Preparation method of transition metal sulfide composite nanometer material

A technology of composite nanomaterials and transition metals, which is applied in the field of preparation of transition metal sulfide composite nanomaterials, can solve the problems of energy density limiting the application of supercapacitors, achieve good pseudocapacitive characteristics and cycle stability, high application value, and preparation The effect of simple method

Inactive Publication Date: 2018-12-11
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But the low energy density limits the application of supercapacitors

Method used

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  • Preparation method of transition metal sulfide composite nanometer material
  • Preparation method of transition metal sulfide composite nanometer material
  • Preparation method of transition metal sulfide composite nanometer material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Preparation of ZIF-67 Nanomaterials

[0024] Dissolve cobalt nitrate hexahydrate (29.1 mg) and 2-methylimidazole (32.8 mg) in 15-25 mL of methanol respectively, then slowly add the cobalt nitrate solution into the 2-methylimidazole solution, stir at room temperature for 2 h, and The mixed solution was left standing at room temperature for 24 hours, the precipitate was collected by centrifugation, washed with methanol and ethanol respectively, and finally dried at 80°C for 24 hours to obtain the precursor ZIF-67 nanomaterial.

[0025] The morphology of the obtained ZIF-67 nanomaterials was characterized by scanning electron microscopy. Such as figure 1 As shown, the obtained ZIF-67 nanomaterial is a dodecahedron with a smooth surface, and the crystal size is about 700 nm.

Embodiment 2

[0027] Preparation of NiCo-LDH intermediate

[0028] Dissolve nickel nitrate hexahydrate (120 mg) in 20-25 mL of ethanol, then add 60 mg of ZIF-67 precursor into the above solution, and ultrasonicate for 5-20 min to make it uniformly dispersed. Stir the dispersion at room temperature for 10 h, centrifuge to collect the precipitate, wash with methanol and ethanol respectively, and finally dry at 80° C. for 24 h to obtain the NiCo-LDH intermediate nanomaterial.

Embodiment 3

[0030] Preparation of NiCo 2 S 4 @MoS 2 nanomaterials

[0031] The NiCo-LDH intermediate nanomaterial (25 mg) in Example 2 was dispersed in deionized water, and then added with a concentration of 20 mg / mL of thioacetamide solution 5 mL and a concentration of 10 mg / mL of sodium molybdate solution, fully After mixing, transfer to a reaction kettle, keep at 120° C. for 4 hours, and then keep at 200° C. for 8 hours. After the reaction, the product is collected by centrifugation and washing with water.

[0032] Its structure was analyzed by X-ray diffractometer, such as figure 2 As shown, the nanomaterial is NiCo in the cubic phase 2 S 4 , due to MoS 2 Low crystallinity and presence of small amounts, NiCo 2 S 4 @MoS 2 There is no obvious MoS in the diffraction pattern 2 diffraction peaks.

[0033] The resulting NiCo was characterized by scanning electron microscopy 2 S 4 @MoS 2 Morphology of nanomaterials. Such as image 3 As shown, the resulting NiCo 2 S 4 @MoS ...

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Abstract

The invention discloses a preparation method of a transition metal sulfide composite nanometer material and belongs to the technical field of preparation of transition metal sulfides. The preparationmethod comprises the following steps of dissolving cobalt nitrate hexahydrate and 2-methylimidazole into methanol, performing stirring at a room temperature, performing still standing on an obtained solution for 12-36h at the room temperature, and preparing an ZIF-67 precursor; dissolving the cobalt nitrate hexahydrate and the ZIF-67 precursor into ethanol, performing dispersion, and performing stirring at the room temperature to form an Ni-Co-LDH intermediate; dispersing the intermediate in deionized water, adding a sulfur source and a molybdenum source, performing full stirring, transferringa mixture into a reaction kettle, adopting a hydrothermal method to perform stepwise temperature rising on the intermediate, then collecting a product through centrifugal washing, and drying at a certain temperature to obtain an NiCo2S4@MoS2 nanometer material. The preparation method provided by the invention is simple and green without pollution and is high in practical degree; and the obtainedNiCo2S4@MoS2 nanometer material can be directly used as an electrode material for a supercapacitor.

Description

technical field [0001] The invention relates to a preparation method of a transition metal sulfide composite nano material, belonging to the technical field of transition metal sulfide preparation. Background technique [0002] In recent years, with the aggravation of environmental pollution and energy consumption, the demand for sustainable energy and green energy has gradually attracted people's attention. As a new energy storage device, supercapacitor has ultra-high power density, good cycle performance and fast charging and discharging characteristics, and is an ideal alternative energy source. But the low energy density limits the application of supercapacitors. The energy density of a supercapacitor depends on the potential window and capacitance of the system. These two properties are determined by the properties of the electrode material, such as particle size, surface morphology, surface area, structure, and porosity. Therefore, research on new nanostructured elec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G53/00C01G39/06B82Y30/00H01G11/30H01G11/26H01G11/86
CPCB82Y30/00C01G39/06C01G53/006C01P2002/72C01P2004/03C01P2004/04C01P2004/82H01G11/26H01G11/30H01G11/86Y02E60/13
Inventor 孟玉兰孙菲菲宋学志王紫薇谭振权
Owner DALIAN UNIV OF TECH
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