Preparation method and application of nanosheet self-assembled microflower-shaped VS2

A self-assembly and nanosheet technology, applied in nanotechnology, chemical instruments and methods, vanadium compounds, etc., to achieve high purity, uniform chemical composition, and low cost

Active Publication Date: 2016-08-03
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are few studies on the electrochemical performance of vanadium disulfide, onl

Method used

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  • Preparation method and application of nanosheet self-assembled microflower-shaped VS2
  • Preparation method and application of nanosheet self-assembled microflower-shaped VS2

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preparation example Construction

[0022] A nanosheet self-assembled microflower-like VS 2 The preparation method comprises the following steps:

[0023] Step 1: Weigh the vanadium source and sulfur source and dissolve them in deionized water, control the vanadium-sulfur molar ratio to 1:1-1:6, stir magnetically for 10-60 minutes to obtain a semi-clear solution A, and the concentration of the vanadium source is 0.1 ~0.5mol / L. Vanadium source is one or more of sodium vanadate, ammonium metavanadate, vanadium pentoxide and potassium metavanadate; sulfur source is thioacetamide, sodium sulfide, ammonium sulfide, sodium diethylthiocarbamate And one or more of the elemental sulfur.

[0024] Step 2: Prepare 1-4 mol / L sodium hydroxide solution B, and then add solution B dropwise to solution A until the pH value of the solution reaches 11-14, and obtain solution C. During this process, solution A needs to be continuously magnetically stirred, and the pH value must be controlled between 11 and 14, so that the presenc...

Embodiment 1

[0029] Step 1: Weigh sodium metavanadate and thioacetamide and dissolve them in deionized water, control the molar ratio of vanadium to sulfur to 1:1, and stir magnetically for 10 minutes to obtain semi-clear solution A. At this time, the concentration of vanadium source is 0.2mol / L.

[0030] Step 2: prepare 3 mol / L sodium hydroxide solution B, then add solution B dropwise to solution A until the pH value of the solution reaches 13, and obtain solution C. During this process, solution A needs to be constantly stirred by magnetic force.

[0031] Step 3: Pour the solution C into the reaction liner, then fix the liner in the outer kettle and place it in a homogeneous reactor, and then react at 160°C for 24 hours under the condition of 10r / min.

[0032] Step 4: Take out the cooled product after the reaction, collect the product after 3 times of water washing and 3 times of alcohol washing, and dry it at 60°C for 12 hours to obtain the nanosheet self-assembled micro flower-shaped...

Embodiment 2

[0036] Step 1: Weigh sodium metavanadate and thioacetamide and dissolve them in deionized water, control the molar ratio of vanadium to sulfur to 1:3, and stir magnetically for 20 minutes to obtain a semi-clear solution A. At this time, the concentration of vanadium source is 0.1mol / L.

[0037] Step 2: prepare 1 mol / L sodium hydroxide solution B, then add solution B dropwise to solution A until the pH value of the solution reaches 11, and obtain solution C. During this process, solution A needs to be constantly stirred by magnetic force.

[0038]Step 3: Pour the solution C into the reaction liner, then fix the liner in the outer kettle and place it in a homogeneous reactor, and then react at 120° C. for 6 hours under the condition of 5 r / min.

[0039] Step 4: Take out the cooled product after the reaction, collect the product after 4 times of water washing and 4 times of alcohol washing, and dry it at 40°C for 18 hours to obtain the nanosheet self-assembled micro flower-shap...

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Abstract

The invention provides a preparation method and application of nanosheet self-assembled microflower-shaped VS2. The preparation method comprises the steps that firstly, the pH of a vanadium source solution and the pH of a sulfur source solution are regulated to be 11-14 under the magnetic stirring state through a sodium hydroxide solution; secondly, the solutions are poured into a reaction inner lining, the inner lining is contained in an outer kettle and fixed, and then the outer kettle is placed in a homogeneous reaction instrument; finally, a product obtained after a reaction is cooled, washed, collected and dried, and then the nanosheet self-assembled microflower-shaped VS2 can be obtained. The technology of the method is simple and easy to control, and the prepared nanosheet self-assembled microflower-shaped VS2 is uniform in chemical constitution and high in purity, has a specific self-assembled structure and shows the excellent electrochemical property when the nanosheet self-assembled microflower-shaped VS2 serves as a lithium-sodium ion battery electrode material. In addition, the method has the advantages that the defect that a traditional calcination method is high in temperature is overcome, large equipment and harsh reaction conditions are not needed, the raw materials are cheap and easy to obtain, the cost is low, the yield is high, aftertreatment is not needed, and the method is friendly to the environment and can be suitable for large-scale production.

Description

【Technical field】 [0001] The invention relates to a preparation method of a transition metal sulfide, in particular to a nanosheet self-assembled micron flower-shaped VS 2 Preparation method and application. 【Background technique】 [0002] Many inorganic compounds such as metal oxides, phosphates, layered silicates, and disulfides have a layered structure similar to graphite. The interlayers of these compounds act with intermolecular forces such as van der Waals force, and the atoms on the laminates interact with each other through strong covalent bonds. We call them intercalation compounds. Inspired by the idea of ​​preparing single-layer graphene by the exfoliation method, Zhang Hua's research group at Nanyang Technological University in Singapore found that by inserting lithium ions into the interlayers of layered disulfide bulk materials, single-layer disulfide materials can also be exfoliated. While the single-layer MoS 2 、WS 2 , VS 2 , SnS 2 It has the unique vol...

Claims

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Application Information

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IPC IPC(8): C01G31/00C01G31/02H01M4/1391B82Y40/00
CPCB82Y40/00C01G31/00C01G31/02H01M4/1391Y02E60/10
Inventor 黄剑锋李文斌王海静李瑞梓费杰曹丽云任一杰罗晓敏闻稼宝程呈
Owner SHAANXI UNIV OF SCI & TECH
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