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Method for preparing crystalline transitional metal boride - cobalt boride

A technology of transition metals and borides, applied in chemical instruments and methods, cobalt compounds, inorganic chemistry, etc., to achieve the effects of simple process, abundant sources, and novel synthesis methods

Inactive Publication Date: 2012-05-09
NANKAI UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to overcome the deficiencies in the prior art and provide a new method for preparing crystalline transition metal boride CoB with simple process and no complicated steps such as high temperature and high pressure.

Method used

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  • Method for preparing crystalline transitional metal boride - cobalt boride
  • Method for preparing crystalline transitional metal boride - cobalt boride
  • Method for preparing crystalline transitional metal boride - cobalt boride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 1. Weigh 0.465 g Co(OH) 2 and 0.540 g KBH 4 , after mixing uniformly in a mortar, press into tablets under a pressure of 20 MPa;

[0022] 2. Keep the pressed sheet at 600°C for 12 h under the protection of argon, and then slowly cool it down to room temperature. The obtained product was fully washed with deionized water and ethanol, and vacuum-dried at 80°C for 12 h to obtain the product crystalline CoB.

[0023] figure 1 is the XRD pattern of the obtained material. Compared with the standard card, it can be seen that the synthesized material is an orthorhombic crystal system.

Embodiment 2

[0025] 1. Weigh 0.512 g Co 3 o 4 and 0.540 g KBH 4 , after mixing uniformly in a mortar, press into tablets under a pressure of 20 MPa;

[0026] 2. Keep the pressed sheet at 600°C for 12 h under the protection of argon, and then slowly cool it down to room temperature. The obtained product was fully washed with deionized water and ethanol, and vacuum-dried at 80°C for 12 h to obtain the product crystalline CoB.

[0027] figure 2 is the TEM image of the as-prepared crystalline CoB. It can be seen from the figure that the crystalline CoB is composed of nanospheres with a diameter of tens to hundreds of nm.

[0028] image 3 and Figure 4 It is the XPS pattern of the as-prepared crystalline CoB. It can be seen from the figure that Co and B exist in the form of CoB, indicating that the obtained CoB is of high purity.

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Abstract

The invention relates to a new method for preparing crystalline transitional metal boride CoB (cobalt boride) with oxide or hydroxide of cobalt and borohydride of cobalt through solid phase reaction. The method provided by the invention comprises the steps as follows: uniformly mixing oxide or hydroxide of cobalt and borohydride of cobalt according to the molar ratio of 1:1 to 1:1.5, tabletting under the pressure of 15 to 20 MPa, keeping the temperature of 400 to 800 DEG C for 6 to 24 hours under the protection of argon gas, and cooling to the ambient temperature slowly; and the obtained product is washed fully with deionized water and alcohol and then vacuum dried, thus the product CoB can be obtained. The method has the characteristics that the synthetic method is novel, the adopted process is simple, and pure crystalline CoB can be obtained without high temperature, high pressure or other complicated procedures; and the used raw materials are simple and easy to obtain, and the cost is low, so that the method is applicable to mass production.

Description

technical field [0001] The present invention relates to a method for preparing crystalline transition metal borides, and more particularly, to a method for preparing crystalline transition metal borides cobalt boride (CoB). Background technique [0002] Transition metal borides are often used as catalysts in hydrogenation reactions. Among them, Co-B has been widely studied and applied due to its good catalytic activity in electrocatalysis and hydrogenation of unsaturated groups. [0003] In addition to its application in catalysis, it has been found in recent years that Co-B has high discharge capacity and good cycle stability as an anode material for alkaline secondary batteries, which has attracted the interest of many researchers. However, previous studies have focused on the study of amorphous Co-B, and the synthesis of crystalline Co-B has not been realized. Therefore, finding a simple method for synthesizing crystalline Co-B has great scientific value and significanc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G51/00B01J23/75
Inventor 王一菁李丽王亚平宋大卫苏振馨蔡洪元焦丽芳袁华堂
Owner NANKAI UNIV
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