Preparation method of superfine zirconia/silicon carbide composite fibers

A technology of ultra-fine zirconia and composite fibers, which is applied in fiber treatment, spinning solution preparation, filament/wire forming, etc., can solve the problems of large diameter of zirconium-containing silicon carbide fibers, and achieve good spinnability and specific surface area Great, easy-to-prepare effects

Active Publication Date: 2011-12-07
NAT UNIV OF DEFENSE TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This Si-Zr-C-O fiber has high strength, good flexibility, and excellent high temperature resistance; but the diameter of the zirconium-containing silicon carbide fiber prepared by this melt spinning method is relatively large, especially the zirconium-containing silicon carbide fiber prepared by melt spinning , the precursor of polyzirconium carbosilane needs to be prepared, and the Si-Zr bonding reaction occurs during the preparation process, and the final fiber does not exist in the form of zirconia / silicon carbide composite fiber

Method used

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  • Preparation method of superfine zirconia/silicon carbide composite fibers
  • Preparation method of superfine zirconia/silicon carbide composite fibers
  • Preparation method of superfine zirconia/silicon carbide composite fibers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Preparation of spinning solution: polycarbosilane solid (softening point 200~220°C) and 85% tetrabutyl zirconate n-butanol solution according to the mass ratio of polycarbosilane and tetrabutyl zirconate to 9 : 1; co-dissolve in xylene, prepare polycarbosilane / tetrabutyl zirconate solution according to the ratio of polycarbosilane and solvent (xylene and n-butanol) at 1.1:1g / ml, and disperse with ultrasonic for 30 minutes;

[0020] (2) Electrospinning: Spinning conditions: the inner diameter of the needle is 0.6mm, the voltage is 15kV, the distance of the wire is 20cm, the feeding rate is 20μl / min, and the aluminum foil is collected to obtain polycarbosilane / tetrabutyl zirconate fibrils;

[0021] (3) Air pre-oxidation: put the above-mentioned fibrils in an oxidation furnace, raise the temperature to 220°C at 20°C / h in an oxidative atmosphere, and keep it at this temperature for 1 hour, and obtain infusible polycarbonate after cooling to room temperature Silane / tetra...

Embodiment 2

[0028] (1) Preparation of spinning solution: polycarbosilane solid (softening point 200~220°C) and 85% tetrabutyl zirconate n-butanol solution according to the mass ratio of polycarbosilane and tetrabutyl zirconate to 11 : 1 co-dissolve in xylene, prepare polycarbosilane / tetrabutyl zirconate solution according to the ratio of polycarbosilane and solvent (xylene and n-butanol) at 1.2:1 g / ml, and disperse by ultrasonic for 30 minutes;

[0029] (2) Electrospinning: Spinning conditions: needle inner diameter 1.0mm, voltage 20kV, take-up distance 25cm, feed rate 30μl / min, aluminum foil take-up, and produce polycarbosilane / tetrabutyl zirconate fibrils;

[0030] (3) Air pre-oxidation: put the above-mentioned fibrils in an oxidation furnace, raise the temperature at 20°C / h in an oxidative atmosphere, keep it at 210°C for 1 hour, and obtain infusible polycarbosilane / zirconic acid after cooling to room temperature tetrabutyl fiber;

[0031] (4) High-temperature firing: put the above-me...

Embodiment 3

[0033] (1) Preparation of spinning solution: polycarbosilane solid (softening point: 200~220°C) and 85% n-butanol solution of tetrabutyl zirconate, according to the mass ratio of polycarbosilane to tetrabutyl zirconate Co-dissolve in xylene at 1:1, polycarbosilane / solvent (xylene and n-butanol) ratio is 1.3:1g / ml to prepare polycarbosilane / tetrabutyl zirconate solution, and disperse with ultrasound for 30 minutes;

[0034] (2) Electrospinning: Spinning conditions: the inner diameter of the needle is 1.2mm, the voltage is 25kV, the wire collection distance is 15cm, the feeding rate is 40μl / min, and the aluminum foil is collected to obtain polycarbosilane / tetrabutyl zirconate fibrils;

[0035] (3) Air pre-oxidation: put the above-mentioned fibrils in an oxidation furnace, raise the temperature at 25°C / h in an oxidative atmosphere, and keep it at 200°C for 1.5 hours, and cool to room temperature to obtain infusible polycarbosilane / zirconic acid tetrabutyl fiber;

[0036] (4) Hig...

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Abstract

The invention discloses a preparation method of superfine zirconia / silicon carbide composite fibers, which comprises the following steps: (1) preparing a polycarbosilane / tetrabutyl zirconate solution by taking polycarbosilane and tetrabutyl zirconate in a mass ratio of 1:1-11:1 and taking xylene as a solvent for carrying out electrostatic spinning; (2) putting protofibers in an oxidizing furnace,heating at 15-25 DEG C / h in an oxidizing atmosphere, insulating at 190-220 DEG C for 0.5-1.5 hours, and cooling to room temperature to obtain infusible polycarbosilane / tetrabutyl zirconate fibers; and (3) putting the infusible fibers into a highly pure argon protected high temperature furnace, heating to 1200-1450 DEG C, and insulating at the temperature for 1 hour to obtain the superfine zirconia / silicon carbide composite fibers with the diameter of 0.5-5 mu m. The composite fibers of the invention is composed of zirconia and silicon carbide and have small fiber diameter and large specific area; and electrostatic spinning is carried out at room temperature with mild condition and good spinning property.

Description

technical field [0001] The invention relates to a preparation method of ultrafine zirconia / silicon carbide composite fiber. Background technique [0002] The Si-Zr-C-O fiber represented by Tyranno ZM produced by Ube Industrial Co., Ltd. of Japan by the precursor conversion method, its precursor polyzirconium carbosilane is composed of Mark III polycarbosilane and zirconium acetylacetonate at 573K, N 2 prepared by reaction under protection; Acta Polymerica Sinica. 2008, (6): 621-625 published "Preparation and Characterization of Polyzirconium Carbosilane Ceramic Precursor" by Cao Shuwei, Xie Zhengfang, Wang Jun, Wang Hao. The liquid phase product polysilocarbosilane obtained by pyrolysis of base silane reacts with zirconium acetylacetonate to prepare the precursor polyzirconium carbosilane and finally obtain zirconium-containing silicon carbide fiber. This Si-Zr-C-O fiber has high strength, good flexibility, and excellent high temperature resistance; but the diameter of the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F9/08D01D1/02D01D5/00D01D10/02
Inventor 王应德郑德钏王浩蓝新艳王军
Owner NAT UNIV OF DEFENSE TECH
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