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Preparation method of ZrB2 powder with uniform and controllable 10B abundance

A powder and uniform technology, applied in the field of ZrB2 powder preparation, can solve the problems of poor abundance stability, uneven distribution of B abundance, and inability to meet the requirements, so as to reduce the content of impurity elements and achieve stable and controllable high uniformity. Effect

Pending Publication Date: 2020-12-11
有研资源环境技术研究院(北京)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the complexity of B isotope chemistry, the 10 B-enriched ZrB 2 powder, powdery 10 B abundance stability is poor, 10 B abundance is unevenly distributed
As shown in Table 1, 10 batches of ZrB prepared by carbothermal reduction reaction 2 Powder, 10 The range of B abundance value was 5.23, and the standard deviation was 1.84, indicating that ZrB prepared in different batches 2 Powder 10 The abundance stability of B is poor, and it cannot meet the needs of nuclear reactors for 10 B-enriched ZrB 2 Material usage requirements

Method used

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  • Preparation method of ZrB2 powder with uniform and controllable 10B abundance
  • Preparation method of ZrB2 powder with uniform and controllable 10B abundance
  • Preparation method of ZrB2 powder with uniform and controllable 10B abundance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1: 10 ZrB with B abundance 10wt.% 2 Powder preparation

[0026] Prepared by carbothermal reduction 10 B abundance ZrB 2 Powder 20kg, ZrB 2 Powder Theory 10 The abundance value of B is 10wt.%, the powder is sampled at 10 points 10 B abundance, the results are shown in Table 3, 10 The maximum deviation of B abundance is 1.36wt.%; use a mixed solution of 1mol / L hydrochloric acid plus 1mol / L nitric acid to treat the above-mentioned ZrB 2 The powder is pickled, wherein the ratio of hydrochloric acid to nitric acid is 3:1 by volume; the powder after pickling is mixed with a high-speed mixer, the mixer speed is 1500r / min, and the mixing time is 10min. 10 ZrB with uniform abundance 2 Powder, powder purity > 99.9% (as shown in Table 2), 10 B abundance deviation <0.4wt.% (as shown in Table 3).

[0027] Table 2 Example 1 related ZrB 2 Analysis results of powder purity

[0028] Impurity elements Content / ppm Impurity elements Content / ppm Impurit...

Embodiment 2

[0031] Example 2: 10 ZrB with B abundance of 30wt.% 2 Powder preparation

[0032] Prepared by sol-gel method 10 ZrB with B abundance of 18.5wt.% 2 Powder 5kg, prepared by carbothermal reduction method 10 ZrB with a B abundance of 55wt.% 2 The powder is 20kg, and the powder is sampled and tested at 10 points respectively. 10 B abundance, the results are shown in table 5; Utilize the mixed solution of 3mol / L hydrochloric acid to add 1mol / L nitric acid to the above two kinds of ZrB 2 The powder is pickled, wherein the ratio of hydrochloric acid to nitric acid is 1:1 by volume; the powder after pickling is mixed by a three-dimensional motion mixer, the spindle speed of the mixer is 25r / min, and the time is 30min to obtain two kinds of 10 ZrB with highly uniform B abundance distribution 2 powder, powdery 10 B abundance deviation values ​​are all10 ZrB with a B abundance of 55wt.% 2 Powder 6.3kg, 10ZrB with B abundance of 18.5wt.% 2 13.7kg of powder was mixed by a high-sp...

Embodiment 3

[0037] Example 3: 10 ZrB with B abundance 50wt.% 2 Powder preparation

[0038] prepared by carbothermal reduction 10 ZrB with B abundance of 95wt.%, 20wt.% and 60wt.% 2 Each powder is 20kg; the prepared powder is pickled with a mixed solution of 3mol / L hydrochloric acid and 1mol / L hydrogen peroxide, wherein the ratio of hydrochloric acid to hydrogen peroxide is 5:1 by volume; The motion mixer is mixed, the spindle speed of the mixer is 20r / min, and the time is 60min, and 3 kinds of 10 ZrB with highly uniform B abundance distribution 2 powder, powdery 10 B abundance deviations are all 10 ZrB with B abundance of 95wt.% 2 Powder 5.714kg, 10 ZrB with B abundance of 20wt.% 2 Powder 10kg, 10 ZrB with a B abundance of 60wt.% 2 Powder 4.286kg, adopt high-speed mixer to mix, mixer speed 1300r / min, mixing time 60min, get 10 ZrB with B abundance 50wt.% 2 Powder 20kg, powder purity > 99.9%, 10 B abundance deviation <0.3wt.%.

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Abstract

The invention discloses a preparation method of ZrB2 powder with uniform and controllable 10B abundance, and belongs to the technical field of boride powder preparation. The method comprises the following steps: (1) preparing ZrB2 powder with different 10B abundance; (2) carrying out purification treatment on the ZrB2 powder with different 10B abundance degrees through acid pickling; (3) carryingout 10B abundance uniformity control mixing on the ZrB2 powder with different 10B abundance by adopting a strong mixing method to obtain ZrB2 powder with highly uniform 10B abundance distribution; and(4) preparing and mixing the ZrB2 powder with different 10B abundance obtained in the step (3) to obtain the ZrB2 powder with the target 10B abundance. According to the invention, the method is simple in process, ZrB2 powder which is stable and controllable in 10B abundance, good in uniformity and high in purity can be obtained, the purity of the powder is larger than 99.9%, the 10B abundance value is controllable in a range of 10 wt.% to 99 wt.%, and the 10B abundance deviation value is smaller than 0.5 wt.%.

Description

technical field [0001] The present invention relates to a 10 ZrB with uniform and controllable B abundance 2 The preparation method of powder belongs to the technical field of boride powder preparation. Background technique [0002] ZrB 2 Ceramics are widely used in the fields of high-temperature structural ceramic materials, composite materials, refractory materials, electrode materials, and nuclear energy materials because of their high melting point, high hardness, and good electrical and thermal conductivity. When ZrB 2 B in 10 When B-enriched form exists, it has excellent neutron absorption capacity, making 10 B-enriched ZrB 2 Fuel elements are used in nuclear reactors. [0003] ZrB 2 There are many methods for the preparation of powders, including direct synthesis, self-propagating high-temperature synthesis, sol-gel method, and carbon thermal reduction method. However, due to the complexity of B isotope chemistry, the 10 B-enriched ZrB 2 powder, powdery 10...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/58C04B35/626
CPCC04B35/58078C04B35/62605
Inventor 王星明杨磊刘宇阳白雪彭程桂涛石志霞孙静
Owner 有研资源环境技术研究院(北京)有限公司
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