Phase-transition intelligent materials with adjustable phase-transition temperature and process for preparing same

A phase transition temperature and smart material technology, applied in the field of phase transition smart materials and their preparation, can solve the problems of vanadium dioxide losing low-temperature phase transition properties, difficult to ensure product uniformity and inhomogeneity, and reduce infrared transmittance. , The effect of reducing reflected light pollution

Inactive Publication Date: 2006-09-27
FUDAN UNIV
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  • Summary
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  • Claims
  • Application Information

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Problems solved by technology

For example, U.S. Patent No. 6,358,307 reports a method for synthesizing tungsten-doped vanadium dioxide. The synthesis route is to add soluble ammonium tungstate solution in ammonium metavanadate, then heat and drop hydrochloric acid solution, ammonium tungstate and ammonium metavanadate After condensation, a mixture of ammonium paratungstate (NH 4 ) 2 V 6 o 16 Paste liquid, filter, wash and dry the precipitate, put it in a sealed tube furnace and heat it to decompose to obtain doped vanadium dioxide; this method may not be uniform due to the fact that ammonium tungstate and ammonium vanadate are not mixed at the atomic level. And the decomposition process is a redox process, it is possible to get V n o 2n+1 and V n o 2n-1 Two sets of non-integer ratio compounds, which make VO 2 The valence state is not accurate enough, and the powder is stacked together, relying on NH 3 Diffusion is difficult to ensure the uniformity of the product
Chinese patent CN 1279211A reports a preparation method of vanadium dioxide nano-powder and nano-ceramic, adopting dropwise excess saturated ammonium bicarbonate solution in vanadyl dichloride solution to form basic ammonium vanadyl carbonate (IV) crystals , put the crystalline material in a tube furnace, heat and decompose it in a nitrogen stream containing a small amount of oxygen to obtain vanadium dioxide powder; this method is due to the fact that the decomposition gas contains NH 3 , while vanadium dioxide strongly adsorbs ammonia at high temperature and undergoes a reduction reaction, and the powder is stacked together, it is difficult to ensure the uniformity of the product by carrier gas diffusion, and it is easy to obtain a non-integral compound, which makes vanadium dioxide lose its low-temperature phase transition performance

Method used

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  • Phase-transition intelligent materials with adjustable phase-transition temperature and process for preparing same
  • Phase-transition intelligent materials with adjustable phase-transition temperature and process for preparing same
  • Phase-transition intelligent materials with adjustable phase-transition temperature and process for preparing same

Examples

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Effect test

Embodiment 1

[0053] In a beaker, control the temperature at 50°C, and prepare 100ml of 0.5mol / L vanadyl sulfate aqueous solution, 100ml of 4mol / L sodium bicarbonate aqueous solution, and 30ml of 0.5mol / L potassium molybdate aqueous solution at 500rpm rotating speed. In a reaction kettle equipped with a stirrer, a dropping funnel, and a condenser, at a speed of 500 rpm, the temperature is controlled at 40-50°C, the vanadyl sulfate aqueous solution and the potassium molybdate aqueous solution are mixed and stirred for 20 minutes, and the temperature is maintained at 40-50°C. After adding sodium bicarbonate solution dropwise for 3-4 hours, a hydrated hydroxide precipitate was obtained, the precipitate was filtered and washed with water until no SO 4 2- , and then washed with methyl amyl ketone for 1-2 times. In a nitrogen atmosphere, the doped amorphous precursor was placed in a muffle furnace, and the temperature was raised to 400-500 ° C for 10 hours at a high temperature to obtain a phase ...

Embodiment 2

[0055] In a beaker, control the temperature at 10-20°C, and prepare 100ml of 0.1mol / L vanadyl sulfate aqueous solution, 200ml of 0.01mol / L sodium hydroxide aqueous solution, 40ml of 0.1mol / L ammonium tantalate, 40ml of 0.01mol / L aluminum chloride aqueous solution, in a reaction kettle equipped with a stirrer, dropping funnel, and condenser, at a speed of 500rpm, control the temperature at 10-20°C, mix vanadyl sulfate aqueous solution and ammonium tantalate aqueous solution and aluminum chloride aqueous solution were mixed and stirred for 20 minutes, and the temperature was maintained at 10-20°C. After adding dropwise sodium hydroxide aqueous solution for 5-6 hours, a hydrated hydroxide precipitate was obtained, and the precipitate was filtered and washed with water until there was no SO 4 2- , and then washed with ethanol for 1-2 times, the obtained doped amorphous precursor was dried in a vacuum oven at 40°C for 6 hours, placed in a muffle furnace in a nitrogen atmosphere, an...

Embodiment 3

[0057] In a beaker, control the temperature at 10-20°C, and prepare 100ml of 5mol / L vanadyl sulfate aqueous solution, 100ml of 10mol / L sodium acetate aqueous solution, 20ml of 1mol / L ammonia aqueous solution, and 1ml of 0.5mol / L aqueous ammonia solution at 1000rpm. L potassium tungstate, 1ml of 0.5mol / L titanyl chloride aqueous solution, 1ml of 0.1mol / L ammonium molybdate aqueous solution, in a reactor equipped with a stirrer, dropping funnel, and condenser, at 500rpm, Control the temperature at 70-80°C, mix and stir vanadyl sulfate aqueous solution, potassium tungstate aqueous solution, titanyl chloride aqueous solution, and ammonium molybdate aqueous solution for 20 minutes, keep the temperature at 70-80°C, and add sodium acetate aqueous solution dropwise in 1-2 hours Mixed solution with aqueous ammonia solution to get hydrated hydroxide precipitate, filter the precipitate, wash with water until no SO 4 2- , the obtained doped amorphous precursor was dried in an oven at 80°...

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Abstract

The invention relates to an intelligent phase-change material with adjustable phase-change temperature and its preparing process, which comprises making doped vanadium dioxide precursor through liquid phase precipitation method, carrying out filtering, scouring, drying, heating and crystallizing. The crystal grain dimension of the obtained phase-change material is less than 100 nanometers, thus can be applied into intelligent window coating material and temperature measurement resistors.

Description

technical field [0001] The invention relates to the field of chemical industry, and relates to a phase-change smart material with adjustable phase-change temperature and a preparation method thereof. Background technique [0002] Scientists have found that vanadium dioxide is equal to (T C =68°C) will undergo crystal transformation from square structure to monoclinic structure, with reversible semiconductor-metal phase transition, low temperature phase has semiconductor properties, high infrared transmittance and low reflectivity, high temperature phase It has metallic properties, low infrared transmittance and high reflectivity, so it is a thermochromic material that can be applied to solar temperature control devices, photoelectric switch materials, thermistor materials, optical information storage, laser Blinding weapon protection devices, large-area thermochromic glass curtain walls, energy-saving coatings, polarizers and variable reflectors, etc. However, because its ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/02C09K3/00
Inventor 武利民施剑秋游波周树学顾广新
Owner FUDAN UNIV
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