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Easy-to-sinter titanium and tungsten co-doped zirconium carbide powder and preparation method thereof

A zirconium carbide powder and co-doping technology, which is applied in the field of ultra-high temperature ceramics, can solve the problems that high-energy ball milling is not suitable for preparing a large number of powders, high oxygen content of zirconium carbide ceramic powder, complex metal impurity removal process, etc., to achieve oxygen content Low, low equipment requirements, small grain size effect

Pending Publication Date: 2020-10-02
SHANDONG ULSTREETCARING FINE CERAMICS +3
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  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Literature 5 (Ceram.Inter.41 (2015) 8397–8401) reported the mechanochemical method of ZrO 2 , C and metal Mg were mixed to prepare ZrC powder by high-energy ball milling for 30 hours. This method is complicated to remove metal impurities and high-energy ball milling is not suitable for preparing a large amount of powder.
Document 6 (J.Ceram.Soc.Japan 124(2016)1171–1174) reported the use of ZrOCl 2 .8H 2 O, C 2 h 8 o 7 .H 2 O, C 2 h 6 o 2 It is a method of synthesizing ZrC powder as raw material through high-temperature microwave heating. Although the size of the synthesized powder is 200-300nm smaller, the oxygen content is as high as 1at%, which is not conducive to high-temperature sintering
[0004] Comparative analysis found that the preparation method or process of the above zirconium carbide ceramic powder is complicated and not suitable for large-scale production, or the prepared zirconium carbide ceramic powder has high oxygen content and low sintering activity

Method used

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  • Easy-to-sinter titanium and tungsten co-doped zirconium carbide powder and preparation method thereof
  • Easy-to-sinter titanium and tungsten co-doped zirconium carbide powder and preparation method thereof
  • Easy-to-sinter titanium and tungsten co-doped zirconium carbide powder and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) the raw material ZrO 2 、TiO 2 and WO 3 Powder and carbon black according to ZrO 2 :TiO 2 :WO 3 : The molar ratio of carbon black=0.91:0.06:0.03:3.21 is weighed, then placed in the zirconia mixing tank, adding dehydrated alcohol, making the ball milling medium with zirconia balls, mixing 12h at 90r / min rotating speed;

[0034] (2) Put the uniformly mixed raw materials into a vacuum drying oven, and dry them at a constant temperature of 30°C for 24 hours;

[0035] (3) Dry press the dried raw material powder into a graphite crucible, heat it to 1450°C at a rate of 15°C / min in a vacuum graphite furnace, keep it warm for 3 hours, cool down to room temperature with the furnace, and grind the obtained powder X-ray diffraction analysis shows that it is pure titanium and tungsten co-doped zirconium carbide Zr 0.91 Ti 0.06 W 0.03 C solid solution powder, no impurity phase, such as figure 1 shown.

[0036] From figure 1 It can be seen that due to the small covalent ...

Embodiment 2

[0039] (1) the raw material ZrO 2 、TiO 2 and WO 3 Powder and carbon black according to ZrO 2 :TiO 2 :WO 3 : The molar ratio of carbon black=0.90:0.08:0.02:3.21 is weighed, then placed in the zirconia mixing tank, adding dehydrated alcohol, making the ball milling medium with zirconia balls, mixing 15h at 120r / min rotating speed;

[0040] (2) Put the homogeneously mixed raw materials into a vacuum drying oven, and dry at a constant temperature of 28°C for 36 hours;

[0041] (3) Dry press the dried raw material powder into a graphite crucible, heat it to 1580°C at a rate of 20°C / min in an argon graphite furnace, keep it warm for 1h, cool to room temperature with the furnace, and grind the obtained powder The body is pure titanium and tungsten co-doped zirconium carbide Zr 0.90 Ti 0.08 W 0.02 C solid solution powder, its scanning electron microscope picture is as follows figure 2 shown.

[0042] From figure 2 It can be seen that titanium and tungsten co-doped zirconi...

Embodiment 3

[0045] (1) the raw material ZrO 2 、TiO 2 and WO 3 Powder and carbon black according to ZrO 2 :TiO 2 :WO 3 : the molar ratio of carbon black=0.85:0.10:0.05:3.21 is weighed, then placed in the zirconia mixing tank, adding dehydrated alcohol, making the ball milling medium with zirconia balls, mixing 20h at 150r / min rotating speed;

[0046] (2) Put the homogeneously mixed raw materials into a vacuum drying oven, and dry at a constant temperature of 25°C for 36 hours;

[0047] (3) Dry press the dried raw material powder into a graphite crucible, heat it to 1500°C at a rate of 15°C / min in a vacuum graphite furnace, keep it warm for 2h, cool to room temperature with the furnace, crush and grind the obtained The powder is pure titanium and tungsten co-doped zirconium carbide Zr 0.85 Ti 0.10 W 0.05 C solid solution powder, the grain size is 200-400nm.

[0048] Codoping titanium and tungsten with zirconium carbide Zr 0.85 Ti 0.10 W 0.05 The C powder was dry-pressed at 80MPa...

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Abstract

The invention relates to the technical field of ultrahigh-temperature ceramics, in particular to easy-to-sinter titanium and tungsten co-doped zirconium carbide powder and a preparation method thereof. The chemical formula of the easy-to-sinter titanium and tungsten co-doped zirconium carbide powder is Zr<1-x-y>Ti<x>WyC, x is larger than 0 and smaller than or equal to 0.05, and y is larger than 0and smaller than or equal to 0.05. The preparation method comprises the following steps: subjecting ZrO2, TiO2, WO3 and carbon black which are adopted as raw materials to high-temperature carbon thermal reduction reaction under the protection of vacuum or argon to prepare the titanium and tungsten co-doped zirconium carbide powder. The titanium and tungsten co-doped zirconium carbide powder easy to sinter is small in grain size, low in oxygen content, high in phase purity, high in sintering activity and wide in application range, and can be used as a raw material for pressureless sintering ofa zirconium carbide body material, an ultrahigh-temperature heat-proof coating material, a solar absorbing material and a base material of an ultrahigh-temperature composite material. The invention also provides the preparation method which is low in raw material cost, simple in technological process, low in equipment requirement and suitable for large-scale production.

Description

technical field [0001] The invention relates to the technical field of ultra-high temperature ceramics, in particular to an easily sinterable titanium and tungsten co-doped zirconium carbide powder and a preparation method thereof. Background technique [0002] Zirconium carbide ceramics have excellent properties such as high melting point, high hardness, corrosion resistance, radiation resistance, ablation resistance, electrical conductivity, and thermal conductivity, and have broad application prospects in the fields of aerospace, aviation, and nuclear industries. Recent studies have shown that zirconium carbide ceramics have good stability in vacuum and argon, anti-volatility, and the characteristics of resistance changing with temperature are similar to those of metal W and Mo. They can be used as new electric heating elements for high vacuum furnace heating. However, the sintering of zirconium carbide ceramics is difficult, and usually requires high-temperature pressuri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/56C04B35/626C04B35/64
CPCC04B35/5622C04B35/6267C04B35/64C04B2235/3244C04B2235/3232C04B2235/424C04B2235/3258C04B2235/5436C04B2235/656C04B2235/668C04B2235/96C04B2235/781C04B2235/785
Inventor 吴事江林杨李拯杨焕顺张合军
Owner SHANDONG ULSTREETCARING FINE CERAMICS
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