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Preparation method of transition metal nano-boride

A nano-boride, transition metal technology, applied in the direction of metal borides, boron/borides, nanotechnology, etc., can solve the problem of inability to obtain crystalline or amorphous particles with nanostructures, and achieve high practical value, The effect of reducing process conditions and mild reaction conditions

Inactive Publication Date: 2013-05-15
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The present invention aims at the disadvantages of relatively harsh reaction conditions in the prior art, such as inability to obtain crystalline or amorphous particles with a nanostructure, and provides a new type of transition metal nanoparticle with mild reaction conditions, simple and reliable operation, and the ability to generate nanoparticles. The preparation method of boride

Method used

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  • Preparation method of transition metal nano-boride

Examples

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Effect test

Embodiment 1

[0029] Preparation of nanocrystalline NbB 2 .

[0030] The raw material used is: anhydrous NbCl 5 (purity 98%), LiBH 4 (purity 98%), LiH (purity 95%), anhydrous LiCl (purity greater than 99%), tetrahydrofuran (purity greater than 99%), metal Na (purity greater than 98%).

[0031] Molar ratio NbCl 5 : LiBH 4 : LiH = 1 : 2 : 3, weigh NbCl in glove box 5 , LiBH 4 and LiH. Weigh anhydrous LiCl, whose mass is 8 times the total mass of the above three samples. NbCl to be weighed 5 Grind evenly with anhydrous LiCl, then weigh the LiBH 4 and LiH into NbCl 5 And LiCl mixture, further grinding evenly. The above uniformly ground sample was transferred into a ball mill jar, the ball-to-material ratio was 40:1, and the speed was set at 400 rpm for ball milling, and the ball milling was performed for 20 h to fully proceed the reaction. The reaction product was collected, washed with tetrahydrofuran, centrifuged, and repeated 4-5 times in order to ensure that all LiCl in the sa...

Embodiment 2

[0034] Preparation of Nano ZrB 2 .

[0035] The raw material used is: anhydrous ZrCl 4 (purity 98%), NaBH 4 (purity 98%), NaH (purity 95%), anhydrous NaCl (purity greater than 99%), glycerin (purity greater than 99%), ethanol (purity greater than 99%).

[0036] Molar ratio of ZrCl 4 : NaBH 4 : NaH = 1 : 2 : 2, weigh ZrCl in the glove box4 , NaBH 4 and NaH. Weigh anhydrous NaCl, its mass is 6 times of the total mass of the above three samples. ZrCl to be weighed 4 Grind evenly with anhydrous NaCl, then weigh the NaBH 4 and NaH into ZrCl 4 And NaCl mixture, further grinding evenly. The uniformly ground sample was transferred into a ball mill jar with a ball-to-material ratio of 30:1, and the ball milling speed was set at 380 rpm for ball milling, and the ball milling was carried out for 25 h to fully proceed the reaction. The reaction product is collected, washed alternately with glycerol and alcohol, centrifuged, and repeated 4-5 times in order to ensure that all N...

Embodiment 3

[0039] Preparation of nano-TiB 2 .

[0040] The raw material used is: TiCl 4 (purity 98%), LiBH 4 (purity 98%), LiH (purity 95%), anhydrous LiCl (purity greater than 99%), tetrahydrofuran (purity greater than 99%), metal Na (purity greater than 98%).

[0041] Molar ratio TiCl 4 : LiBH 4 : LiH = 1 : 2 : 3, weigh TiCl in the glove box 4 , LiBH 4 and LiH. Weigh anhydrous LiCl, whose mass is 8.5 times the total mass of the above three samples. LiBH to be weighed 4 Grind with LiH and anhydrous LiCl evenly, then transfer the above-mentioned uniformly ground sample into a ball mill jar, and add the weighed TiCl drop by drop 4 . The ball-to-material ratio was 40:1, and the set speed was 350 rpm for ball milling, and the ball milling was carried out for 30 h to fully proceed the reaction. The reaction product was collected, washed with tetrahydrofuran, centrifuged, and repeated 4-5 times in order to ensure that all LiCl in the sample was dissolved by tetrahydrofuran. Prio...

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Abstract

The invention relates to the technical field of material synthesis and discloses a preparation method of a transition metal nano-boride. The preparation method comprises the following specific steps of: mixing a transition metal halide with a reducing agent I and a reducing agent II in a protective atmosphere of inert gas; placing an obtained mixture into a ball milling tank, and performing ball milling in the protective atmosphere of the inert gas; and removing the metal halide in a product of ball milling to get the transition metal nano-boride. The preparation method disclosed by the invention has the advantages of overcoming the shortcomings of high energy consumption, complex process and the like of the traditional preparation method, realizing mild reaction conditions and short reaction period, being capable of generating the product with a nano-structure, enabling the purity of the reaction product to be high and simultaneously precisely controlling the particle size of the product.

Description

technical field [0001] The invention relates to the technical field of material synthesis, in particular to a preparation method of transition metal nano borides. Background technique [0002] In transition metal borides, transition metals and non-metallic boron are covalently bonded, but at the same time have partial metal bond properties. The special bond valence and atomic combination provide a wide range of uses for transition metal borides. For example, niobium boride can be used as a wear-resistant material, cerium boride can be used as a thermoelectric material, lanthanum boride has been widely used in cathode components in electron microscopes and energy spectrometers, and titanium boride can be used in various hydrogen storage materials catalyst. At present, the methods for producing transition metal borides in industry mainly include boron thermal reduction method, carbothermal reduction method, pure element chemical synthesis method and molten salt electrolysis m...

Claims

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Application Information

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IPC IPC(8): C01B35/04B82Y30/00
Inventor 陈立新范修林肖学章邵杰张刘挺
Owner ZHEJIANG UNIV
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