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Method for preparing fine niobium powder through calcium thermal reduction of niobium chloride in calcium chloride molten salt

A technology of calcium chloride molten salt and niobium chloride, applied in the field of calcithermal reduction of niobium chloride to prepare fine niobium powder, which can solve the problems of high energy consumption, low current efficiency, uneven particle size distribution, etc.

Inactive Publication Date: 2021-10-15
ANHUI UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Electrochemical reduction methods include EMR method (electrochemically mediated molten salt calcithermal reduction reaction), OS method (combination reaction of calcithermal reduction and electrolysis) and FFC method (electrolytic metal oxide cathode reaction), the prepared Nb powder particles Large diameter and uneven particle size distribution, low current efficiency and high energy consumption

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  • Method for preparing fine niobium powder through calcium thermal reduction of niobium chloride in calcium chloride molten salt
  • Method for preparing fine niobium powder through calcium thermal reduction of niobium chloride in calcium chloride molten salt

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Embodiment 1

[0023] A method for preparing fine niobium powder by calcithermal reduction of niobium chloride in calcium chloride molten salt, carried out according to the following steps:

[0024] S1. Vacuumize and dehydrate anhydrous calcium chloride in an atmosphere furnace. The vacuum dehydration temperature is 500° C., and the dehydration time is 12 hours; then add metallic calcium, and the mass ratio of added metallic calcium to anhydrous calcium chloride is 1. :50, raise the atmosphere furnace to the specified reaction temperature of 900°C and stir with argon gas to promote the dissolution of calcium metal in the molten calcium chloride salt. At the same time, the calcium metal in the molten calcium chloride salt is saturated before the calcium metal reacts. state;

[0025] S2, and then use argon gas to pass the evaporated niobium pentachloride gas into the calcium chloride molten salt that dissolves metallic calcium, so that a calcithermal reaction occurs to obtain a reduction produ...

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Abstract

The invention discloses a method for preparing fine niobium powder through calcium thermal reduction of niobium chloride in calcium chloride molten salt. The method for preparing the fine niobium powder through calcium thermal reduction of the niobium chloride in the calcium chloride molten salt comprises the following steps of: introducing niobium pentachloride gas into calcium chloride molten salt dissolved with metal calcium by adopting argon, leaching a reaction product by adopting diluted hydrochloric acid after the reaction is finished, washing with deionized water and absolute ethyl alcohol, and finally, performing vacuum drying to obtain fine niobium powder. The method for preparing the fine niobium powder through calcium thermal reduction of the niobium chloride in the calcium chloride molten salt has the advantages that the niobium powder prepared through the method is high in purity, the particle size is small, the sphericity degree is good, the preparation process can be carried out continuously, and the method can be popularized to preparation of other fine metal powder.

Description

technical field [0001] The invention relates to the technical field of preparation of functional metal powder materials, in particular to a method for preparing fine niobium powder by calcithermal reduction of niobium chloride in calcium chloride molten salt. Background technique [0002] Tantalum anodes for high-performance capacitors are made from high-purity fine tantalum (Ta) powder. However, due to limited resources in the earth's crust, tantalum is expensive. Niobium (Nb) has similar physical and chemical properties to tantalum, is abundant in reserves, and its price is 1 / 20 of that of tantalum. Therefore, the development of niobium capacitors is of great significance. Since the capacitance is proportional to the surface area of ​​the anode, it has been reported that the specific surface area of ​​the anode is greater than 5.0 m 2 / g (equivalent to an average anode particle size of less than 70 nm) with a high capacitance of over 0.2 FV / g for Ta capacitors. Therefo...

Claims

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Application Information

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IPC IPC(8): B22F9/28
CPCB22F9/28
Inventor 杜超潘育松潘成岭黄润
Owner ANHUI UNIV OF SCI & TECH
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