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A kind of high-purity ultrafine amorphous boron powder and preparation method thereof

An amorphous boron powder, high-purity technology, applied in the direction of boron, boron/boride, etc., can solve the problems of low purity of amorphous boron powder, low product purity, poor impurity removal effect, etc., and achieve good particle size control effect and high purity High, the effect of improving the purity

Active Publication Date: 2022-03-11
BEIJING MINING & METALLURGICAL TECH GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to overcome the defect of low purity of the amorphous boron powder prepared by the existing method and further improve the use effect of the amorphous boron powder, the invention provides a high-purity ultrafine amorphous boron powder and a preparation method thereof. Amorphous boron powder has the advantages of high purity, high porosity ratio and ultra-fine particle size
[0008] The inventors of the present invention found in the research process that the boron powder directly prepared by the self-propagating method has low purity, and at least there are problems in the following aspects: ① The reaction raw materials are mechanically mixed, and then subjected to high-temperature sintering reaction, and complete mixing cannot be achieved due to mechanical mixing The purpose of uniformity will lead to incomplete reaction, more impurities generated, and lower purity; ②The impurity removal stage of pickling and water washing generally adopts conventional pickling and water washing, and there are no other specific process control points to further improve the impurity removal effect. Less effective, resulting in less pure final product

Method used

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Effect test

preparation example Construction

[0032] In the first aspect, the present invention provides a method for preparing high-purity ultrafine amorphous boron powder, comprising: mixing a boron source and a reducing agent to obtain a mixture; and then making the mixture undergo a self-propagating reaction through a two-step heating method ; Then cooling and impurity removal;

[0033] Wherein, the process of the two-step heating method includes: under a protective atmosphere, the mixture is firstly preheated, kept warm, and then heated up to perform the self-propagating reaction; the temperature of the preheating is lower than the temperature of the self-propagating reaction .

[0034] The present invention adopts the above-mentioned two-step heating method, specifically, through the preheating to a temperature lower than the temperature at which the self-propagating reaction occurs, and heat preservation, so that before the self-propagating reaction occurs, the liquid boron source and reducing agent Interdiffusion...

Embodiment approach

[0046] According to a preferred embodiment of the present invention, the preparation method further includes: introducing calcium chloride into the mixing.

[0047] In the above-mentioned preferred embodiment, the calcium chloride is introduced during the mixing, so that the calcium chloride can be more evenly distributed around the boron source and the reducing agent, and when the self-propagating reaction is carried out, the temperature around the reaction substance rises sharply, Calcium chloride melts into a liquid state and evenly disperses on the surface of the material. After the reaction is completed and the temperature drops, the calcium chloride recondenses into a solid state and is evenly distributed with impurities generated during the reaction process (such as magnesium oxide, boron-magnesium-oxygen ternary compounds, etc.) Around the generated boron particles. In the subsequent pickling, the calcium chloride around the boron particles contacts with water, dissolv...

Embodiment 1

[0094] Boron oxide, magnesium powder, and calcium chloride are mixed for 1.5 hours by roller milling (the mass of the balls is 8 times the total mass of the reaction raw materials, and the rotation speed is 30Hz), and then put into the tray, and preheated to 680°C, heat preservation for 15 minutes, after the end of the heat preservation, continue to heat up to 780°C for self-propagating reaction. Among them, based on the total amount of boron oxide, magnesium powder and calcium chloride, the mass proportion of boron oxide is 70%, the mass proportion of magnesium powder is 20%, and the mass proportion of calcium chloride is 10%.

[0095] When the temperature does not continue to rise during the self-propagating reaction (the self-propagating reaction time is about 2 minutes), the sintered material obtained by the self-propagating reaction is directly pushed into the cooling zone and cooled by water in a nitrogen atmosphere (the temperature of the cooling water is 5°C ) and air ...

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Abstract

The invention belongs to the technical field of amorphous boron powder preparation, and in particular relates to a high-purity ultrafine amorphous boron powder and a preparation method thereof. The preparation method comprises: mixing a boron source and a reducing agent to obtain a mixture; and then heating in two steps method to make the mixture self-propagating reaction; then cooling and impurity removal; wherein, the process of the two-step heating method includes: under a protective atmosphere, the mixture is firstly preheated, kept warm, and then heated up for self-propagation reaction. Propagating reaction; the temperature of the preheating is lower than the temperature of the self-propagating reaction. The two-step heating method adopted in the present invention can make the liquid boron source and reducing agent more fully mixed through interdiffusion through preheating and heat preservation, the self-propagating reaction is more thorough, and the formation of impurity phases is significantly reduced. And in the preferred scheme of adding calcium chloride in the present invention, the purity of the prepared boron powder can be further improved, and at the same time, by controlling the cooling, the prepared boron powder has the characteristics of high purity, fine particle size, and large loose ratio.

Description

technical field [0001] The invention belongs to the technical field of preparation of amorphous boron powder, and in particular relates to a high-purity ultrafine amorphous boron powder and a preparation method thereof. Background technique [0002] Amorphous boron powder has high energy characteristics and is an important national strategic resource. It is mainly used in the fields of JG fuel, civil explosives and pyrotechnic product manufacturing, especially in rocket propellant fuel, propellant fuel, igniter and pyrotechnic products. A large number of applications in industrial products and other industries can greatly improve the energy level of my country's new fuels. In addition, this product can also be used as detonating agent for automobile airbags, high-temperature anti-oxidation coatings, synthetic boride raw materials, special alloy components, deoxidizers for oxygen-free copper smelting, steelmaking additives, welding aids and high-end ceramic sintering additives...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B35/02
CPCC01B35/023
Inventor 张鑫张思源王彦军阴荫冀国娟贾坤乐胡晓蕾
Owner BEIJING MINING & METALLURGICAL TECH GRP CO LTD
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