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Preparation method of high-performance zirconia ceramic fibers

A zirconia ceramic, high-performance technology, applied in the direction of inorganic raw material rayon, etc., can solve the problems of large investment in equipment, high corrosion, and difficult to recycle.

Inactive Publication Date: 2013-07-10
绍兴市圣诺超高温晶体纤维材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, public information shows that by the end of 2012, the length of the zirconia ceramic fiber produced by the representative company in the world - Zircar of the United States was only in the millimeter range.
Domestic research on the preparation of zirconia ceramic fibers of several centimeters to tens of centimeters mostly uses the sol-gel method, but most of the process routes are too long, the equipment investment is large, the energy consumption is large, and the process conditions are harsh; what is more serious is that many of them are used as Zr 4+ Ligands use a large amount of organic solvents, which are highly corrosive, costly and difficult to recycle, and are likely to cause environmental pollution and safety hazards, so industrialization is particularly difficult

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Weigh 322 grams of zirconium oxychloride, 120 grams of acetic acid, and 324 grams of pure water (molar ratio 1:2:18); yttrium oxide is used as a stabilizer, and 39 grams of yttrium nitrate (molar ratio Zr 4+ : Y 3+ =1:0.1, partly stable tetragonal phase).

[0013] First mix and stir the above-mentioned zirconium oxychloride, yttrium nitrate, and pure water to dissolve, then slowly add acetic acid dropwise to the solution, and stir vigorously for 2 to 5 hours. The gas is discharged during the reaction, and the polymerized long chain containing Zr-O-Zr is obtained. Transparent sol.

[0014] Continue to stir the above sol, heat to 65~75℃, turn on the vacuum to -0.095MPa, concentrate under reduced pressure to remove part of the water, sol polycondensation for 5 hours and gradually reach the viscosity of the material 20~25Pa·s, stop concentration, take out the material and place at room temperature After 10 days of static aging, a gel with good spinnability is obtained.

[0015] T...

Embodiment 2

[0017] Weigh 322 grams of zirconium oxychloride, 180 grams of acetic acid, and 260 grams of pure water (molar ratio 1:3:20); yttrium oxide is used as a stabilizer, and 76 grams of yttrium nitrate (molar ratio Zr 4+ : Y 3+ =1:0.2, fully stable cubic phase).

[0018] First stir the above-mentioned zirconium oxychloride, yttrium nitrate, and pure water into a mixed solution, then slowly add acetic acid dropwise to the mixed solution, stir vigorously, and discharge the gas from the reaction until it is completely dissolved, that is, a polymerized long chain containing Zr-O-Zr is obtained. The colorless transparent sol.

[0019] Continue to stir and heat the above transparent sol to 65~75℃, turn on the vacuum to -0.095MPa, concentrate the sol under reduced pressure to remove part of the water, and polycondensate the sol for 6 hours to gradually reach the viscosity of the material 20~25Pa·s, stop the concentration, take out the material and place After 15 days of static aging at room tem...

Embodiment 3

[0022] The gel of Example 1 above is spun out at high speed by a high-speed centrifugal spinning device to become gel fibers with a length of several centimeters to several tens of centimeters. The diameter of the small hole of the spinning disc on the high-speed centrifugal spinning device is 0.2mm, and the linear speed of gel spinning is 60m / s. The gel can spin out the silk from several centimeters to tens of centimeters; the tangential direction of the spinning disc is 80 ℃ hot air blowing, stretching and drying.

[0023] Put the above-mentioned spray-dried gel fiber into a program-controlled atmosphere furnace, inject water vapor into the furnace, and complete the analytical crystallization at a heating rate of 0.5°C / min to 600°C; then, a heating rate of 2°C / min to 1600 Dense sintering is completed at ℃ to obtain a partially stable high-performance zirconia ceramic fiber with a diameter of 3-8 microns, a large aspect ratio, high tensile strength, and a soft hand.

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Abstract

The invention relates to a preparation method of high-performance zirconia ceramic fibers. The preparation method comprises the steps of: dissolving zirconium oxychloride, ethylic acid and yttrium nitrate into pure water according to a certain mole ratio, reacting and synthesizing into Zr-O-Zr polymerization long chain-containing sol through heating, then performing decompression and distillation to obtain gel, namely a spinning solution, performing mechanical thread throwing, drying gel fibers, and performing ligand atmosphere analysis, high-temperature calcining and the like to obtain the long high-performance zirconia ceramic fibers with high strength. The sol-gel is prepared at a step, so that the energy consumption is less, the yield is high, the cost is low, the technological processes are environment-friendly, and further large-scale production can be easily realized.

Description

Technical field [0001] The invention relates to a preparation method of zirconia ceramic fiber, in particular to a preparation method of high-performance zirconia ceramic fiber mainly used in the field of aerobic ultra-high temperature thermal insulation, and belongs to the technical field of inorganic refractory and thermal insulation materials. Background technique [0002] Compared with carbon fiber and silicon carbide fiber, the stabilized zirconia ceramic fiber has the characteristics of not being oxidized under high temperature in an aerobic environment. Zirconia ceramic fiber is compatible with the widely used aluminum silicate, mullite, and oxide Compared with oxide fibers such as aluminum, it has high melting point, low thermal conductivity, low high-temperature vapor pressure, strong acid and alkali corrosion resistance, good chemical stability and strong thermal shock resistance, making it a new generation of ultra-high temperature insulation Thermal insulation materia...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/48C04B35/624D01F9/08
Inventor 章宝土张永坚缪锡飞章宝华陈卫东潘军标
Owner 绍兴市圣诺超高温晶体纤维材料有限公司