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
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[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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