Preparation method of transition metal carbide material
A transition metal and carbide technology, applied in the field of preparation of transition metal carbide powder, coating, fiber and nanotubes, can solve the problems of high preparation cost, high conversion temperature, difficult purification, etc., and achieve controllable form and raw materials The effect of low cost and low synthesis temperature
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[0023] The invention relates to a preparation method of a transition metal carbide material. The process is to place the carbon material in the crucible, and cover the alkali metal or alkaline earth metal chloride, fluoride, nitrate, sulfate or transition metal fluorate material as an auxiliary agent without mixing or mixing with the transition metal material. On the carbon material in the crucible, under the condition of argon atmosphere or isolated air, heat the crucible at a heating rate of 0.1-30°C / min to 600°C-1300°C, keep it warm for 0.1-200 hours, and then cool it to room temperature; After the salt crucible is boiled in water, the insoluble transition metal carbide or the transition metal carbide supported on the carbon material is taken out, washed with water and dried. In essence, the present invention uses different molten salts as auxiliary media to prepare related transition metal carbide (VC, ZrC, NbC, MoC, HfC, TaC, WC) powders, coatings, fibers and new techniqu...
Embodiment 1
[0026] The preparation of embodiment 1 TaC coating
[0027] (1) Cover the carbon block in the crucible after the auxiliary agent is mixed with transition metal material tantalum powder, the carbon block, auxiliary agent, and tantalum powder are respectively 1-20wt%, 50-85wt%, 1-35wt%; Sodium chloride and potassium fluorotantalate are 50-60wt% and 40-50wt% of their consumption respectively;
[0028] (2) Heating to 1100-1300°C at a heating rate of 0.5-5°C / min under an argon atmosphere, maintaining the temperature for 0.1-0.5 hours, and then cooling down to room temperature;
[0029] (3) Boil the molten salt crucible in water, dissolve and remove the metal salt therein, and take out the insoluble carbon block coated with tantalum carbide. Further desalination is carried out by washing with water, and after drying, a tantalum carbide coating with a thickness of 1-10 μm is formed on the surface of the carbon block.
Embodiment 2
[0030] The preparation of embodiment 2 ZrC fiber
[0031] (1) Cover the carbon fiber in the crucible after the auxiliary agent is mixed with transition metal material zirconium powder, the carbon fiber, auxiliary agent, and zirconium powder are respectively 10-25wt%, 40-75wt%, 5-35wt%; Agent sodium chloride, sodium sulfate are respectively 80~90wt%, 10~20wt% of its consumption;
[0032] (2) Heating to 700-900°C at a heating rate of 10-15°C / min under an argon atmosphere, maintaining the temperature for 180-200 hours, and then cooling down to room temperature;
[0033] (3) Boil the molten salt crucible in water, dissolve and remove the metal salt therein, and take out the insoluble carbon fiber coated with zirconium carbide. It is further desalted by water washing and dried.
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