CN105540667A - Preparation method of doping modified vanadium dioxide powder with lower phase transition temperature - Google Patents

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

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Publication number
CN105540667A
CN105540667A CN201511011913.4A CN201511011913A CN105540667A CN 105540667 A CN105540667 A CN 105540667A CN 201511011913 A CN201511011913 A CN 201511011913A CN 105540667 A CN105540667 A CN 105540667A
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preparation
vanadium dioxide
presoma
powder
doping
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陈伟
李植开
刘相
王雨琦
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Shandong Hairong Energy Saving New Material Co Ltd
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Shandong Hairong Energy Saving New Material Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G31/00—Compounds of vanadium
    • C01G31/02—Oxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G41/00—Compounds of tungsten
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM

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

There is the doping vario-property hypovanadic oxide powder preparation method of more low transformation temperature
Technical field
The present invention relates to a kind of preparation method with the vanadium dioxide ultrafine powder of low transformation temperature, the present invention is exactly a kind of preparation method with the hypovanadic oxide powder more vanadium dioxide ultrafine powder of low transformation temperature compared with prior art of W/Mo doping vario-property.
Background technology
Nineteen fifty-nine Morin has found VO 2the one-level reversible transformation of metal-semi-conductor can be there is at about 68 DEG C.In phase transformation simultaneously, VO 2stuctures and properties undergo mutation within the scope of nsec, the tetragonal of high temperature is changed to from the monocline of low temperature, simultaneously with the sudden change of optical property, electrical properties, such as, change in resistance 4-5 the order of magnitude, optics through (espespecially infrared band) will by high transmission change into low through even close to not through.Because phase transformation fore/aft properties there occurs leap, VO 2can be applied to different fields, the vanadium dioxide such as such as thermistor, thermic switch, variable mirror, CD media material, intelligent glass are a kind of phase-change metal compounds.Excellent vanadium dioxide film binary states transmissivity can reach 85% and 1% respectively.Can be used for the lasing safety of detector.Be arranged on infrared photoelectric sensor and photodetector window, the optical system preventing high power laser or thermal infrared ripple from damaging and optical element are also among development.
But VO 2transformation temperature higher than room temperature, this point limits the scope that material can be applied, and thus how to reduce VO 2transformation temperature become study hotspot.The method of usual employing is that the elements such as doping W, Mo, Ta, Nb reduce its transformation temperature.
There is the preparation VO of bibliographical information 2the method of nanometer powder doping first prepares VO 2powder, then carries out solid phase doping with doping agent by ratio requirement.This method will introduce impurity when ball milling, and some raw material used is inherently not easily prepared, and there is certain shortcoming.
The Zheng Chenmou of Zhongshan University etc. utilize presoma (NH 4) 5{ (VO) 6(CO 3) 4(OH) 910H 2o synthesizing blender parent, decomposes and obtains V in nitrogen 1-xm xo 2powder.
The wavelength region of solar radiation flow is at 350 ~ 2500nm, and wherein the energy of visible ray accounts for 1/3, all the other 2/3 mainly thermal radiation energy.Conventional clear glass transmission range is between 300 ~ 5000nm.Wherein transmissivity that is visible and near-infrared band is greater than 80%, and the transmissivity about 10% of middle-infrared band, just in time overlaps with solar radiation spectral region.
Before and after vanadium dioxide intensification phase transformation, the change of its visible light transmissivity is not obvious, but infrared transmittivity declines and can reach 50%; And reflectivity rises to high reverse--bias gradually by low reflection simultaneously.Therefore, vanadium dioxide is excellent energy-saving glass material, can realize energy-conservation object with simple glass compound.Relative to commercial building energy conservation glass, reach by controlling vanadium dioxide phase critical point the object regulating room temp, thus realize the intellectuality of building energy conservation glass.And the doping vario-property of vanadium dioxide ultrafine powder material, be one of prerequisite realizing smart window Practical Performance.
Therefore, find green, easy synthetic method prepares the VO of phase transformation temperature points close to room temperature 2nano material is also current research focus.
Summary of the invention
The invention provides a kind of VO 2the preparation method of nano material, the VO prepared by the method 2its transformation temperature of nano material can reduce by more than 10 DEG C.
The preparation method with the doping vario-property hypovanadic oxide powder of more low transformation temperature of the present invention, be with tungstenic and containing the compound of molybdenum for adulterating in tungsten source and molybdenum source, W and Mo is with VO 2atomic percent 1 ~ 10% adulterate, utilize coprecipitation method adulterate prepare W-VO 2or Mo-VO 2presoma, then by obtained W-VO 2or Mo-VO 2presoma inert atmosphere protection under 450 ~ 700 DEG C carry out calcination process, then under protective atmosphere, slowly automatically cool to room temperature, then carry out the nano vanadium dioxide superfine powder that dispersion treatment obtains W or Mo doping vario-property.
In the preparation method of the doping vario-property hypovanadic oxide powder with more low transformation temperature of the present invention, be by V 2o 5with W or V 2o 5with vanadium at H 2sO 4, HCl or HNO 3in system, system pH=3 ~ 10, use SO 2, NaBH 4, hydrazine, azanol, oxalic acid, formic acid, formaldehyde, methyl alcohol, in ethanol, the reductive agent of one or both arbitrary proportion combination reduces, and obtains W-VO 2or Mo-VO 2presoma, tungsten source used of adulterating is soluble tungstate salt or WO 3or WOCl 4in any one or appoint several combination; Described molybdenum source such as is at soluble molybdenum hydrochlorate or the MoO 3or MOCl 4in any one or appoint several combination; Dispersion treatment refers to grinding.
The preparation method with the doping vario-property hypovanadic oxide powder of more low transformation temperature of the present invention, is adulterate under the condition of pH=4, obtains W-VO 2or Mo-VO 2presoma, W-VO 2or Mo-VO 2presoma under high pure nitrogen or argon shield 550-650 DEG C carry out calcination process 1 ~ 7 hour.
This preparation method by chemical doping at VO 2introducing hetero-atoms in lattice, because heteroatoms ionic radius is slightly larger than V 4 +ionic radius, when its replace V 4+impel unit cell volume to there occurs change during position on lattice point, result in original V-V key and V-O key extends, make the changes in crystal structure of vanadium dioxide, thus change its transformation temperature.
Method of the present invention owing to not being physical doping, the VO of therefore prepared W/Mo doping 2nano material cost is low, and purity is high.
Accompanying drawing explanation
Fig. 1 vanadium dioxide powder DTA schemes,
Fig. 2 VO of the present invention 2the stereoscan photograph of nano-powder,
Fig. 3 VO of the present invention 2the various temperature IR figure of nano-powder,
Fig. 4 is through the VO of 500 DEG C of process 2the stereoscan photograph of nano-powder and electron-diffraction diagram, wherein the upper left corner is electron-diffraction diagram,
Fig. 5. W doping VO of the present invention 2the differential thermal figure of nano-powder material.
Embodiment
W/Mo of the present invention doping VO is below provided 2the preparation embodiment of nano-powder material and sign.
The preparation method of doping vario-property hypovanadic oxide powder of the present invention is by V 2o 5with W or V 2o 5with vanadium at H 2sO 4, HCl or HNO 3in system, system pH=3 ~ 10, use SO 2, NaBH 4, hydrazine, azanol, oxalic acid, formic acid, formaldehyde, methyl alcohol, in ethanol, the reductive agent of one or both arbitrary proportion combination reduces, and obtains W-VO 2or Mo-VO 2presoma, tungsten source used of adulterating is soluble tungstate salt or WO 3or WOCl 4in any one or appoint several combination; Described molybdenum source such as is at soluble molybdenum hydrochlorate or the MoO 3or MOCl 4in any one or appoint several combination; Dispersion treatment refers to grinding.
Embodiment 1: nanometer VO 2preparation
V 2O 5+H 2SO 4+Red→2VOSO 4+H 2O
VOSO 4+2KOH→VO 2+K 2SO 4
Wherein, Red is SO 2, NaBH 4, hydrazine, azanol, oxalic acid, formic acid, formaldehyde, methyl alcohol, in the reductive agents such as ethanol one or more, in this example, with SO 2for example.
1.8g Vanadium Pentoxide in FLAKES, 3.0 ~ 5.0ml vitriol oil and 4 – 8ml deionized waters mix, and heating in water bath 20-60 minute, thin up is to 40-50ml.Under the condition stirred, constantly pass into brand-new sulfurous gas, until the Vanadium Pentoxide in FLAKES suspension liquid in acidic medium is completely reduced au bleu VO 2+solution.
After having reacted, vanadium dioxide residual in solution is driven in ventilation out of.Then slowly dropping KOH solution or ammonia soln adjust ph are 4-6.Now have brown-green to precipitate to generate.
Precipitation suction filtration gained sample is transferred in quartz boat, then quartz boat is put into silica tube.At high vacuum (0.5-5pa), 600-900h obtains heat-treatment of annealing 6-9h under condition, can obtain well-crystallized and obtain nano vanadium dioxide powder after cooling.This nano vanadium dioxide powder DTA characterizes and confirms that its transformation temperature is 69 DEG C, see Fig. 1.Prepared nano vanadium dioxide powder TEM characterizes and confirms that its median size is 30-40nm, see Fig. 2.The corresponding Temperature-dependent IR of prepared nano vanadium dioxide powder characterizes as shown in Figure 3, as seen from Figure 3, and 682cm in infrared spectrum -1, 527cm -1the absorption peak at place is warmed up to more than 68 DEG C disappearances, again occurs when being cooled to below 68 DEG C, shows 68 DEG C of transformation temperatures for sample.And fit like a glove with the spectral line of being down to room temperature before heating up, illustrate that this sample has reversible transformation character.
The nanometer VO of embodiment 2W doping vario-property 2preparation
As obtained blue VO in embodiment 1 2+after solution, in this system, add WO 3, or soluble tungstate salt, wherein W=1 ~ 7%, control pH4 ~ 6, by W and VO 2+co-precipitation.This coprecipitated product is heat-treatment of annealing 6-9h under 600-900h obtains condition, obtains W dopen Nano VO 2powder.This nano material xps energy spectrum characterizes and confirms, the absorption peak being positioned at 516.2eV in spectrogram is attributed to V 2p3/2, and V is+4 valencys; The absorption peak being positioned at 35.30eV belongs to W 4f7/2(W is+6 valencys), thus show that W is atom doped in VO 2in.Corresponding TEM characterizes see Fig. 4, and the differential thermal of this nano material characterizes its transformation temperature and has been reduced to 58 DEG C, and comparatively previous materials has reduced 10 degree.
Change tungsten source in embodiment 2 into corresponding MoO 3or soluble molybdenum hydrochlorate, the nanometer VO of Mo doping can be obtained 2particulate, the nanometer VO that its relevant phase transformation and optical property and W adulterate 2particulate similar nature.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.

Claims (3)

1. there is the preparation method of the doping vario-property hypovanadic oxide powder of more low transformation temperature, it is characterized in that with VO 2for presoma, with tungstenic and containing the compound of molybdenum for adulterating in tungsten source and molybdenum source, W and Mo is with VO 2atomic percent 1 ~ 10% adulterate, utilize coprecipitation method adulterate prepare W-VO 2or Mo-VO 2presoma, then by obtained W-VO 2or Mo-VO 2presoma inert atmosphere protection under 450 ~ 700 DEG C carry out calcination process, then under protective atmosphere, slowly automatically cool to room temperature, then carry out the nano vanadium dioxide superfine powder that dispersion treatment obtains W or Mo doping vario-property.
2. the preparation method with the doping vario-property hypovanadic oxide powder of more low transformation temperature according to claim 1, is characterized in that V 2o 5with W or V 2o 5with vanadium at H 2sO 4, HCl or HNO 3in system, system pH=3 ~ 10, use SO 2, NaBH 4, hydrazine, azanol, oxalic acid, formic acid, formaldehyde, methyl alcohol, in ethanol, the reductive agent of one or both arbitrary proportion combination reduces, and obtains W-VO 2or Mo-VO 2presoma, tungsten source used of adulterating is soluble tungstate salt or WO 3or WOCl 4in any one or appoint several combination; Described molybdenum source such as is at soluble molybdenum hydrochlorate or the MoO 3or MOCl 4in any one or appoint several combination; Dispersion treatment refers to grinding.
3. the preparation method with the doping vario-property hypovanadic oxide powder of more low transformation temperature according to claims 1 or 2, is characterized in that adulterating under the condition of pH=4, obtains W-VO 2or Mo-VO 2presoma, W-VO 2or Mo-VO 2presoma under high pure nitrogen or argon shield 550-650 DEG C carry out calcination process 1 ~ 7 hour.
CN201511011913.4A 2015-12-30 2015-12-30 Preparation method of doping modified vanadium dioxide powder with lower phase transition temperature Pending CN105540667A (en)

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Cited By (7)

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CN108659812A (en) * 2018-05-11 2018-10-16 中国科学院广州能源研究所 A kind of efficient thermochromism composite nano-powder of nucleocapsid and preparation method thereof
CN109192934A (en) * 2018-07-24 2019-01-11 北京理工大学 A kind of porous silica vanadium micron ball composite material and preparation method of graphene support
CN112574602A (en) * 2020-11-20 2021-03-30 深圳市奥拓电子股份有限公司 Automatic temperature control LED display screen, mask and manufacturing method
CN112978798A (en) * 2021-02-02 2021-06-18 昆明理工大学 Method and device for preparing molybdenum oxide nano material with adjustable phase, shape and size
CN113173599A (en) * 2021-05-07 2021-07-27 南京理工大学 Preparation method and application of vanadium dioxide material containing oxygen vacancies
CN113754307A (en) * 2021-09-29 2021-12-07 中山市中佳新材料有限公司 Thermochromic film and preparation method thereof
CN114672094A (en) * 2022-04-02 2022-06-28 兰州大学 Modified nanometer VO of intelligence window2High polymer composite membrane and preparation method thereof

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108659812A (en) * 2018-05-11 2018-10-16 中国科学院广州能源研究所 A kind of efficient thermochromism composite nano-powder of nucleocapsid and preparation method thereof
CN108659812B (en) * 2018-05-11 2020-07-03 中国科学院广州能源研究所 Efficient thermochromic nano composite powder with core-shell structure and preparation method thereof
CN109192934A (en) * 2018-07-24 2019-01-11 北京理工大学 A kind of porous silica vanadium micron ball composite material and preparation method of graphene support
CN112574602A (en) * 2020-11-20 2021-03-30 深圳市奥拓电子股份有限公司 Automatic temperature control LED display screen, mask and manufacturing method
CN112978798A (en) * 2021-02-02 2021-06-18 昆明理工大学 Method and device for preparing molybdenum oxide nano material with adjustable phase, shape and size
CN113173599A (en) * 2021-05-07 2021-07-27 南京理工大学 Preparation method and application of vanadium dioxide material containing oxygen vacancies
CN113173599B (en) * 2021-05-07 2022-03-11 南京理工大学 Preparation method and application of vanadium dioxide material containing oxygen vacancies
CN113754307A (en) * 2021-09-29 2021-12-07 中山市中佳新材料有限公司 Thermochromic film and preparation method thereof
CN114672094A (en) * 2022-04-02 2022-06-28 兰州大学 Modified nanometer VO of intelligence window2High polymer composite membrane and preparation method thereof

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