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Ultra-high temperature zrsi/zrc composite nanofiber and its preparation method

A composite nanofiber and ultra-high temperature technology, applied in fiber processing, fiber chemical characteristics, filament/wire forming, etc., can solve the problems of high raw material cost, coarse carbide particles, high energy consumption, etc., and achieve cheap raw materials and reduce Energy consumption and cost saving effects

Active Publication Date: 2021-05-04
INNER MONGOLIA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The cost of raw materials is high, the energy consumption is high, and the high reaction temperature leads to coarsening of carbide particles, making it difficult to obtain ultrafine carbide ceramic phases

Method used

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  • Ultra-high temperature zrsi/zrc composite nanofiber and its preparation method
  • Ultra-high temperature zrsi/zrc composite nanofiber and its preparation method
  • Ultra-high temperature zrsi/zrc composite nanofiber and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0031] 97wt% zirconium silicate powder and 3wt% carbon powder were mixed, press-molded, and sintered at 950° C. for 4 hours under an inert atmosphere such as nitrogen or argon to obtain a sintered product.

[0032] The sintered product is made into a cathode, graphite is used as an anode, and connected to a constant voltage power supply; CaCl with a mass ratio of 7:3 2 -NaCl mixed salt is used as a molten salt medium to form an electrolysis system.

[0033] Under an inert atmosphere, in a molten salt at 850° C., a 2.8V constant voltage was used for 20 hours to obtain an electrolysis product.

[0034] The electrolysis product was cleaned, followed by XRD, SEM, TEM and SAED detection.

[0035] Such as figure 1 As shown, the electrolysis product of this example is composed of ZrSi and ZrC.

[0036] Depend on figure 2 It can be seen that the electrolysis product in this example is mainly composed of nanofibers with uneven thickness, and the diameter of the fibers is about 100...

example 2

[0045] 94wt% zirconium silicate powder and 6wt% carbon powder were mixed, press-molded, and sintered at 1050° C. for 5 hours under an inert atmosphere such as nitrogen or argon to obtain a sintered product.

[0046] The sintered product is made into a cathode, graphite is used as an anode, and connected to a constant voltage power supply; CaCl with a mass ratio of 7:3 2 -NaCl mixed salt is used as a molten salt medium to form an electrolysis system.

[0047] Under an inert atmosphere, in a molten salt at 885° C., 2.82 V constant voltage was used for 20 h to obtain an electrolysis product. Subsequently, the electrolyzed product was washed several times with ethanol and deionized water to obtain the sample to be tested.

[0048] After testing, the sample to be tested is composed of zirconium silicide with a columnar core and tubular zirconium carbide coated on the zirconium silicide, and its fiber diameter is in the range of about 120-370 nm.

example 3

[0050] 95wt% zirconium silicate powder and 5wt% carbon powder were mixed, press-molded, and sintered at 9000° C. for 8 hours under an inert atmosphere such as nitrogen or argon to obtain a sintered product.

[0051] The sintered product is made into a cathode, graphite is used as an anode, and connected to a constant voltage power supply; CaCl with a mass ratio of 7:3 2 -NaCl mixed salt is used as a molten salt medium to form an electrolysis system.

[0052] Under an inert atmosphere, in a molten salt at 820° C., a constant voltage of 2.84 V was used for electrolysis for 19 hours to obtain an electrolysis product. Subsequently, the electrolyzed product was washed several times with ethanol and deionized water to obtain the sample to be tested.

[0053] After testing, the sample to be tested is composed of zirconium silicide with a columnar core and tubular zirconium carbide coated on the zirconium silicide, and the diameter of its fiber is in the range of about 110-360 nm.

...

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Abstract

The invention provides an ultra-high temperature ZrSi / ZrC composite nanofiber and a preparation method thereof. The method includes: mixing zirconium silicate powder and carbon powder, pressing and molding, and sintering under an inert atmosphere to obtain a sintered product; using the sintered product as a cathode and graphite as an anode, under an inert atmosphere, the In the molten salt, a constant voltage of 2.8-2.85V is used to electrolyze until the reaction is sufficient to obtain a nanocomposite fiber with a ZrSi core / ZrC coating. The present invention does not need to prepare zirconium carbide and high-melting silicide separately, and directly converts cheap ZrSiO 4 / Carbon powder mixture is used as a solid cathode, and ZrC / ZrSi composite fiber material is prepared by one-step electrochemical reduction, and electric deoxidation, alloying and carbonization are simultaneously realized during the electrolysis process; and it has short process, low cost, low energy consumption, and economic value High, conducive to the comprehensive utilization of silicate-type zirconium ore resources and other advantages.

Description

technical field [0001] The invention relates to the technical field of preparation of zirconium composite materials, in particular to a method capable of synthesizing a ZrC / ZrSi nanometer composite fiber material in situ by a molten salt electrochemical reduction method, and a ZrC / ZrSi nanometer composite fiber material. Background technique [0002] Zirconium carbide (ZrC) is considered to be the most potential ultra-high temperature structural material, solar thermoelectric receiver material and nuclear fuel cladding material. However, the high brittleness of ZrC ceramic materials leads to low fracture toughness and poor thermal shock resistance, and it is prone to damage during rapid temperature rise, causing catastrophic failure. And its low-temperature oxidation resistance is poor, and the sintering densification temperature is high. The refractory metal silicide has a high melting point (>2000°C), has good thermal stability, oxidation resistance and good mechanical...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F8/18D01D5/34
Inventor 刘红霞苏娟
Owner INNER MONGOLIA UNIV OF TECH