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Preparation method of metal sulfide porous single crystal

A metal sulfide and sulfide technology, which is applied in chemical instruments and methods, single crystal growth, single crystal growth, etc., can solve problems that have not been seen in the literature, and achieve the effect of simple process and easy operation

Pending Publication Date: 2022-01-04
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Up to now, the method of using prefabricated templates to prepare porous metal sulfide single crystals has not been found in the literature and published patents.

Method used

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  • Preparation method of metal sulfide porous single crystal
  • Preparation method of metal sulfide porous single crystal
  • Preparation method of metal sulfide porous single crystal

Examples

Experimental program
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Effect test

preparation example Construction

[0034] Porous single crystal NiS 2 As a case, the implementation of the scheme is introduced in detail: take 2g of SiO 2 Nanosphere close-packed template, added to NiCl with a concentration of 0.01mmol / L 2 ·6H 2 In O aqueous solution, stir at room temperature for 12 hours; pour off the liquid after standing for 3 minutes, rinse the template with deionized water for 3 to 5 times, and dry the template at 60° C. to fully adsorb Ni substances on the template. Take the dried template and heat it in a tube furnace at 600°C for 60 minutes, use nitrogen or argon as the carrier gas, the carrier gas flow rate is 50 sccm, place 1 g of thiourea in the upstream of the carrier gas flow, and the carrier gas will drive the thiourea to decompose by heat The gas passes through the template to vulcanize the Ni substance adsorbed on the template, so that the template becomes a uniform gray pre-seeded template, indicating that the pre-seeded crystal is completed.

[0035] Among them, SiO 2 The...

Embodiment 1

[0039] Porous single crystal NiS prepared by adding silica nanospheres (50nm) close-packed templates pre-seeded by impregnation method 2 (MSC-NiS 2 ) and non-porous single crystal NiS prepared without prefabricated templates 2 (Solid-NiS 2 ) As a comparison, the phases of samples prepared according to this method were studied.

[0040] X-ray testing equipment and conditions: Rigaku D / max 2500, Cu Ka rays. Such as figure 1 As shown, it is porous single crystal NiS 2 with nonporous single crystal NiS 2 X-ray diffraction pattern of . It can be seen from the figure that the added template has no effect on the phase of the sample, and it is still a blazonite structure with a single phase; at the same time, compared with the non-porous single-crystal sample, the diffraction of the porous single-crystal sample The peak broadens obviously, which can be understood as the scattering effect of the porous structure on X-rays.

Embodiment 2

[0042] Porous single crystal NiS prepared by adding silica nanospheres (50nm) close-packed templates pre-seeded by impregnation method 2 (MSC-NiS 2 ) and non-porous single crystal NiS prepared without prefabricated templates 2 (Solid-NiS 2 ) as a comparison to study the relationship between the prefabricated template and the particle pore structure.

[0043] Morphological characterization equipment: scanning electron microscope, FEI Nova620. Such as figure 2 As shown, it can be clearly seen that MSC-NiS 2 There are a large number of porous structures on the particles, while Solid-NiS 2 There are no pores on the particles, which proves the effectiveness of the preparation method of the sulfide porous single crystal.

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Abstract

The invention relates to the field of nano material preparation, in particular to a preparation method of a metal sulfide porous single crystal. The preparation method comprises the following steps: implanting a seed crystal corresponding to a target sulfide on a prefabricated template by using an impregnation-vulcanization method, then growing the sulfide in the template by using a hydrothermal method, and finally removing the template to obtain the metal sulfide porous single crystal particle with the prefabricated template reverse structure. On the basis of special requirements of a catalyst on active sites and electron transmission in electrochemical reaction, the metal sulfide which can expose the inner surface and the outer surface, is beneficial to electron transmission and has a three-dimensional porous single-crystal structure is obtained by utilizing cheap and easily available raw materials through a simple and easy-to-operate method. The method makes preparation of the metal sulfide porous single crystal possible, is simple and convenient to operate and simple in process, and has the potential of large-scale application.

Description

technical field [0001] The invention relates to the field of nanomaterial preparation, in particular to a method for preparing a metal sulfide porous single crystal. Background technique [0002] Metal sulfides have higher ion and electron conductivity than metal oxides, and are widely used in electrochemical energy storage and electrocatalysis. The morphology and surface structure of metal sulfides directly affect their contact with the electrolyte, which has a key impact on performance. The introduction of a pore structure is a powerful means to improve the electrochemical performance of metal sulfides: the specific surface area of ​​the porous sample is large, both the inner and outer surfaces can participate in the electrochemical reaction, and the utilization rate of the sample is high; after the introduction of the pore structure, the inner and outer surfaces can be Contact with the electrolyte can increase the number of reaction sites and bring significant performanc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B7/10C30B7/14C30B25/00C30B9/00C30B29/46C30B29/60C25B11/075C25B11/031C25B1/04
CPCC30B7/10C30B7/14C30B25/00C30B9/00C30B29/46C30B29/60C25B11/075C25B11/031C25B1/04Y02E60/36
Inventor 刘岗张露露杨勇强成会明
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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