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A kind of preparation method of selenium/vanadium selenide composite phase material

A composite material, vanadium selenide technology, applied in the field of electrocatalytic energy material preparation, can solve the problems of small ionization energy, etc., and achieve the effects of improving catalytic activity, short preparation cycle, and easy control of reaction

Active Publication Date: 2020-02-21
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, selenium and sulfur are in different periods of the periodic table, so there are many differences: 1) selenium has stronger metallicity than sulfur, and thus has better electrical conductivity; 2) selenium is more metallic than sulfur Has a larger atomic radius; 3) Selenium atoms have smaller ionization energy than sulfur atoms

Method used

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  • A kind of preparation method of selenium/vanadium selenide composite phase material
  • A kind of preparation method of selenium/vanadium selenide composite phase material
  • A kind of preparation method of selenium/vanadium selenide composite phase material

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Experimental program
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Effect test

Embodiment 1

[0030] 1) Take by weighing selenium dioxide and vanadium pentoxide in a molar ratio of 5:1, that is, the quality of the two is 554.79mg and 182.00mg respectively, and it is dissolved in deionized water and anhydrous water with a volume ratio of 3:1. In a solution composed of ethanol (35 mL in total), magnetically stirred for 30 min to obtain a mixed solution;

[0031] 2) Transfer the resulting mixed solution in step 1) to a 50mL autoclave with p-polyphenyl liner, then add 0.038g of hexamethylenetetramine, 0.324g of dodecane to the reactor Sodium sulfate, 0.023g of polyvinylpyrrolidone and 0.087g of N,N-dimethylformamide morphology regulator, the reaction kettle was sealed, and placed in an oven at 220°C for 18 hours;

[0032] 3) After the reaction is finished, cool to room temperature naturally to obtain a black product, which is repeatedly centrifuged 3 times with ultrapure water and absolute ethanol;

[0033] 4) Finally, vacuum-dry the obtained sample at 50° C. to obtain a ...

Embodiment 2

[0036] 1) Take sodium selenide and ammonium metavanadate with a molar ratio of 3:1, namely the quality of the two is 374.82mg and 116.99mg respectively, and it is dissolved in deionized water and anhydrous water with a volume ratio of 4:1. In a solution composed of ethanol (35 mL in total), magnetically stirred for 30 min to obtain a mixed solution;

[0037]2) Transfer the resulting mixed solution in step 1) to a 50mL autoclave with p-polyphenyl liner, then add 0.059g of hexamethylenetetramine, 0.226g of dodecane to the reactor Sodium sulfate, 0.035g of polyvinylpyrrolidone and 0.056g of N,N-dimethylformamide morphology regulator, the reaction kettle was sealed, and placed in an oven at 200°C for 24 hours;

[0038] 3) After the reaction is finished, cool to room temperature naturally to obtain a black product, which is repeatedly centrifuged 3 times with ultrapure water and absolute ethanol;

[0039] 4) Finally, vacuum-dry the obtained sample at 120° C. to obtain a selenium / v...

Embodiment 3

[0042] 1) Take by weighing selenium powder and vanadium chloride in a molar ratio of 4:1, that is, the quality of the two is 315.84mg and 157.30mg respectively, and it is dissolved in deionized water and absolute ethanol with a volume ratio of 3:1. in the solution (totally 35mL), magnetically stirred for 30min to obtain a mixed solution;

[0043] 2) Transfer the resulting mixed solution in step 1) to a 50mL autoclave with p-polyphenyl liner, then add 0.048g of hexamethylenetetramine, 0.275g of dodecane to the reactor Sodium sulfate, 0.029g of polyvinylpyrrolidone and 0.072g of N,N-dimethylformamide morphology regulator, the reaction kettle was sealed, and placed in an oven at 210°C for 21 hours;

[0044] 3) After the reaction is finished, cool to room temperature naturally to obtain a black product, which is repeatedly centrifuged 3 times with ultrapure water and absolute ethanol;

[0045] 4) Finally, vacuum-dry the obtained sample at 90° C. to obtain a selenium / vanadium sele...

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Abstract

The invention discloses a method for preparing a selenium / vanadium selenide composite phase material. The method comprises the following steps: weighing a selenium source and a vanadium source in a mole ratio of (2-6):1, dissolving into a solution consisting of deionized water and absolute ethyl alcohol, carrying out magnetic stirring to sufficiently dissolve the components, adding a morphology regulation agent into a mixed liquid, sealing a reaction kettle, carrying out a reaction for 18-24 hours in an oven at 200-220 DEG C, repeatedly centrifuging the obtained black product with super pure water and absolute ethyl alcohol for multiple times, and carrying out vacuum drying, thereby obtaining the selenium / vanadium selenide composite phase material. A solvothermal method which is simple inprocess, short in preparation cycle and easy in reaction control is adopted, an idea is provided for design of a composite material electric catalyst; compared with vanadium selenide, the prepared selenium / vanadium selenide composite phase material has a large surface area, and the catalysis activity of the selenium / vanadium selenide composite phase material can be improved.

Description

technical field [0001] The invention belongs to the field of preparation of electrocatalytic energy materials, and in particular relates to a preparation method of a selenium / vanadium selenide composite phase material. Background technique [0002] In recent years, with the rapid development of graphene materials, other two-dimensional materials have attracted more and more attention and research. Two-dimensional materials usually exhibit unique electrical, optical, and magnetic properties, and have their own unique structural advantages, which provide new ideas and guide new directions for exploring new electrocatalysts and energy storage materials. Due to the unique physical and chemical properties of two-dimensional transition metal dichalcogenides (TMDs), the research on TMDs has gradually attracted attention, and metal selenides, especially two-dimensional layered metal selenides, are becoming a new hotspot in material research, attracting attention. It has attracted e...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B19/02C01B19/00C01B3/04C01B13/02
CPCC01B3/042C01B13/0207C01B19/007C01B19/02C01P2002/72C01P2004/03Y02E60/36
Inventor 曹丽云何丹阳冯亮亮黄剑锋吴建鹏刘倩倩
Owner SHAANXI UNIV OF SCI & TECH