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Method for preparing fully-stabilized tetragonal-phase zirconia crystal fibers

A technology of crystalline fiber and phase zirconia, applied in the field of refractory materials and heat preservation, can solve the problems of low fiber strength, low zirconia content, and difficult densification of zirconia fibers, and achieves the effect of simple process and short production cycle.

Inactive Publication Date: 2012-11-14
安徽同和晶体新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008]The zirconia fiber precursor prepared by impregnation method, zirconium polymer method, colloid method and previous mixing method contains a large amount of organic components or water, and the zirconia The content is not high. During the calcination process, a large amount of volatile substances are removed, so that the prepared zirconia fibers are not easy to be dense, and the fiber strength is not high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Pour 30g of zirconium hydroxide powder into 90g of water and stir to form a suspension. Then mix 5.7g of yttrium nitrate and 48g of 50% nitric acid solution, stir well to make it evenly mixed, and then slowly add this mixture into the zirconium hydroxide aqueous solution under the stirring condition of 25°C, and keep stirring for 2.5h after the addition is completed , concentrated at 78°C until the viscosity reached 20 Pa.s, and finally aged to 80 Pa.s at 10°C to obtain a spinnable precursor sol. The spinnable precursor sol is passed through high-speed centrifugal spinning equipment to obtain zirconium-containing gel fibers. The zirconium-containing gel fibers are heated in a shuttle high-temperature kiln, and the temperature is raised to 500°C at a rate of 1.5°C / min. After 1 hour, the temperature was raised to 1100°C at a rate of 5°C / min, and then kept at a constant temperature for 1 hour, then rapidly cooled to room temperature to obtain zirconia crystal fibers. The ...

Embodiment 2

[0022] Pour 30g of zirconium hydroxide powder into 90g of water and stir to form a suspension. Then mix 7.8g of yttrium nitrate and 48g of 50% concentration nitric acid solution, stir fully to make it evenly mixed, then slowly add this mixed solution into the zirconium hydroxide aqueous solution at 26°C under stirring conditions, and continue stirring for 2.2h after the slow addition , concentrated at 75°C until the viscosity reached 21Pa.s, and finally aged to 85Pa.s at 10°C to obtain a spinnable precursor sol. The spinnable precursor sol is passed through high-speed centrifugal spinning equipment to obtain zirconium-containing gel fibers. The zirconium-containing gel fibers are heated in a shuttle high-temperature kiln, and the temperature is raised to 500°C at a rate of 1.6°C / min. 1h, then the temperature was raised to 1100°C at a rate of 6°C / min, kept at a constant temperature for 1h, and rapidly cooled to room temperature to obtain zirconia crystal fibers. The crystal fo...

Embodiment 3

[0024] Pour 30g of zirconium hydroxide powder into 90g of water and stir to form a suspension. Mix 5.7g of yttrium nitrate and 96g of 50% nitric acid solution, stir well to make it evenly mixed, then slowly add the mixed solution into the zirconium hydroxide aqueous solution at 27°C under stirring conditions, and continue stirring for 2.4h after the slow addition is completed. Concentrate at 76°C until the viscosity reaches 22 Pa.s, and finally age at 10°C to 90 Pa.s to obtain a spinnable precursor sol. The spinnable precursor sol is passed through high-speed centrifugal spinning equipment to obtain zirconium-containing gel fibers. The zirconium-containing gel fibers are heated in a shuttle high-temperature kiln, and the temperature is raised to 500°C at a rate of 1.7°C / min. After 1 hour, the temperature was raised to 1100°C at a rate of 7°C / min, and then kept at a constant temperature for 1 hour, and then rapidly cooled to room temperature to obtain zirconia crystal fibers. ...

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Abstract

The invention discloses a method for preparing fully-stabilized tetragonal-phase zirconia crystal fibers. The invention aims to provide a method for preparing fully-stabilized tetragonal phase zirconia crystal fibers, which is simple in process and short in product manufacturing cycle, and prepared zirconia crystal fibers are high in purity, good in strength, small in diameter, uniform in product, low in thermal conductivity and good in long-term high-temperature-resistant performance. The method comprises the following steps of: 1, preparing a spinnable precursor zirconium oxynitrate sol by using an inorganic material zirconium hydroxide, pure water, yttrium nitrate and a salpeter solution with the concentration of 50%; 2, forming of gelatinous fiber: enabling the prepared spinnable precursor zirconium oxynitrate sol to pass through a high-speed centrifugal spinner so as to obtain a zirconium-containing gelatinous fiber; and 3, carrying out heat treatment on a zirconia crystal fiber so as to obtain a fully-stabilized tetragonal-phase zirconia crystal fiber with a diameter of 3-6mu m.

Description

technical field [0001] The invention relates to a method for preparing zirconia crystal fibers, in particular to a method for preparing fully stable tetragonal zirconia crystal fibers, and belongs to the technical fields of thermal insulation and refractory materials. Background technique [0002] Refractory ceramic fiber has become a hot spot for development due to its excellent thermal insulation performance. Carbon fiber is a kind of thermal insulation material with excellent performance. ; Alumina fiber is also a commonly used thermal insulation material with excellent performance, which can be used in an oxidizing atmosphere, but its maximum service temperature is 1800 ° C, which restricts its use in higher temperature environments; zirconia ceramic fiber and Compared with other types of inorganic fiber materials, it has a high melting point (2710 ± 15 ℃), large thermal resistance coefficient, good burning resistance (it can still maintain a good fiber shape at 2500 ℃ i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/48C04B35/624
Inventor 任克诚许元虎任叶强周小平
Owner 安徽同和晶体新材料股份有限公司