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A low-cost method for preparing molybdenum silicide without sulfur-containing gas emissions

A technology of gas emission and molybdenum silicide, applied in the direction of metal silicide, etc., can solve the problems of difficulty, environmental pollution, gas collection, etc., and achieve the effect of avoiding the roasting process, shortening the production process, and shortening the production process

Active Publication Date: 2022-04-15
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

SiS and SiS 2 The gas is difficult to collect, and after being released into the air, it will undergo hydrolysis reaction to form H 2 S gas causes environmental pollution, so it is difficult to be applied to the industrial preparation of MoSi 2

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] molybdenum concentrate (MoS 2 The mass fraction is 95%) and Si powder according to the actual MoS 2 The molar ratio of the content to Si is 1:2.33 and the ingredients are mixed uniformly and pressed into shape as an inner layer sample, and then the outer layer of the inner layer sample is covered (cover the inner layer sample with desulfurizer lime) with a layer of desulfurizer, the amount of desulfurizer lime Corresponding to MoS in molybdenum concentrate 2 The molar ratio to the CaO content in lime is 1:4, and react in an inert atmosphere at 1100°C for 0.5 hours. After cooling to room temperature, peel off the outer desulfurizer layer to obtain Mo 3 Si. Carry out XRD analysis to the sample of different positions of the exfoliated outer layer material, the result shows that the main phase of matter in the position of contact with the inner layer sample is CaS, which shows that the lime in the present invention can convert the sulfur element in the molybdenum concent...

Embodiment 2

[0025] Put molybdenum disulfide and high-purity Si powder into the actual MoS 2 The molar ratio of the content to C is 1:4, and the ingredients are mixed uniformly and pressed into the inner layer sample, and then a layer of desulfurization agent is coated on the outside of the inner layer sample. The amount of desulfurization agent lime corresponds to MoS2 in molybdenum disulfide 2 The molar ratio to the CaO content in lime is 1:3, and reacted in an inert atmosphere at 1200°C for 10 hours. After cooling to room temperature, peel off the outer desulfurizer layer to obtain pure MoSi 2 . In addition, XRD analysis was performed on the outer surface of the outer desulfurization layer, and only CaO was detected, which indicated that no sulfur-containing gas was emitted during the reaction.

Embodiment 3

[0027] molybdenum concentrate (MoS 2 The mass fraction is 95%) and Si powder according to the actual MoS 2 The molar ratio of the content to Si is 1:2.6 and the ingredients are mixed uniformly and pressed into the inner layer sample, and then a layer of desulfurization agent is coated on the outside of the inner layer sample. The amount of desulfurization agent lime corresponds to MoS in molybdenum concentrate 2 The molar ratio to the CaO content in lime is 1:4, and react in an inert atmosphere at 1300°C for 5 hours. After cooling to room temperature, peel off the outer desulfurizer layer to obtain Mo 5 Si 3 . In addition, XRD analysis was performed on the outer surface of the outer desulfurization layer, and only CaO was detected, which indicated that no sulfur-containing gas was emitted during the reaction.

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Abstract

The invention discloses a low-cost method for preparing molybdenum silicide without sulfur-containing gas emissions, directly using MoS 2 The material as the main component, such as molybdenum concentrate is the molybdenum source, the material with Si as the main component is used as the reducing agent, and lime is used as the sulfur fixing agent. Molybdenum silicide is prepared in the next step under high temperature and inert atmosphere conditions. During the reaction, MoS 2 The S in the desulfurization layer is all captured by the desulfurizer lime and stored in the external desulfurization layer in the form of CaS, and the desulfurization layer can be separated from the internal molybdenum silicide (MoSi 2 、Mo 5 Si 3 or Mo 3 Si). The present invention can directly use molybdenum concentrate as the molybdenum source, avoiding the roasting process of the molybdenum concentrate, and greatly shortening the production process of the molybdenum source; the present invention uses lime as the desulfurizer, which can avoid the use of molybdenum concentrate as the molybdenum source. The sulfur element is discharged into the atmosphere in the form of sulfur-containing gas. After the reaction is completed, the desulfurization layer and the inner layer product can be easily crushed and separated, which is suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to the field of material preparation and discloses a method for preparing a molybdenum silicide material. Background technique [0002] Silicon and molybdenum can generate Mo under different conditions 3 Si, Mo 5 Si 3 and MoSi 2 Three intermetallic compounds, currently only MoSi 2 Has a wide range of applications. MoSi 2 With anti-oxidation properties under high temperature conditions, it is mainly used as heating element and high temperature structural material of industrial furnaces. Compared to MoSi 2 , Mo 5 Si 3 and Mo 3 Si has a higher melting point and better high temperature creep resistance, but poor high temperature oxidation resistance. In addition, Mo 3 Si has the highest Mo content (about 91%) among the three compounds, Mo 5 Si 3 The Mo content of the two is 79.7%, and the Mo content of the two is higher than that of the conventional molybdenum additive ferromolybdenum, so it is expected to be used as a m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/06
CPCC01B33/06
Inventor 张国华常贺强
Owner UNIV OF SCI & TECH BEIJING
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