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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

Inactive Publication Date: 2002-11-20
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

to VS 2 for the precursor at 725°C and NH 3 Heating in airflow for 12 hours can produce 0.5μm VN with a purity of about 96%, but VS 2 Precursors are not readily available
Apply VCl 4 with NH 3 and H 2 By gas phase reaction, VN with a particle size of 1.0-500nm, uniform particle size distribution, and an oxygen content of less than 100ppm can be obtained, but the production efficiency of the gas phase reaction is low, and the gaseous hydrogen chloride produced by the reaction severely corrodes the equipment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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%.

[...

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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Abstract

The preparation method of vanadium nitride nano powder body includes the following steps: using industrial-grade V2O5 to make reduction reaction to prepare VOCl2 solution, making said solution react with (NH4)2CO3 or NH4HCO3 to synthesize vanadyl (IV) basic ammonium carbonate precursor, in the atmosphere of NH3 and under the moderate condition making the above-mentioned precursor undergo the processes of ammonization and nitrogenation so as to obtain the invented vanadium nitride nano powder body whose grain size is 20nm-1 micrometer, distribution of particle size is uniform and vanadium nitride content is greater than 98%.

Description

technical field [0001] The invention relates to a preparation method of vanadium nitride (VN) nanometer powder. Background technique [0002] Vanadium nitride has a high melting point (2350°C), high hardness (Mohs hardness is 9-10), has very high thermal and chemical stability and strong mechanical properties, and is widely used in engineering technology. Vanadium nitride is widely used in extremely hard cutting tools, abrasives and structural materials. The coating made of vanadium nitride has extremely high hardness, which can greatly improve the surface performance of the workpiece. It not only has higher hardness and better wear resistance, but also has the characteristics of heat resistance, corrosion resistance and fatigue resistance. The coating made of fine vanadium nitride powder can also improve the toughness of the material surface. Vanadium Nitride is a conductor and an essential component of many magnetic and electronic compone...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/06
Inventor 郑臣谋雷德铭
Owner SUN YAT SEN UNIV
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