CN105858725A - Method for preparing silica-coated vanadium dioxide nanoparticles through alcohol-water solution method - Google Patents
Method for preparing silica-coated vanadium dioxide nanoparticles through alcohol-water solution method Download PDFInfo
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- CN105858725A CN105858725A CN201610230734.8A CN201610230734A CN105858725A CN 105858725 A CN105858725 A CN 105858725A CN 201610230734 A CN201610230734 A CN 201610230734A CN 105858725 A CN105858725 A CN 105858725A
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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
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- 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
- C01P2002/88—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by thermal analysis data, e.g. TGA, DTA, DSC
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- 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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
- C01P2004/84—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases one phase coated with the other
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
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Abstract
The invention relates to a method for preparing silica-coated vanadium dioxide nanoparticles through an alcohol-water solution method. The method comprises the steps that 1, an alcohol-water mixed solution containing 2-15 ml of water and 400 ml of alcohol is prepared; 2, 0.1-5 g of vanadium dioxide (VO2) is weighed and put into a ball mill to be milled for 10 min; 3, milled VO2 particles are ultrasonically dispersed in the alcohol-water mixed solution for an ultrasonic reaction, and a VO2 dispersion mixed solution is obtained; 4, 2-15 ml of ammonia water is added into the dispersion mixed solution, and magnetic stirring is conducted; 5, under the stirring condition, 0.15-0.5 ml of ethyl orthosilicate is dripped to the stirred dispersion mixed solution according to the dripping speed of 0.5 ml/h to 6 ml/h, and room-temperature stirring is conducted for 6 h to 12 h; 6, high-speed centrifugation is conducted after stirring is conducted; 7, cleaning is conducted with ethyl alcohol and water in sequence; 8, freeze-drying is conducted on the cleaned reaction product, and the silica-coated vanadium dioxide (VO2@SiO2) nanoparticles are obtained. The method is easy and convenient to operate, no surfactant is used, and the environment is not polluted; the silica-coated vanadium dioxide nanoparticles are spin-coated into films, and the visible light transmittance is increased by 20%.
Description
Technical field
The present invention relates to a kind of normal temperature, surfactant-free alcohol-water dissolving prepares coated with silica vanadium dioxide nano particle method, belongs to energy-saving material preparing technical field.
Background technology
People regulate being mainly of indoor temperature and regulate indoor temperature by heating, electric fan, air-conditioning, and this regulative mode energy consumption is big, does not meets energy-saving and emission-reduction and the theory of sustainable Green Development.Therefore, using high-performance energy-saving heat-insulating glass is one of effective way reducing energy consumption.
The energy-saving heat-insulating glass of regulation indoor temperature is by preparing transparent heat insulating dope and film.The nano particle of energy-saving heat-insulating glass mainly has alundum (Al2O3), titanium dioxide, vanadium dioxide etc. at present.Pure vanadium dioxide is as a kind of phase-change material, when low temperature with M phase in the presence of, near infrared light transmitance is high, when reaching its phase transition temperature, its near infrared light transmitance drastically declines, and we can carry out Intelligent adjustment to its near infrared light transmitance thus reach the effect of smart window " cool in summer and warm in winter " to utilize this feature.But, VO2The deficiencies such as high (68 DEG C) poor chemical stability of own phase transition temperature, oxidizable, visible light transmissivity is low greatly limit the application in smart window field.Pertinent literature is reported, by elemental tungsten (W) doped vanadium dioxide, phase transition temperature can be reduced to room temperature, simultaneously in order to improve chemical stability, by being coated with one layer of high material of chemical stability (such as TiO in nanoparticle surface2、ZrO2、SiO2) improve VO2The chemical stability of material and non-oxidizability.Owing to material that one layer of chemical stability of nanoparticle surface coated silica is high has, optical transmittance is good, chemically stable, raw material feature simple and easy to get so that silica SiO2It is better than other covering materials as a kind of covering material.But, the preparation method of current coated with silica vanadium dioxide nano particle is by surfactant modified and be coated with by St ber method, and preparation process is complicated, and with a lot of silica SiO2Homogeneous nucleation, reunites serious, causes material scatter to decline.
Summary of the invention
It is an object of the invention to there are provided a kind of employing normal temperature surfactant-free alcohol-water dissolving and quickly prepare coated with silica vanadium dioxide nano particle method, the method is the most easy and simple to handle, free from environmental pollution, and the coated with silica vanadium dioxide nano particle prepared has higher visible light transmissivity.
A kind of normal temperature surfactant-free alcohol-water dissolving of the present invention prepares coated with silica vanadium dioxide nano particle method, comprises the steps:
(1). configuration 2～15ml water and the alcohol-water mixture of 400ml alcohol, put it in wide-mouth bottle；
(2). weigh the vanadium dioxide VO of 0.1～5 g2It is placed in ball mill, grinds 10 minutes, obtain vanadium dioxide VO2Particle；
(3). the vanadium dioxide VO after grinding2Particle ultrasonic disperse carries out ultrasonic reaction, ultrasonic time 0.5～3 hours in above-mentioned alcohol-water mixture, obtains vanadium dioxide VO2Dispersion mixing liquid；
(4). the ammoniacal liquor adding 2～15ml again in above-mentioned dispersion mixing liquid carries out magnetic agitation, and magnetic agitation speed is 150～500 r/min, and mixing time is 5～30 minutes；
(5). under agitation, it is 0.5～6ml/h according to rate of addition, the tetraethyl orthosilicate of 0.15～0.5ml is added drop-wise in the dispersion mixing liquid after above-mentioned stirring, 6～12 hs are stirred at room temperature；
(6). high speed centrifugation after stirring, obtain product；
(7). clean 3～4 times successively with second alcohol and water again；
(8). the product after cleaning is carried out freeze-drying, and baking temperature be-10～-70 DEG C, prepared coated with silica vanadium dioxide (VO2@SiO2) nano particle.
Alcohol described in above-mentioned steps (1) is one or more in methyl alcohol, ethanol, propyl alcohol, isopropanol, glycerine, n-butanol.
Vanadium dioxide VO described in above-mentioned steps (3)2Dispersion mixing liquid, wherein, vanadium dioxide VO2Mass body fraction and alcohol-water mixture mark be 1～5%.
The preparation method of the present invention compared with prior art, has remarkable result, has the following characteristics that
1. the method for the present invention does not use any surfactant, free from environmental pollution；
2. the method for the present invention uses tetraethyl orthosilicate and water to be raw material, low cost；
3. the method for the present invention is easy and simple to handle；
4. using coated with silica vanadium dioxide nano particle spin-coating film prepared by the present invention, its visible light transmissivity improves 20% after tested.
Accompanying drawing explanation
Fig. 1 is the (VO that embodiment 1 prepares2@SiO2) the transmission electron microscope TEM diffraction pattern of nano particle.
Fig. 2 is the (VO that embodiment 1 prepares2@SiO2) the transmission electron microscope HRTEM diffraction pattern of nano particle.
Fig. 3 is the (VO that embodiment 1 prepares2@SiO2) nano particle thermogravimetric analysis TG figure.
Fig. 4 is the (VO that embodiment 1 prepares2@SiO2) the oxidizing temperature figure of nano particle.
Fig. 5 is that embodiment 1 prepares standby (VO2@SiO2) the optical transmittance figure of nano particle.
Detailed description of the invention
The present invention is made the most in detail below in conjunction with embodiment, comparative example and accompanying drawing, intactly illustrates.
Embodiment one
A kind of alcohol-water dissolving prepares coated with silica vanadium dioxide nano particle method, its step:
(1). configure 10 ml water and the alcohol-water mixture of 400ml alcohol, put it in wide-mouth bottle；
(2). weigh the vanadium dioxide VO of 0.1 g2It is placed in ball mill, grinds 10 minutes, obtain vanadium dioxide VO2Particle；
(3). the vanadium dioxide VO after grinding2Particle ultrasonic disperse carries out ultrasonic reaction, ultrasonic time 0.5 hour in above-mentioned alcohol-water mixture, obtains vanadium dioxide VO2Dispersion mixing liquid；
(4). the ammoniacal liquor adding 6ml again in above-mentioned dispersion mixing liquid carries out magnetic agitation, and magnetic agitation speed is 300 r/min, and mixing time is 10 minutes；
(5). under agitation, it is 6ml/h according to rate of addition, the tetraethyl orthosilicate of 0.15ml is added drop-wise in the dispersion mixing liquid after above-mentioned stirring, 8 hs are stirred at room temperature；
(6). high speed centrifugation after stirring, obtain product；
(7). clean 3～4 times successively with second alcohol and water again；
(8). the product after cleaning is carried out freeze-drying, and baking temperature is-50 DEG C, prepares coated with silica vanadium dioxide (VO2@SiO2) nano particle.
With TEM, the HRTEM coated with silica vanadium dioxide (VO to above-mentioned preparation2@SiO2) pattern of nano particle and performance be tested.Fig. 1 is coated with silica vanadium dioxide (VO2@SiO2) the TEM photo of nano particle, the nano particle favorable dispersibility after display cladding, cladding thickness is uniform, without silica homogeneous nucleation.Fig. 2 is coated with silica vanadium dioxide (VO2@SiO2) the HRTEM photo of nano particle, display coated with silica layer thickness is uniform, and a size of 5nm.Fig. 3 is coated with silica vanadium dioxide (VO2@SiO2) nano particle TG figure, show vanadium dioxide (VO after coated silica2@SiO2) nano particle starts oxidation reaction at 330 DEG C.Fig. 4 is coated with silica vanadium dioxide (VO2@SiO2) nano particle different in atmosphere heating rates under oxidizing temperature figure, the curve from Fig. 4 shows, oxidation onset temperature is above 310 DEG C, and along with the oxidation onset temperature improving nano particle of heating rate declines。
In order to detect the coated with silica vanadium dioxide (VO of the present invention2@SiO2)
VO2@SiO2) the optical transmittance performance of nano particle, using ultraviolet near infrared spectrum tester to test, be dispersed in by material in the PVP aqueous solution of 1:1, ultra-clear glasses is substrate, with 600rmp/min spin-coating film, UH4150 type spectrophotometer (Spectrophotometer (Direct
Light Detector)) detection.Fig. 5 is coated with silica vanadium dioxide (VO2@SiO2) optical transmittance of nano particle, the optics visible light transmissivity after display coated with silica vanadium dioxide improves 20%.
Claims (3)
1. alcohol-water dissolving prepares a coated with silica vanadium dioxide nano particle method, it is characterized in that, comprises the steps:
Configuration 2～15ml water and the alcohol-water mixture of 400ml alcohol, put it in wide-mouth bottle；
Weigh 0.1～5 g's
Vanadium dioxide VO2It is placed in ball mill, grinds 10 minutes, obtain vanadium dioxide VO2Particle；
Vanadium dioxide VO after grinding2Particle ultrasonic disperse carries out ultrasonic reaction, ultrasonic time 0.5～3 hours in above-mentioned alcohol-water mixture, obtains vanadium dioxide VO2Dispersion mixing liquid；
The ammoniacal liquor adding 2～15ml again in above-mentioned dispersion mixing liquid carries out magnetic agitation, and magnetic agitation speed is 150～500 r/min, and mixing time is 5～30 minutes
；
Under agitation, it is 0.5～6ml/h according to rate of addition, the tetraethyl orthosilicate of 0.15～0.5ml is added drop-wise in the dispersion mixing liquid after above-mentioned stirring, 6～12 hs are stirred at room temperature；
High speed centrifugation after stirring, obtains product；
3～4 times are cleaned successively again with second alcohol and water
；
Product after cleaning is carried out freeze-drying, and baking temperature be-10～-70 DEG C, prepared coated with silica vanadium dioxide (VO2@SiO2) nano particle.
2. prepare coated with silica vanadium dioxide nano particle method according to a kind of alcohol-water dissolving described in claim 1, it is characterized in that, the alcohol described in above-mentioned steps (1) is one or more in methyl alcohol, ethanol, propyl alcohol, isopropanol, glycerine, n-butanol.
3. prepare coated with silica vanadium dioxide nano particle method according to a kind of alcohol-water dissolving described in claim 1, it is characterised in that the vanadium dioxide VO described in above-mentioned steps (3)2Dispersion mixing liquid, wherein, vanadium dioxide VO2Mass body fraction and alcohol-water mixture mark be 1～5%.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106675115A (en) * | 2016-11-28 | 2017-05-17 | 江南大学 | Preparation method of high-transmittance thermochromatic intelligent recoating |
| CN108394907A (en) * | 2018-05-29 | 2018-08-14 | 中国科学院青岛生物能源与过程研究所 | A kind of silicon vanadium oxides composite and preparation method thereof |
| CN108751256A (en) * | 2018-05-15 | 2018-11-06 | 清华大学 | A kind of preparation method of high performance lithium ion battery anode material vanadium oxide |
| CN109294277A (en) * | 2017-07-25 | 2019-02-01 | 上海大学 | A kind of vanadium dioxide and preparation method thereof that surface is modified |
| CN110003882A (en) * | 2019-04-04 | 2019-07-12 | 东华大学 | A kind of structure of controlling temperature color dyestuff and its preparation and application |
| CN110937819A (en) * | 2019-12-09 | 2020-03-31 | 东莞深圳清华大学研究院创新中心 | Preparation method of transparent super-hydrophobic intelligent temperature control glass |
| CN111039261A (en) * | 2019-12-12 | 2020-04-21 | 上海大学 | Liquid-phase high-concentration nano particle coating method |
| CN111725334A (en) * | 2020-06-30 | 2020-09-29 | 浙江晶科能源有限公司 | Coating liquid for photovoltaic module, preparation method of coating liquid and photovoltaic module |
| CN112059172A (en) * | 2020-09-16 | 2020-12-11 | 浙江工业大学 | SiO is carried out to micron order granule2Method of coating |
| CN113130745A (en) * | 2021-04-16 | 2021-07-16 | 中国人民解放军陆军工程大学 | VO2@SiO2Nano particle filled type electric field phase change composite material and its preparation method |
| CN113956864A (en) * | 2021-09-22 | 2022-01-21 | 河南龙德福新材料科技研究院有限公司 | Low-density high-strength ceramsite proppant coated by silicon dioxide and preparation method thereof |
| CN114890473A (en) * | 2022-06-10 | 2022-08-12 | 济南大学 | VO (volatile organic compound) 2 /SiO 2 Method for preparing composite material |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106675115A (en) * | 2016-11-28 | 2017-05-17 | 江南大学 | Preparation method of high-transmittance thermochromatic intelligent recoating |
| CN109294277A (en) * | 2017-07-25 | 2019-02-01 | 上海大学 | A kind of vanadium dioxide and preparation method thereof that surface is modified |
| CN108751256A (en) * | 2018-05-15 | 2018-11-06 | 清华大学 | A kind of preparation method of high performance lithium ion battery anode material vanadium oxide |
| CN108751256B (en) * | 2018-05-15 | 2020-12-29 | 清华大学 | Preparation method of high-performance lithium ion battery cathode material vanadium oxide |
| CN108394907A (en) * | 2018-05-29 | 2018-08-14 | 中国科学院青岛生物能源与过程研究所 | A kind of silicon vanadium oxides composite and preparation method thereof |
| CN108394907B (en) * | 2018-05-29 | 2021-06-22 | 中国科学院青岛生物能源与过程研究所 | Silicon-vanadium composite oxide and preparation method thereof |
| CN110003882A (en) * | 2019-04-04 | 2019-07-12 | 东华大学 | A kind of structure of controlling temperature color dyestuff and its preparation and application |
| CN110937819A (en) * | 2019-12-09 | 2020-03-31 | 东莞深圳清华大学研究院创新中心 | Preparation method of transparent super-hydrophobic intelligent temperature control glass |
| CN111039261A (en) * | 2019-12-12 | 2020-04-21 | 上海大学 | Liquid-phase high-concentration nano particle coating method |
| CN111039261B (en) * | 2019-12-12 | 2022-09-23 | 上海大学 | Liquid-phase high-concentration nano particle coating method |
| CN111725334B (en) * | 2020-06-30 | 2022-08-16 | 浙江晶科能源有限公司 | Coating liquid for photovoltaic module, preparation method of coating liquid and photovoltaic module |
| CN111725334A (en) * | 2020-06-30 | 2020-09-29 | 浙江晶科能源有限公司 | Coating liquid for photovoltaic module, preparation method of coating liquid and photovoltaic module |
| CN112059172A (en) * | 2020-09-16 | 2020-12-11 | 浙江工业大学 | SiO is carried out to micron order granule2Method of coating |
| CN113130745A (en) * | 2021-04-16 | 2021-07-16 | 中国人民解放军陆军工程大学 | VO2@SiO2Nano particle filled type electric field phase change composite material and its preparation method |
| CN113956864A (en) * | 2021-09-22 | 2022-01-21 | 河南龙德福新材料科技研究院有限公司 | Low-density high-strength ceramsite proppant coated by silicon dioxide and preparation method thereof |
| CN114890473A (en) * | 2022-06-10 | 2022-08-12 | 济南大学 | VO (volatile organic compound) 2 /SiO 2 Method for preparing composite material |
| CN114890473B (en) * | 2022-06-10 | 2024-02-06 | 济南大学 | VO (Voice over Internet protocol) 2 /SiO 2 Preparation method of composite material |
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Application publication date: 20160817 |