A kind of preparation method of pure phase metal silicide

A metal silicide, pure-phase technology, applied in the direction of metal silicide, etc., can solve the problem of difficulty in the target silicide product, and achieve the effect of flexible and convenient method, mild synthesis conditions, and lower reaction enthalpy

Active Publication Date: 2021-07-20
合肥动量守恒绿色能源有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although there are some methods that can prepare silicides under relatively mild conditions, they are only applicable to individual metal elements and crystal phase structures
Moreover, since many silicides have only slight stoichiometric differences between the different crystalline phases, it is particularly difficult to synthesize phase-pure target silicide products

Method used

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  • A kind of preparation method of pure phase metal silicide
  • A kind of preparation method of pure phase metal silicide
  • A kind of preparation method of pure phase metal silicide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Preparation of RuSi. RuCl 3 (103.8mg, 0.5mmol), Si powder (14.0mg, 0.5mmol) and Mg powder (29.2mg, 1.2mmol) were fully ground and mixed under the irradiation of an infrared lamp, and then transferred to a quartz tube. The quartz tube that raw material mixture is housed is connected with vacuum pumping device, when vacuum degree is drawn to less than 1Pa, seal this quartz tube ( figure 1 ). The sealed quartz tube was calcined at 700° C. for 4 h with a heating rate of 3° C. / min. After the quartz tube was cooled to room temperature, the obtained black powder was dissolved in 0.5mol / L H 2 SO 4 Soak in the solution for 1h to remove the by-product MgCl 2 and excess Mg powder. After three times of centrifugal cleaning with water and ethanol, put it in a vacuum drying oven and dry it at 50°C. After drying, a RuSi sample with a mass of about 60 mg can be obtained.

[0025] Some structural and morphological studies were carried out on the samples prepared by the above meth...

Embodiment 2

[0027] Preparation of IrSi. IrCl 3 (149.3mg, 0.5mmol), Si powder (14.0mg, 0.5mmol) and Mg powder (18.2mg, 0.75mmol) were fully ground and mixed under the irradiation of an infrared lamp, and then transferred to a quartz tube. Connect the quartz tube containing the raw material mixture to a vacuum device, and seal the quartz tube when the vacuum is lower than 1 Pa. The sealed quartz tube was calcined at 800° C. for 4 h with a heating rate of 3° C. / min. After the quartz tube was cooled to room temperature, the obtained black powder was dissolved in 0.5mol / L H 2 SO 4 Soak in the solution for 1h to remove the by-product MgCl 2 . After three times of centrifugal cleaning with water and ethanol, put it in a vacuum drying oven and dry it at 50°C. After drying, an IrSi sample with a mass of about 110 mg is obtained. The XRD pattern of this sample is shown in figure 2 .

Embodiment 3

[0029] Preparation of PtSi. PtCl 4(168.4mg, 0.5mmol), Si powder (14.0mg, 0.5mmol) and Mg powder (24.3mg, 1.0mmol) were fully ground and mixed under the irradiation of an infrared lamp, and then transferred to a quartz tube. Connect the quartz tube containing the raw material mixture to a vacuum device, and seal the quartz tube when the vacuum is lower than 1Pa. The sealed quartz tube was calcined at 800° C. for 4 h with a heating rate of 3° C. / min. After the quartz tube was cooled to room temperature, the obtained black powder was dissolved in 0.5mol / L H 2 SO 4 Soak in the solution for 1h to remove the by-product MgCl 2 . After three times of centrifugal cleaning with water and ethanol, put it in a vacuum drying oven and dry it at 50°C. After drying, a PtSi sample with a mass of about 110 mg is obtained. The XRD pattern of this sample is shown in figure 2 .

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Abstract

The invention discloses a method for preparing a pure-phase metal silicide, which belongs to the field of inorganic chemistry. The present invention utilizes the magnesium thermal reduction reaction of metal chloride, silicon powder and magnesium powder as raw materials to synthesize metal silicides of different phases, including TiS i2 , ZrSi 2 、VSi 2 , NbSi 2 、TaSi 2 、CrSi 2 、MoSi 2 、WSi 2 、FeSi 2 、CoSi 2 、NiSi 2 , PtSi, IrSi, RuSi and Pd 2 Si et al. Compared with the traditional single-substance reaction pathway, this method significantly reduces the reaction enthalpy, and the synthesis conditions are relatively mild. The side reaction product MgCl of this method 2 Easy to clean, easy to obtain pure phase; short synthesis cycle, good repeatability, easy to mass production.

Description

technical field [0001] The invention belongs to the field of inorganic chemistry, and in particular relates to a simple and universal preparation method of a pure-phase metal silicide. Background technique [0002] Silicide refers to the intermetallic compound formed by metal and silicon, which has an ordered crystal structure and a definite stoichiometric ratio, and is a huge family of compounds. They usually have excellent chemical stability and high-temperature thermal stability, corrosion resistance, and good electrical conductivity, and have been widely studied in electric heating elements, high-temperature anti-oxidation layers, integrated circuits, and electrode anti-corrosion layers. In recent years, metal silicides have demonstrated important performance in the fields of catalysis and energy storage, showing a very broad application prospect. For example, TiSi 2 As a photocatalyst for water splitting hydrogen production (Angew.Chem.Int.Ed., 2007, vol. 46, page 777...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/06
CPCC01B33/06C01P2002/72C01P2004/03C01P2004/04C01P2004/62
Inventor 邹晓新陈辉刘旺
Owner 合肥动量守恒绿色能源有限公司
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