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Preparation method of nano hafnium boride powder

A nano-boron and hafnium boride technology, applied in chemical instruments and methods, nanotechnology, inorganic chemistry, etc., can solve the problems of high production cost, difficult to balance purity and particle size, etc., and achieve short production cycle and good morphology characteristics. , the effect of uniform distribution

Active Publication Date: 2021-12-21
HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The technical problem to be solved by the present invention is to provide a method for preparing nano hafnium boride powder in order to overcome the disadvantages of the existing technology that the hafnium boride powder is difficult to balance the purity and particle size and the production cost is high

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  • Preparation method of nano hafnium boride powder
  • Preparation method of nano hafnium boride powder
  • Preparation method of nano hafnium boride powder

Examples

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Effect test

Embodiment 1

[0032] A method for preparing hafnium boride powder by coprecipitation, comprising the following steps:

[0033] Step S1, weigh 2.0g of boric acid and 3.5g of sorbitol, put them into the same beaker and mix them, then pour 10mL of acetic acid (analytical pure) into it, and use a magnetic stirrer to gradually heat up to 80°C under the condition of heating in an oil bath, Stir at constant temperature until boric acid and sorbitol are completely dissolved in acetic acid, and the solution is completely clear, thereby obtaining a clear mixed solution A and cooling to room temperature;

[0034] Step S2, measure 6mL of acetic acid (analytical grade) and pour it into a beaker, weigh 3.2g of hafnium chloride and slowly pour it into it with continuous stirring to obtain a light yellow transparent mixed solution B;

[0035] Step S3, under the continuous stirring state of the mixed solution A, slowly drop the mixed solution B into it at a rate of 1 mL / min at a constant speed, so as to obt...

Embodiment 2

[0039] A kind of co-precipitation method prepares the method for 100 grams level hafnium boride powder, comprises the following steps:

[0040] Step S1. Weigh 20g of boric acid and 35g of sorbitol, put them into the same beaker and mix them, then pour 100mL of acetic acid (analytical grade) into it, and use an oil bath magnetic stirrer to gradually raise the temperature to 80°C, and stir at a constant temperature until Boric acid and sorbitol are completely dissolved in acetic acid, and the solution is completely clear, thereby obtaining clear mixed solution A and cooling to room temperature;

[0041] Step S2, measure 80mL of acetic acid (analytical grade) and pour it into a beaker, weigh 32g of hafnium chloride and slowly pour it into it and keep stirring to obtain a light yellow transparent mixed solution B;

[0042] Step S3, under continuous stirring of the mixed solution A, slowly drop the mixed solution B into it at a rate of 5 mL / min at a constant speed, so as to obtain ...

Embodiment 3

[0046] A method for preparing hafnium boride powder by coprecipitation, comprising the following steps:

[0047] Step S1, weigh 2.0g boric acid and 3.8g sorbitol, put them into the same beaker and mix them, then pour 10mL acetic acid (analytical grade) into it, and use a magnetic stirrer to gradually heat up to 60°C under oil bath heating conditions, Stir at constant temperature until boric acid and sorbitol are completely dissolved in acetic acid, and the solution is completely clear, thereby obtaining a clear mixed solution A and cooling to room temperature;

[0048] Step S2, measure 8 mL of acetic acid (analytical pure) and pour it into a beaker, weigh 3.0 g of hafnium chloride and slowly pour it into it and continue stirring to obtain a light yellow transparent mixed solution B;

[0049] Step S3, under the continuous stirring state of the mixed solution A, slowly drop the mixed solution B into it at a rate of 1 mL / min at a constant speed, so as to obtain a white hafnium bo...

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Abstract

The invention belongs to the field of nano material preparation, and particularly relates to a novel method for preparing hafnium boride powder through a coprecipitation method. The specific process comprises the following steps: (1) dissolving HfCl4 in acetic acid to obtain a transparent solution A; dissolving boric acid and D-sorbitol in acetic acid, and stirring until the boric acid and the D-sorbitol are completely dissolved to obtain a transparent solution B; (2) after the solution B is cooled to room temperature, dropwise adding the solution A into the solution and stirring until white floccules are separated out and the solution becomes milk white; (3) drying an obtained sol; (4) fully grinding to obtain a white powdery hafnium boride precursor; and (5) calcining the hafnium boride precursor at a high temperature to obtain the nano hafnium boride powder. The preparation method is easy to operate, conditions are easy to control, and the production period is short; the prepared hafnium boride powder has nano-scale particle size and uniform distribution, and has good morphological characteristics, ultrahigh purity and high yield. And a technical basis is provided for realizing engineering and industrial preparation of high-performance, high-strength and ultrahigh-temperature ceramic materials.

Description

technical field [0001] The invention relates to the technical field of nanomaterial preparation, in particular to a method for preparing nano hafnium boride powder by a novel co-precipitation method. Background technique [0002] Hafnium diboride (HfB 2 ) has a hexagonal AlB 2 type layered structure, containing B atoms in two-dimensional graphitic rings, and alternately forming hexagonal densely packed Hf layers, strong Hf–B ionic bonds and B–B covalent bonds lead to an extremely high melting point of 3250 °C It is one of the best candidate materials for hypersonic vehicles, rocket propulsion systems, cutting tools, wear-resistant coatings, molten metal crucibles, plasma arc electrodes, and nuclear reactor neutron absorbers. . However, the particle size of the existing commercial boride powder is tens of microns, and the purity of the product is generally lower than 90wt% after testing, and there is basically a blank in the development of high-purity ultra-fine sub-micron...

Claims

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Application Information

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IPC IPC(8): C01B32/914B82Y40/00C04B35/56C04B35/626
CPCC01B32/914B82Y40/00C04B35/5622C04B35/62675C01P2004/62C01P2002/72C01P2002/85C01P2004/03C04B2235/3409C04B2235/444C04B2235/95
Inventor 王振黄竹林李昕扬胡晨光胡小晔李越
Owner HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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