Unlock instant, AI-driven research and patent intelligence for your innovation.

Preparation method of superfine zirconium oxide/silicon carbide fiber with radial and gradient distribution

A technology of ultra-fine zirconia and radial gradient, applied in fiber treatment, fiber chemical characteristics, spinning solution preparation, etc., can solve the problems of large fiber diameter, spinnability constraints, difficult control of distillation process, etc., and achieve specific surface area Large, easy to prepare, good spinnability

Active Publication Date: 2011-08-31
NAT UNIV OF DEFENSE TECH
View PDF4 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This fiber has the advantages of high strength, high temperature resistance, and high oxidation resistance; however, the diameter of the fiber prepared by this melt spinning method is still large, especially the radial gradient distribution of zirconia / silicon carbide prepared by melt spinning Fibers need to prepare polycarbosilane / tetrabutyl zirconate precursors, whose spinnability is restricted by factors such as tetrabutyl zirconate content and its dispersibility
In addition, since polycarbosilane (softening point: 200-220°C) is solid at room temperature and tetrabutyl zirconate (boiling point: 310°C) is liquid at room temperature, it is difficult to control the distillation process when preparing precursors

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of superfine zirconium oxide/silicon carbide fiber with radial and gradient distribution
  • Preparation method of superfine zirconium oxide/silicon carbide fiber with radial and gradient distribution
  • Preparation method of superfine zirconium oxide/silicon carbide fiber with radial and gradient distribution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (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 4 : 1 co-dissolve in xylene, prepare polycarbosilane / tetrabutyl zirconate solution according to the ratio of polycarbosilane and solvent (xylene and n-butanol) at 1.1:1 g / ml, and disperse by ultrasonic for 30 minutes;

[0021] (2) Electrospinning: The spinning conditions are: the inner diameter of the needle is 0.8mm, the voltage is 15kV, the distance of the wire is 20cm, the feeding rate is 20μl / min, and the wire is collected by aluminum foil to obtain polycarbosilane / tetrabutyl zirconate Ester fibrils;

[0022] (3) Maturation heat treatment: put the above-mentioned fibrils in an oven and keep them warm at 80°C for 120 hours under the air to obtain polycarbosilane / tetrabutyl zirconate matured fibers;

[0023] (4) Air pre-oxidation: put the above-mentioned matu...

Embodiment 2

[0032] (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-dissolved in xylene, prepared polycarbosilane / tetrabutyl zirconate solution according to the ratio of polycarbosilane and solvent (xylene and n-butanol) at 1.3:1g / ml, and dispersed it by ultrasonic for 30 minutes;

[0033] (2) Electrospinning: The spinning conditions are: the inner diameter of the needle is 1.2mm, the voltage is 20kV, the distance of the wire is 15cm, the feeding rate is 30μl / min, and the aluminum foil is collected to obtain polycarbosilane / tetrabutyl zirconate fiber;

[0034] (3) Maturation heat treatment: put the above-mentioned fibrils in an oven and keep them warm at 80°C for 120 hours under the air to obtain polycarbosilane / tetrabutyl zirconate matured fibers;

[0035] (4) Air pre-oxidation: put the above-mentioned mature fiber in ...

Embodiment 3

[0038] (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 1.5 : 1 co-dissolved in xylene, according to polycarbosilane and solvent (xylene and n-butanol) ratio of 1.1: 1g / ml preparation polycarbosilane / tetrabutyl zirconate solution, and ultrasonically dispersed for 30 minutes;

[0039] (2) Electrospinning: The spinning conditions are: the inner diameter of the needle is 0.8mm, the voltage is 25kV, the distance of the wire is 25cm, the feeding rate is 40μl / min, and the aluminum foil is collected to obtain the polycarbosilane / tetrabutyl zirconate fibrils ;

[0040] (3) Maturation heat treatment: put the above-mentioned fibrils in an oven, and heat them at 120°C under air for 80 hours to obtain polycarbosilane / tetrabutyl zirconate matured fibers;

[0041] (4) Air pre-oxidation: put the above-mentioned mature fiber in an ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
softening pointaaaaaaaaaa
softening pointaaaaaaaaaa
quality scoreaaaaaaaaaa
Login to View More

Abstract

The invention discloses a preparation method of superfine zirconium oxide / silicon carbide fiber with the radial and gradient distribution. The method comprises the following steps: using polycarbosilane and tetrabutyl zirconate, which weight ratio is 1:1-9:1 and solvent xylene to prepare a polycarbosilane / tetrabutyl zirconate solution, performing electrostatic spinning to prepare polycarbosilane / tetrabutyl zirconate protofiber; placing the protofiber in an oven, maintaining the temperature to 80-120 DEG C for 120-30 hours in the air to obtain polycarbosilane / tetrabutyl zirconate cured fiber; performing air pre-oxidation to the cured fiber, and firing at a high temperature to obtain the superfine zirconium oxide / silicon carbide fiber with the radial and gradient distribution finally. The method of the invention uses silicon carbide as matrix and zirconium oxide as the surface layer, the content of zirconium oxide is lowered along the radial direction, the product of the invention has small diameter and large specific area; and electrostatic spinning is performed at the room temperature, the preparation conditions are mild and the spinnability of the fiber is good.

Description

technical field [0001] The invention relates to a preparation method of superfine zirconia / silicon carbide radial gradient distribution fibers. Background technique [0002] T. Ishikawa, H. Yamaoka, Y. Harada, T. Fujii and T. Nagasawa. A general process for in situ formation of functional surface layers on ceramics[J]. Nature, 2002, 416: 64-67. Precursor in situ transformation method, using polycarbosilane as raw material, synthesized precursor with low molecular additive tetrabutyl zirconate, and then made continuous polycarbosilane / tetrabutyl zirconate fiber through melt spinning, the fiber The non-melting fiber is obtained by placing it in the air for non-melting treatment, and the non-melting fiber is placed in a high-temperature furnace under the protection of an inert atmosphere for high-temperature firing to obtain a radial gradient distribution fiber of zirconia / silicon carbide. This fiber has the advantages of high strength, high temperature resistance, and high ox...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): D01D1/02D01F9/10D01D10/00D01D10/02D01D5/00D01F1/10
Inventor 王应德郑德钏王浩蓝新艳王军
Owner NAT UNIV OF DEFENSE TECH