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Preparation method of doping modified vanadium dioxide powder with lower phase transition temperature

A phase transition temperature, vanadium dioxide technology, applied in vanadium oxide, chemical instruments and methods, tungsten compounds, etc., can solve problems such as difficult preparation, and achieve the effect of low cost and high purity

Inactive Publication Date: 2016-05-04
SHANDONG HAIRONG ENERGY SAVING NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method will introduce impurities during ball milling, and some raw materials used are not easy to prepare, so there are certain shortcomings

Method used

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  • Preparation method of doping modified vanadium dioxide powder with lower phase transition temperature
  • Preparation method of doping modified vanadium dioxide powder with lower phase transition temperature
  • Preparation method of doping modified vanadium dioxide powder with lower phase transition temperature

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1: Nano VO 2 preparation of

[0023] V 2 o 5 +H 2 SO 4 +Red→2VOSO 4 +H 2 o

[0024] VOSO 4 +2KOH→VO 2 +K 2 SO 4

[0025] Among them, Red is SO 2 , NaBH 4 , one or more of reducing agents such as hydrazine, hydroxylamine, oxalic acid, formic acid, formaldehyde, methanol, ethanol, etc. In this example, SO 2 as an example.

[0026] Mix 1.8g vanadium pentoxide, 3.0~5.0ml concentrated sulfuric acid and 4–8ml deionized water evenly, heat in a water bath for 20-60 minutes, add water to dilute to 40-50ml. Under the condition of stirring, the newly produced sulfur dioxide is continuously introduced until the suspension of vanadium pentoxide in the acidic medium is completely reduced to blue VO 2+ solution.

[0027] After the reaction is completed, ventilate to drive out the residual vanadium dioxide in the solution. Then slowly drop KOH solution or ammonia solution to adjust the pH value to 4-6. At this time, a brown-green precipitate formed.

[00...

Embodiment 2W

[0029] The nanometer VO of embodiment 2W doping modification 2 preparation of

[0030] Obtain blue VO as in embodiment 1 2+ solution, add WO to the system 3 , or soluble tungstate, where W=1~7%, control pH4~6, mix W and VO 2+ Total precipitation. The co-precipitated product is annealed for 6-9h under the condition of 600-900h to obtain W-doped nano-VO 2 Powder. The XPS energy spectrum characterization of the nanomaterials confirmed that the absorption peak at 516.2eV in the spectrum is assigned to V 2p3 / 2 , and V is +4 valence; the absorption peak at 35.30eV is attributed to W 4f7 / 2 (W is +6 valence), thus indicating that W atoms are doped in VO 2 middle. For the corresponding TEM characterization see Figure 4 According to the differential thermal analysis of the nanomaterial, its phase transition point has been reduced to 58°C, which is 10 degrees lower than that of the aforementioned materials.

[0031] Change the tungsten source into corresponding MoO in embodime...

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Abstract

The invention discloses a preparation method of vanadium dioxide ultrafine powder modified by doping W / Mo and having the phase transition temperature lower than that of the vanadium dioxide powder of the prior art. The preparation method of the vanadium dioxide powder comprises the following steps: doping by adopting a tungsten containing compound and a molybdenum containing compound as a tungsten source and a molybdenum source and by using a co-precipitation method to prepare a W-VO2 or Mo-VO2 precursor, roasting the obtained W-VO2 or Mo-VO2 precursor under the protection of an inert atmosphere at 450 to 700 DEG C, slowly and automatically cooling to the room temperature under the protection atmosphere, and then dispersing to obtain the W or Mo doped modified nano vanadium dioxide ultrafine powder. Since the method adopts no physical doping, the prepared W / Mo doped VO2 nano material is relatively low in cost and high in purity, and the obtained powder has much lower phase transition temperature compared with the VO2 nano material in the prior art.

Description

technical field [0001] The present invention relates to a preparation method of vanadium dioxide ultrafine powder with low phase transition temperature. Specifically, the present invention is a kind of vanadium dioxide powder modified with W / Mo doping and has higher vanadium dioxide powder than the prior art. A method for preparing vanadium dioxide ultrafine powder with low phase transition temperature. Background technique [0002] In 1959 Morin discovered VO 2 A metal-semiconductor first-order reversible phase transition can occur at about 68°C. At the same time as the phase change, VO 2 The structure and performance of the structure and properties of the nanometer change suddenly in the time range of nanoseconds, from the monoclinic structure at low temperature to the tetragonal structure at high temperature, accompanied by the sudden change of optical and electrical properties, for example, the resistivity changes by 4-5 orders of magnitude, the optical transparency P...

Claims

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Application Information

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IPC IPC(8): C01G31/02C01G41/00B82Y30/00
CPCB82Y30/00C01G31/02C01G41/00C01P2002/80C01P2002/82C01P2004/03
Inventor 陈伟李植开刘相王雨琦
Owner SHANDONG HAIRONG ENERGY SAVING NEW MATERIAL CO LTD
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