.

For example, in CN1584155A and CN101498063A patent documents, zirconium oxychloride, triethylamine and acetylacetone are used as raw materials, and methanol and ethanol are used as solvents respectively to react and synthesize zirconium polyacetylacetonate precursors, and then dissolve the precursors in methanol The spinning solution is obtained, the precursor fiber is prepared by high-speed centrifugal spinning, and then the zirconia crystal fiber is obtained by special atmosphere treatment and high-temperature sintering. The two methods of rubber making process are more complicated, with many operating steps and strict requirements.

CN102181962A patent document uses basic zirconium carbonate, glacial acetic acid, water, and yttrium nitrate as raw materials to prepare polyzirconium sol spinning liquid, and obtains fine-diameter polyzirconium gel fibers through high-speed centrifugal spinning and hot air jet drawing, and then heat treatment Fine-diameter zirconia fibers are obtained by sintering. Although this method simplifies the synthesis steps, the gel fibers that are thrown out at a high speed by using water as a solvent contain a lot of water. It is necessary to increase the hot air blowing to obtain relatively dry gel fibers, otherwise The gel fiber is easy to absorb moisture and form a cake; if it is sintered directly in the heat treatment, the acetate in the gel fiber will generate a large amount of gas during the sintering process, and there will be more pores in the fiber, resulting in a decrease in the mechanical strength of the zirconia fiber. decline

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