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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 conventional chemical methods (such as sol-gel method, hydrothermal method, microemulsion method, chemical co-precipitation method, chemical vapor deposition method, electrolysis method) are not suitable for refractory metals. For high-purity ultra-fine powder, it is either difficult to obtain high-purity powder, or the cost is high
In addition, due to the large specific surface area and high activity of ultrafine powder, the lack of low-cost powder product surface passivation treatment technology suitable for industrial production is also one of the obstacles

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] S1: Weigh 100g of analytically pure NbCl 5 , heated to 200°C in the evaporation container to make its vapor pressure 0.35atm;

[0036] S2: NbCl to be produced 5 The steam is introduced into a reactor with a temperature of 1000°C, and argon with a purity of 99.99% is used as NbCl during the introduction process 5 Vapor carrier, adjusted NbCl 5 The steam flow rate is 4×10 -4 mol / min, hydrogen with a purity of 99.99% is introduced into the reactor through a separate pipeline, and the hydrogen flow rate is adjusted to 5×10 -2 mol / min, and for the introduction of NbCl 5 The pipeline of steam and hydrogen is preheated to 600°C to obtain ultrafine powder of metal Nb and HCl, and introduce NbCl 5 The cross-sectional area of ​​the outlet end of the steam pipeline is reduced, so that the NbCl 5 When the steam enters the reactor, the flow rate increases and is fully mixed with hydrogen;

[0037] S3: At the tail of the reactor, the reaction by-product HCl gas is discharged o...

Embodiment 2

[0043] S1: Weigh 100g of analytically pure NbCl 5 , heated to 200°C in the evaporator to make its saturated vapor pressure 0.35atm.

[0044] S2: NbCl to be produced 5 The steam is introduced into a reactor with a temperature of 1000°C, and argon with a purity of 99.99% is used as NbCl during the introduction process 5 Vapor carrier, adjusted NbCl 5 The steam flow rate is 4×10 -4 mol / min, hydrogen with a purity of 99.99% is introduced into the reactor through a separate pipeline, and the hydrogen flow rate is adjusted to 5×10 -2 mol / min, and for the introduction of NbCl 5 The steam and hydrogen pipelines are preheated to 600°C to obtain ultrafine powder of metal Nb and HCl gas;

[0045] S3: At the tail of the reactor, the reaction by-product HCl gas is discharged out of the reactor along with the tail gas, and the tail gas is absorbed with 1% NaOH solution, and the metal powder stays at the tail of the reactor through the barrier of the filter screen, and the reactor is ev...

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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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