CN109457228A - A kind of temperature automatically controlled smart membranes and preparation method thereof - Google Patents
A kind of temperature automatically controlled smart membranes and preparation method thereof Download PDFInfo
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- CN109457228A CN109457228A CN201811549418.2A CN201811549418A CN109457228A CN 109457228 A CN109457228 A CN 109457228A CN 201811549418 A CN201811549418 A CN 201811549418A CN 109457228 A CN109457228 A CN 109457228A
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
- C23C16/513—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges using plasma jets
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/083—Oxides of refractory metals or yttrium
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/34—Nitrides
- C23C16/345—Silicon nitride
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B10/00—Integration of renewable energy sources in buildings
- Y02B10/20—Solar thermal
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Abstract
A kind of temperature automatically controlled smart membranes and preparation method thereof.A kind of vanadium oxide composite film, including the first fexible film, vanadium oxide film and the second fexible film；Wherein, the vanadium oxide film is formed between the first fexible film and the second fexible film；When the temperature of the vanadium oxide composite film reduces, the vanadium oxide composite film increases the transmissivity of the infrared light in incident light；When the temperature of the vanadium oxide composite film increases, decrease in transmission of the vanadium oxide composite film to the infrared light in incident light.The flexible material that above-mentioned vanadium oxide composite film uses high temperature resistant, corrosion-resistant, environmental-friendly, light transmittance is high forms stepped construction by one layer of vanadium oxide film as substrate, centre.The rigid basements such as this film and glass, silicon wafer adaptability is good, has a good characteristics such as flexibility, tortuosity, wide adaptability, light, while easy to disassemble, cleaning and assembly, can also Bidirectional temperature-controlling, it is good to the modulating performance of infrared light.
Description
Technical field
The present invention relates to a kind of intelligent temperature control film, especially a kind of vanadium oxide flexible intelligent temperature control film.
Background technique
The development of global economy constantly consumes limited non-renewable energy resources, and the mankind will be faced with the danger of energy shortage
Machine.In the growing energy consumption in the whole world, either developed country or developing country, building energy consumption are all countries
More great one in total energy consumption, the building energy consumption of developed country even accounts for the one third or so of national total energy consumption.
In all kinds of energy consumptions, the energy consumption of heating and air-conditioning accounts for 55% or so of building total energy consumption, and China's construction unit
Area energy consumption is 2 to 3 times of developed country, and in trend is risen year by year, energy waste is extremely serious.In modern building,
Window is the indispensable important component of building, it substantially improve the daylighting of building and ventilation can, and energy
So that house has certain open area, expand the visual field.With the modernization of construction style, the light-transmission types such as exterior window and glass curtain wall
The ratio that building enclosure accounts for exterior surface area is higher and higher, and the thermal energy of solar radiation is mainly entered the room by window.
According to measuring and calculating, the heat exchange carried out by ordinary glazed window is lost accounts for 58% and 73% in winter and summer respectively, thus
It can be seen that caused by the major part of thermal losses under construction is all heat exchange by windowpane, the especially loss of summer
Up to 73%.This is because solar energy about 99% be distributed in wavelength be 0.2-2.5 μm in the range of, wherein 0.2~0.38
μm ultraviolet region account for about the 8% of gross energy, 0.38~0.76 μm of visible light accounts for about 43%, 0.76~2.5 μm of infrared light
48% is accounted for, and simple glass does not have ability of regulation and control to the sunlight of different wave length, when outdoor temperature is higher, cannot effectively end
Near-infrared sunlight increases the cooling load of air-conditioning, and when outdoor temperature is low, indoor heat passes through glass again in the form of heat radiation
Glass surface is scattered and disappeared, and the heat preservation load of air-conditioning is increased.In the case where adjusting room temperature using air-conditioning, according to measurement, refrigeration temperature
Degree improves 2 DEG C, and cooling load reduces about 20%；Heating temperature turns down 2 DEG C, and heating load reduces about 30%.It can be seen from the above, changing
Kind glass pane heat-insulating property will be the key point for improving building energy consumption.
Existing structure mainly uses low-E (Low-E) plated film of the passive tune heat type of simple glass and business application
Glass can effectively reduce the radiance of glass surface, and then reduce corresponding heat loss through radiation, improve the property of glass pane insulation
Energy.But these glass once structure formation after, optical characteristics is difficult to change, cannot with seasonal variations into
Row bidirectional modulation, and be difficult to re-assembly, change.In addition, the existing glass curtain wall of China has accounted for the 85% of global total amount.According to not
Statistics completely, in nearly 20 years time, light glass curtain wall has broken through 500,000,000 square metres in China.So huge quantity is difficult to
Novel glass is replaced in a short time.In addition, cleaning and replacement that glass is frequent, not only increase the cost of manual maintenance,
Also increase security risk.
The prior art " a kind of intelligent glass of automatic temperature-control " (CN204020142U) discloses one kind by one or more layers
The assembly of transparent material layer and the stepped construction of at least one layer of vanadium dioxide film composition, but its light transmittance is unknown, performance
It is not high, it is difficult to bidirectional modulation temperature.In addition, the cleaning for the intelligent glass that this method obtains and replacement not only increase manual maintenance
Cost, also increase security risk.
Summary of the invention
For the above technical problem of the existing technology, the present invention proposes a kind of new flexible intelligent temperature control film, makes
Use high temperature resistant, the flexible material that corrosion-resistant, environmental-friendly, light transmittance is high is as substrate, centre is made of one layer of vanadium oxide film
Stepped construction.The rigid basements such as this film and glass, silicon wafer adaptability is good, has flexibility, tortuosity, wide adaptability, light
Just equal good characteristics, while easy to disassemble, cleaning, assembly, can also Bidirectional temperature-controlling, it is good to the modulating performance of infrared light.
The present invention relates to a kind of preparation methods of vanadium oxide composite film, including, high temperature resistant is formed on the substrate in step 1
The first flexible material film, to form substrate；Step 2 forms oxidation on first flexible material on the substrate
Vanadium precursor thin-film；Step 3 carries out high annealing to the substrate for being formed with the vanadium oxide precursor thin-film, and being formed has oxygen
Change the laminated film of vanadium film；Step 4 forms the second flexible material film on the vanadium oxide film.
It preferably, further include substrate preparation process before the step 1；Wherein, the substrate is silicon substrate.
Preferably, the substrate preparation process further comprises forming silicon nitride layer on the silicon substrate, to form tool
There is the silicon substrate of silicon nitride layer；First flexible material film described in step 1 is formed in the silicon nitride layer on the substrate
On.
It preferably, further include strip step after the step 3；Wherein, the strip step includes, by described first
Flexible material film, vanadium oxide film and the second flexible material film are removed from the substrate, are obtained flexible described first
The laminated film of vanadium oxide film is formed in material film and the second flexible material film.
Preferably, the thermal decomposition temperature of first flexible material resistant to high temperature is higher than the temperature of step 3 high temperature annealing
Degree.
Preferably, the first flexible material film and the second flexible material film are by visible, infrared band
The translucent material for all having highly transmissive is formed.
Preferably, first flexible material is fire resistant resin material.
Preferably, the fire resistant resin material is polyimides.
Preferably, the thermal decomposition temperature of the polyimides is greater than 400 DEG C.
Preferably, the first flexible material film is made of with the second flexible material film identical material.
Preferably, in step 2, before forming the vanadium oxide on first flexible material by magnetically controlled sputter method
Drive body thin film.
Preferably, the condition of the magnetron sputtering are as follows: substrate temperature is 100-400 DEG C, and vacuum degree is lower than 5.0 × 10-4Pa,
Target and substrate distance are 80mm, argon flow 15-30sccm, oxygen flow 0.3-2.0sccm, and argon oxygen ratio is 7.5:1-
39:1, sputtering operating air pressure are 0.3Pa, sputtering power 150-200W, sedimentation time 60min.
Preferably, in step 3 carry out high annealing condition be, in vacuum or inert environments to the vanadium oxide before
Body thin film is driven to anneal.
Preferably, the temperature of high annealing is carried out in step 3 within the scope of 420-480 DEG C.
Preferably, the environment of the annealing is that vacuum degree is the argon atmosphere of 0.1-0.3Pa.
Preferably, the step 2 further includes that the method for polyimide solution blade coating or spin coating is uniformly applied to institute
It states on substrate, is toasted at 25-60 DEG C 3 hours, then heat 8 hours and anneal at 300-400 DEG C, on a silicon substrate
To uniform Kapton, to form the first flexible material film.
Preferably, the step 4 further includes that the method for polyimide solution blade coating or spin coating is uniformly applied to institute
It states on vanadium oxide film, is toasted at 25-60 DEG C 3 hours, then heat 8 hours and anneal at 300-400 DEG C, described
Uniform Kapton is obtained on vanadium oxide film, to form the second flexible material film.
Preferably, the first flexible material film with a thickness of 10-20 μm, the thickness of vanadium oxide film is less than 100nm, second
Flexible material film with a thickness of 10-20 μm.
The invention further relates to a kind of preparation methods of vanadium oxide composite film, including, step 1, preparing substrate, in silicon substrate
Silicon nitride layer is formed on bottom；The substrate is sequentially placed into deionized water, dehydrated alcohol, surpassed in acetone solvent respectively by step 2
Sound cleans 10 minutes, and dries；Step 3 prepares substrate, forms the first Kapton over the substrate；Step 4,
The substrate is sequentially placed into deionized water, dehydrated alcohol, is cleaned by ultrasonic respectively 10 minutes in acetone solvent, and is dried；Step
Five, it is 5.0 × 10 that cleaned substrate, which is placed in vacuum degree,-4In the high vacuum rf magnetron sputtering equipment of Pa, in substrate temperature
It is 7.5:1-39:1 for 100-400 DEG C, argon flow 15-30sccm, oxygen flow 0.3-2.0sccm, argon oxygen ratio, sputtering
Under conditions of operating air pressure is 0.3Pa, sputtering power 150-200W, target and substrate distance are 80mm, 60min is deposited, with
Vanadium oxide precursor thin-film is formed on the substrate；The target is vanadium metal target；Step 6 is annealed at 420-480 DEG C
30min or more, the vanadium oxide film of acquisition are stratiform polycrystalline film；Step 7 forms second on the vanadium oxide film
Kapton.
It preferably, further include strip step after the step 7；Wherein, the strip step includes, by described first
Flexible material film, vanadium oxide film and the second flexible material film are removed from the substrate, are obtained flexible described first
The laminated film of vanadium oxide film is formed in material film and the second flexible material film.Preferably, the step 3
It further include that the method for polyimide solution blade coating or spin coating is uniformly smeared over the substrate, toasts 3 at 25-60 DEG C
Hour, it then heats 8 hours and anneals at 300-400 DEG C, obtain uniform Kapton, on a silicon substrate with shape
At the first Kapton.
Preferably, the step 7 further includes that the method for polyimide solution blade coating or spin coating is uniformly applied to institute
It states on vanadium oxide film, is toasted at 25-60 DEG C 3 hours, then heat 8 hours and anneal at 300-400 DEG C, described
Uniform Kapton is obtained on vanadium oxide film, to form the second Kapton.
Preferably, the first flexible material film with a thickness of 10-20 μm, the thickness of vanadium oxide film is less than 100nm, second
Flexible material film with a thickness of 10-20 μm.
The invention further relates to a kind of vanadium oxide composite film, including the first fexible film, vanadium oxide film and second soft
Property film；Wherein, the vanadium oxide film is formed between the first fexible film and the second fexible film；When the vanadium oxide is multiple
When the temperature of conjunction film is lower than the phase transition temperature of vanadium oxide, the infrared light in incident light can penetrate the vanadium oxide composite film
And it is transmitted through the other side；It is red in incident light when the temperature of the vanadium oxide composite film is higher than the phase transition temperature of vanadium oxide
Outer light can be reflected by the vanadium oxide composite film.
Preferably, first fexible film and the second tenderness film are formed from the same material.
Preferably, first fexible film and second fexible film are formed by polyimide material.
Preferably, there is the transmissivity of infrared light of the laminated film to wave-length coverage in 750-1700nm modulation to make
With.
Preferably, the first flexible material film with a thickness of 10-20 μm, the thickness of vanadium oxide film is less than 100nm, second
Flexible material film with a thickness of 10-20 μm.
Preferably, prepared by vanadium oxide composite film method as described in any one of aforementioned approaches method forms.
Compared with prior art, the beneficial effects of the present invention are with high temperature resistant, corrosion-resistant, environmental-friendly, light transmittance is high
Flexible material polyimides as two sides substrate, the good vanadium oxide film of high temperature processability is used in centre, so that whole
Body thin film is bigger for the modulation amplitude of infrared light, and the rigid basements such as film proposed by the present invention and glass, silicon wafer adhere to
Property is good, and the scope of application is wider.
Detailed description of the invention
Attached drawing 1: schematic diagram under vanadium oxide composite film low temperature environment；
Attached drawing 2: schematic diagram under vanadium oxide composite film hot environment；
Attached drawing 3: the vanadium oxide film scanning electron microscope diagram of 1 method of embodiment preparation；
Attached drawing 4: modulating action of the vanadium oxide composite film of 1 method of embodiment preparation to infrared band.
Specific embodiment
The temperature automatically controlled smart membranes of one kind of the present embodiment use high temperature resistant, corrosion-resistant, environmental-friendly, saturating
The high flexible material of light rate is as substrate, and centre is by one layer of vanadium oxide (VOx) film composition stepped construction assembly.It is this thin
The rigid basements such as film and glass, silicon wafer adaptability is good, has flexibility, tortuosity, wide adaptability, and also having has made with reality
There is characteristic compatible very well with glass, easy to disassemble, cleaning, assembly, the film can Bidirectional temperature-controlling, it is light, to infrared light
Modulating performance is good.Wherein, the vanadium oxide is not limited only to VO2Or V2O5, that is, include the oxide of various forms of vanadium, i.e., usually
VOx is denoted as by those skilled in the art.
Preparation method mainly includes that the first flexible material film resistant to high temperature is formed on the substrate, and so as to form substrate,
The substrate can be used in forming vanadium oxide film in subsequent step；It is formed on first flexible material on the substrate
Then vanadium oxide precursor thin-film further carries out high annealing to the substrate for being formed with the vanadium oxide precursor thin-film, with
Form the laminated film of vanadium oxide film；The second flexible material film is further formed on the vanadium oxide film.
In some embodiments, further include the steps that preparing substrate, usually select silicon substrate as the laminated film
Substrate is directly combined the laminated film with facilitating with semiconductor device fabrication processes.
In some embodiments, the step of preparing substrate further comprises forming silicon nitride layer on the silicon substrate, with
Form the silicon substrate with silicon nitride layer；And described in further the first flexible material film is formed on the substrate
On silicon nitride layer.Silicon nitride layer can play the role of insulating layer, so that the whole preferably MEMS suitable for device fabrication
Technique preparation.During the reaction, the silicon nitride layer is only used as the carrier of fexible film together with silicon wafer, is not involved in directly anti-
It answers.
It in some embodiments, further include strip step；Wherein, the strip step includes, by the described first flexible material
Material film, vanadium oxide film and the second flexible material film are removed from the substrate, are obtained thin in first flexible material
The laminated film of vanadium oxide film is formed in film and the second flexible material film.By this step, can individually obtain
Vanadium oxide composite film flexible can be adapted under different use environments and use condition as individual flexible thin-film material
It uses.
In some embodiments, the high-temperature flexible material is preferably fire resistant resin material, and further preferably
Polyimide resin material, and the thermal decomposition temperature of the polyimides is greater than 400 DEG C.Preferably, the high-temperature flexible material
The thermal decomposition temperature of material is higher than the temperature of high annealing.So that being formed in the oxidation of the first flexible material film surface
Vanadium film can anneal under conditions of high temperature, and formed surface uniformly, compact structure, quality of forming film be good, well-crystallized,
And vanadium oxide and polyimides are tightly combined vanadium oxide composite film not easily to fall off.
In some embodiments, the first flexible material film and the second flexible material film by visible light and
The translucent material that highly transmissive is all had in infrared band is formed.Due to the first flexible material film and described second soft
Property material film formed for translucent material so that flexible vanadium oxide composite film can be suitable for as window needs light transmission
In environment.
In some embodiments, the first flexible material film and the second flexible material film are by identical material
It constitutes.It is possible thereby to reduce preparation cost of the flexible vanadium oxide composite film in whole preparation process.
In some embodiments, the vanadium oxide forerunner is formed on first flexible material by magnetically controlled sputter method
Body thin film；And the condition of the magnetron sputtering is preferably, substrate temperature is 100-400 DEG C, and vacuum degree is lower than 5.0 × 10-4Pa, target
Material and substrate distance are 80mm, argon flow 15-30sccm, oxygen flow 0.3-2.0sccm, and argon oxygen ratio is 7.5:1-
39:1, sputtering operating air pressure are 0.3Pa, sputtering power 150-200W, sedimentation time 60min；Wherein, used described
Target is vanadium metal target, quality purity >=99.99%, purity >=99.999% of argon gas, purity >=99.99% of oxygen.
With this obtain surface uniformly, compact structure, quality of forming film be good, well-crystallized, and vanadium oxide is tightly combined with polyimides and is not easy
The vanadium oxide film to fall off.
In some embodiments, the condition of high annealing is, to the vanadium oxide presoma in vacuum or inert environments
Film is annealed；Further preferably, it in the argon atmosphere that vacuum degree is 0.1-0.3Pa, anneals at 420-480 DEG C
30min or more, the vanadium oxide film of acquisition are stratiform polycrystalline film.High annealing is carried out under vacuum or inert conditions, is had
Help improve quality of forming film, formed surface uniformly, compact structure, well-crystallized, vanadium oxide film not easily to fall off.
In some embodiments, the preparation step of the first flexible material film are as follows: scratch polyimide solution
Or the method for spin coating is uniformly smeared over the substrate, is toasted 3 hours at 25-60 DEG C, is then heated 8 at 300-400 DEG C
Hour anneals, and obtains uniform Kapton, on a silicon substrate to form the first flexible material film；It is described
Second flexible material film is preferably also formed on the vanadium oxide film using identical step.It is possible thereby to form high temperature resistant
Kapton, using identical method formed two flexible material films, can reduce whole preparation cost.It is preferred that
For the dielectric constant of resulting Kapton is 3.4, and thermal decomposition temperature is 494 DEG C.
In some embodiments, the first flexible material film with a thickness of 10-20 μm, the thickness of the vanadium oxide film
Degree be less than 100nm, the second flexible material film with a thickness of 10-20 μm.The laminated film being consequently formed can either guarantee
Enough translucency and flexibility, and enough infrared light modulation effects can be played.
In some embodiments, specific vanadium oxide film preparation method includes step 1, preparing substrate, in silicon base
Upper formation silicon nitride layer；The substrate is sequentially placed into deionized water, dehydrated alcohol, ultrasound respectively in acetone solvent by step 2
Cleaning 10 minutes, and dry；Step 3 prepares substrate, forms the first Kapton over the substrate；Step 4, will
The substrate is sequentially placed into deionized water, dehydrated alcohol, is cleaned by ultrasonic respectively 10 minutes in acetone solvent, and dries；Step 5,
It is 5.0 × 10 that cleaned substrate, which is placed in vacuum degree,-4In the high vacuum rf magnetron sputtering equipment of Pa, it is in substrate temperature
100-400 DEG C, argon flow 15-30sccm, oxygen flow 0.3-2.0sccm, argon oxygen ratio be 7.5:1-39:1, sputtering work
Under conditions of air pressure is 0.3Pa, sputtering power 150-200W, target and substrate distance are 80mm, deposit 60min, with
Vanadium oxide precursor thin-film is formed on the substrate；The target is the vanadium metal target of quality purity >=99.99%；Step 6,
In 420-480 DEG C of annealing 30min or more, the vanadium oxide film of acquisition is stratiform polycrystalline film；Step 7, in the vanadium oxide
The second Kapton is formed on film.With this obtain surface uniformly, compact structure, quality of forming film be good, well-crystallized and oxygen
Change vanadium and polyimides is tightly combined vanadium oxide film not easily to fall off.
It in some embodiments, further include strip step after the step 7；Wherein, the strip step includes,
The first flexible material film, vanadium oxide film and the second flexible material film are removed from the substrate, obtained in institute
State the laminated film that vanadium oxide film is formed in the first flexible material film and the second flexible material film.It is walked by this
Suddenly, vanadium oxide composite film flexible can be individually obtained, can be adapted under different use environments and use condition as single
Only flexible thin-film material uses.
In some embodiments, the step 3 further includes scratching polyimide solution or the method for spin coating being uniform
It smears over the substrate, 3 is toasted at 25-60 DEG C, then heats 8 hours and anneals at 300-400 DEG C, in silicon base
On obtain uniform Kapton.By this step, the Kapton with high thermal decomposition temperature can be obtained, it is excellent
It is selected as, the thermal decomposition temperature of the Kapton is greater than 400 DEG C.Preferably, the dielectric of resulting Kapton is normal
Number is 3.4, and thermal decomposition temperature is 494 DEG C.
The vanadium oxide composite film prepared by method made above, including the first fexible film, vanadium oxide film,
And second fexible film；Wherein, the vanadium oxide film is formed between the first fexible film and the second fexible film；Work as institute
When stating the temperature of vanadium oxide composite film and being lower than the phase transition temperature of vanadium oxide, the infrared light in incident light can penetrate the oxidation
Vanadium laminated film is simultaneously transmitted through the other side；When the temperature of the vanadium oxide composite film is higher than the phase transition temperature of vanadium oxide, enter
The infrared light penetrated in light can be reflected by the vanadium oxide composite film.Make the infrared light of the vanadium oxide composite film with this
Transmissivity can with temperature change, the infrared light of transmission is realized it is intelligent automatic regulated, to play auxiliary to a certain extent
Adjust the effect of room temperature.When outdoor temperature is higher, room temperature is quickly increased, after reaching vanadium oxide phase transition temperature,
So that it is changed into tetragonal phase by original monoclinic phase, i.e., all band reflection infrared light is transformed by all band transmitted infrared light, from
And reduce and account for the energy of the infrared region of solar radiation energy 48% and enter the room, the burden of air-conditioning is alleviated, energy has been saved
Source.When outdoor temperature is lower than vanadium oxide phase transition temperature, vanadium oxide is the monoclinic phase of semiconductor form at this time, and all band transmission is infrared
Light, so that warm sunlight is entered the room through glass pane, temperature rises.And interior when reaching phase transition temperature vanadium oxide occur
Mutually it is turned into the tetragonal phase of metallic state, all band reflects infrared light.To firmly lock indoors indoor heat radiation, room is reduced
Interior heat is scattered and disappeared by glass pane, and then mitigates the load of heating of house, energy saving.
In addition, the stepped construction of the laminated film is followed successively by transparent material layer, vanadium oxide membrane, lower light transmission from top to bottom
Material layer.Such structure is clipped in vanadium oxide film among upper layer and lower layer transparent material layer, protects vanadium oxide well
Film will not contact other impurities or sharp object to cause the pollution or breakage of vanadium oxide film, while also avoid because long
Phase ingress of air is oxidized vanadium oxide film and reduces its control action to the solar energy entered the room.
In some embodiments, first fexible film and second fexible film are formed from the same material, excellent
It is selected as first fexible film and second fexible film is formed by polyimide material.So that the vanadium oxide
Laminated film can have the effect of reflecting ultraviolet light while visible light wave range has high transmittance, and enable to oxygen
Changing vanadium laminated film integrally has flexibility, and the vanadium oxide film can be bonded, not easily to fall off.
In some embodiments, the first flexible material film with a thickness of 10-20 μm, the thickness of the vanadium oxide film
Degree be less than 100nm, the second flexible material film with a thickness of 10-20 μm.The laminated film being consequently formed can either guarantee
Enough translucency and flexibility, and enough infrared light modulation effects can be played.Wherein, the work of laminated film of the invention
Make wavelength preferably in the range of 750-1500nm.
Embodiment 1
The preparation method for the vanadium oxide composite film that the present embodiment is related to is specific as follows:
Step 1, preparing substrate.Silicon base is provided, and heavy by plasma enhanced chemical vapor in the silicon base
Area method forms silicon nitride layer.Silicon base is having a size of 33mm × 33mm used in it.Silicon nitride layer can play the work of insulating layer
With so that the whole preferably MEMS technology preparation suitable for device fabrication.During the reaction, the silicon nitride layer only with
Silicon wafer is used as the carrier of fexible film together, is not involved in direct reaction.
The substrate is sequentially placed into deionized water, dehydrated alcohol, is cleaned by ultrasonic 10 points respectively in acetone solvent by step 2
Clock, and dry.
Step 3 prepares substrate.It is dry that the method for polyimides (PI) solution blade coating or spin coating is uniformly applied to cleaning
It on the net substrate, is toasted 3 hours at 25-60 DEG C, removes the organic principle in polyimides, then in high temperature 300-400
It is heated 8 hours at DEG C, imidization occurs, finally obtains uniform first Kapton over the substrate.Gained
Polymide dielectric constant be 3.4, thermal decomposition temperature be 494 DEG C.
The substrate is sequentially placed into deionized water, dehydrated alcohol, is cleaned by ultrasonic 10 points respectively in acetone solvent by step 4
Clock, and dry.
Step 5 prepares vanadium oxide precursor thin-film.It is lower than 5.0 × 10 that cleaned substrate, which is placed in vacuum degree,-4Pa
High vacuum rf magnetron sputtering equipment in, using the mixed gas of oxygen and argon gas as working gas, sputter the vacuum of work
Degree is 2.5~4.0 × 10-4Pa, for vanadium metal as target, target and substrate distance are 80mm, argon flow 30sccm, oxygen
Flow is 0.83sccm, and argon oxygen ratio is 36:1, and sputtering operating air pressure is 0.3Pa, sputtering power 190W, substrate temperature when growth
It is 400 DEG C, sedimentation time 60min.Wherein, the quality purity of vanadium metal target is 99.99%, the purity of argon gas >=
99.999%, purity >=99.99% of oxygen.Resulting vanadium oxide (VOx) be stratiform amorphous VOxFilm.
Step 6, high annealing.It is preferred that annealing in vacuum or argon atmosphere high temperature.Atmosphere is adjusted to 0.1-
The argon atmosphere of 0.3Pa, in 480 DEG C or so annealing 30min, the vanadium oxide (VO of acquisitionx) it is stratiform polycrystalline film.
It is thin to be uniformly applied to the vanadium oxide prepared by step 7 for the method for polyimides (PI) solution blade coating or spin coating
On film, uniform second Kapton is prepared in the same method of step 3, obtains compound vanadium oxide film.
Step 8, the first Kapton that step 3 to step 7 is formed, vanadium oxide film and the second polyamides
Imines film is removed from the substrate together, to form vanadium oxide composite film flexible.
Referring to attached Fig. 1 and 2 it is found that thus method obtain vanadium oxide composite film 1 include the first Kapton 11,
Vanadium oxide film 12 and the second Kapton 13, the vanadium oxide film 12 are formed in first Kapton
Between 11 and second Kapton 13.Wherein, first Kapton 11 with a thickness of 10-20 μm, institute
State vanadium oxide film 12 thickness be less than 100nm, second Kapton 13 with a thickness of 10-20 μm.The oxidation
The flexible material Kapton that vanadium laminated film 1 uses high temperature resistant, corrosion-resistant, environmental-friendly, light transmittance is high as substrate,
Centre forms stepped construction by one layer of vanadium oxide film.The rigid basements such as this laminated film and glass, silicon wafer adaptability is good,
Have the good characteristics such as flexibility, tortuosity, wide adaptability, light.
Fig. 3 is shown, and the vanadium oxide film in flexible vanadium oxide composite film that the present embodiment method finally obtains exists
The ZEISS that Carl Zeiss Corporation company producesThe scanning of the standard obtained under the scanning electron microscope of 55 models
Electron microscope picture.It can be seen from the figure that the vanadium oxide film has the characteristic of layer growth, membrane structure is fine and close, and
Crystallization effect is good, and the quality of film is high.
Fig. 4 is shown, and the vanadium oxide composite film 1 that the present embodiment method obtains illustrates the modulating action of infrared band
Figure.The vanadium oxide composite film 1 is set forth at 25 DEG C and 80 DEG C in figure for the tune of the light of infrared band different wave length
Production is used, and obviously shows to gradually decrease the transmissivity of infrared band light at 80 DEG C.
As illustrated in fig. 1 and 2, the vanadium oxide composite film 1 has the visible light 22 in the natural light 2 from the sun
Higher transmissivity allows visible light 22 to penetrate the vanadium oxide composite film 1 and be transmitted through the other side；The vanadium oxide is compound
Film 1 is for the reflectivity with higher of ultraviolet light 23 in the natural light 2 from the sun, i.e. ultraviolet light 23 in natural light 2
With lower transmissivity.With the reduction of the temperature of the vanadium oxide composite film 1, the vanadium oxide composite film 1 for
The transmissivity of infrared light 21 in incident natural light 2 gradually increases, so that showing characteristic as shown in Figure 1, that is, comes from
Infrared light 21 and visible light 22 in the natural light 2 of the sun can penetrate the vanadium oxide composite film 1 and be transmitted to the other side,
And the transmissivity of the ultraviolet light 23 in natural light 2 is lower, reflectivity is higher.With the temperature of the vanadium oxide composite film 1
It increasing, the vanadium oxide composite film 1 gradually decreases the transmissivity of the infrared light 21 in incident natural light 2, so that
Characteristic as shown in Figure 2 is shown, i.e. visible light 22 in the natural light 2 from the sun can penetrate the vanadium oxide THIN COMPOSITE
Film 1 is simultaneously transmitted to the other side, and the transmissivity of infrared light 21 and ultraviolet light 23 in natural light 2 is lower, reflectivity is higher.
Since the vanadium oxide composite film 1 has characteristic so, if the vanadium oxide composite film 1 is applied
It, can be under relative low temperature environment as shown in Figure 1 and high relative humidity environment as shown in Figure 2 onto existing windowpane
Under, automatic adjusument is carried out to indoor amount of infrared light is injected, effective auxiliary adjustment can be played the role of to room temperature.
In addition, the high temperature resistant of vanadium oxide composite film 1, the flexible material that corrosion-resistant, environmental-friendly, light transmittance is high are poly-
Acid imide uses the good vanadium oxide of high temperature processability as substrate, in centre, so that tune of the monolithic film membrane for infrared light
Amplitude processed is obvious.Since the vanadium oxide composite film 1 is flexible composite film, it is easy to apply to glass, silicon wafer
Etc. in rigid basements, and there is good adhesiveness to be not only easy to install in use, it is easier to maintenance and replacement.
The present invention proposes a kind of flexible intelligent temperature control film, and using high temperature resistant, corrosion-resistant, environmental-friendly, light transmittance is high
Flexible material forms stepped construction by one layer of vanadium oxide film as substrate, centre.The rigidity base such as this film and glass, silicon wafer
Bottom adaptability is good, has the good characteristics such as flexibility, tortuosity, wide adaptability, light, and easy to disassemble, cleaning, assembly,
Simultaneously can also Bidirectional temperature-controlling, it is good to the modulating performance of infrared light.Compared with prior art, laminated film of the invention it is whole for
The modulation amplitude of infrared light is bigger.
It is recited above only to illustrate some embodiments of the present invention, due to the ordinary skill people to same technique field
It is easy to carry out several modifications and change on this basis for member, therefore this specification is not intended to for the present invention to be confined to institute
Show in the specific structure, method and step, process flow, the scope of application, therefore it is all it is all may be utilized accordingly repair
Change and equivalent, belongs to the applied the scope of the patents of the present invention.
Claims (29)
1. a kind of preparation method of vanadium oxide composite film, including,
The first flexible material film resistant to high temperature is formed on the substrate, to form substrate in step 1；
Step 2 forms vanadium oxide precursor thin-film on first flexible material on the substrate；
Step 3 carries out high annealing to the substrate for being formed with the vanadium oxide precursor thin-film, and being formed has vanadium oxide film
Laminated film；
Step 4 forms the second flexible material film on the vanadium oxide film.
2. the method as described in claim 1, which is characterized in that further include substrate preparation process before the step 1；Its
In, the substrate is silicon substrate.
3. method according to claim 2, which is characterized in that the substrate preparation process further comprises serving as a contrast in the silicon
Silicon nitride layer is formed on bottom, to form the silicon substrate with silicon nitride layer；First flexible material film described in step 1 is formed
In on the silicon nitride layer on the substrate.
4. the method as described in claim 1, which is characterized in that further include strip step after the step 3；Wherein, institute
Stating strip step includes, by the first flexible material film, vanadium oxide film and the second flexible material film from the substrate
Upper removing, acquisition are formed with answering for vanadium oxide film in the first flexible material film and the second flexible material film
Close film.
5. the method as described in claim 1, which is characterized in that the thermal decomposition temperature of first flexible material resistant to high temperature is high
In the temperature of step 3 high temperature annealing.
6. method as claimed in claim 5, which is characterized in that the first flexible material film and second flexible material
Film is formed by the translucent material for all having highly transmissive in visible light and infrared band.
7. such as method described in claim 5 or 6, which is characterized in that first flexible material is fire resistant resin material.
8. the method for claim 7, which is characterized in that the fire resistant resin material is polyimides.
9. method according to claim 8, which is characterized in that the thermal decomposition temperature of the polyimides is greater than 400 DEG C.
10. method as claimed in any one of claims 1-9 wherein, which is characterized in that the first flexible material film with it is described
Second flexible material film is made of identical material.
11. such as method of any of claims 1-10, which is characterized in that in step 2, pass through magnetically controlled sputter method
The vanadium oxide precursor thin-film is formed on first flexible material.
12. method as claimed in claim 11, which is characterized in that the condition of the magnetron sputtering are as follows: substrate temperature 100-
400 DEG C, vacuum degree is lower than 5.0 × 10-4Pa, target and substrate distance are 80mm, argon flow 15-30sccm, oxygen flow
For 0.3-2.0sccm, argon oxygen ratio is 7.5:1-39:1, and sputtering operating air pressure is 0.3Pa, sputtering power 150-200W, deposition
Time is 60min.
13. such as method of any of claims 1-12, which is characterized in that carry out the condition of high annealing in step 3
To anneal in vacuum or inert environments to the vanadium oxide precursor thin-film.
14. such as method of any of claims 1-13, which is characterized in that carry out the temperature of high annealing in step 3
Within the scope of 420-480 DEG C.
15. method according to claim 13 or 14, which is characterized in that the environment of the annealing is vacuum degree 0.1-
The argon atmosphere of 0.3Pa.
16. the method as described in any one of claim 1-15, which is characterized in that the step 2 further includes, by polyamides Asia
Amine aqueous solution blade coating or the method for spin coating are uniformly smeared over the substrate, are toasted 3 hours at 25-60 DEG C, then in 300-
It heats 8 hours and anneals at 400 DEG C, obtain uniform Kapton on a silicon substrate, it is flexible to form described first
Material film.
17. the method as described in any one of claim 1-16, which is characterized in that the step 4 further includes, by polyamides Asia
Amine aqueous solution blade coating or the method for spin coating are uniformly applied on the vanadium oxide film, toast 3 hours at 25-60 DEG C, then
It heats 8 hours and anneals at 300-400 DEG C, obtain uniform Kapton, on the vanadium oxide film with shape
At the second flexible material film.
18. the method as described in any one of claim 1-17, which is characterized in that the thickness of the first flexible material film
It is 10-20 μm；The thickness of the vanadium oxide film is less than 100nm；The second flexible material film with a thickness of 10-20 μm.
19. a kind of preparation method of vanadium oxide composite film, including,
Step 1, preparing substrate form silicon nitride layer on a silicon substrate；
The substrate is sequentially placed into deionized water, dehydrated alcohol, is cleaned by ultrasonic respectively 10 minutes in acetone solvent by step 2,
And it dries；
Step 3 prepares substrate, forms the first Kapton over the substrate；
The substrate is sequentially placed into deionized water, dehydrated alcohol, is cleaned by ultrasonic respectively 10 minutes in acetone solvent by step 4,
And it dries；
Step 5, it is 5.0 × 10 that cleaned substrate, which is placed in vacuum degree,-4In the high vacuum rf magnetron sputtering equipment of Pa,
Substrate temperature is 100-400 DEG C, argon flow 15-30sccm, oxygen flow 0.3-2.0sccm, argon oxygen ratio are 7.5:1-
Under conditions of 39:1, sputtering operating air pressure are 0.3Pa, sputtering power 150-200W, target and substrate distance are 80mm, deposition
60min, to form vanadium oxide precursor thin-film on the substrate；The target is vanadium metal target；
Step 6, in 420-480 DEG C of annealing 30min or more, the vanadium oxide film of acquisition is stratiform polycrystalline film；
Step 7 forms the second Kapton on the vanadium oxide film.
20. method as claimed in claim 19, which is characterized in that further include strip step after the step 7；Wherein,
The strip step includes, by the first flexible material film, vanadium oxide film and the second flexible material film from the lining
It is removed on bottom, acquisition is formed with vanadium oxide film in the first flexible material film and the second flexible material film
Laminated film.
21. the method as described in claim 19 or 20, which is characterized in that the step 3 further includes, by polyimide solution
It is uniformly smeared over the substrate, is toasted 3 hours at 25-60 DEG C, then at 300-400 DEG C with the method for blade coating or spin coating
Heating is annealed for 8 hours, obtains uniform Kapton, on a silicon substrate to form the first Kapton.
22. the method as described in claim 19 or 21, which is characterized in that the step 7 further includes, by polyimide solution
It is uniformly applied on the vanadium oxide film, is toasted 3 hours at 25-60 DEG C, then in 300- with the method for blade coating or spin coating
It heats 8 hours and anneals at 400 DEG C, uniform Kapton is obtained on the vanadium oxide film, to form second
Kapton.
23. the method as described in any one of claim 18-22, which is characterized in that the thickness of the first flexible material film
Degree is 10-20 μm；The thickness of the vanadium oxide film is less than 100nm；The second flexible material film with a thickness of 10-20 μ
m。
24. a kind of vanadium oxide composite film, including the first fexible film, vanadium oxide film and the second fexible film；Wherein, institute
Vanadium oxide film is stated to be formed between the first fexible film and the second fexible film；When the temperature of the vanadium oxide composite film is low
When the phase transition temperature of vanadium oxide, the infrared light in incident light can penetrate the vanadium oxide composite film and be transmitted through another
Side；When the temperature of the vanadium oxide composite film is higher than the phase transition temperature of vanadium oxide, the infrared light in incident light can be by institute
State vanadium oxide composite film reflection.
25. vanadium oxide composite film as claimed in claim 24, which is characterized in that first fexible film and described second
Tenderness film is formed by identical transparent material, and the transparent material is the material transparent in visible light wave range and infrared band.
26. vanadium oxide composite film as claimed in claim 25, which is characterized in that first fexible film and described second
Fexible film is formed by polyimide material.
27. the vanadium oxide composite film as described in any one of claim 24-26, which is characterized in that the laminated film pair
The transmissivity of infrared light of the wave-length coverage in 750-1700nm has modulating action.
28. the vanadium oxide composite film as described in any one of claim 24-27, which is characterized in that the described first flexible material
Expect film with a thickness of 10-20 μm；The thickness of the vanadium oxide film is less than 100nm；The thickness of the second flexible material film
Degree is 10-20 μm.
29. the vanadium oxide composite film as described in any one of claim 24-28, which is characterized in that the vanadium oxide is compound
Prepared by film method as described in any one of claim 1-23 forms.
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| WO2020125438A1 (en) * | 2018-12-18 | 2020-06-25 | 深圳先进技术研究院 | Vanadium oxide composite film and preparation method therefor |
| WO2020125440A1 (en) * | 2018-12-18 | 2020-06-25 | 深圳先进技术研究院 | Method for preparing flexible vanadium oxide thin film by means of two-step method |
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