CN102464354A - Rutile-phase vanadium dioxide composition, coating containing same and performance of rutile-phase vanadium dioxide composition - Google Patents
Rutile-phase vanadium dioxide composition, coating containing same and performance of rutile-phase vanadium dioxide composition Download PDFInfo
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- CN102464354A CN102464354A CN2010105333385A CN201010533338A CN102464354A CN 102464354 A CN102464354 A CN 102464354A CN 2010105333385 A CN2010105333385 A CN 2010105333385A CN 201010533338 A CN201010533338 A CN 201010533338A CN 102464354 A CN102464354 A CN 102464354A
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Abstract
The invention provides a rutile-phase vanadium dioxide particle composition, wherein the particle composition has a microstructure capable of generating a nano-scale effect, wherein the particle size is not more than 120nm on at least one dimensionality. The invention also provides a dispersion system containing the rutile-phase vanadium dioxide particle composition. The nano-scale effect generated by the microstructure of the particle composition disclosed by the invention can adjust the phase-change temperature, and thus the energy-saving efficiency is achieved.
Description
Technical field
The present invention relates to chemical field and field of materials, specifically originally deliver the microstructure that relates to a kind of intelligent power saving material, nanometer size effect and in the application aspect the transformation temperature adjusting (comprising the intelligent power saving coating).
Background technology
Under the situation that the global energy supply is becoming tight, energy-conservationly become another important topic that construction industry must be faced.The total amount of China's building energy consumption rises year by year, in energy aggregate consumption shared ratio from last century late nineteen seventies 10%, rise in recent years 27.45%.And the building energy consumption of developed country generally accounts for about 33% of national total energy consumption in the world.The energy-conservation of construction industry is mainly reflected on window design and the illuminating energy-saving at present.At building window glass and car and boat surface-coated one energy-saving coating, change the through performance of material, intercept solar irradiation, reduce the injury of ultraviolet ray to human body, reach improve people by bus, living environment, reduce the purpose of air conditioning energy consumption.
Material with optics barrier property is a lot, but the passive obstruct infrared light of these material intelligence can't be accomplished intelligent response.Rutile phase (R phase) vanadium dioxide is because of its character 68 ℃ of reversible metal semiconductor phase transformations of generation; Have higher room temperature transmitance and very low high temperature transmitance respectively before and after the phase transformation, become material thereby become the most promising intelligent thermic look of present application, its transformation temperature is 68 ℃; A little more than room temperature; Generally be reduced to room-temperature applications to the intelligent power saving field at present, but doping can cause the deterioration of its high low temperature phase transition property, thereby reduce its energy-saving efficiency through elements such as Doped Tungsten, molybdenums.
In sum, this area lacks a kind of material that reduces energy-saving efficiency.
Summary of the invention
First purpose of the present invention is to obtain a kind of material compositions that reduces energy-saving efficiency.
Second purpose of the present invention is to obtain a kind of dispersed system that reduces energy-saving efficiency.
The 3rd purpose of the present invention is to obtain a kind of preparation method who reduces the material compositions of energy-saving efficiency.
The 4th purpose of the present invention is to obtain a kind of preparation method who reduces the dispersed system of energy-saving efficiency.
The 5th purpose of the present invention is to obtain a kind of application of described rutile phase hypovanadic oxide particulate compsn.
The 6th purpose of the present invention is to obtain a kind of goods that contain described rutile phase hypovanadic oxide particulate compsn.
In first aspect of the present invention, a kind of rutile phase hypovanadic oxide particulate compsn is provided, said particulate compsn has the following microstructure that produces nanometer size effect:
Said particle size is not more than 120nm at least one dimension.
Said particle size is between 0.5nm～120nm at least one dimension, more preferably is in 3nm～70nm, most preferably 8nm～50nm.
In an embodiment of the present invention, said particle size is not more than 120nm at least three dimensions, be in particularly between 0.5nm～120nm, more preferably is in 3nm～70nm, most preferably 8nm～50nm.
In an embodiment of the present invention, said particle size is not more than 120nm at least three dimensions, be in particularly between 0.5nm～120nm, more preferably is in 3nm～70nm, most preferably 8nm～50nm.
In an embodiment of the present invention, said particulate length-to-diameter ratio scope is 1: 1～100: 1.
Most preferably, the shortest direction length of said particle (also being radial width) is not less than 5% of length direction.
In an embodiment of the present invention, the halfwidth at 110 peaks that said rutile phase xrd method records is not less than 0.1 °.
In an embodiment of the present invention, the gross weight that the particle of said monocrystalline form accounts for particulate compsn is no less than 80%, and preferably, each rutile phase hypovanadic oxide particle is monocrystalline.
In second aspect of the present invention, a kind of preparation method of rutile phase hypovanadic oxide particulate compsn, said preparation method is selected from hydrothermal method, thermal decomposition method or hydrogen reduction method.
The third aspect of the invention, a kind of rutile phase hypovanadic oxide dispersed system that contains the rutile phase hypovanadic oxide particulate compsn of significant quantity.
In a preference, said dispersed system is selected from solid dispersed system, liquid dispersion system or gas dispersion system.
In a preference, dispersed system is meant that adopting the vanadium dioxide particle is core material, and it is disperseed formed dispersion system in base-materials such as inorganic, organic, polymer.This dispersed system can be a solid (glass, pottery, gel, resin, plastics and solid mixture), (like the various suspension-s that contain vanadium dioxide, its solvent can be a water, also can be organic solvents such as alcohol, toluene in liquid dispersion system.) also can be gas dispersion system (comprising aerosol).
In a preference, in the said dispersed system, vanadium dioxide nano particle shared quality in dispersed system is 0.001%-100 weight % than scope.
Fourth aspect of the present invention provides the preparation method of rutile phase hypovanadic oxide dispersed system of the present invention, and said method is selected from sol-gel method, magnetron sputtering method or chemical Vapor deposition process.
The application that the 5th aspect of the present invention provides a kind of rutile phase hypovanadic oxide particulate compsn of the present invention or described rutile phase hypovanadic oxide dispersed system to regulate in the vanadium dioxide transformation temperature makes transformation temperature not be higher than 68 ℃;
Preferably, said transformation temperature is adjusted to 30～68 ℃;
More preferably, said transformation temperature is adjusted to 5～68 ℃;
Most preferably, said transformation temperature is adjusted to-14.5～68 ℃.
The goods that the 6th aspect of the present invention provides a kind of rutile phase hypovanadic oxide particulate compsn of the present invention or described rutile phase hypovanadic oxide dispersed system to obtain, said goods comprise intelligent power saving coating, sun power temperature control unit, micro optical switch device, thermistor or optical information storage spare.
Description of drawings
Fig. 1 is the XRD figure spectrum of nano vanadium dioxide powder.
The said longitudinal axis " intensity " is meant intensity.
The HRTEM of Fig. 2 nano vanadium dioxide (high power transmission electron microscope) photo
The DSC temperature lowering curve that Fig. 3 Fig. 2 nanoparticle is corresponding
The TEM photo of Fig. 4 nano vanadium dioxide
Fig. 5 is the temperature-rise period DSC curve of different transformation temperature hypovanadic oxide powders
The TEM photo of Fig. 6 embodiment 3 pairing nano vanadium dioxides
The transmission electron microscope photo of Fig. 7 film
The high resolution transmission electron microscopy photo of Fig. 8 film
Fig. 9 is that the high low temperature Visible-to-Near InfaRed that makes film sees through spectrum.
Test condition: instrument is the Japanese Hitachi U-4100 of company UV, visible light near infrared spectrometer; Through temperature conditioning unit heating and cooling sample; Thereby the transmitance of measuring 2000nm place film in the heating and cooling process obtains the thermic loop line, confirms transformation temperature.Temperature measurement range is 20-90 ℃, and temperature rate is 5 ℃/minute.
Embodiment
The inventor is through extensive and deep research, through improving preparation technology, obtained a kind ofly to regulate the method for vanadium dioxide phase transformation problem through regulating dimensional effect, and its energy-saving efficiency is excellent especially.Accomplished the present invention on this basis.
Technical conceive of the present invention is following:
Provide a kind of method and this dimensional effect of directly regulating vanadium dioxide phase transformation problem with the regulation and control rutile phase hypovanadic oxide powder size and the microstructure that can produce this dimensional effect in the application aspect the adjusting of vanadium dioxide transformation temperature.Above-mentioned vanadium dioxide with dimensional effect can be the vanadium dioxide particle, also can be to be prepared into to contain vanadium dioxide nano particulate film and dispersed system.Its preparation can realize through physics method, chemical method or additive method.Can be applied to the intelligent power saving coating, also can be applied to the preparation of sun power temperature control unit, micro optical switch device, thermistor or optical information storage spare etc.
Among this paper, said " dimensional effect " is meant transformation temperature is adjusted to necessary requirement.For example transformation temperature is adjusted to and is not higher than 68 ℃.
Among this paper, rutile phase hypovanadic oxide is meant and has the rutile phase structure vanadium dioxide particle of (corresponding X diffraction standard card 43-1051 or 440252,440253).Vanadium dioxide can be that other element dopings are arranged, and can be have other element dopings yet.
Among this paper, said rutile phase hypovanadic oxide particulate compsn is meant that the crystalline phase at least 90% of said compsn is the rutile phase, and by weight, preferably, the crystalline phase at least 95% of said compsn is the rutile phase.
The rutile phase hypovanadic oxide particle
A kind of rutile phase hypovanadic oxide particle of the present invention can be regarded as a kind of compsn.Said composition has the following microstructure that produces nanometer size effect:
Said particle size is not more than 120nm at least one dimension, be in particularly between 0.5nm～120nm, more preferably is in 3nm～70nm, most preferably 8nm～50nm.The contriver finds that the nanometer size effect that said particle size produces can make transformation temperature be controlled at 30～68 ℃.
Among this paper, said particle size is measured by the transmission electron microscope photo.Said dimension has the well-known definitions in this area, also is length, width or height.
In an embodiment, said particle size is not more than 120nm at least two dimensions, is in particularly between 0.5nm～120nm, more preferably is in 3nm～70nm, most preferably 8nm～50nm.The contriver finds that the nanometer size effect that said particle size produces can make transformation temperature be controlled at 5～68 ℃.
In an embodiment, said particle size is not more than 120nm at least three dimensions, is in particularly between 0.5nm～120nm, more preferably is in 3nm～70nm, most preferably 8nm～50nm.The contriver finds that the nanometer size effect that said particle size produces can make transformation temperature be controlled at-14.5～68 ℃.
In sum, transformation temperature of the present invention is adjusted to below 68 ℃, minimum can be to-16 ℃.And transformation temperature is the key of energy-saving efficiency.
In an embodiment, said particulate length-to-diameter ratio scope is 1: 1～100: 1.Most preferably, the shortest direction length of said particle is not less than 5% of length direction.
In an embodiment, the halfwidth at 110 peaks that said rutile phase xrd method records is not less than 0.1 °.
In an embodiment, the gross weight that the particle of said monocrystalline form accounts for particulate compsn is no less than 80%, and preferably, each rutile phase hypovanadic oxide particle is monocrystalline.
In order to obtain the more said compsn of good dispersibility, hard aggregation-free phenomenon, said preparation method is selected from hydrothermal method, thermal decomposition method or hydrogen reduction method.These methods are known to those skilled in the art.
The hydrothermal method concrete operation method makes reference to the text-book, concrete example as, can be through controlled temperature 200-300 ℃, pH value 1.5～12, factors such as 2 hours～36 hours reaction times are controlled the pattern of rutile phase hypovanadic oxide.But said method is not limited thereto.
Particularly, thermal decomposition method can be passed through 400～900 degrees centigrade of control decomposition temperatures, and oxygen partial pressure 0.1pa-10
-6Factor systems such as Pa rutile phase hypovanadic oxide particulate size.But said method is not limited thereto.
Particularly, hydrogen reduction method is with through factor system rutile phase hypovanadic oxide particulate sizes such as control 400～900 degrees centigrade of decomposition temperatures and depositing time 0.1～24h.But said method is not limited thereto.
The rutile phase hypovanadic oxide dispersed system
The present invention also provides a kind of rutile phase hypovanadic oxide dispersed system that contains the rutile phase hypovanadic oxide particulate compsn of significant quantity.
Said significant quantity is meant the content that makes said vanadium dioxide nano particle (or being called the vanadium dioxide nano particulate compsn) in the content of dispersed system, keep nanometer size effect.Particularly, vanadium dioxide nano particle shared quality in dispersed system is 0.001%-100 weight % than scope.
In a preference, said dispersed system is selected from solid dispersed system, liquid dispersion system or gas dispersion system.
In a preference, dispersed system is meant that adopting the vanadium dioxide particle is core material, and it is disperseed formed dispersion system in base-materials such as inorganic, organic, polymer.This dispersed system can be a solid (glass, pottery, gel, resin, plastics and solid mixture), (like the various suspension-s that contain vanadium dioxide, its solvent can be a water, also can be organic solvents such as alcohol, toluene in liquid dispersion system.) also can be gas dispersion system (comprising aerosol).
Particularly, said dispersed system can be to contain rutile phase hypovanadic oxide particulate coating, film or block structure.
The preferred method that said dispersed system can adopt is selected from sol-gel method, magnetron sputtering method or chemical Vapor deposition process.Said method is known to those skilled in the art.
Particularly, sol-gel method can be 1～4 through the viscosity of control colloidal sol, and factors such as 300～700 ℃ of follow-up Heating temperatures and digestion time 2 hours～30 days are controlled the size of rutile phase hypovanadic oxide.But said method is not limited thereto.
Particularly, magnetron sputtering method can be through 200～700 degrees centigrade of control underlayer temperatures, and oxygen partial pressure 0.1pa～factors such as 10-6Pa are controlled rutile phase hypovanadic oxide particulate size.But said method is not limited thereto.
Particularly, chemical Vapor deposition process is through 400～900 degrees centigrade of underlayer temperatures of control, and factor system rutile phase hypovanadic oxide particulate size such as depositing time 1h-24h.But said method is not limited thereto.
Purposes
The application that the present invention also provides a kind of rutile phase hypovanadic oxide particulate compsn or rutile phase hypovanadic oxide dispersed system to regulate in the vanadium dioxide transformation temperature makes transformation temperature not be higher than 68 ℃;
Preferably, said transformation temperature is adjusted to 30～68 ℃;
More preferably, said transformation temperature is adjusted to 5～68 ℃;
Most preferably, said transformation temperature is adjusted to-14.5～68 ℃.
Goods
The goods that described rutile phase hypovanadic oxide particulate compsn or described rutile phase hypovanadic oxide dispersed system obtain, said goods comprise intelligent power saving coating, sun power temperature control unit, micro optical switch device, thermistor or optical information storage spare.
The present invention compares with existing traditional method, and it has following advantage:
Transformation temperature is regulated and need not to adopt element doping;
Transformation temperature can be regulated through size or microstructure control as required continuously.
The present invention adopts particle size, the microstructure of control rutile phase hypovanadic oxide; Utilize the nanometer size effect that produces to regulate transformation temperature; (for example three dimensions all are between 0.5nm～120nm through nano particle; More preferably be in 3nm～70nm, most preferably the dimensional effect of the 8nm～50nm) method of regulating transformation temperature is not appeared in the newspapers in existing document, patent.
The present invention also provides an optimal way; Also be that nano particle of the present invention all requires to be controlled on three dimensions and is in particularly between 0.5nm～120nm; More preferably be in 3nm～70nm, most preferably 8nm～50nm just has the transformation temperature of adjusting to subzero performance under this yardstick; Its transformation temperature regulation range is-16～68 ℃ (more preferably-14.5～68 ℃, as shown in Figure 3).The present invention both can be independent nano vanadium dioxide particle regulating the transformation temperature application facet, also can be to contain vanadium dioxide nano particulate dispersed system.The present invention can be applicable to fields such as thermochromism film, energy-saving coatings, energy saving paint, intelligent power saving glass curtain wall, temperature control unit and energy-saving coating, also can be applied to the reducing energy consumption on existing building, car and boat surface.
Compound provided by the present invention can be synthetic through marketable material and traditional chemical transform mode.
Other aspects of the present invention are because the disclosure of this paper is conspicuous to those skilled in the art.
Below in conjunction with specific embodiment, further illustrate the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in the restriction scope of the present invention.The experimental technique of unreceipted actual conditions in the following example usually according to normal condition, for example is " condition in the smooth organic chemistry handbook of Bel Si (Chemical Industry Press, 1996), or the condition of advising according to manufacturer.Ratio and per-cent are based on weight, unless stated otherwise.
Only if definition or explanation are arranged in addition, the same meaning that all specialties used herein and scientific words and those skilled in the art are familiar with.Any in addition with the institute similar content of putting down in writing or the equalization method and material all can be applicable in the inventive method.
Testing method of the present invention is specific as follows:
Transmission electron microscope (TEM), model JEM2010JEOL, Japanese Tokyo company
X-ray diffraction (XRD), model D/max 2550V, Japanese Rigaku adopts Cu K alpha-ray, λ=0.15406nm 4 degree/min.
DSC (DSC), model DSC200F3, NETZSCH company, TR-30-90 ℃, 10 ℃ of min of temperature rate
-1
Embodiment 1:
With 0.36g V
2O
5Powder is put into the small beaker of the oxalic acid solution that contains 80ml concentration 0.15M, and constantly stirs, in the 100ml water heating kettle of packing into then, and 260 ℃ of hydro-thermals 8 hours, whiz obtains rutile phase hypovanadic oxide powder.Its crystalline phase is rutile (shown in Fig. 1 XRD spectra); Each vanadium dioxide particle is a single crystal particle; Its grain-size is 5-12nm, and length-to-diameter ratio is 1: 1-3: (shown in Fig. 2 TEM photo) its temperature-fall period transformation temperature is-14.5 ℃ (shown in Fig. 3 DSC curves) between 1
Embodiment 2:
With 0.36g V
2O
5Powder is put into the small beaker of the oxalic acid solution that contains 80ml concentration 0.15M, and constantly stirs, in the 100ml water heating kettle of packing into then, and 260 ℃ of hydro-thermals 24 hours, whiz obtains rutile phase hypovanadic oxide powder.Its crystalline phase is the rutile phase, and grain-size is 90-120nm, and length-to-diameter ratio is 1: 1-3: between 1 (shown in Fig. 4 TEM photo), its temperature-rise period transformation temperature is 68 ℃ (shown in DSC curves among Fig. 6).
Embodiment 3:
With 0.36g V
2O
5Powder is put into the small beaker of the oxalic acid solution that contains 80ml concentration 0.15M, and constantly stirs, in the 100ml water heating kettle of packing into then, and 260 ℃ of hydro-thermals 12 hours, whiz obtains rutile phase hypovanadic oxide powder.Its crystalline phase is rutile (shown in Fig. 1 XRD spectra); Each vanadium dioxide particle is a single crystal particle; Its grain-size is 40-50nm, and length-to-diameter ratio is 3: 1-10: (shown in Fig. 6 TEM photo) its temperature-rise period transformation temperature is 28 ℃ (shown in DSC curves among Fig. 4) between 1
Embodiment 4:
With 0.1g embodiment 3 prepared V O
2The powder grinding is put into the small beaker that contain 5ml water later, and constantly stir, and adds 0.25g Vinylpyrrolidone polymer K-30, and ultrasonic 60min behind the stirring 30min makes suspension-s.Adopt spin coating method that gained suspension-s is coated on the glass substrate, in room temperature or baking oven, after the drying, can obtain vanadium dioxide film again.The phase transformation front and back curve of spectrum that makes vanadium dioxide film is as shown in Figure 7.
Embodiment 5:
(1) coating liquid preparation:
Get methyl ethyl diketone vanadyl 13.3g, dissolving in the 100ml volume ratio is 2: 4: 1: in the mixing solutions of 1 ethanol, terepthaloyl moietie, chloroform, water, in magnetic stirring apparatus, stirred 3 hours, obtain the coating liquid of vanadium dioxide film through ageing after 3 hours.
(2) clean substrate:
The selection substrate is a silica glass, adopts the RCA technology of standard to clean, and takes out organism, dust and the impurity metal ion on surface.It is subsequent use afterwards substrate to be put into 60 ℃ of oven dryings processing backs.
(3) coating liquid plated film
Choose the coating liquid of above-mentioned steps (1) gained, adopt the spin coater plated film.The resulting film of spin coating is put into 60 ℃ of baking ovens, after dry ten minutes, repeat the film that above spin coating process can obtain desired thickness.
(4) vanadium dioxide film sintering
The resulting film of step (3) is put into vacuum oven, and the long-pending ratio of control oxysome is 3 * 10
-7Oxygen-argon mixture gas under sintering, sintering temperature is 380 ℃, sintering time is 4 hours.To be sintered finishing; When dropping to below 80 ℃, film temperature takes out; Two kinds of films of changing vanadium particle microstructure are like (shown in Figure 7) mutually to obtain containing rutile, and its rutile phase hypovanadic oxide particle (shown in Fig. 8 high power TEM photo) that consists of about diameter 40nm is 42.1 ℃ through the transformation temperature that detects this vanadium dioxide film.
All documents in that the present invention mentions are all quoted as a reference in this application, are just quoted such as a reference separately as each piece document.Should be understood that in addition after having read above-mentioned teachings of the present invention, those skilled in the art can do various changes or modification to the present invention, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Claims (11)
1. a rutile phase hypovanadic oxide particulate compsn is characterized in that, said particulate compsn has the following microstructure that produces nanometer size effect:
Said particle size is not more than 120nm at least one dimension.
2. particulate compsn as claimed in claim 1 is characterized in that said particle size is not more than 120nm at least two dimensions, is in particularly between 0.5nm～120nm, more preferably is in 3nm～70nm, most preferably 8nm～50nm.
3. particulate compsn as claimed in claim 1 is characterized in that said particle size is not more than 120nm at least three dimensions, is in particularly between 0.5nm～120nm, more preferably is in 3nm～70nm, most preferably 8nm～50nm.
4. particulate compsn as claimed in claim 1 is characterized in that, said particulate length-to-diameter ratio scope is 1: 1～100: 1; Most preferably, the shortest direction length of said particle is not less than 5% of length direction.
5. particulate compsn as claimed in claim 1 is characterized in that, the halfwidth at 110 peaks that said rutile phase xrd method records is not less than 0.1 °.
6. particulate compsn as claimed in claim 1 is characterized in that the gross weight that the particle of said monocrystalline form accounts for particulate compsn is no less than 80%, and preferably, each rutile phase hypovanadic oxide particle is monocrystalline.
7. the preparation method of a rutile phase hypovanadic oxide particulate compsn is characterized in that, said preparation method is selected from hydrothermal method, thermal decomposition method or hydrogen reduction method.
8. rutile phase hypovanadic oxide dispersed system that contains the rutile phase hypovanadic oxide particulate compsn as claimed in claim 1 of significant quantity.
9. the preparation method of a rutile phase hypovanadic oxide dispersed system as claimed in claim 8 is characterized in that, said method is selected from sol-gel method, magnetron sputtering method or chemical Vapor deposition process.
10. the application regulated in the vanadium dioxide transformation temperature of rutile phase hypovanadic oxide particulate compsn as claimed in claim 1 or the described rutile phase hypovanadic oxide dispersed system of claim 8 makes transformation temperature be lower than 68 ℃;
Preferably, said transformation temperature is adjusted to 30～68 ℃;
More preferably, said transformation temperature is adjusted to 5～68 ℃;
Most preferably, said transformation temperature is adjusted to-14.5～68 ℃.
11. the goods that rutile phase hypovanadic oxide particulate compsn as claimed in claim 1 or the described rutile phase hypovanadic oxide dispersed system of claim 8 obtain, said goods comprise intelligent power saving coating, sun power temperature control unit, micro optical switch device, thermistor or optical information storage spare.
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| CN108390112A (en) * | 2018-01-30 | 2018-08-10 | 中国电力科学研究院有限公司 | A kind of analogy method and device of battery internal short-circuit |
| CN109266103A (en) * | 2018-10-11 | 2019-01-25 | 扬州市祥华新材料科技有限公司 | Reversible temperature becomes water-based ink and its preparation method and application |
| CN109502643A (en) * | 2018-11-26 | 2019-03-22 | 深圳大学 | A kind of boron magnesium codope VO2Powder and its preparation method and application |
| CN109502643B (en) * | 2018-11-26 | 2021-03-16 | 深圳大学 | Boron-magnesium co-doped VO2Powder and preparation method and application thereof |
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