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Method for preparing zirconium oxide fibers through inorganic hybridization of organic polymer

A zirconia fiber and polymer technology, which is applied in the field of inorganic fiber preparation, can solve the problems of complex spinning process, short zirconia fiber fiber, and difficulty in stabilizing, and achieves expanded application range, excellent fiber processing performance, and production stability Improved effect

Inactive Publication Date: 2011-09-21
ZHONGYUAN ENGINEERING COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is that the fiber of zirconia fiber is short, the spinning process is complicated, and it is difficult to stabilize, and it provides a kind of raw material that is easy to get, and can use the conventional industrial spinning method to prepare zirconia by using organic polymer inorganic hybridization fiber method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] (1) Weigh 300g of zirconium oxychloride, add 50g of ammonia water, stir for 60 minutes at 75-80°C, and gradually form a transparent sol, then wash with water and ethanol respectively until no chloride ions are detected with silver nitrate reagent. Dry at 100°C, grind again, and bake in a microwave sintering furnace at a temperature of 1000°C for 1 hour to obtain nano-zirconia powder with an average particle size of 92±21nm;

[0018] (2) blending the deionized nano zirconia powder in step (1) with polyacrylonitrile resin resin, and then preparing organic-inorganic hybrid zirconia fibers with higher mechanical properties through solution spinning;

[0019] (3) The zirconia fibers in step (2) are thermally stabilized at a temperature of 210 to 320° C. at a heating rate of 10° C. / hour, and carbonized at a temperature of 1200 to 1500° C. at a heating rate of 20-40°C / hour to obtain inorganic zirconia fibers. The tensile strength is tested with a universal material testing ma...

Embodiment 2

[0021] (1) Weigh 300g of zirconium oxychloride, add 150g of oxalic acid, stir at 80-85°C for 40 minutes, gradually form a transparent sol, and then wash with water and ethanol respectively until no chloride ions are detected with silver nitrate reagent. Dry at 120°C, grind again, and bake in a microwave sintering furnace at a temperature of 1000°C for 1 hour to obtain nano-zirconia powder with an average particle size of 68±20nm;

[0022] (2) blending the deionized nano zirconia powder in step (1) with polyacrylonitrile resin resin, and then preparing organic-inorganic hybrid zirconia fibers with higher mechanical properties through solution spinning;

[0023] (3) The zirconia fibers in step (2) are thermally stabilized at a temperature of 210 to 320° C. at a heating rate of 10° C. / hour, and carbonized at a temperature of 1200 to 1500° C. at a heating rate of 20-40°C / hour to obtain inorganic zirconia fibers. The tensile strength is tested with a universal material testing mac...

Embodiment 3

[0025] (1) Weigh 300g of zirconium oxychloride, add 105g of dimethylformamide, stir at 85-90°C for 60 minutes, gradually form a transparent sol, then wash with water and ethanol respectively until chlorine-free is tested with silver nitrate reagent. ions, dried at a temperature of 110°C, then ground, and roasted in a microwave sintering furnace at a temperature of 800°C for 1 hour to obtain nano-zirconia powder with an average particle size of 77±28nm;

[0026] (2) blending the deionized nano zirconia powder in step (1) with polyacrylonitrile resin resin, and then preparing organic-inorganic hybrid zirconia fibers with higher mechanical properties through solution spinning;

[0027] (3) The zirconia fibers in step (2) are thermally stabilized at a temperature of 210 to 320° C. at a heating rate of 10° C. / hour, and carbonized at a temperature of 1200 to 1500° C. at a heating rate of 20-40°C / hour to obtain inorganic zirconia fibers. The tensile strength is tested with a univers...

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Abstract

The invention discloses a method for preparing zirconium oxide fibers through inorganic hybridization of organic polymer, which comprises the following steps of: adding one of dimethylformamide, ammonia water and oxalic acid into zirconium oxychloride, and stirring to form transparent sol; washing with water and ethanol sequentially until chloride ions are absent through detection of a silver nitrate reagent, drying and grinding, and roasting in a microwave sintering furnace to obtain nano zirconium oxide powder; blending the nano zirconium oxide powder and organic polymer resin, and preparing organic / inorganic hybrid fibers through solvent spinning, melting spinning or electrostatic spinning; and performing thermal stabilization and carbonization on the zirconium oxide fibers to obtain inorganic zirconium oxide fibers. Raw materials are cheap and readily available; the prepared zirconium oxide fibers can be short fibers and continuous fibers, and also can be nano zirconium oxide fibrous membranes; the zirconium oxide fibers can be prepared by several pieces of conventional process equipment, and the manufacturing cost is reduced; and the product stability is improved and continuous filament fibers are easily obtained.

Description

technical field [0001] The invention relates to a method for preparing inorganic fibers, in particular to a method for preparing zirconia fibers by inorganic hybridization of organic polymers. Background technique [0002] Ceramic fiber is a lightweight refractory material, which combines the textile processing characteristics of fiber and the high temperature resistance of ceramics. It has the characteristics of high temperature resistance, good thermal stability, oxidation resistance, corrosion resistance, and good heat insulation performance. It has been widely used in aerospace, atomic energy, metallurgy and petrochemical, transportation and other industries. Ceramic fibers are mainly used in fields that require high temperature resistance and high mechanical properties. They are used in aerospace for ablation-resistant material components, such as heat shields for spacecraft re-entering the atmosphere, rocket nose cones, nozzles, exhaust ports and Separators, etc.; use...

Claims

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Application Information

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IPC IPC(8): C04B35/48C04B35/622
Inventor 张旺玺王艳芝王志新孙礼武桑向东焦明立袁祖培
Owner ZHONGYUAN ENGINEERING COLLEGE
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