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(001)-oriented nanosheet self-assembled three-dimensional VS2 microrod and preparation method thereof

A nanosheet and microrod technology, applied in the field of three-dimensional self-assembled VS2 and its preparation, can solve the problems of insignificant electrochemical performance improvement, complex synthesis process, high cost, etc., and achieve a simple synthesis path, simple reaction process, and low temperature. Effect

Active Publication Date: 2018-04-13
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these materials have no effect on VS 2 The suppression of volume expansion occurs only in the direction of the contact point, resulting in an insignificant improvement in electrochemical performance
Currently VS 2 The preparation methods are mainly hydrothermal method and calcination method, the vanadium sources are mainly sodium orthovanadate and ammonium metavanadate, etc., and the morphology is mainly nano-flower-like (Wu Changzheng, Sun Xu, Xie Yi. A kind of preparation of vanadium disulfide The method of nanopowder: CN, CN102010004A[P].2011.), and mostly appear in the form of composite material (Zhong Mianzeng, Tang Xinping, Li Shushen, etc. A kind of vanadium disulfide / graphene composite material and its preparation method: , CN105355865A[P].2016.), in addition, these materials need to be prepared or purchased separately, which will make the whole synthesis process complicated, inefficient and costly

Method used

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  • (001)-oriented nanosheet self-assembled three-dimensional VS2 microrod and preparation method thereof
  • (001)-oriented nanosheet self-assembled three-dimensional VS2 microrod and preparation method thereof
  • (001)-oriented nanosheet self-assembled three-dimensional VS2 microrod and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Step 1: Add 1g of sodium metavanadate and 3.6g of thioacetamide to 50ml of absolute ethanol at the same time, and stir magnetically to obtain a semi-clear solution A;

[0037] Step 2: Pour solution A into the reaction liner at a filling ratio of 50% and seal it, install the liner in the outer kettle and fix it, then place it in a homogeneous reactor, and conduct a hydrothermal reaction at 30r / min at 180°C 24h;

[0038] Step 3: After the hydrothermal reaction is completed, the reaction kettle is naturally cooled to room temperature, and then the cooled product after the reaction is taken out, washed alternately with water and alcohol for 3 times, and the product is collected, and dried at 60°C to obtain (001) Oriented nanosheet self-assembled 3D VS 2 micron rods.

[0039] Change the filling ratio of step 2 to 20%, 30%, 40% and 60% respectively to get figure 1 The experimental data from figure 1 It can be found that when the filling ratio is 30-50%, the synthesized pr...

Embodiment 2

[0050] Step 1: Add 0.8g of sodium metavanadate and 3.0g of thioacetamide to 45ml of absolute ethanol at the same time, and magnetically stir to obtain a semi-clear solution A;

[0051] Step 2: Pour solution A into the reaction liner at a filling ratio of 45% and seal it, install the liner in the outer kettle and fix it, then place it in a homogeneous reactor, and conduct hydrothermal reaction at 170°C at 20r / min 25h;

[0052] Step 3: After the hydrothermal reaction is completed, the reaction kettle is naturally cooled to room temperature, and then the cooled product after the reaction is taken out, washed alternately with water and alcohol for 3 times, and the product is collected, and dried at 70°C to obtain (001) Oriented nanosheet self-assembled 3D VS 2 micron rods.

Embodiment 3

[0054] Step 1: Add 0.9g of sodium metavanadate and 3.2g of thioacetamide to 48ml of absolute ethanol at the same time, and magnetically stir to obtain a semi-clear solution A;

[0055] Step 2: Pour the solution A into the reaction liner at a filling ratio of 52% and seal it, install the liner in the outer kettle and fix it, then place it in a homogeneous reactor, and conduct a hydrothermal reaction at 40r / min at 190°C 23h;

[0056] Step 3: After the hydrothermal reaction is completed, the reaction kettle is naturally cooled to room temperature, and then the cooled product after the reaction is taken out, washed alternately with water and alcohol for 3 times, and the product is collected, and dried at 75°C to obtain (001) Oriented nanosheet self-assembled 3D VS 2 micron rods.

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Abstract

A preparation method of a (001)-oriented nanosheet self-assembled three-dimensional VS2 microrod comprises the following steps: simultaneously adding sodium metavanadate and thioacetamide into anhydrous ethanol to obtain a solution A; and pouring the solution A into a reaction liner, sealing the reaction liner, carrying out a hydrothermal reaction in a homogeneous reactor, naturally cooling the obtained reaction product to room temperature, taking out the obtained cooled reaction product, alternately cleaning the product with water and alcohol, collecting the product, and drying the product toobtain the (001)-oriented nanosheet self-assembled three-dimensional VS2 microrod. The center of the microrod is obtained through mutually interlacing large VS2 nanosheets in a radial form, the edgeof the microrod is formed by small flaky VS2 nanosheets, the nanosheets are monocrystalline structures and grow along the (001) crystal face orientation, the diameter of the microrod is 2-15 [mu]m, and the thickness of the nanosheets is 5-20 nm. The highly-pure three-dimensional self-assembled VS2 is synthesized through a one-step solvothermal technology. The method has the advantages of simple reaction process, low temperature, easiness in control, and no large devices or strict reaction conditions.

Description

technical field [0001] The invention relates to a three-dimensional self-assembled VS 2 And preparation method thereof, be specifically related to a kind of (001) oriented nanosheet self-assembled three-dimensional VS 2 Microrods and methods for their preparation. Background technique [0002] Transition metal dichalcogenides such as MoS 2 、WS 2 and VS 2 The large interlayer space of the layered structure makes them a very promising anode material for Na-ion batteries. Although recent studies have shown that MoS 2 and WS 2 They can exhibit excellent sodium storage properties, but poor electron transport caused by semiconducting limits their further development. As a typical member of the transition metal dichalcogenide family, the metallic state VS with excellent conductivity 2 It will exhibit excellent electron transport performance during cycling. At the same time, VS 2 The spatial distance between layers is It can provide sufficient space for the intercalation...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/00B82Y30/00B82Y40/00
Inventor 黄剑锋李文斌何枢薇曹丽云冯亮亮畅珣伟范海鑫王娜
Owner SHAANXI UNIV OF SCI & TECH
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