Method for preparing ultrafine high-purity refractory metal powder

A technology for refractory metals and ultrafine powders, applied in the field of preparation of ultrafine high-purity refractory metal powders, which can solve the problems of large specific surface area, high cost, and high melting point of refractory metals for ultrafine powders, so as to improve the powder yield , less environmental pollution, and the effect of avoiding reactions

Pending Publication Date: 2021-06-25
宁夏德运创润钛业有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation of high-purity ultra-fine powders of refractory metals is still basically at the level of theoretical research and laboratory-scale pilot tests.
The reason is that refractory metals have high melting points and high hardness, and general physical methods (such as mechanical ball milling, jet mill pulverization, plasma rotating electrode method, physical vapor deposition method, atomization method, sputtering method) are difficult to Prepare powders with purity and particle size that meet the requirements at the same time; while con

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0034] Example 1

[0035] S1: Weigh 100g analysis pure NBCL 5 The evaporation container was heated to 200 ° C to make the vapor pressure of 0.35 atm;

[0036] S2: NBCL will be generated 5 The steam introduction temperature is 1000 ° C reactor, and the purity of 99.99% is used as NBCl during the introduction. 5 Vapor carrier adjustment NBCL 5 The flow rate of the vapor is 4 × 10 -4 Mol / min, hydrogen having a purity of 99.99% is introduced into the reactor by a separate line, and the hydrogen flow is 5 × 10. -2 Mol / min, and import NBCL 5 The pipe and hydrogen are preheated to 600 ° C to give the ultrafine powder and HCl of the metal Nb, introduced into NBCL. 5 The cross-sectional area of ​​the outlet end of the vapor is reduced, making NBCL 5 The flow rate is increased when the vapor enters the reactor and is mixed with hydrogen;

[0037] S3: In the reactor tail, the reaction by-product HCl gas discharges the reactor with the exhaust gas, using a 1% NaOH solution to absorb the e...

Example Embodiment

[0042] Example 2

[0043] S1: Weigh 100g analysis pure NBCL 5 The evaporation container was heated to 200 ° C, and the saturated vapor pressure was 0.35 atm.

[0044] S2: NBCL will be generated 5 The steam introduction temperature is 1000 ° C reactor, and the purity of 99.99% is used as NBCl during the introduction. 5 Vapor carrier adjustment NBCL 5 The flow rate of the vapor is 4 × 10 -4 Mol / min, hydrogen having a purity of 99.99% is introduced into the reactor by a separate line, and the hydrogen flow is 5 × 10. -2 Mol / min, and import NBCL 5 The pipe and hydrogen are preheated to 600 ° C to give the ultrafine powder of the metal Nb and the HCl gas;

[0045] S3: In the reactor tail, the reaction by-product HCl gas discharges the reactor with the exhaust gas, using a 1% NaOH solution to absorb the exhaust gas, and the metal powder is left in the reactor tail by the barrier of the filter, and the reactor is vacuumed to 5 Pa, and Heat until 1000 ° C for 4 h, then cooled to room ...

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PUM

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Abstract

The invention provides a method for preparing ultrafine high-purity refractory metal powder, and belongs to the technical field of metallurgy and material preparation. The method comprises the following steps: heating and evaporating refractory metal halide in an evaporation container to enable the vapor pressure to reach 0.1-1 atm; conveying the refractory metal halide steam and high-purity hydrogen into a reactor to be subjected to homogeneous phase reduction reaction, and obtaining superfine powder of refractory metal and reaction tail gas; separating reaction tail gas, collecting the refractory metal ultrafine powder, and carrying out vacuum heat treatment on the refractory metal ultrafine powder; carrying out surface passivation treatment on the refractory metal superfine powder treated in the third step; and finally taking out the metal powder product.

Description

technical field [0001] The invention relates to a method for preparing metal powder, in particular to a method for preparing ultrafine high-purity refractory metal powder. Background technique [0002] Refractory metals generally refer to metals with a melting point higher than 1650°C and have certain reserves in the earth's crust, mainly including: tungsten (W), molybdenum (Mo), vanadium (V), titanium (Ti), tantalum (Ta), niobium ( Nb), zirconium (Zr), hafnium (Hf), chromium (Cr), etc. Refractory metal materials have extremely high application prospects in aerospace, microelectronic devices, biomedicine, intelligent manufacturing and other fields. However, these high-tech applications have extremely strict requirements on refractory metal materials, such as extreme service conditions, high purity greater than 99.9%, and controllable microstructure. my country is very rich in refractory metal resources. The reserves of titanium, molybdenum and tungsten are among the top in...

Claims

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Application Information

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IPC IPC(8): B22F9/28B22F1/00
CPCB22F9/28B22F2301/20B22F1/142B22F1/145
Inventor 朱骏焦树强朱鸿民罗乙娲刘勇
Owner 宁夏德运创润钛业有限公司
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