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Preparation method of vanadium oxides with different valence states, crystal forms and appearances

A technology of vanadium oxide and crystal form, which is applied in the field of preparation of vanadium oxide, can solve the problems of inability to obtain vanadium oxide, adverse environmental impact, energy consumption, etc., and achieve the effects of performance improvement, investment reduction, and uniform reaction

Active Publication Date: 2015-03-25
HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this preparation method can also obtain granular vanadium dioxide, it also has shortcomings. First, it cannot obtain vanadium oxides with different valence states, crystal forms and shapes; secondly, adding surface active substances to the mixed solution It needs to be stirred for at least 2 hours after the preparation, and the precursor solution needs to be reacted for at least 1 day in a closed state, which is time-consuming and energy-consuming; thirdly, the oxalic acid in the raw materials is likely to cause adverse effects on the environment

Method used

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  • Preparation method of vanadium oxides with different valence states, crystal forms and appearances
  • Preparation method of vanadium oxides with different valence states, crystal forms and appearances
  • Preparation method of vanadium oxides with different valence states, crystal forms and appearances

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Experimental program
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Effect test

Embodiment 1

[0029] The concrete steps of preparation are:

[0030] Step 1: Firstly mix vanadium pentoxide, 28wt% hydrogen peroxide and deionized water according to the weight ratio of 0.16:3:26 to obtain a mixed solution. This mixed solution is used as a precursor solution.

[0031] Step 2, first place the precursor solution in an airtight container, and react at 180° C. for 34 minutes to obtain a reaction liquid; wherein, the airtight container is a polytetrafluoroethylene container, and the heating source is microwave. Then the reaction solution is subjected to solid-liquid separation, washing and drying in sequence; wherein, the solid-liquid separation process is centrifugation, the rotating speed is 6000r / min, and the time is 3min, and the washing process is obtained by using deionized water and ethanol to separate The solid matter is washed alternately twice, the separation of the solid matter during washing is centrifugation, and the drying process is to dry the washed solid matter...

Embodiment 2

[0033] The concrete steps of preparation are:

[0034] In step 1, vanadium pentoxide, 30wt% hydrogen peroxide and deionized water are mixed according to a weight ratio of 1:2.8:28 to obtain a mixed solution. Add polyethylene glycol to the mixed liquid; wherein, the weight ratio of polyethylene glycol to vanadium pentoxide in the mixed liquid is 0.1:1, and the polyethylene glycol is polyethylene glycol 600 to obtain a precursor solution.

[0035]Step 2, first place the precursor solution in an airtight container, and react at 200°C for 32 minutes to obtain a reaction liquid; wherein, the airtight container is a polytetrafluoroethylene container, and the heating source is microwave. Then the reaction solution is subjected to solid-liquid separation, washing and drying in sequence; wherein, the solid-liquid separation process is centrifugation, the rotating speed is 7000r / min, and the time is 2min, and the washing process is obtained by using deionized water and ethanol to separa...

Embodiment 3

[0037] The concrete steps of preparation are:

[0038] Step 1: Firstly mix vanadium pentoxide, 32wt% hydrogen peroxide and deionized water according to the weight ratio of 2:2.6:30 to obtain a mixed solution. Add polyethylene glycol to the mixed liquid; wherein, the weight ratio of polyethylene glycol to vanadium pentoxide in the mixed liquid is 0.2:2, and the polyethylene glycol is polyethylene glycol 600 to obtain a precursor solution.

[0039] Step 2, first place the precursor solution in an airtight container, and react at 220° C. for 30 minutes to obtain a reaction liquid; wherein, the airtight container is a polytetrafluoroethylene container, and the heating source is microwave. Then the reaction solution is subjected to solid-liquid separation, washing and drying in sequence; wherein, the solid-liquid separation process is centrifugation with a rotating speed of 8000r / min and a time of 1min, and the washing process is obtained by using deionized water and ethanol to sep...

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Abstract

The invention discloses a preparation method of vanadium oxides with different valence states, crystal forms and appearances. The preparation method comprises the following steps: firstly mixing vanadium pentoxide, hydrogen peroxide and deionized water to obtain a mixed solution, and further adding polyethylene glycol into the mixed solution to obtain a precursor solution; then putting the precursor solution into a closed container, and reacting at the temperature of 180-220 DEG C for at least 30min to obtain a reaction solution, wherein the closed container is a polytetrafluoroethylene container and a heating source is microwaves; further sequentially performing solid-liquid separation, washing and drying treatment on the reaction solution to prepare alpha-V2O5 nanowires with valence state of 5, crystal form of orthorhombic alpha phase, space group of Pmmn and appearance of 40nm diameter and 100mu m length or VO2(D) nanoparticles with valence state of 4, crystal form of monoclinic D phase, space group of P2 / c and appearance of 30-40nm particle size or nanorods with valence state of 4, crystal form of monoclinic B phase, space group of C2 / m and appearance of 60nm diameter and 500nm length. The preparation method can be widely used for preparing vanadium oxides with different valence states, crystal forms and appearances.

Description

technical field [0001] The invention relates to a method for preparing vanadium oxides, in particular to a method for preparing vanadium oxides with different valence states, crystal forms and shapes. Background technique [0002] Vanadium oxide is a complex system of multivalent states and polycrystalline phases; among them, there are more than 10 kinds of crystals of vanadium dioxide, mainly including A phase, B phase, C phase, D phase, M phase, R phase and hydrated phase. crystalline phases. Vanadium pentoxide and B-phase vanadium dioxide are good cathode materials for lithium batteries, and M-phase vanadium dioxide is a typical phase-change compound, which can be applied to intelligent temperature-controlled glass for buildings, photoelectric switches and other fields. Both D phase and B phase vanadium dioxide can be annealed in an inert gas to form M phase vanadium dioxide, and both vanadium dioxide can be annealed in air to form vanadium pentoxide. The size and shape...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/02
CPCC01G31/02C01P2002/72C01P2004/03C01P2004/16C01P2004/62C01P2004/64
Inventor 潘静李明罗媛媛钟莉王强吴昊李广海
Owner HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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