CN107651860A - Tungsten oxide film with infrared barrier function and preparation method thereof - Google Patents
Tungsten oxide film with infrared barrier function and preparation method thereof Download PDFInfo
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- CN107651860A CN107651860A CN201610589510.6A CN201610589510A CN107651860A CN 107651860 A CN107651860 A CN 107651860A CN 201610589510 A CN201610589510 A CN 201610589510A CN 107651860 A CN107651860 A CN 107651860A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
- C03C17/3429—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating
- C03C17/3435—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating comprising a nitride, oxynitride, boronitride or carbonitride
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Abstract
The present invention relates to tungsten oxide film with infrared barrier function and preparation method thereof; the tungsten oxide film with infrared barrier function includes matrix, is formed and mixes the tungsten oxide film formed and the first protective layer formed on the tungsten oxide film surface by crystalline state tungsten oxide and amorphous state tungsten oxide on matrix, and the valence state composition of wolfram element includes+6 valency tungsten ions and+5 valency tungsten ions in the tungsten oxide film.Tungsten oxide film of the present invention with infrared barrier function includes matrix, formation and mixes the tungsten oxide film formed and the first protective layer formed on the tungsten oxide film surface by crystalline state tungsten oxide and amorphous state tungsten oxide on matrix; crystalline state tungsten oxide mainly has good shield effectiveness to more than 1500nm infrared light, and amorphous state tungsten oxide has good shield effectiveness to 900 1200nm infrared light.
Description
Technical field
The invention belongs to fields such as energy conservation, infrared barrier device, stealth technologies, it is related to infrared shielding multi-layer thin
The preparation method of film.
Background technology
Building energy consumption typically occupies more than 1/3rd of social total energy consumption, meanwhile, energy for building is to world greenhouse gas
" contribution rate " of body discharge is up to 25%, is one of emphasis rich and influential family of reduction of greenhouse gas discharge.Windowpane enters as building with the external world
The main thoroughfare that row photo-thermal exchanges, data show that the 50% of building energy consumption is carried out by windowpane；And skin etc.
Heat absorption also exacerbate the heat island phenomenon of down town.So realize that building energy conservation will rise to reducing building greenhouse gas emission
Decisive role.Equally, the window of the moving body such as automobile or the energy-saving of outer surface, also will be to comfortably making with energy-saving and emission-reduction
Contribution.
At present, the energy-saving glass of market sale or energy-conservation pad pasting (abbreviation Energy Saving Windows) belong to low-launch-rate (Low-E)
Category, be characterized in that there is higher visible light transmissivity and relatively low far infrared transmissivity (winter is heat-insulated), can realize every
While heat insulation, carry out the infrared part in sunshine high blocking (being suitable for hot area) or high transmission (is suitable for trembling with fear
Cryogenic region).But because current Energy Saving Windows generally use argentiferous composition, cost is high, price, and encapsulation technology requirement compared with
Height, researchers are pursuing in the research and development without silver-colored infrared barrier functional material always.
The tungsten oxide class material of sub-stoichiometric ratio has its preferable visible light transmissivity, relatively low infrared light transmission,
With ultraviolet cut-on characteristic.But further oxidation easily occurs for the oxidation tungsten product of the sub-stoichiometric ratio for preparing, and leads
Cause performance degradation.
The content of the invention
In view of the above-mentioned problems, it is an object of the invention to provide a kind of oxidation with infrared barrier function and sandwich construction
W film.
On the one hand, it is described that there is infrared barrier the invention provides a kind of tungsten oxide film with infrared barrier function
The tungsten oxide film of function includes matrix, formation and mixes what is formed by crystalline state tungsten oxide and amorphous state tungsten oxide on matrix
Tungsten oxide film and the first protective layer on the tungsten oxide film surface is formed, wolfram element in the tungsten oxide film
Valence state composition includes+6 valency tungsten ions and+5 valency tungsten ions.
Tungsten oxide film of the present invention with infrared barrier function include matrix, formed on matrix by crystalline state
Tungsten oxide and the amorphous state tungsten oxide mixing tungsten oxide film formed and formed on the tungsten oxide film surface first
Protective layer, crystalline state tungsten oxide mainly have a good shield effectiveness to more than 1500nm infrared light, and amorphous state tungsten oxide pair
900-1200nm infrared light has good shield effectiveness.Tungsten oxide film has a very high transmitance in visible region, but
Infrared light district transmitance is relatively low, i.e., with good infrared barrier function.In addition, positioned at the matrix of tungsten oxide film both sides and
One protective layer can prevent tungsten oxide from further aoxidizing, and improve corrosion-resistant function, can make the military service of tungsten oxide film
Performance improves a lot.
It is preferred that visible light transmissivity >=50% and infrared light transmittance≤50% of the tungsten oxide film.
It is preferred that the thickness of the tungsten oxide film is 50~1000nm, preferably 50~500nm.
It is preferred that also include the second protective layer being arranged between described matrix and tungsten oxide film.Above-mentioned matrix material
Surface redeposition layer protecting film, there is anti-oxidant, corrosion-resistant function, can make tungsten oxide film military service performance have it is very big
Improve.
It is preferred that first protective layer and/or the second protective layer are silicon nitride, aluminum oxide, silica, zinc oxide, oxygen
Change at least one of titanium, zirconium oxide, magnesia, magnesium fluoride.
It is preferred that the refractive index of first protective layer and/or the second protective layer is between 1.3-2.6, thickness is 50~
1000nm, preferably 50~500nm.
It is preferred that described matrix is one kind in glass, crystalline ceramics, silicon chip, sheet metal.
On the other hand, present invention also offers a kind of preparation method of the tungsten oxide film with infrared barrier function, adopt
Sputtered in matrix surface to obtain amorphous state tungsten oxide film with magnetron sputtering technique, then make annealing treatment 1 at 300~700 DEG C
~30 minutes, so that amorphous state tungsten oxide portions turn is crystalline state tungsten oxide in amorphous state tungsten oxide film, obtain the tool
There is the tungsten oxide film of infrared barrier function.
The present invention carries out the amorphous state tungsten oxide film of acquisition the heat treatment of 1-30 minutes, heat during 300-700 DEG C
The treated tungsten oxide film has very high transmitance in visible region, but relatively low in infrared light district transmitance, that is, has
Good infrared barrier function, it is that crystalline state tungsten oxide and the mixing of amorphous state tungsten oxide are formed in structure composition.The present invention is also logical
Control sputtering time length and sputtering power size are crossed, amorphous state tungsten oxide film (sub-stoichiometric ratio is prepared in matrix surface
Tungsten oxide).Or before amorphous state tungsten oxide film is prepared, first prepare one layer of second protective layer (note in matrix surface：Substrate
Glassy layer is also believed to the second protective layer).Then one layer of fine and close transparent silicon nitride film is sputtered again as screen layer (
One protective layer), obtain the film article with energy-saving effect.
It is preferred that it is preferred that the heating rate of the annealing is 4 DEG C/sec.
It is preferred that carrying out reactive magnetron sputtering using metal tungsten target prepares amorphous state tungsten oxide film, or use oxygen
Change tungsten ceramic target and directly prepare amorphous state tungsten oxide film through magnetron sputtering in an inert atmosphere.
It is preferred that the tungsten oxide film is sub-stoichiometric ratio tungsten oxide, consisting of WOx, wherein 2≤x≤3.
The technology path that the present invention prepares the tungsten oxide film with infrared barrier function can be divided into two categories below：One,
Amorphous state tungsten oxide film is prepared using metal targets, sputters one layer of silicon nitride as the second protective layer in glass surface, then
On silicon nitride sputter one layer of amorphous state tungsten oxide film, finally sputter one layer of silicon nitride, after by annealing etc. processing.Two, adopt
By the use of tungsten oxide ceramic target as sputtering target material, sputtered in the glass surface for sputtering silicon nitride, after sputter one layer of nitridation again
Silicon, then by annealing.Both the above technology path, implementing process and its simple, especially the first, metal targets system
Standby cost is much lower compared with ceramic target.Two kinds of technology paths are all the tungsten oxides for sputtering hundred nanometer thickness, and dosage is minimum, and cost is cheap,
And technical process is simple, controllability is strong.
Tungsten oxide film material of the present invention with infrared barrier function is expected applied to heat-insulated smart window, aviation
Aircraft, automobile heat-insulating glass, the heat-insulated field such as stealth technology and transparent optical device.
Brief description of the drawings
Fig. 1 is the XRD of the tungsten oxide film before annealing prepared by embodiment 1；
Fig. 2 is the XRD of the tungsten oxide film by annealing prepared by embodiment 1；
Fig. 3 is the SEM figures of the tungsten oxide film before annealing prepared by embodiment 1；
Fig. 4 is the SEM figures of the tungsten oxide film by annealing prepared by embodiment 1；
Fig. 5 is the visible ray infrared transmittivity spectrum of glass/silicon nitride/tungsten oxide/silicon nitride before annealing prepared by embodiment 1
Figure；
Fig. 6 is the visible ray infrared transmittivity light of glass/silicon nitride/tungsten oxide/silicon nitride by annealing prepared by embodiment 1
Spectrogram；
Fig. 7 is the visible ray infrared transmittivity spectrogram of glass/tungsten oxide/silicon nitride by annealing prepared by embodiment 2；
Fig. 8 is glass/silicon nitride/tungsten oxide/silicon nitride structure schematic diagram prepared by embodiment 1；
Fig. 9 is glass/tungsten oxide/silicon nitride structure schematic diagram prepared by embodiment 2.
Embodiment
The present invention is further illustrated below by way of following embodiments, it should be appreciated that following embodiments are merely to illustrate this
Invention, is not intended to limit the present invention.
The present invention by using magnetron sputtering technique with glass, crystalline ceramics, silicon chip, sheet metal etc. for matrix, had
There is the tungsten oxide film of energy-saving effect, including：Matrix and the oxidation with infrared barrier function for being formed at matrix surface
W film.The valence state composition of wolfram element includes+6 valency tungsten ions and+5 valencys in the tungsten oxide film with infrared barrier function
Tungsten ion.Or the first protective layer for also including being arranged on the tungsten oxide film surface (can also claim transparent protective film, protect
Cuticula etc.).Or both include the first protective layer being arranged on the tungsten oxide film surface, in addition to it is arranged on described matrix
The second protective layer (can also claim transparent protective film, diaphragm etc.) between tungsten oxide film.Wherein, first protective layer
Or/and second protective layer can be silicon nitride, aluminum oxide, silica, zinc oxide, titanium oxide, zirconium oxide, magnesia, in magnesium fluoride
At least one.
The invention provides it is a kind of including the second protective layer for being arranged between matrix and tungsten oxide film have it is infrared
The preparation method of the tungsten oxide film (referring to Fig. 8) of barriers function.Illustrate to following exemplary provided by the invention with infrared
The preparation method of the tungsten oxide film of barriers function.
Matrix surface is cleaned and dried.The example detailed as one, simple glass is put into detergent solution and soaked
Several minutes, brush brushing surface is used afterwards, removes the greasy dirt and attachment impurity of glass surface.Glass is rinsed with clear water, removes washing
Essence residual, afterwards with deionized water rinsing, is removed the foreign ion on surface, is dried up using high pressure dry air.
Before matrix (for example, glass, crystalline ceramics, silicon chip, sheet metal etc.) surface prepares amorphous state tungsten oxide film,
Can first matrix surface sputter one layer of second protective layer, such as can be silicon nitride, aluminum oxide, silica, zinc oxide, titanium oxide,
At least one of zirconium oxide, magnesia, magnesium fluoride.The thickness of second protective layer can be 50~1000nm, preferably 50
~500nm.The example detailed as one, when the second protective layer elects silicon nitride as, using silicon target, or silicon nitride target shielding power supply
Using direct current or radio frequency, Power Control is in 1.2w/cm2, using 1:1 argon nitrogen mixed gas, Stress control 0.2Pa to 1.5Pa are left
The right side, sputtering thickness 50nm-1000nm or so, preferably 50~500nm.
Then one layer of amorphous state tungsten oxide is sputtered on the second protective layer as sputtering target material using tungsten oxide or tungsten
Film, its color is translucent blue brown or black-and-blue, consisting of WOx, wherein 2≤x≤3.For preparing amorphous state oxidation
W film, carry out reactive magnetron sputtering using metal tungsten target and be prepared, or using tungsten oxide ceramic target in inert atmosphere
In be directly prepared through magnetron sputtering.During from metal tungsten target, shielding power supply can use direct current, intermediate frequency, radio frequency etc.；From
During tungsten oxide ceramic target, shielding power supply selects radio frequency.Power Control is in 1.2w/cm during sputtering2To 2.4w/cm2Between, using argon
As working reaction gas, oxygen proportion controls between 3% to 8% oxygen gas mixture, Stress control 0.2pa to 1.5pa it
Between, sputtering thickness is between 50nm to 1000nm, preferably 50~500nm.
Finally one layer of first protective layer is sputtered (for example, silicon nitride, aluminum oxide, oxidation in gained amorphous state tungsten oxide film
Silicon, zinc oxide, titanium oxide, zirconium oxide, magnesia, magnesium fluoride etc.), using 4 DEG C/s heating rate, it is heated to 300 DEG C to 700
Between DEG C, after being incubated 1 to 30 minutes, room temperature cooling, tungsten oxide film (the transparent pale blue with infrared barrier function is obtained
Color).For the refractive index of first protective layer between 1.3-2.6, thickness can be 50~1000nm, preferably 50~500nm.Make
For a detailed example, when the first protective layer elects silicon nitride as, using silicon target, or silicon nitride target shielding power supply using direct current or
Radio frequency, Power Control is in 1.2w/cm2, using 1:1 argon nitrogen mixed gas, Stress control 0.2Pa to 1.5Pa or so, sputter thickness
50nm-1000nm or so, preferably 50~500nm.
Wherein, it is amorphous state tungsten oxide film before the annealing of described amorphous state tungsten oxide film, after annealing
The tungsten oxide film mixed as crystalline state and amorphous state.
Do not include being arranged on the second protective layer between matrix and tungsten oxide film present invention also offers another
The preparation method of tungsten oxide film (referring to Fig. 9) with infrared barrier function.Illustrate to following exemplary provided by the invention
The preparation method of tungsten oxide film with infrared barrier function.
Matrix surface is cleaned and dried.The example detailed as one, simple glass is put into detergent solution and soaked
Several minutes, brush brushing surface is used afterwards, removes the greasy dirt and attachment impurity of glass surface.Glass is rinsed with clear water, removes washing
Essence residual, afterwards with deionized water rinsing, is removed the foreign ion on surface, is dried up using high pressure dry air.
Using tungsten oxide or tungsten as sputtering target material, directly amorphous state is prepared on matrix (for example, glass etc.) surface
Tungsten oxide film (is now amorphous state tungsten oxide film, blue brown or black-and-blue is now relatively low to visible light transmissivity, red
External shield poor-performing).For preparing amorphous state tungsten oxide film, using the reactive magnetron sputtering preparation of metal tungsten target progress
Into, or be directly prepared in an inert atmosphere through magnetron sputtering using tungsten oxide ceramic target.During from metal tungsten target, sputtering
Power supply can use direct current, intermediate frequency, radio frequency etc.；During from tungsten oxide ceramic target, shielding power supply selects radio frequency.Power control during sputtering
System is in 1.2w/cm2To 2.4w/cm2Between, arrived using argon oxygen gas mixture as working reaction gas, oxygen proportion control 3%
Between 8%, Stress control sputters thickness between 50nm to 1000nm between 0.2pa to 1.5pa, preferably 50~
500nm。
At 300-700 DEG C after one layer of first protective layer (transparent protective film) of gained amorphous state tungsten oxide film surface sputtering
Lower annealing 1-30 minutes, obtain the tungsten oxide film with infrared barrier function.Either gained amorphous state tungsten oxide is thin
After film annealing, layer of transparent diaphragm is sputtered again on its surface.The main purpose of annealing is so that amorphous state oxygen
Change amorphous state tungsten oxide portions turn in W film and obtain having the tungsten oxide of infrared barrier function thin for crystalline state tungsten oxide
Film (transparent light blue).If annealing time more than 30 minutes, can cause amorphous state tungsten oxide ratio too low, influence near red
The shielding action of exterior domain.The example detailed as one, when the first protective layer elects silicon nitride as, using silicon target, or silicon nitride
Target shielding power supply uses direct current or radio frequency, and Power Control is in 1.2w/cm2, using 1:1 argon nitrogen mixed gas, Stress control 0.2Pa
Arrive 1.5Pa or so, sputtering thickness 50nm-1000nm or so.
For the present invention when sputtering amorphous state tungsten oxide film, the first protective layer and the second protective layer, first pre-sputtering removes target
Material surface impurity, then just formal sputtering.Tungsten oxide film with infrared barrier function prepared by the present invention it is described with
Visible light transmissivity >=50% and infrared light transmittance≤50% of the tungsten oxide film of infrared barrier function.It is heretofore described
First protective layer, the second protective layer, amorphous state tungsten oxide film thickness are measured using SEM.
Embodiment is enumerated further below to describe the present invention in detail.It will similarly be understood that following examples are served only for this
Invention is further described, it is impossible to is interpreted as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright the above is made belong to protection scope of the present invention.Following examples are specific
Technological parameter etc. is also only an example in OK range, i.e. those skilled in the art can be done properly by this paper explanation
In the range of select, and do not really want to be defined in the concrete numerical value of hereafter example.
Embodiment 1
Simple glass is put into detergent solution and soaked several minutes, brush brushing surface is used afterwards, removes the greasy dirt of glass surface
With attachment impurity.Rinse glass with clear water, remove detergent residual, afterwards with deionized water rinsing, remove the impurity on surface from
Son, dried up using high pressure dry air；
Magnetic control sputtering device background is extracted into 10-5The order of magnitude starts to sputter.Sputtering tungsten oxide uses dc source, power setting 100W,
Target selects high purity metal tungsten target, and gas uses Ar and O2Gaseous mixture, purity are better than 99.9%, its O2Proportion is 5%,
Stress control 0.5Pa during sputtering；
Sputtered silicon nitride uses radio-frequency power supply, power setting 100W, and target selects the silicon target of general purity, and gas uses Ar and N2
Gaseous mixture, purity is due to 99%, ratio 1:1, sputtering pressure control 0.5Pa；
Pre-sputtering 10 minutes.Formal sputtering, sputtered silicon nitride, thickness 100nm, sputter tungsten oxide, thickness 150nm, sputtering
Silicon nitride, thickness 100nm, sputtering finish；
Glass plate is taken out after sputtering, is put into quick anneal oven and is made annealing treatment.The rate of heat addition is 4 DEG C/s, target temperature
500 DEG C of degree, it is incubated 2.5min.After heating, natural cooling in air is placed in.
Determine spectrum, quality inspection.Its membrane structure provides in Fig. 8.Fig. 5 is glass/silicon nitride/oxidation before annealing
The visible ray infrared transmittivity spectrum of tungsten/silicon nitride, as can be known from Fig. 5, the film visible light transmissivity before annealing is relatively low, and red
Outer transmitance is higher.Fig. 6 is the visible ray infrared transmittivity spectrum of glass/silicon nitride/tungsten oxide/silicon nitride after annealing, from
Understood in Fig. 6, after annealing, the visible light transmissivity of film is significantly raised, while infrared transmittivity is relatively low.
Embodiment 2
Simple glass is put into detergent solution and soaked several minutes, brush brushing surface is used afterwards, removes the greasy dirt of glass surface
With attachment impurity.Rinse glass with clear water, remove detergent residual, afterwards with deionized water rinsing, remove the impurity on surface from
Son, dried up using high pressure dry air；
Magnetic control sputtering device background is extracted into 10-5The order of magnitude starts to sputter.Sputtering tungsten oxide uses dc source, power setting 100W,
Target selects high purity metal tungsten target, and gas uses Ar and O2Gaseous mixture, purity are better than 99.9%, its O2Proportion is 5%,
Stress control 0.5Pa during sputtering；
Sputtered silicon nitride uses radio-frequency power supply, power setting 100W, and target selects the silicon target of general purity, and gas uses Ar and N2
Gaseous mixture, purity is due to 99%, ratio 1:1, sputtering pressure control 0.5pa；
Pre-sputtering 10 minutes.Formal sputtering, tungsten oxide is sputtered, thickness 150nm, sputtered silicon nitride, thickness 100nm, has been sputtered
Finish；
Glass plate is taken out after sputtering, is put into quick anneal oven and is made annealing treatment.The rate of heat addition is 4 DEG C/s, target temperature
500 DEG C of degree, it is incubated 5min.After heating, natural cooling in air is placed in.
Determine spectrum, quality inspection.Its membrane structure provides in Fig. 9.The optical characteristics of 350-2600nm scopes is in Fig. 7
In provide, the visible light transmissivity of film is higher as can be known from Fig. 7, and infrared transmittivity is relatively low.
Fig. 1 is the XRD of the tungsten oxide film before annealing prepared by embodiment 1.Tungsten oxide film is not as can be known from Fig. 1
Sharp diffraction maximum is occurred, illustrates that film is mainly made up of amorphous state tungsten oxide.Fig. 2 is the preparation of embodiment 1 by annealing
The XRD of the tungsten oxide film of processing, as can be known from Fig. 2 by annealing, crystalline state tungsten oxide is formed in tungsten oxide film, in diffraction
Sharp diffraction maximum is shown as on collection of illustrative plates.
Fig. 3 is the SEM figures of the tungsten oxide film before annealing prepared by embodiment 1, as can be known from Fig. 3 the film master before annealing
To be that amorphous state tiling accumulation forms, no crystalline morphology.Fig. 4 is the tungsten oxide film by annealing prepared by embodiment 1
SEM figures, as can be known from Fig. 4, after annealing, form crystalline state oxidation tungsten grain, membrane structure develops again.
Claims (9)
- A kind of 1. tungsten oxide film with infrared barrier function, it is characterised in that the oxidation with infrared barrier function W film includes matrix, the tungsten oxide film being made up of crystalline state tungsten oxide and the mixing of amorphous state tungsten oxide formed on matrix And the first protective layer on the tungsten oxide film surface is formed, the valence state composition bag of wolfram element in the tungsten oxide film Include+6 valency tungsten ions and+5 valency tungsten ions.
- 2. the tungsten oxide film according to claim 1 with infrared barrier function, it is characterised in that the tungsten oxide is thin Visible light transmissivity >=50% and infrared light transmittance≤50% of film.
- 3. the tungsten oxide film according to claim 1 or 2 with infrared barrier function, it is characterised in that the oxidation The thickness of W film is 50~1000nm, preferably 50~500nm.
- 4. the tungsten oxide film with infrared barrier function according to any one of claim 1-3, it is characterised in that also Including the second protective layer being arranged between described matrix and tungsten oxide film.
- 5. the tungsten oxide film according to claim 4 with infrared barrier function, it is characterised in that first protection Layer and/or the second protective layer are in silicon nitride, aluminum oxide, silica, zinc oxide, titanium oxide, zirconium oxide, magnesia, magnesium fluoride At least one.
- 6. the tungsten oxide film according to claim 5 with infrared barrier function, it is characterised in that first protection For the refractive index of layer and/or the second protective layer between 1.3-2.6, thickness is 50~1000nm, preferably 50~500nm.
- 7. the tungsten oxide film with infrared barrier function according to any one of claim 1-6, it is characterised in that institute Matrix is stated as one kind in glass, crystalline ceramics, silicon chip, sheet metal.
- 8. a kind of preparation method of the tungsten oxide film with infrared barrier function as any one of claim 1-7, its It is characterised by, sputters in matrix surface to obtain amorphous state tungsten oxide film using magnetron sputtering technique, then at 300~700 DEG C Lower annealing 1~30 minute, so that amorphous state tungsten oxide portions turn is crystalline state tungsten oxide in amorphous state tungsten oxide film, Obtain the tungsten oxide film with infrared barrier function.
- 9. preparation method according to claim 8, it is characterised in that the tungsten oxide film aoxidizes for sub-stoichiometric ratio Tungsten, consisting of WOx, wherein 2≤x≤3.
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| CN108516699A (en) * | 2018-04-17 | 2018-09-11 | 武汉理工大学 | A kind of low radiation coated glass |
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| CN109650741A (en) * | 2019-02-21 | 2019-04-19 | 合肥工业大学 | A kind of tungsten trioxide nano bowl electrochromic material and preparation method thereof |
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| WO2023144222A1 (en) * | 2022-01-27 | 2023-08-03 | Saint-Gobain Glass France | Transparent substrate provided with a functional stack of thin layers |
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| CN108516699A (en) * | 2018-04-17 | 2018-09-11 | 武汉理工大学 | A kind of low radiation coated glass |
| CN109097733A (en) * | 2018-08-21 | 2018-12-28 | 中国科学院上海硅酸盐研究所 | A kind of oxygen-containing hydrogenation yttrium light thermochromism multilayered film material that can quickly fade |
| CN109097734A (en) * | 2018-08-21 | 2018-12-28 | 中国科学院上海硅酸盐研究所 | Oxygen-containing hydrogenation yttrium light thermochromism multilayered film material |
| CN109650741A (en) * | 2019-02-21 | 2019-04-19 | 合肥工业大学 | A kind of tungsten trioxide nano bowl electrochromic material and preparation method thereof |
| CN109650741B (en) * | 2019-02-21 | 2021-09-10 | 合肥工业大学 | Tungsten trioxide nanometer bowl electrochromic material and preparation method thereof |
| CN113943928B (en) * | 2021-10-18 | 2023-09-12 | 哈尔滨工业大学 | Preparation method of tungsten oxide electrochromic film with controllable ordered structure |
| CN113943928A (en) * | 2021-10-18 | 2022-01-18 | 哈尔滨工业大学 | Preparation method of tungsten oxide electrochromic film with controllable ordered structure |
| FR3132096A1 (en) * | 2022-01-27 | 2023-07-28 | Saint-Gobain Glass France | Transparent substrate provided with a functional stack of thin layers |
| WO2023143884A1 (en) * | 2022-01-27 | 2023-08-03 | Saint-Gobain Glass France | Transparent substrate provided with a functional stack of thin layers |
| WO2023144222A1 (en) * | 2022-01-27 | 2023-08-03 | Saint-Gobain Glass France | Transparent substrate provided with a functional stack of thin layers |
| WO2023144223A1 (en) * | 2022-01-27 | 2023-08-03 | Saint-Gobain Glass France | Transparent substrate provided with a functional stack of thin layers |
| WO2023144221A1 (en) * | 2022-01-27 | 2023-08-03 | Saint-Gobain Glass France | Transparent substrate provided with a functional stack of thin layers |
| FR3132095A1 (en) * | 2022-01-27 | 2023-07-28 | Saint-Gobain Glass France | Transparent substrate provided with a functional stack of thin layers |
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