Preparation method of three-dimensional reticular ammonium vanadate nanometer crystals

A nanocrystal, three-dimensional network technology, applied in the field of preparation of three-dimensional network ammonium vanadate nanocrystals, to achieve the effect of good dispersion and easy control of shape

Active Publication Date: 2017-09-15
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Pure phase NH is currently prepared 4 V 3 o 8 There are mainly precipitation method, hydrothermal method, solvothermal method and sol-gel method. As long as the prepared morphology is one-dimensional nanorods, nanobelts, nanowires and two-dimensional sheet morphology, these materials with unique structures are effective. Raised NH 4 V 3 o 8 electrochemical performance, but NH 4 V 3 o 8 There are relatively few reports on the three-dimensional network morphology of nanomaterials. Compared with low-dimensional materials, the three-dimensional network morphology can promote the contact area with the electrolyte and accelerate the transmission rate of lithium ions and electrons.

Method used

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  • Preparation method of three-dimensional reticular ammonium vanadate nanometer crystals
  • Preparation method of three-dimensional reticular ammonium vanadate nanometer crystals

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Experimental program
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Effect test

Embodiment 1

[0031] Preparation of three-dimensional network ammonium vanadate nanocrystals, the specific process is:

[0032] Step 1, the NH 4 VO 3 Uniformly dissolved in 100% ethylene glycol solvent and heated to 30°C to obtain NH at a concentration of 0.05mol / L 4 VO 3 solution;

[0033] Step 2, use 0.1mol / L HCl solution to NH 4 VO 3 The pH of the solution was adjusted to 3, and then reacted for 2 hours under a 300W ultrasonic environment to obtain a solution;

[0034] Step 3, the A solution is placed in a polytetrachlorethylene-lined reactor, the filling ratio in the reactor is 50%, and the reactor is set in a homogeneous hydrothermal reaction, and reacted at 180 ° C for 6 hours, Suspension is obtained in the reactor;

[0035] Step 4: centrifuge the suspension to obtain a powder product, wash the powder product alternately with deionized water and absolute ethanol, and then dry the cleaned product in an electric vacuum drying oven for 8 hours to obtain a three-dimensional netwo...

Embodiment 2

[0037] Preparation of three-dimensional network ammonium vanadate nanocrystals, the specific process is:

[0038] Step 1, the NH 4 VO 3 Uniformly dissolved in 100% ethylene glycol solvent and heated to 50°C to obtain NH with a concentration of 0.03mol / L 4 VO 3 solution;

[0039] Step 2, use 0.1mol / L HCl solution to NH 4 VO 3 The pH of the solution was adjusted to 3, and then reacted for 1 hour under a 300W ultrasonic environment to obtain A solution;

[0040] Step 3, place A solution in a polytetrachlorethylene-lined reactor, the filling ratio in the reactor is 60%, and set the reactor in a homogeneous hydrothermal reaction, and react at 160°C for 8 hours, Suspension is obtained in the reactor;

[0041] Step 4: centrifuge the suspension to obtain a powder product, wash the powder product alternately with deionized water and absolute ethanol, and then dry the cleaned product in an electric vacuum drying oven for 8 hours to obtain a three-dimensional network NH 4 V 3 o ...

Embodiment 3

[0043] Preparation of three-dimensional network ammonium vanadate nanocrystals, the specific process is:

[0044] Step 1, the NH 4 VO 3 Uniformly dissolved in 100% ethylene glycol solvent and heated to 35°C to obtain NH with a concentration of 0.08mol / L 4 VO 3 solution;

[0045] Step 2, use 0.2mol / L HCl solution to NH 4 VO 3 The pH of the solution was adjusted to 1, and then reacted for 2 hours under a 200W ultrasonic environment to obtain a solution;

[0046] Step 3, the A solution is placed in a polytetrachlorethylene-lined reactor, the filling ratio in the reactor is 40%, and the reactor is set in a homogeneous hydrothermal reaction, and reacted at 170 ° C for 7 hours, Suspension is obtained in the reactor;

[0047] Step 4: Centrifuge the suspension to obtain a powder product, wash the powder product alternately with deionized water and absolute ethanol, and then dry the cleaned product in an electric vacuum drying oven for 5 hours to obtain a three-dimensional net...

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Abstract

The invention discloses a preparation method of three-dimensional reticular ammonium vanadate nanometer crystals. The method comprises the following steps of uniformly dissolving NH4VO3 into ethylene glycol to obtain NH4VO3 solution with the NH4<+> concentration being 0.01 to 0.1 mol/L; using HCl solution for regulating the pH of the NH4VO3 solution to be 1 to 3.5; then, performing reaction for 0.5 to 2h in the ultrasonic environment to obtain a solution A; putting the solution A into a reaction kettle with an inner liner being polytetrafluoroethylene; installing the reaction kettle into homogeneous hydrothermal reaction; performing reaction for 4 to 8h at 160 to 200 DEG C; obtaining suspension liquid in the reaction kettle; performing centrifugation separation on the suspension liquid to obtain a powder product; using deionized water and absolute ethyl alcohol for alternately cleaning the powder product; then, drying the cleaned product to obtain the three-dimensional reticular NH4V3O8 nanometer crystals. The three-dimensional reticular ammonium vanadate nanometer crystals prepared by the method are used as a positive electrode material of the lithium battery, and have the characteristics that good electrochemical performance, great multiplying power and good performance. The method has the advantages that the process is simple; the chemical composition of the product is uniform.

Description

technical field [0001] The invention belongs to the technical field of positive electrode materials of lithium ion batteries, and relates to a preparation method of a three-dimensional network ammonium vanadate nanocrystal. Background technique [0002] Since the beginning of human civilization, the development, utilization and storage of energy have been closely related to human life style and quality of life. The long-term use of fossil fuels increases the greenhouse effect of the earth, exacerbates the deterioration of the environment, and poses a great threat to the living environment of human beings. In order to make full use of natural energy, such as wind energy, tidal energy, solar energy, etc., it is necessary to have a suitable energy storage device, so the recyclable secondary battery, as a medium that can effectively store energy, realizes chemical energy and electrical energy. mutual conversion. With the development of secondary batteries, lithium-ion batterie...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/00
CPCC01G31/00C01P2002/72C01P2004/03C01P2004/30C01P2006/80
Inventor 曹丽云寇领江黄剑锋杨军李嘉胤吴建鹏
Owner SHAANXI UNIV OF SCI & TECH
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