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Superfine 10B-rich titanium diboride powder and preparation method thereof

The technology of titanium diboride and titanium dioxide is applied in the field of 10B-rich titanium diboride powder and its preparation, which can solve the problem of high cost of raw materials, and achieve the effects of stable product components, strong operability and fast synthesis speed.

Inactive Publication Date: 2015-09-30
LAIWU ADVANCED CERAMIC TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has simple process, uniform powder, and is suitable for large-scale production, but its essence is the physical pulverization of titanium diboride itself, and the cost of raw materials is relatively high

Method used

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  • Superfine 10B-rich titanium diboride powder and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] a super fine 10 The preparation method of B titanium diboride powder comprises steps as follows:

[0041] (1) will 10 B abundance 85% rich10 B boron carbide powder (average particle size 10-30μm) 25.5kg, anatase titanium dioxide (average particle size 20-40μm) 64kg, carbon black (average particle size 10-30μm) 10kg and calcium oxide (average particle size (10-20μm in diameter) 0.5kg is mixed in a dry color mixer for 40min;

[0042] (2) Transfer the dry mixed raw materials to a medium frequency induction sintering furnace, raise the temperature to 2000°C in an argon atmosphere, hold the temperature for 27 hours, and heat up at a rate of 10°C / min;

[0043] (3) The calcined product was wet-milled with a sand mill for 7 hours, filtered and dried for 15 hours to obtain titanium diboride powder with a particle size of 0.6 μm. The main crystal phase is TiB 2 phase, with a purity of 98%, 10 B abundance is 85%.

Embodiment 2

[0045] a super fine 10 The preparation method of B titanium diboride powder comprises steps as follows:

[0046] (1) will 10 B abundance 65% rich 10 B boron carbide powder (average particle size 10-30μm) 30kg, anatase titanium dioxide (average particle size 20-40μm) 64kg, carbon black (average particle size 10-30μm) 8kg and calcium oxide (average particle size 10-20μm) 0.5kg in a dry color mixer for 35min;

[0047] (2) Transfer the dry-mixed raw materials to an intermediate frequency induction sintering furnace, raise the temperature to 1850°C in an argon atmosphere, hold the temperature for 22 hours, and heat up at a rate of 8°C / min;

[0048] (3) The calcined product was wet ball-milled with a sand mill for 6 hours, filtered and dried for 10 hours to obtain titanium diboride powder with a particle size of 0.8 μm. The main crystal phase is TiB 2 phase, with a purity of 96%, 10 B abundance is 65%.

Embodiment 3

[0050] a super fine 10 The preparation method of B titanium diboride powder comprises steps as follows:

[0051] (1) will 10 B abundance 80% rich 10 B boron carbide powder (average particle size 10-30μm) 28kg, anatase titanium dioxide (average particle size 20-40μm) 64kg, carbon black (average particle size 10-30μm) 9kg and calcium oxide (average particle size 10-20μm) 0.5kg in the dry color mixer for 30min;

[0052] (2) Transfer the dry-mixed raw materials to an intermediate frequency induction sintering furnace, raise the temperature to 1950°C in an argon atmosphere, hold the temperature for 24 hours, and heat up at a rate of 10°C / min;

[0053] (3) The calcined product was wet-milled with a sand mill for 7 hours, filtered and dried for 20 hours to obtain titanium diboride powder with a particle size of 0.7 μm. The main crystal phase is TiB 2 phase, with a purity of 97%, 10 B abundance is 80%.

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Abstract

The invention relates to a superfine 10B-rich titanium diboride powder and a preparation method thereof. The powder is prepared by mixing, calcining, milling and drying the following raw materials in percentage by mass: 15-40 wt.% of 10B-rich boron carbide with the 10B abundance of 60-90%, 45-75 wt.% of titanium dioxide, 5-15 wt.% of carbon black and 0.2-1 wt.% of calcium oxide, totaling 100%. The preparation method comprises the following steps: dryly mixing the 10B-rich boron carbide, titanium dioxide, carbon black and calcium oxide for 30-60 minutes; heating to 1600-2200 DEG C in an argon atmosphere, keeping the temperature for 20-30 hours, and naturally cooling; carrying out wet-process ball milling for 5-7 hours, filtering the ball-milled slurry, and drying for 10-30 hours. The carbothermic method for synthesizing the 10B-rich titanium diboride powder does not need the gelation process, and has the advantages of simple technique, high synthesis speed and low production cost.

Description

technical field [0001] The present invention relates to a rich 10 B Titanium diboride powder and a preparation method thereof belong to the technical field of new materials. Background technique [0002] Neutron absorbing materials play a pivotal role in the development and application of nuclear power technology. The control rods, safety rods, regulating rods and shielding rods produced by them are important functional components in nuclear reactor core components next to fuel components. [0003] Element B has excellent neutron absorption, wide absorption energy spectrum, and weak secondary radiation of gamma rays, so it is widely used in the field of neutron absorption. At present, nuclear reactors mostly use boron, boron carbide and boron metal compounds as neutron absorbing materials. [0004] Boron has two isotopes, namely: 10 B and 11 b. 11 B does not have the ability to absorb neutrons, can absorb neutrons 10 B only accounts for about 19% in natural boron raw m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B35/04
Inventor 张玉军余锦程谭砂砾
Owner LAIWU ADVANCED CERAMIC TECH
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