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Method for preparing nano vanadium nitride (VN) electrode material for super capacitor

A nanometer vanadium nitride, supercapacitor technology, applied in capacitors, electrolytic capacitors, nitrogen-metal/silicon/boron binary compounds, etc., can solve the problems of unsuitable supercapacitor materials, harsh reaction conditions, and coarse VN grains. , to achieve the effect of fine grain size, short reaction time and simple method

Inactive Publication Date: 2009-12-09
SICHUAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example using VS 2 As a precursor, relatively pure VN can be obtained; but the raw material VS 2 Difficult to prepare, and the reaction conditions are very harsh
There is a pair of Nano V 2 o 5 high temperature ammonia reduction, or by adding nano V 2 o 5 After mixing carbon, VN can be obtained by reducing in high temperature nitrogen, but the VN obtained in this way usually has coarse grains and small specific surface area, which is not suitable for supercapacitor materials

Method used

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  • Method for preparing nano vanadium nitride (VN) electrode material for super capacitor
  • Method for preparing nano vanadium nitride (VN) electrode material for super capacitor
  • Method for preparing nano vanadium nitride (VN) electrode material for super capacitor

Examples

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Embodiment 1

[0029] Embodiment 1: take a certain amount of analytically pure V 2 o 5 Raw materials, preparation of VOCl 2 Solution: weigh V 2 o 5 (99%) 50g, oxalic acid 37g, dilute hydrochloric acid (1:1) 300ml, V 2 o 5 Mix it with oxalic acid and add it to distilled water, stir and heat it to boiling with a magnetic device, then add 1:1 dilute hydrochloric acid dropwise to it until the reaction is complete, and finally add 20 drops of hydrazine hydrochloride to the solution to obtain blue-green VOCl 2 solution. Precursor preparation: to self-made VOCl 2 Add ammonia water dropwise to the solution to make an excess of 2ml of ammonia water to ensure that the reaction is complete; during the dripping process, keep stirring to adjust the pH of the solution to about 9; Chloride ions; place the precipitate in a vacuum oven and dry at 80°C for 12h. Grind the dry precursor and fully mix it with activated carbon according to a certain mass ratio (1:0.3), spread it into a thin layer in a qua...

Embodiment 2

[0030] Embodiment 2: take a certain amount of analytically pure V 2 o 5 Raw materials, preparation of VOCl 2 Solution: weigh V 2 o 5 (99%) 100g, oxalic acid 75g, dilute hydrochloric acid (1:1) 600ml, V 2 o 5 Mix it with oxalic acid and add it to distilled water, stir it with a magnetic device and heat it to boiling, then add 1:1 dilute hydrochloric acid dropwise to it until the reaction is complete, and finally add 30 drops of hydrazine hydrochloride to the solution to obtain blue-green VOCl 2 solution. Precursor preparation: to self-made VOCl 2 Add ammonia water dropwise to the solution, and ensure that the excess amount of ammonia water is 4ml to ensure complete reaction; during the dripping process, keep stirring, and adjust the pH of the solution to about 10; the obtained precipitate is washed and filtered with alcohol for many times; the precipitate is placed in vacuum drying In the oven, dry at 100°C for 10h. Grind the dry precursor and fully mix it with nano-car...

Embodiment 3

[0031] Embodiment 3: prepare VOCl 2 The solution method was as described in Example 1. to VOCl 2 Add ammonia water dropwise to the solution, and ensure that the excess amount of ammonia water is 6ml to ensure complete reaction; during the dropping process, keep stirring, and adjust the pH of the solution to about 11; the obtained precipitate is washed and filtered with alcohol for many times; the precipitate is placed in vacuum drying In the oven, dry at 90°C for 12h. Grind the dry precursor, put it into the acetone solution with acetylene black in a certain ratio (1:0.2), and stir it with a magnetic stirrer to make it fully mixed. Put it in the oven to dry for about 2 hours. Then put it into a quartz tube, and carry out nitriding heat treatment for 1.5 h under an ammonia gas atmosphere at 700°C. Then get nano VN powder. The obtained product is made into an electrode material for constant-current charge-discharge and cyclic voltammetry tests, and the specific capacity aft...

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Abstract

The invention discloses a method for preparing a nano vanadium nitride electrode material for a super capacitor. The method is applied to analyzing pure vanadium pentoxide as an initial raw material, and comprises the following steps: preparing a precursor (NH4)2V4O9 of nano vanadium nitride by a chemical precipitation method, washing and filtering the precursor, drying the precursor for 10 to 15 hours in vacuum at the temperature of between 60 and 120 DEG C, then using activated carbon, acetylene black, nano-carbon black, citric acid or glucose and the like as a reducing agent, reacting the mixture for 1 to 4 hours at the temperature of between 600 and 800 DEG C under the atmosphere of ammonia gas, and nitriding and reducing a reaction product to obtain nano-scale vanadium nitride granules. The method is simple to operate, and can prepare the spherical vanadium nitride granules of about 12 nanometers; and the vanadium nitride granules used as the electrode material for the super capacitor have specific capacity of 340 to 480 F / g.

Description

technical field [0001] The invention relates to a preparation method of nano-scale vanadium nitride (VN) as an electrode material of a supercapacitor, and belongs to the field of preparation of energy storage materials. technical background [0002] With the growth of the world's population and the development of the social economy, the resources and energy that human beings rely on for survival are becoming increasingly scarce, and the ecological environment is gradually deteriorating. Human beings will rely more on clean and renewable new energy. Therefore, the development of new energy and new materials is a hot topic in the world today. Electrochemical capacitor is a new type of energy storage device that has emerged in recent years. It uses the electric double layer formed between the electrode surface and the electrolyte or the two-dimensional or quasi-two-dimensional Faraday reaction to store electrical energy. The capacitance can reach the Farad level. Therefore, it...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/06H01G9/042
CPCY02E60/13
Inventor 刘恒吕玲
Owner SICHUAN UNIV