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CN-121974309-A - High-purity nanoscale tungsten nitride powder and preparation method thereof

CN121974309ACN 121974309 ACN121974309 ACN 121974309ACN-121974309-A

Abstract

The invention provides high-purity nanoscale tungsten nitride powder and a preparation method thereof. The tungsten nitride is WN or W 2 N or a mixed phase of the WN and the W 2 N, the purity of the powder is more than or equal to 99.99 percent, and the particle size of the powder is 20-200nm. The preparation method comprises the following steps of taking tungsten as a raw material, firstly sintering the tungsten in a radio frequency furnace at 900-1200 ℃ for 3-10 hours, then pretreating the treated raw material in a box furnace, then sintering the pretreated powder in a rotary furnace at 550-700 ℃ for 5-10 hours in an NH 3 environment, cooling to room temperature, discharging the powder out of the furnace, and then performing planetary ball milling, crushing and sieving in an inert atmosphere to obtain the high-purity tungsten nitride powder. The tungsten nitride powder prepared by the method has the advantages of stable structure, high purity, simple preparation process, easy breaking, low operation cost and wide process window, and is suitable for large-scale industrial production. The prepared tungsten nitride can be widely used in the fields of catalysis, wear-resistant coatings, electronics, optics and the like.

Inventors

  • LIU XUEQIAN
  • LI XUANXUAN
  • YANG ZHIPING
  • YOU YONG
  • ZHAO JINXIN
  • LI XU
  • LI PANLAI
  • WANG DAWEI

Assignees

  • 河北利福光电技术有限公司

Dates

Publication Date
20260505
Application Date
20260306

Claims (9)

  1. 1. A high-purity nano-grade tungsten nitride powder is characterized in that the purity of the powder is more than or equal to 99.99 percent and the particle size is 20nm-200nm.
  2. 2. The high purity nanoscale tungsten nitride powder of claim 1, wherein the high purity nanoscale tungsten nitride is WN or W 2 N or a mixed phase of both.
  3. 3. The preparation method of the high-purity nanoscale tungsten nitride powder is characterized by comprising the following steps of: (1) Taking metal tungsten powder as a raw material, and firstly sintering in a radio frequency furnace at 900-1200 ℃; (2) Then pretreating the material obtained in the step (1) in a box-type furnace at 800-1000 ℃; (3) Sintering the pretreated powder in a rotary furnace at 550-700 ℃ in an NH 3 environment; (4) Finally, cooling to room temperature, discharging, and performing planetary ball milling, crushing and sieving under the protection of inert gas to obtain the high-purity nanoscale tungsten nitride powder.
  4. 4. The method for preparing high-purity nano-grade tungsten nitride powder according to claim 3, wherein the sintering condition in the radio frequency furnace is that the temperature is raised to 900-1200 ℃ at the temperature rising rate of 50-80 ℃ per minute, the temperature rising and heat preservation process is carried out under vacuum conditions, the flow rate of O 2 ,O 2 is 0.5-1.5L/min after heat preservation is carried out for 3-5h, the heat preservation time is 3-5h after the O 2 is carried out, and the condensed fine powder is obtained after the heat preservation is finished.
  5. 5. The method for preparing high purity nano tungsten nitride powder according to claim 3, wherein the pretreatment conditions in step (2) are that the temperature is raised to 800 ℃ to 1000 ℃ at a temperature rising rate of 10 ℃ to 15 ℃ per minute in a box furnace, sintering is carried out for 5 to 10 hours, air in the box furnace is discharged by N 2 during sintering, and sufficient carbon powder is placed around the box furnace.
  6. 6. The method for preparing high-purity nano-sized tungsten nitride powder according to claim 4, wherein the pretreated product of step (2) is WO 3 and/or W 18 O 49 .
  7. 7. The method for preparing high-purity nano-grade tungsten nitride powder according to claim 3, wherein the sintering process in step (3) is to heat up to 550-700 ℃ at a temperature rising rate of 5-10 ℃ per minute for 5-10 hours, NH 3 is introduced during sintering, the air flow is 1.5-2L per minute, the pressure is 0.3-0.5Mpa, and the rotating speed is controlled at 5-10rpm.
  8. 8. The method for preparing high purity nano-sized tungsten nitride powder according to claim 4, wherein the temperature is reduced at a rate of 20-30 ℃ per minute during the temperature reduction in step (1) and step (4).
  9. 9. The method for preparing high-purity nano-sized tungsten nitride powder according to claim 3, wherein the inert gas filled in the planetary ball milling process is nitrogen or argon.

Description

High-purity nanoscale tungsten nitride powder and preparation method thereof Technical Field The invention relates to the technical field of tungsten nitride and preparation thereof, in particular to high-purity nanoscale tungsten nitride powder and a preparation method thereof. Background Tungsten nitride is an inorganic compound composed of metal tungsten and nitrogen, has excellent mechanical properties and thermal stability, and can be widely applied to various technical fields such as catalysis field, wear-resistant coating field, electronic device, optical field and the like. As a novel catalytic material, the catalytic performance of the catalyst is superior to that of sulfide catalysts, and sulfur pollution caused by industrial catalysts can be avoided. Because of high hardness and excellent wear resistance, the wear-resistant coating can obviously improve the wear resistance of the material and prolong the service life. The material can be used for manufacturing semiconductor materials, optical films, optical filters and the like, and the excellent optical performance of the material makes the material have important significance in the preparation of optoelectronic devices. With the development of scientific technology, the application field of tungsten nitride is further expanded and deepened, and the purity requirement of each industrial field on tungsten nitride is higher and higher. In view of the current data, high purity tungsten nitride has no mature process, and has high requirements on raw materials, and still faces some technical and cost challenges in its preparation. The Chinese patent application CN 104743529A provides a method for preparing nano tungsten nitride, the method can obtain nitride powder with granularity of 30-120nm, the method adopts ammonium metatungstate, ammonium nitrate, auxiliary agent and ethylenediamine tetraacetic acid as raw materials, impurity C is easy to introduce into the product and is not easy to remove, and the produced product is unstable and has great spontaneous combustion risk. In the Chinese patent application CN 101786610A, tungstic acid and organic amine are adopted to prepare a tungstic acid-based inorganic-organic mixed lamellar compound precursor, and then the tungsten acid-based inorganic-organic mixed lamellar compound precursor is sintered under the ammonia gas condition to obtain nano tungsten nitride powder. Disclosure of Invention The invention aims to provide high-purity nanoscale tungsten nitride powder and a preparation method thereof, so as to solve the problem that the purity of a product is low due to the fact that impurities are easy to introduce in the preparation of tungsten nitride in the existing method. The invention is realized in the following way: A high-purity nano-class tungsten nitride powder with the purity more than or equal to 99.99% and granularity of 20-200 nm. Further, the high purity nanoscale tungsten nitride is WN or W 2 N or a mixed phase of the WN and the W 2 N. Further, the preparation method of the high-purity nanoscale tungsten nitride powder comprises the following steps: (1) Taking high-purity tungsten powder as a raw material, and firstly sintering the high-purity tungsten powder in a radio frequency furnace at 900-1200 ℃ for 3-10h; (2) Then pretreating the material obtained in the step (1) in a box-type furnace at 800-1000 ℃; (3) Sintering the pretreated powder in a rotary furnace at 550-700 ℃ in an NH 3 environment; (4) Finally, cooling to room temperature, discharging, and performing planetary ball milling, crushing and sieving under the protection of inert gas to obtain the high-purity nanoscale tungsten nitride powder. Further, the sintering condition of the step (1) in a radio frequency furnace is that the temperature is quickly increased to 900-1200 ℃ at the temperature increasing rate of 50-80 ℃ per minute, the heating and heat preservation process is carried out under vacuum condition, the flow of O 2,O2 is 0.5-1.5L/min after heat preservation for 3-5h, the heat preservation time is 3-5h, and the condensed fine powder is obtained after heat preservation is finished. Further, the pretreatment product in the step (2) is high-purity WO 3 or W 18O49 or a mixture of the two, the pretreatment conditions are that the temperature is raised to 800-1000 ℃ at the temperature rising rate of 10-15 ℃ per minute, the sintering is carried out for 5-10 hours, the air in the box-type furnace is discharged by N 2 during the sintering, and sufficient carbon powder is placed around the box-type furnace. Further, in the step (3), the sintering process is that the temperature is raised to 550-700 ℃ at the temperature rising rate of 5-10 ℃ per minute, the temperature is kept for 5-10 hours, NH 3 is introduced in the sintering process, the air flow is 1.5-2L per minute, the pressure is 0.3-0.5Mpa, and the rotating speed is controlled at 5-10rpm. Further, in the step (1) and the step (4), the temperature is rapidly reduce