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Preparation method of metal phase molybdenum disulfide

A technology of molybdenum disulfide and metal phase, applied in the direction of molybdenum sulfide, etc., can solve problems such as danger and time-consuming

Active Publication Date: 2018-01-30
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the past few decades, molybdenum disulfide with the coexistence of metal and semiconductor phases can be obtained by Li ion intercalation, but this method is dangerous and time-consuming.

Method used

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  • Preparation method of metal phase molybdenum disulfide
  • Preparation method of metal phase molybdenum disulfide
  • Preparation method of metal phase molybdenum disulfide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A preparation method of metal phase molybdenum disulfide, the steps are as follows:

[0020] (1) Mix ammonium molybdate and thiourea at a molar ratio of 1:14, then stir in deionized water to form a homogeneous solution. Wherein, the concentration of ammonium molybdate is 1mmol / L;

[0021] (2) The solution was transferred to a stainless steel reaction kettle, reacted at 220°C for 18h, and then cooled naturally to room temperature.

[0022] (3) Centrifuge the reaction solution, wash the precipitate, and dry it in vacuum to obtain MoS 2 powder.

[0023] (4) The vacuum-dried MoS 2 The powder is dispersed into a saturated copper salt solution, MoS 2 The concentration is 1.14mmol / L; ultrasonic treatment 24h;

[0024] (5) Centrifuge the above solution, wash the precipitate, and dry it in vacuum to obtain metal phase molybdenum disulfide powder.

[0025] figure 1 is the scanning electron microscope image (SEM) of the prepared metal phase molybdenum disulfide. It can be s...

Embodiment 2

[0029] This embodiment is the same as embodiment 1, the MoS in step 4 2 The concentration is 0.11mmol / L, the Raman of the product is as follows Figure 6 shown. It can be seen from the figure that the samples prepared at this concentration have undergone a phase transition to form molybdenum disulfide in the metal phase.

Embodiment 3

[0031] This embodiment is the same as embodiment 1, the MoS in step 4 2 Concentration is 2.84mmol / L, the Raman of product is as follows Figure 7 shown. It can be seen from the figure that the samples prepared at this concentration are still in the semiconductor phase.

[0032] It can be seen from the above examples that when MoS 2 The concentration is 2.84mmol / L, and the molybdenum disulfide of the metal phase cannot be generated. The reason is that the concentration is too large, resulting in uneven dispersion between the nanoparticles, and the copper ions and MoS 2 The contact is hindered, the stress effect caused by copper ions becomes smaller, MoS 2 The slip of the middle S layer is hindered, so it does not produce a phase transition; when MoS 2 When the concentration is 0.11mmol / L, metal phase molybdenum disulfide can be generated, so when the concentration is lower than 1.14mmol / L, it can lead to the generation of metal phase molybdenum disulfide.

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Abstract

The invention discloses a preparation method of metal-phase molybdenum disulfide, belongs to the field of nano materials, and aims to achieve the effect of preparing the metal-phase molybdenum disulfide according to an ion ultrasonic assistance process. The preparation method comprises the following steps: synthesizing semiconductor-phase molybdenum disulfide through a hydrothermal process, and then carrying out ultrasonic treatment in a copper salt solution to enable semiconductor-phase molybdenum disulfide atoms to be rearranged and enable the atomic surface to slide, thus generating the metal-phase molybdenum disulfide. The preparation method has the advantages of simplicity, safety, economy, efficiency, batch synthesis and the like.

Description

technical field [0001] The invention relates to a method for preparing metal phase molybdenum disulfide, and the prepared material can be used in the fields of electrochemical hydrogen evolution, lithium ion batteries and the like. Background technique [0002] Two-dimensional layered molybdenum disulfide is a typical transition metal sulfide, which has attracted extensive attention of researchers because of its special graphene-like structure and unique physical and chemical properties. The molybdenum disulfide currently studied mainly includes semiconductor phase, metallic phase and semi-metallic phase. The semi-metallic phase of molybdenum disulfide only exists in bulk molybdenum disulfide. Stable phase, essentially can not exist stably, but the metal phase molybdenum disulfide has many active sites and good conductivity, therefore, in the fields of electrocatalytic hydrogen production and supercapacitors, the metal phase molybdenum disulfide is a A very promising materi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G39/06
CPCC01G39/06C01P2002/72C01P2002/82C01P2002/85C01P2004/03C01P2004/04C01P2004/20C01P2004/51C01P2004/62
Inventor 崔小强魏淑婷祁琨徐延超张海燕张雷
Owner JILIN UNIV