Preparation method of vanadium nitride nano powder body
A technology of vanadium nitride nano and vanadium nitride, which is applied in the field of preparation of vanadium nitride nano powder, can solve the problems of difficult access to precursors, low production efficiency of gas phase reaction, corrosion of equipment by gaseous hydrogen chloride, etc., and achieve continuous production The effect of modernization, low equipment requirements, and environmental friendliness
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Embodiment 1
[0018] Weigh 91g V 2 o 5 , add about 100mL distilled water to adjust slurry, add 38g H 2 C 2 o 4 2H 2 O, heat, add 140~160mL concentrated hydrochloric acid in portions under stirring, boil slightly for a few minutes, then add N 2 h 4 ·H 2 O turns the solution dark blue. with a small amount of V 2 o 5 or N 2 h 4 2HCl adjusted to the solution can not detect VO 2 + and V 3+ ion. If necessary, filter out the insoluble matter, and then dilute to 500mL.
[0019] Weigh 14~16g(NH 4 )HCO 3 or 8.5~10g(NH 4 ) 2 CO 3 , add a small amount of distilled water, pass CO 2 or N 2 Or Ar gas drives oxygen. Then add 28-30mL of the above VOCl dropwise under stirring 2 solution. Let it stand for 0.5-2 hours, or it can be placed overnight under the isolation of air. Suction filtration, with a small amount of (NH 4 )HCO 3 The crystal is washed with the solution, and then washed with a small amount of ethanol to obtain 8.0-9.5 g of the precursor, with a yield of 80-95%.
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Embodiment 2
[0022] In Example 1, the precursor was ultrasonically crushed in absolute ethanol to a particle size ≤ 2 μm, and then directly heated to 850°C in a quartz boat and kept for 12 hours, and the quartz tube was pulled out and cooled to room temperature in an ammonia flow , the particle size is about 25nm, and the particle size distribution is uniform. The vanadium nitride content of the powder is higher than 97%, and the nitriding time is prolonged, and the vanadium nitride content can be as high as 98%.
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