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Preparation method and application of vanadium tetrasulfide @ reduced graphene oxide composite powder

A graphene composite, vanadium tetrasulfide technology, applied in chemical instruments and methods, physical/chemical process catalysts, electrochemical generators, etc. Sparse distribution and other problems, to achieve the effect of simple synthesis path, low synthesis temperature, and low cost

Active Publication Date: 2019-06-14
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the composite materials that have been reported above, a part of VS 4 Not grown on the carbon material surface, only for VS 4 Composite with carbon materials, although the other part grows on the surface of carbon materials, but the distribution is relatively sparse and irregular, and VS 4 The shape is also irregular and uniform
This inadequate and inefficient recombination makes VS 4 The high performance of the

Method used

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  • Preparation method and application of vanadium tetrasulfide @ reduced graphene oxide composite powder
  • Preparation method and application of vanadium tetrasulfide @ reduced graphene oxide composite powder
  • Preparation method and application of vanadium tetrasulfide @ reduced graphene oxide composite powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Step 1: Weigh 50 mg of graphene oxide and add it to 60 ml of deionized water, and ultrasonicate for 2.0 h with an ultrasonic power of 400-600 W to obtain a uniformly dispersed black solution A.

[0042] Step 2: Weigh 1.0 g of sodium metavanadate and 3.6 g of thioacetamide and add them to solution A at the same time, stir magnetically for 30 minutes at a speed of 500 r / min, and obtain solution B.

[0043] Step 3: Pour solution B into the reaction liner and seal it, then install the liner in the outer kettle and fix it, then place it in a homogeneous reactor with a filling ratio of 60%, and then at a speed of 10r / min, Reaction at 180°C for 24h.

[0044] Step 4: After the hydrothermal reaction is completed, the reactor is naturally cooled to room temperature, and then the cooled product after the reaction is taken out, and the product is collected after 6 times of alternate washing with water and alcohol.

[0045] Step 5: Place the collected product in the cold well of a ...

Embodiment 2

[0047] Step 1: Weigh 20mg of graphene oxide and add it to 58ml of deionized water, ultrasonic for 1.5h, with ultrasonic power of 400W, to obtain a uniformly dispersed black solution A;

[0048] Step 2: Weigh 0.9g of sodium metavanadate and 3.5g of thioacetamide and add them into solution A at the same time, stir magnetically for 30-60min at a speed of 400r / min to obtain solution B;

[0049] Step 3: Pour solution B into the reaction liner and seal it, then install the liner in the outer kettle and fix it, then place it in a homogeneous reactor with a filling ratio of 58%, and then at a speed of 5r / min, React at 175°C for 12h;

[0050] Step 4: After the hydrothermal reaction is completed, the reaction kettle is naturally cooled to room temperature, and then the product cooled after the reaction is taken out, and the product is collected after being washed alternately with water and alcohol for 4 times;

[0051] Step 5: Place the collected product in the cold well of a freeze dr...

Embodiment 3

[0053] Step 1: Weigh 120mg of graphene oxide and add it to 62ml of deionized water, and ultrasonicate for 2.5h with an ultrasonic power of 600W to obtain a uniformly dispersed black solution A;

[0054] Step 2: Weigh 1.1g of sodium metavanadate and 3.7g of thioacetamide and add them to solution A at the same time, stir magnetically for 60min at a speed of 600r / min to obtain solution B;

[0055] Step 3: Pour solution B into the reaction liner and seal it, then install the liner in the outer kettle and fix it, then place it in a homogeneous reactor with a filling ratio of 62%, and then at a speed of 10r / min, React at 185°C for 30h;

[0056] Step 4: After the hydrothermal reaction is completed, the reaction kettle is naturally cooled to room temperature, and then the product cooled after the reaction is taken out, and the product is collected after 10 times of alternate washing with water and alcohol;

[0057] Step 5: Place the collected product in the cold well of a freeze drye...

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Abstract

The invention relates to a preparation method of vanadium tetrasulfide @ reduced graphene oxide composite powder. The preparation method comprises the steps of: weighing 20 to 120mg of graphene oxideinto 58 to 62ml of deionized water to carry out ultrasonic processing to obtain black solution A uniformly dispersed; weighing 0.9 to 1.1g of sodium metavanadate and 3.5 to 3.7g of thioacetamide, simultaneously adding into the solution A, and carrying out magnetic stirring to obtain solution B; after pouring the solution B into a reaction liner, sealing up, then placing the liner in an outer kettle, after fixing the outer kettle, placing the outer kettle into a homogeneous reactor, and then performing a reaction under a rotational speed condition; after a hydrothermal reaction is ended, naturally cooling the reaction kettle to the room temperature, then taking out a cooled product after the reaction, and after alternatively cleaning the product with water and alcohol, collecting the product; and placing the collected product into a cold well of a freezer dryer to carry out freezing, then placing the frozen product into a tray, covering a sealing hood, and after vacuumizing and drying,collecting the product to obtain the vanadium tetrasulfide @ reduced graphene oxide composite powder. The preparation method has the characteristics of simple reaction process, low temperature, easiness for control and no requirement for large-sized equipment and harsh reaction conditions.

Description

technical field [0001] The invention relates to the technical field of vanadium tetrasulfide@reduced graphene oxide composite powder, in particular to a preparation method and application of vanadium tetrasulfide@reduced graphene oxide composite powder. Background technique [0002] As a typical transition metal sulfide, VS 4 Has a one-dimensional chain structure. Among them, two S 2 2- The group (four S) tightly surrounds V and expands along the c direction to form VS 4 Molecular chain, two adjacent VS 4 The molecular chains are connected by weak van der Waals force, and the distance between the chains can reach (Rout CS, Kim B-H, et al. J Am ChemSoc. 2013, 135:8720-8725.). Similar to FeS 2 , VS 4 It is derived from the natural mineral green sulfur vanadite, and the valence state of S is -1, and the valence state of V is +4. The above structural properties make VS 4 It has been applied in photocatalysis, hydrorefining reaction, lithium ion battery, supercapacitor...

Claims

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Application Information

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IPC IPC(8): H01M4/36H01M4/58H01M4/62H01M10/0525H01M10/054B01J27/04B82Y40/00
CPCY02E60/10
Inventor 黄剑锋李文斌冯亮亮曹丽云孙震石泓彬马闯刘代源
Owner SHAANXI UNIV OF SCI & TECH
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