Method for microwave hydrothermal preparation of 1T@2H-MoS2

A microwave hydrothermal and deionized water technology, applied in chemical instruments and methods, chemical/physical/physicochemical processes of energy application, molybdenum sulfide, etc., can solve problems such as hidden safety hazards, difficult conditions to control, and complicated operations. Achieve the effects of easy popularization, simple operation and low reaction temperature

Inactive Publication Date: 2018-02-02
XINJIANG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] From the above reports, it can be seen that the existing preparation of 1T@2H-MoS 2 The traditional method: the operation is complicated, the sample preparation time is long, some methods require carrier gas, the conditions are not easy to control, and there are potential safety hazards

Method used

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  • Method for microwave hydrothermal preparation of 1T@2H-MoS2
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  • Method for microwave hydrothermal preparation of 1T@2H-MoS2

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Embodiment 1

[0030] Dissolve 1mmol of ammonium heptamolybdate and 15mmol of thiourea in 35ml of distilled water, and continue magnetic stirring at room temperature for 30min to form a homogeneous solution. Transfer the solution to a polytetrafluoroethylene-lined microwave instrument, and set the microwave program to at 200°C for 10 min, and then cooled to room temperature after the end of the program. A microwave-one-step sample (denoted as M1) was collected by centrifugation. For the second time, the M1 sample was dissolved in 25 ml of alcohol and transferred to a Teflon-lined microwave instrument. At this time, the program was set at 220 °C for 4 min, and cooled to room temperature after the program ended. After centrifugation, the collected product was dissolved in ethanol and sonicated for 20 min and vacuum-dried at 60 °C to obtain 1T@2H-MoS 2 . (marked as M-1T@2H-MoS 2 ). Such as figure 1 Shown is the XRD pattern of the resulting product. Compared to 2H-MoS 2 , 1T@2H-MoS 2 New...

Embodiment 2

[0032] Dissolve 1mmol of ammonium heptamolybdate and 15mmol of thiourea in 35ml of distilled water, and continue magnetic stirring at room temperature for 30min to form a homogeneous solution. Transfer the solution to a polytetrafluoroethylene-lined microwave instrument, and set the microwave program to at 200°C for 10 min, and then cooled to room temperature after the end of the program. A microwave-one-step sample (denoted as M1) was collected by centrifugation. For the second time, the M1 sample was dissolved in 25 ml of alcohol and transferred to a Teflon-lined microwave instrument. At this time, the program was set at 220 °C for 6 min, and cooled to room temperature after the program was completed. After centrifugation, the collected product was dissolved in ethanol and sonicated for 20 min and vacuum-dried at 60 °C to obtain 1T@2H-MoS 2 . (marked as M-1T@2H-MoS 2 ). Such as image 3 Shown; is the TEM image of the obtained product, proving that the prepared MoS 2 ar...

Embodiment 3

[0034] Dissolve 1mmol of ammonium heptamolybdate and 15mmol of thiourea in 35ml of distilled water, and continue magnetic stirring at room temperature for 30min to form a homogeneous solution. Transfer the solution to a polytetrafluoroethylene-lined microwave instrument, and set the microwave program to at 200°C for 10 min, and then cooled to room temperature after the end of the program. A microwave-one-step sample (denoted as M1) was collected by centrifugation. For the second time, the M1 sample was dissolved in 25 ml of alcohol and transferred to a Teflon-lined microwave instrument. At this time, the program was set at 220 °C for 8 min, and cooled to room temperature after the program ended. After centrifugation, the collected product was dissolved in ethanol and sonicated for 20 min and vacuum-dried at 60 °C to obtain 1T@2H-MoS 2 . (marked as M-1T@2H-MoS 2 ).

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Abstract

The invention discloses a microwave hydrothermal preparation method of 1T@2H‑MoS2. The preparation method comprises: firstly, using deionized water as a solvent, stirring ammonium heptamolybdate and thiourea for 30 minutes, adjusting the temperature to 200 ° C for 10 minutes, Secondly, using alcohol as a solvent, the product obtained in the first step was reacted at 220 °C for 4-10 min to obtain 1T@2H‑MoS2 nanospheres. The method of the invention uses a microwave hydrothermal instrument, which is simple, safe and fast, has good repeatability and low cost, and the obtained sample has uniform morphology and two phase structures of 1T and 2H.

Description

technical field [0001] The invention belongs to the field of nano-semiconductor phase transition, and specifically relates to microwave hydrothermal preparation of 1T@2H-MoS 2 Methods. Background technique [0002] Currently, MoS 2 Due to its unique photoelectric properties, it has been widely used in fields including catalysis, optoelectronics, spintronics, biological and chemical sensors, capacitors, and solar cells. MoS 2 There are two main crystal structures, 1T and 2H. The 2H phase is a stable structure with semiconductor properties, and its band gap is 1.2-1.9 eV. The 1T phase is a metastable structure with metallic properties, good electrical conductivity and high electron concentration. In photocatalytic applications, the narrow bandgap of the 2H phase can be used as a photosensitizer, and the metallic nature of the 1T phase can be used as a cocatalyst. Combination of two phases (1T@2H-MoS 2 ) and applied to photocatalysis has greater advantages. First, use 2...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/06B01J19/12
CPCC01G39/06B01J19/126C01P2002/72C01P2004/03C01P2004/04C01P2004/32C01P2004/84
Inventor 吴荣刘海洋杨茜范鸿梅孔洋洋
Owner XINJIANG UNIVERSITY
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