Method and equipment of preparing high performance zirconium oxide continuous fiber

A technology of continuous fiber and zirconia, which is applied in the direction of zirconia and inorganic raw material artificial filament, etc. It can solve the problems that continuous fiber cannot be prepared by melting method, zirconium dispersion is not uniform enough in the mixing method, and can not be used continuously, etc., to achieve shortening Molecular weight distribution range, reducing performance unevenness, and improving fiber performance

Inactive Publication Date: 2005-06-15
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

Because the melting point of zirconia is too high, its continuous fiber cannot be prepared by melting method, only various precursor methods as mentioned above can be used, and the existing technologies all have their own shortcomings.
From the perspective of the precursor system, the zirconium content in the impregnation method is too low, and it is difficult to prepare high-strength zirconia fibers; from the performance of the spinning solution, the dispersion of zirconium in the mixing method is not uniform enough, the spinning is easy to block and the preparation of nano-sized zirconia The microparticle process is very complicated. The properties of the sol spinning solution in the sol-gel method are not stable, and it is easy to spontaneously turn into a gel, which affects spinning or even cannot be used continuously; in terms of heat treatment, there are also certain deficiencies.
Therefore, the existing technology is difficult to ensure that the prepared zirconia fibers are as continuous as carbon fibers and quartz fibers and can have high strength.

Method used

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  • Method and equipment of preparing high performance zirconium oxide continuous fiber
  • Method and equipment of preparing high performance zirconium oxide continuous fiber
  • Method and equipment of preparing high performance zirconium oxide continuous fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] (1) 97.0 grams of high-purity zirconium oxychloride (ZrOCl 2 ·8H 2 O) be dissolved in 1000 milliliters of methanol, under ice bath at 0~4 ℃, according to the ratio of zirconium oxychloride: acetylacetone: triethylamine=1: 1.5: 2 in molar ratio, successively add 46.0 milliliters of acetylacetone dropwise and 84.0 ml of triethylamine, stirring continuously during the dropwise addition, after the dropwise addition, remove the ice bath, continue to stir at room temperature for 2 hours, evaporate the solvent methanol with a rotary evaporator, until dry, add 500 ml of tetrahydrofuran, stir vigorously After 1 hour, filter with suction to remove the white precipitate, then use a rotary evaporator to evaporate the solvent tetrahydrofuran from the filtrate until a dried light yellow hardened substance is obtained, add 700 ml of n-hexane, stir vigorously for 24 hours, filter with suction, and dry the precipitated filter cake to obtain 61.2 grams of zirconium polyacetylacetonate w...

Embodiment 2

[0059] As described in Example 1, the difference is that 97.0 grams of high-purity zirconium oxychloride is replaced by 97.0 grams of commercially pure zirconium oxychloride in step (1), and the tensile strength of the continuous zirconia fiber obtained is the result of comparative example 1 slightly worse.

Embodiment 3

[0061] As described in Example 1, the difference is that the ratio of zirconium oxychloride in step (1): the molar ratio of acetylacetone=1:1.5 is changed to 1:1, that is, 46.0 milliliters of acetylacetone is changed to 30.7 milliliters of acetylacetone , The tensile strength of the obtained zirconia continuous fiber is slightly higher than that of Example 1.

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Abstract

A preparation method and equipment for high-performance zirconia continuous fibers belong to the field of structural and functional fiber materials. Including using acetylacetone and zirconium oxychloride as the main raw materials to synthesize the precursor zirconium acetylacetonate polymer, dissolving it in methanol to obtain spinning solution, using dry spinning to obtain continuous precursor fiber, heat treatment and sintering to obtain continuous zirconia fiber , a special atmosphere heat treatment process is adopted for the precursor fiber, and the zirconia continuous fiber is blown by air at high temperature to make the fiber stretch and strengthen. The heat treatment is carried out in a multifunctional sintering furnace, which includes an inner tube, an outer tube, and a heating furnace wire wound on the outer tube. When ventilating, the airflow can be blown radially from the inner tube through small slits to the outside of the tube. The process of the invention is simple and easy, and the smooth and uniform zirconia continuous fiber can be prepared with a tensile strength exceeding 2.6 GPa and a continuous length of several kilometers.

Description

(1) Technical field [0001] The invention relates to a method for preparing high-performance high-temperature oxide fibers, in particular to a method for preparing continuous zirconia fibers with high strength, high toughness, high temperature resistance and good heat insulation, belonging to the field of structural and functional fiber materials . (2) Background technology [0002] With the development of economy and science and technology, fiber materials such as quartz fiber, carbon fiber, glass fiber and oxide ceramic fiber are playing an increasingly important role in optical communication, aerospace, military and other high-tech and cutting-edge technology fields. important role. [0003] Zirconia continuous fiber is a structural and functional material with great application potential. Compared with other fibers, it has many unique and irreplaceable superior properties. The thermal conductivity of zirconia is the smallest among all metal oxides, which determines that...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G25/02C04B35/48D01F9/08
Inventor 许东刘和义侯宪钦王彦玲汪晨吕孟凯袁多荣陈代荣刘久荣潘梅
Owner 绍兴市圣诺超高温晶体纤维材料有限公司
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