Metal sulfide single crystal material and preparation method

A technology of metal sulfides and single crystal materials, which is applied in the growth of polycrystalline materials, chemical instruments and methods, and single crystal growth, etc. The effect of improving reaction kinetics

Active Publication Date: 2010-08-04
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method can obtain the target product, the use of high pressure and organic solvents not only increases the risk but also increases the difficulty of operation.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Example 1: Cobalt sulfide CoS 2 preparation of

[0016] Weigh the sulfur powder and cobalt powder according to the molar ratio S: Co=5:1, put them into a sealed ceramic ball mill jar, use ceramic balls with a diameter of 10mm and 20mm, and a quantity ratio of 1:1. 1. Under an argon atmosphere, perform ball milling; ball mill at room temperature at a speed of 400 rpm for 10 hours; place the powder obtained after ball milling in a tube furnace, and roast at 200°C for 48 hours in an argon atmosphere , and then roasted at 380°C for 10 hours; the process of ball milling and roasting was repeated 6 times to obtain the product CoS 2 .

[0017] The obtained product was detected by XRD, and the spectrum showed that the product was pure phase CoS 2 ; After high-resolution transmission electron microscopy (HRTEM) detection, the photo shows that the material has a single crystal structure, and the particle diameter is about 20nm; after EDS detection, the energy spectrum shows th...

Embodiment 2

[0018] Example 2: Indium sulfide In 2 S 3 preparation of

[0019] Weigh the sulfur powder and indium powder according to the molar ratio S:In=8:1, put them into a sealed polyurethane ball mill jar, use polyurethane grinding balls with a diameter of 10mm and 20mm, and a quantity ratio of 1:1. 1. Under an argon atmosphere, perform ball milling. The ball mill was ball milled at room temperature at a speed of 200 rpm for 10 hours. The powder obtained after ball milling was placed in a tube furnace, and calcined at 130°C for 12 hours in a mixed atmosphere of argon and air, and then calcined at 300°C for 5 hours. Repeat the ball milling and roasting process twice to get the product In 2 S 3 . The detection results of XRD, HRTEM, EDS and thermogravimetric curve of this material are similar to embodiment 1, and the material after secondary firing has single crystal structure, and the product In of gained 2 S 3 It is still a single crystal structure with a particle size of abou...

Embodiment 3

[0020] Example 3: Tin Sulfide SnS 2 preparation of

[0021] Weigh the sulfur powder and tin powder according to the molar ratio S:Sn=7:1, put them into a sealed polyurethane ball mill jar, use polyurethane grinding balls with a diameter of 10mm and 20mm, and a quantity ratio of 1:1. 1. Under an argon atmosphere, perform ball milling. The ball mill was ball milled at room temperature at a speed of 200 rpm for 5 hours. The powder obtained after ball milling was placed in a tube furnace, and calcined at 130° C. for 12 hours in an argon atmosphere, and then calcined at 450° C. for 5 hours. Repeat the ball milling and roasting process 4 times to get the product SnS 2 . The detection results of XRD, HRTEM, EDS and thermogravimetric curve of this material are similar to embodiment 1, and the material after second firing has single crystal structure, and the product SnS of gained 2 It is still a single crystal structure with a particle size of about 25nm.

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Abstract

A metal sulfide single crystal material comprises metal element M and sulfur element S; the chemical formula thereof is MSx, wherein x is not more than 3 and not less than 1, the metal elements are In, Sn, Sb, Ti, V, Mo, Mn, Co, Cu or Zn; the material is prepared with a method in combination with high energy ball milling method and high temperature solid phase method, comprising the following steps: mixing the sulfur powder with metal powder, and placing in a ball mill tank to carry out ball milling in argon atmosphere; thermostatically baking at low temperature and high temperature for a long time in the argon atmosphere and mixed atmosphere of argon atmosphere and air; cooling, and repeating the steps of 2-6. The preparation method uses simple device, the process conditions are simple and easy, the production cost is low, and the process is environment-friendly and is suitable for production in a large scale. The material can be widely applied to the fields such as high temperature lubricant, hydrogenation catalyst, high energy power supply, hydrogen storage material, semiconductor material, or even super conductive material.

Description

technical field [0001] The invention relates to a metal sulfide material and a preparation method thereof, in particular to a metal sulfide single crystal material and a preparation technology thereof. Background technique [0002] Due to their excellent properties, metal sulfide materials have been widely used in high-temperature lubricants, hydrogenation catalysts, high-energy power supplies, hydrogen storage materials, semiconductor materials and even superconductor materials, so they have attracted the attention of researchers. The traditional preparation methods of sulfide mainly include solid-phase method and liquid-phase method. The solid-phase method is the high-temperature sintering method, and the liquid-phase method mainly includes the homogeneous deposition method and the hydrothermal synthesis method. The traditional high-temperature solid-phase method usually takes a long time to complete the reaction, and the product particles are coarse. The liquid phase me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/46C30B1/10
Inventor 杨化滨齐洁
Owner NANKAI UNIV
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