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Preparation method of transition metal sulfide nano composite electrode material

A transition metal and nanocomposite technology, which is applied in battery electrodes, nanotechnology, nanotechnology, etc., can solve the problems of long preparation time, large size, uneven material shape, etc., and achieve the effect of short preparation time and improved cycle

Active Publication Date: 2021-02-09
NANJING UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to overcome the problems of complex preparation operation, long preparation time, uneven material appearance, large size and low specific capacity of transition metal sulfides, and propose an easy-to-operate, material appearance A new rapid preparation method for metal sulfide nanocomposite electrode materials with uniformity, small product size and high specific capacity, and this method is applicable to various transition metal sulfides

Method used

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  • Preparation method of transition metal sulfide nano composite electrode material
  • Preparation method of transition metal sulfide nano composite electrode material
  • Preparation method of transition metal sulfide nano composite electrode material

Examples

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Embodiment 1

[0036] According to metal salt Cr(NO 3 ) 3 9H 2 The molar ratio of O to PTA was 1:1, and 0.1 g of urea was weighed as a nitrogen source. 3.2mmol Cr(NO 3 ) 3 9H 2 Dissolve O and urea in 20mL of deionized water, stir to fully dissolve, adjust the pH to 1 with concentrated HF solution, then put the weighed 3.2mmol of PTA into a microwave hydrothermal reaction tank, and react at 210°C for 0.5 h, after the reaction, the product was washed three times with deionized water. The obtained MOFs precursor was mixed with 20 mL of DMF solution, and the dried MOFs precursor was obtained in an oven at 80 °C. The MOFs precursor powder and sulfur powder were ground and mixed at a mass ratio of 1:3, and a porcelain boat was put into a tube furnace with argon gas for sintering. The sintering temperature was 700 °C and the holding time was 2 h. The mass specific capacity of the prepared material is 450mAh / g.

Embodiment 2

[0038] According to metal salt Cr(NO 3 ) 3 9H 2 The molar ratio of O to PTA was 1:1.5, and 0.1 g of urea was weighed as a nitrogen source. 4.5mmol Cr(NO 3 ) 3 9H 2 Dissolve O and urea in 20mL of deionized water, stir to fully dissolve, adjust the pH to 1 with concentrated HF solution, then put the weighed 3.2mmol of PTA into a microwave hydrothermal reaction tank, and react at 210°C for 0.5 h, after the reaction, the product was washed three times with deionized water. The obtained MOFs precursor was mixed with 20 mL of N,N-dimethylamide solution, and dried in an oven at 80 °C to obtain a dry MOFs precursor. The MOFs precursor powder and sulfur powder were ground and mixed at a mass ratio of 1:3, and a porcelain boat was put into a tube furnace with argon gas for sintering. The sintering temperature was 800 °C and the holding time was 2 h. The mass specific capacity of the prepared material is 550mAh / g.

Embodiment 3

[0040] According to metal salt Cr(NO 3 ) 3 9H 2The molar ratio of O to PTA was 1:1.5, and 0.1 g of urea was weighed as a nitrogen source. 4.5mmol Cr(NO 3 ) 3 9H 2 Dissolve O and urea in 20mL of deionized water, stir to make it fully dissolved, adjust the pH to 1 with concentrated HF solution, then put the weighed 3.2mmol of PTA into a microwave hydrothermal reaction tank, and react at 210°C for 1h After the reaction, the product was washed three times with deionized water. The obtained MOFs precursor was mixed with 20 mL of DMF solution, and the dried MOFs precursor was obtained in an oven at 80 °C. The MOFs precursor powder and sulfur powder were ground and mixed at a mass ratio of 1:3, and a porcelain boat was put into a tube furnace with argon gas for sintering. The sintering temperature was 900 °C and the holding time was 2 h. The mass specific capacity of the prepared material is 450mAh / g.

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Abstract

The invention discloses a preparation method of a transition metal sulfide nano composite electrode material. The method comprises the following steps: dissolving a metal salt in deionized water, stirring until the metal salt is completely dissolved, respectively putting PTA and a metal salt solution into a microwave hydrothermal reaction kettle, dropwise adding hydrofluoric acid, and reacting at210 DEG C for 1 hour to obtain an MOFs precursor; and carrying out annealing treatment on the metal organic framework precursor and sublimed sulfur at 700-900 DEG C for 1-8 hours to obtain the metal sulfide and carbon composite material. According to the method, the MOFs precursor is synthesized and serves as a hard template, the structural characteristics of the MOFs precursor are kept while themetal sulfide is prepared through one-step carbonization and vulcanization, the method is suitable for various transition metal sulfides, the prepared material is small in size and uniform in carbon material distribution, the migration distance of ions is shortened, and the conductivity of the material is improved; and the structure of the MOFs precursor before vulcanization is maintained after vulcanization, so that the prepared material has relatively high reversible capacity, relatively good rate capability and cycling stability in energy storage application.

Description

technical field [0001] The invention belongs to the technical field of secondary batteries, and in particular relates to a preparation method of a transition metal sulfide nanocomposite electrode material. Background technique [0002] With the rapid development of mobile portable electronic devices and electric vehicles and power grids, the requirements for energy storage are getting higher and higher. Moreover, energy storage devices restrict the development of some electronic equipment to a large extent. Therefore, there is an urgent need for further development of energy storage devices. [0003] Lithium-ion batteries (LIBs), as one of the most reliable energy storage technologies, have been widely used in portable electronics, electric vehicles, and even large-scale grid energy storage. However, due to the uneven distribution of lithium resources, the reserves of lithium resources are relatively small. The cost of lithium raw materials remains high. This is hardly r...

Claims

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Application Information

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IPC IPC(8): H01M4/36H01M4/58H01M4/62B82Y30/00H01M10/0525
CPCH01M4/362H01M4/5815H01M4/625B82Y30/00H01M10/0525Y02E60/10
Inventor 夏晖孙铭卿刘子恒杨梅徐萌
Owner NANJING UNIV OF SCI & TECH
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