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Method for directly synthesizing M-phase vanadium dioxide nano particles by liquid phase method

A technology of vanadium dioxide nanometer and liquid phase method, which is applied in the field of preparation of functional inorganic materials, can solve the problems of large particle size of M-phase VO2, high preparation cost, complicated process, etc., achieve significant competitive advantages and profit margins, and mild production conditions Effect

Active Publication Date: 2012-08-01
DALIAN NATIONALITIES UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

By comparison, it is found that the current method is either complicated in process and high in preparation cost; or the prepared M-phase VO 2 Larger particle size, usually at the micron level

Method used

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  • Method for directly synthesizing M-phase vanadium dioxide nano particles by liquid phase method

Examples

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Effect test

Embodiment 1

[0015] Take 0.3637g of vanadium pentoxide and 30-60mL of distilled water on a heating magnetic stirrer (60-100°C, 450-1100r / min) and mix for 10-30min to form a uniform suspension; then add 4mL of the prepared hydrazine hydrochloride solution ( V: hydrazine hydrochloride=1: 3) is slowly added dropwise in the vanadium pentoxide suspension that mixes homogeneously, continues reaction 1~6 hour, uses hydrochloric acid to regulate pH value in the reaction process and remains in the scope of 1~3; The reaction product is subjected to centrifugation (8000-12000 rad / min, 10-15 min) to obtain a precipitate of the reaction precursor. Mix the precursor precipitate with 50mL of distilled water and transfer it to a reaction steel kettle with a polytetrafluoroethylene liner. After the filling rate is 60-70%, the reaction temperature is 240°C, and the reaction time is 36h, it is cooled at room temperature and centrifuged (8000~ 12000rad / min, 10~15min), washing (washing with distilled water and...

Embodiment 2

[0017] Take 0.3637g of vanadium pentoxide and 30-70mL of distilled water on a heating magnetic stirrer (60-100°C, 450-1100r / min) and mix for 20-30min to form a uniform suspension; then add 10mL of the prepared oxalic acid solution (V : oxalic acid=1: 2) is slowly added dropwise in the mixed ammonium metavanadate solution, adjusts pH to be 2~3 with sulfuric acid solution, continues reaction 1~3 hour; Reaction product is carried out centrifugation (8000~12000rad / min, 10-15min) to obtain the precipitation of the reaction precursor. Mix the precursor precipitate with 70mL of distilled water and transfer it to a reaction steel kettle with a polytetrafluoroethylene liner. After the filling rate is 60-70%, the reaction temperature is 260°C, and the reaction time is 48 hours, it is cooled at room temperature and centrifuged (8000~ 12000rad / min, 10~15min), washing (washing with distilled water and absolute ethanol for 2~4 times respectively), drying (temperature not higher than 100°C,...

Embodiment 3

[0019] Take 0.4680g of ammonium metavanadate and 10-40mL of distilled water on a heated magnetic stirrer (60-120°C, 450-1100r / min) and mix for 20-30min to form a uniform suspension; then mix 5mL of the prepared hydrazine hydrate solution ( V: hydrazine hydrate = 1: 1) is slowly added dropwise in the uniformly mixed ammonium metavanadate solution, and the pH is adjusted to about 3 with hydrochloric acid, and the reaction is continued for 4 to 6 hours; the reaction product is centrifuged (8000 to 12000 rad / min, 10-15min) to obtain the precipitation of the reaction precursor. Mix the precursor precipitate with 40mL of distilled water and transfer it to a reaction steel kettle with a polytetrafluoroethylene liner. After the filling rate is 70-80%, the reaction temperature is 220 ° C, and the reaction time is 24 hours, it is cooled at room temperature and centrifuged (8000~ 12000rad / min, 10~15min), washing (washing with distilled water and absolute ethanol for 2~4 times respective...

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Abstract

The invention provides a method for directly synthesizing M-phase vanadium dioxide nano particles by a liquid phase method. The method comprises the following steps of: dissolving one or a mixture of vanadium pentoxide and metavanadate, which is taken as a raw material in water, heating under normal pressure with stirring, slowly dripping a reducing agent, and reacting at constant temperature to obtain precursor substance; and centrifuging and precipitating the precursor substance, mixing with distilled water, transferring into a reaction steel kettle with a teflon lining, and controlling phase purity and the particle size of a product by controlling reaction temperature, reaction time, reaction kettle filling rate, substance concentration and the like to obtain black blue M-phase vanadium dioxide nano particles. The preparation process is performed under the condition of liquid phase, a solid-phase high-temperature heating step is eliminated, and the method belongs to a low-carbon technology; and moreover, the generation condition of M-phase vanadium dioxide is mild and easy to control, and the particle size of the product is in a nano level. The method has obvious competition advantages and profit margins in the aspects of manufacturing cost, product performance, environment-friendliness and the like.

Description

technical field [0001] The invention belongs to the technical field of preparation of functional inorganic materials, in particular to a low-cost and rapid preparation method of nano-scale M-phase vanadium dioxide temperature-sensitive phase-change nanomaterials. Background technique [0002] M phase vanadium dioxide (VO 2 ) is a phase-change metal oxide, at temperature T c = 68°C, a reversible crystal phase transition (from M-phase monoclinic crystal structure to R-phase rutile structure) occurs, and at the same time, its resistivity and infrared light transmittance undergo a sudden change. Therefore, in intelligent windows that automatically adjust temperature, Infrared detectors, laser protective layers and other fields have been widely used. But VO 2 It has a variety of crystal phase structures such as B phase, M phase, R phase and A, and they belong to allotropes, of which only M phase VO 2 It has a temperature-sensitive phase transition function. At the same time,...

Claims

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Application Information

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IPC IPC(8): C01G31/02B82Y40/00
Inventor 齐济牛晨
Owner DALIAN NATIONALITIES UNIVERSITY
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