Preparation method and application of nanometer rod-shaped V3S4

A technology of nanorods and nanomaterials, applied in nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve rare problems and achieve high crystallinity, excellent performance, and uniform chemical composition

Active Publication Date: 2016-09-07
SHAANXI UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, in recent years about V 3 S 4 There are few reports, especially about the controllable preparation of V by a hydrothermal-calcination two-step method 3 S 4 Reports are even rarer

Method used

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  • Preparation method and application of nanometer rod-shaped V3S4
  • Preparation method and application of nanometer rod-shaped V3S4
  • Preparation method and application of nanometer rod-shaped V3S4

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preparation example Construction

[0025] A preparation method of nanorod-shaped vanadium tetrasulfide, comprising the following steps:

[0026] Step 1: Take 10-20mL of ethylene glycol and pour it into 30-50mL of deionized water, and magnetically stir for 10-30min to obtain solution A. Then weigh a certain amount of V 2 o 5 Dissolve in solution A and stir magnetically for 30-60 minutes to obtain vanadium source solution B, wherein the concentration of vanadium source is 0.01-0.10 mol / L. The ethylene glycol is replaced with one or more of oxalic acid, ethanol and isopropanol.

[0027] Step 2: Pour the prepared solution B into the reaction polytetrafluoroethylene liner, put the liner into the outer kettle, and place it in the homogeneous reactor after being fixed. Then, under the conditions that the rotation speed is controlled at 5-50 r / min, the filling ratio of the reactor is controlled at 40-70%, and the reaction temperature is controlled at 120-200° C., the temperature is kept for 12-48 hours. The reactio...

Embodiment 1

[0034] Step 1: Take 15mL of ethylene glycol and pour it into 45mL of deionized water, and magnetically stir for 10min to obtain solution A. Then weigh 0.8gV 2 o 5 Dissolve in solution A and stir magnetically for 30 minutes to obtain solution B, wherein the concentration of vanadium source is 0.02mol / L.

[0035] Step 2: Pour the prepared solution B into the reaction polytetrafluoroethylene liner, put the liner into the outer kettle, and place it in the homogeneous reactor after being fixed. Then, the temperature is kept at 180° C. for 24 hours at a rotating speed of 5 to 10 r / min, a filling ratio of the reactor of 60 percent, and a reaction temperature of 180° C.

[0036] Step 3: After the hydrothermal reaction is completed, cool the reactor to room temperature naturally, take out the reaction liquid and wash it with deionized water for 3 times and with absolute ethanol for 3 times. Then the washed samples were collected and frozen at a cold trap temperature of -70 to -65°C ...

Embodiment 2

[0044] Step 1: Take 10mL of ethylene glycol and pour it into 30mL of deionized water, and magnetically stir for 15min to obtain solution A. Then weigh 0.5gV 2 o 5 Dissolve in solution A and stir magnetically for 40 minutes to obtain solution B, wherein the concentration of vanadium source is 0.01mol / L.

[0045] Step 2: Pour the prepared solution B into the reaction polytetrafluoroethylene liner, put the liner into the outer kettle, and place it in the homogeneous reactor after being fixed. Then, keep the temperature for 48 hours under the condition that the rotating speed is 10-20 r / min, the filling ratio of the reactor is 40%, and the reaction temperature is 120°C.

[0046] Step 3: After the hydrothermal reaction is completed, cool down the reactor naturally to room temperature, take out the reaction solution and wash it twice with deionized water and twice with absolute ethanol. Then collect the washed samples and freeze them for 12 to 24 hours at a cold trap temperature ...

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Abstract

The invention provides a preparation method and application of a nanometer rod-shaped V3S4. The preparation method comprises the following steps of firstly, carrying out hydrothermal reaction of a vanadium source solution to obtain a vanadium oxide nanometer material, wherein the concentration of a vanadium source is 0.01-0.10mol / L; and finally, roasting the vanadium oxide nanometer material whose mole ratio of vanadium to sulfur is (1:8)-(1:12) and a sulfur source substance in a tubular atmosphere furnace, cooling the roasted sample, and washing, cooling and drying the sample to obtain the nanometer rod-shaped V3S4. The method process is simple and is easy to control, and the prepared V3S4 nanometer powder is uniform in chemical constitution, relatively high in purity and relatively high in crystallinity, and shows excellent performance when taken as a ferromagnetic material and an electrode material of a lithium / sodium ion battery. Meanwhile, by the method, a V3S4 structure is controlled by a two-step method, and the controllable preparation of the nanometer rod-shaped V3S4 is further achieved; and further, the raw material is low in cost and is available, the cost is low, the yield is high, subsequent processing is not needed, and the method is friendly to an environment and can be suitable for mass production.

Description

【Technical field】 [0001] The invention relates to a preparation method of vanadium sulfide, in particular to a nanorod V 3 S 4 Preparation method and application. 【Background technique】 [0002] As an important layered inorganic material, vanadium sulfide has attracted more and more attention in recent years, and its application has involved the response ability of moisture, catalytic properties, hydrogen storage properties, lubricating properties and lithium-ion battery electrode materials. Electrochemical properties and other fields [Zhang Y, Wu X.Vanadium sulfide nanoribbons: Electronic and magnetic properties[J].Physics Letters A,2013,377(43):3154-3157]. [0003] At present, more studies are mainly on vanadium disulfide [Yin X.A novel VS 2 nanosheet-based biosensor for rapidfluorescence detection of cytochrome c[J].New Journal of Chemistry,2015,39:1892-1898] and vanadium tetrasulfide[Lui G,Jiang G,Duan A,et al.Synthesis and Characterization of Template- Free VS 4 Na...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58H01M10/0525H01M10/054B82Y30/00B82Y40/00C01G31/00H01F1/01
CPCB82Y30/00B82Y40/00C01G31/00H01F1/01H01M4/5815H01M10/0525H01M10/054Y02E60/10
Inventor 黄剑锋李文斌王海静李瑞梓费杰曹丽云任一杰闻稼宝程呈罗晓敏
Owner SHAANXI UNIV OF SCI & TECH
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