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Superfine zirconium carbide ceramic fiber and preparation method thereof

A technology of ceramic fiber and zirconium carbide, which is applied in the field of ultrafine zirconium carbide ceramic fiber and its preparation, and achieves the effects of adjustable rheology, convenient operation and maintaining fiber morphology

Active Publication Date: 2017-10-20
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The purpose of the present invention is to overcome the deficiencies of the prior art. By optimizing the zirconium source precursor and introducing a new type of carbon source allyl phenolic, the problem of compatibility and stability of each component in the prior art is solved, and the production of ceramics is improved. Rate

Method used

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  • Superfine zirconium carbide ceramic fiber and preparation method thereof
  • Superfine zirconium carbide ceramic fiber and preparation method thereof
  • Superfine zirconium carbide ceramic fiber and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0047] (1) At 25°C, 5.85g of allylphenolic (AN) with an allylation degree of 80%, 50g of yttrium-containing polyzirconium (PNZ-Y), and a molar ratio of yttrium to zirconium of 2 : 25, zirconium element is 11.70g, polyvinylpyrrolidone (PVP) 3.34g is dissolved in ethylene glycol monoethyl ether (EE), stirs until forming brown transparent homogeneous solution, adjusts viscosity to 442mPa s, obtains zirconium carbide ceramic precursor Spinning solution (PNZ-Y-AN-2), wherein the mass ratio of each component Zr:AN:PVP=3.5:1.75:1, the resulting precursor spinning solution placed at 25°C for one month has a viscosity of 463mPa·s.

[0048] (2) At a temperature of 25°C and a humidity of 49%, the rotating speed of the centrifuge is 2000r / min, and the aperture of the spinning machine is 0.4mm, and the spinning liquid is thrown out at a high speed from the spinning hole to obtain the precursor fiber and the fiber macro photo as figure 1 As shown, the precursor fiber was placed in a tube ...

Embodiment 2

[0052] (1) At 25°C, 4.68g of allylphenolic (AN) with a degree of allylation of 85%, 50g of yttrium-containing polyzirconium (PNZ-Y), and a molar ratio of yttrium to zirconium of 3 : 100, the zirconium element is 11.70g, polyvinyl acetate (PVAc) 3.90g is dissolved in ethylene glycol monomethyl ether, stirs until forming brown transparent homogeneous solution, adjusts viscosity to 405mPa s, obtains zirconium carbide ceramic precursor spinning Silk liquid (PNZ-Y-AN-2.5), wherein the mass ratio of each component Zr:AN:PVAc=3:1.2:1, the resulting precursor spinning liquid has a viscosity of 430mPa after being placed at 25°C for one month ·s.

[0053] (2) Under the conditions of a temperature of 15°C and a humidity of 49%, the rotating speed of the centrifuge is 3000r / min, and the aperture of the spinning machine is 0.1mm. The body fiber is placed in a tube furnace, the temperature is raised at 1°C / min, and the temperature is kept at 140°C for 0.5h, at 160°C for 1h, at 180°C for 1h...

Embodiment 3

[0056] (1) At 25°C, 3.90g of allylphenolic (AN) with a degree of allylation of 90%, 50g of yttrium-containing polyzirconium (PNZ-Y), and a molar ratio of yttrium to zirconium of 1 :20, the zirconium element is 11.70g, polyvinyl butyral (PVC) 3.90g is dissolved in a mixed solvent of n-propanol and ethylene glycol monoethyl ether, the volume ratio is 1:1, stir until a brown transparent uniform solution is formed, adjust Viscosity to 365mPa·s, obtain zirconium carbide ceramic precursor spinning solution (PNZ-Y-AN-3), wherein the mass ratio of each component Zr:AN:PVP=3:1:1, the precursor spinning that will obtain The viscosity of the silk liquid is 380mPa·s after being placed at 25°C for one month.

[0057] (2) At a temperature of 30°C and a humidity of 49%, the rotating speed of the centrifuge is 8000r / min, and the aperture of the spinning machine is 0.5mm. The body fiber is placed in a tube furnace, the temperature is raised at 1°C / min, and the temperature is kept at 140°C for...

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Abstract

The invention provides a superfine zirconium carbide ceramic fiber. The fiber adopts yttrium-containing PNZ as a zirconium source and adopts allyl phenolic aldehyde as a carbon source, and a structural formula of allyl phenolic aldehyde is represented as a formula (I). The invention further provides a preparation method of the superfine zirconium carbide ceramic fiber. Yttrium-containing PNZ is adopted as the zirconium source, allyl phenolic aldehyde is adopted as the carbon source, the components have better compatibility and stability, and elements reach molecular-level and are uniformly distributed; a prepared zirconium carbide precursor thread-throwing solution has adjustable rheological property, is good in spinning property and can be stored in a sealed manner at the room temperature for 1 month or longer. A centrifugal thread throwing method is adopted, equipment is simple, operation is convenient, cost is low, the superfine fiber with the diameter smaller than 3 mu m can be obtained, and up-scale production can be realized rapidly.

Description

technical field [0001] The invention belongs to the field of ultra-high temperature resistant ceramic fibers, and in particular relates to an ultrafine zirconium carbide ceramic fiber and a preparation method thereof. Background technique [0002] With the advancement of science and technology, the next generation of spacecraft represented by near-space vehicles is developing in the direction of long endurance, hypersonic flight in the atmosphere and reusability, and there is an urgent need for new anti-oxidation structural materials. Ultra-high temperature ceramics and their composites have excellent ultra-high temperature oxidation resistance, and are the most promising material systems. [0003] The development of ultra-high temperature ceramic matrix composites is inseparable from high-performance reinforcing fibers. Carbon fiber has the advantages of high strength and high temperature resistance, but limited by the nature of carbon materials, it starts to oxidize at 45...

Claims

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Application Information

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IPC IPC(8): C04B35/56C04B35/622
CPCC04B35/5622C04B35/62277
Inventor 潘飞韩伟健邱文丰叶丽孙娅楠赵彤
Owner INST OF CHEM CHINESE ACAD OF SCI
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