Silicon disulfide and preparation method thereof

A silicon disulfide and silicon powder technology, applied in chemical instruments and methods, inorganic chemistry, silicon compounds, etc., can solve the problems of low powder phase purity and chemical purity, poor safety, complex equipment and procedures, etc.

Active Publication Date: 2022-05-27
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0032] The technical problem to be solved by the present invention is that the existing elemental silicon powder and elemental sulfur powder are synthesized to obtain SiS 2 The preparation cost of the powder is high, the safety is poor, the equipment and process are complex, and the phase purity and chemical purity of the powder are low, which cannot meet the important needs of basic research and applied research, especially related sulfide-based solid electrolytes

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  • Silicon disulfide and preparation method thereof
  • Silicon disulfide and preparation method thereof
  • Silicon disulfide and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] The present embodiment provides a preparation method of silicon disulfide, specifically:

[0075] S1) Weigh a certain amount of solar (or above) grade (>99.9999wt.%) silicon block, crush it with a tungsten steel or steel device, and pass it through a 20-mesh (<0.85mm) sieve to obtain coarse Si powder;

[0076] S2) place the coarse Si powder in a planetary ball mill to carry out wet ball milling, use a stainless steel tank as the ball milling tank, use tungsten carbide-cobalt (WC-Co) balls as the ball milling medium, use anhydrous ethanol as the ball milling liquid, and the ball milling speed is Revolve at 150rpm, rotate at 300rpm, and ball mill for 2h to obtain Si slurry;

[0077] S3) ultrasonically clean the Si slurry prepared in S2) with 10 wt.% hydrochloric acid (HCl) three times, each 10 min; ultrasonically clean it with 6 wt.% hydrofluoric acid (HF) three times, each 10 min; use ultrapure water (resistance rate 18MΩ·cm, impurities - And it is neutral; vacuum-dryin...

Embodiment 2

[0082] The present embodiment provides a preparation method of silicon disulfide, specifically:

[0083] In the second embodiment, except that the holding temperature in the fifth step is different from that of the first embodiment, the rest are the same as those of the first embodiment.

[0084] The 5th step of embodiment two is as follows:

[0085] Mix and grind high-purity silicon powder and high-purity sulfur powder at the ratio of Si:S=1:3.3 (mol%), protect and seal it in a vacuum (≤10Pa) quartz tube with argon gas, set an inclination angle of 20°, and set the inclination angle of 20°. The tube was placed in a high-temperature furnace, raised to 800°C at 5°C / min, kept for 3 hours, mainly for solid / gas two-phase chemical reaction synthesis, then cooled to room temperature at 5°C / min, passed through a 200-mesh (<74μm) sieve, A rod-shaped silicon disulfide powder was obtained.

[0086] ICP tested, SiS 2 The impurity content is 3174ppm (mg / L), and the K / Na content is extre...

Embodiment 3

[0088] The present embodiment provides a preparation method of silicon disulfide, specifically:

[0089] In Example 3, except for the addition of the last step (surface treatment and modification of benzene to silicon disulfide), the rest are the same as in Example 1.

[0090] The last step of embodiment three is as follows:

[0091] The synthesized product was surface-treated and modified with benzene (≥99.5 wt.%), filtered, vacuum-dried at 80° C. for 5 h, and passed through a 200-mesh (2 The impurity content is 3227ppm (mg / L), and the impurity content without K / Na is 2141ppm (mg / L).

[0092] XRD test ( figure 1 ) showed that the polycrystalline particles had high phase purity and were preferentially aligned perpendicular to the (101) / (002) / (112) crystal planes; SEM tests ( figure 2 ) show that the rod-shaped particles have an aspect ratio of 2-7 and a size distribution of L9-35 × D3-10 μm.

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Abstract

The invention discloses silicon disulfide and a preparation method thereof, and the preparation method comprises the following steps: taking silicon powder and powdered sulfur in a molar ratio of 1: (3.0-4.0) as reaction raw materials, converting sulfur in the reaction raw materials into sulfur steam at the temperature of 725-825 DEG C, and calcining for more than 2 hours under the condition that the pressure of the sulfur steam is 2.2-3.2 MPa. According to the method, the raw materials are economical and safe, the preparation process is simple, the preparation time is short, the process stability is high, and the obtained SiS2 powder has a controllable rod-shaped microstructure and high phase purity and chemical purity, so that the method has a very strong industrial application prospect.

Description

technical field [0001] The invention relates to a silicon disulfide and a preparation method thereof, and belongs to the field of silicon disulfide material preparation. Background technique [0002] Silicon Disulfide (SiS 2 ) is an important artificial compound for basic and applied research, and one of the important raw materials for sulfide-based solid electrolytes. 2 S is toxic gas, the existing preparation technology and process are complicated, and the yield is low, which leads to its high price, which greatly hinders the research and development progress in related fields. [0003] SiS 2 There are five kinds of homogeneous polycrystals, of which the most stable phase (normal temperature and normal pressure phase) is the NP phase of the orthorhombic system, which is synthesized under normal pressure or low pressure (1-32 atmospheres, 390-1500 ° C), and another Four metastable high-pressure phases are HP1 and HP2 phases of monoclinic system, HP3 phase of tetragonal c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/00
CPCC01B33/00C01P2002/72C01P2004/03C01P2004/10C01P2004/61C01P2006/80Y02E60/10
Inventor 邵刚勤谢梦祥张继伟吴厚燃王炎培王文豪
Owner WUHAN UNIV OF TECH
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