CN110331366A - A kind of preparation method of hypovanadic oxide-based composite film - Google Patents
A kind of preparation method of hypovanadic oxide-based composite film Download PDFInfo
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- CN110331366A CN110331366A CN201910700292.2A CN201910700292A CN110331366A CN 110331366 A CN110331366 A CN 110331366A CN 201910700292 A CN201910700292 A CN 201910700292A CN 110331366 A CN110331366 A CN 110331366A
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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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0688—Cermets, e.g. mixtures of metal and one or more of carbides, nitrides, oxides or borides
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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
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
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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
- C23C14/5846—Reactive treatment
- C23C14/5853—Oxidation
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Abstract
The invention discloses a kind of preparation methods of hypovanadic oxide-based composite film, comprising the following steps: with vanadium metal target and zinc-oxide ceramic target sputtering target material, argon gas is reaction gas, and deposition obtains the vanadium film mixed with zinc oxide on quartz glass；Gained is put into annealing in annealing furnace mixed with the vanadium film of zinc oxide and obtains hypovanadic oxide-based composite film.It does not need to heat chip bench in magnetron sputtering process of the present invention, sputtering process is simple, and the vanadium film by preparation mixed with zinc oxide is separately handled with hypovanadic oxide-based composite film process is prepared, so that preparation process is easier to manipulate, subsequent annealing process is easy to operate, it does not need to be passed through other gases, meets the requirement of large-scale production.There is Zinc vanadate generation on the basis of guaranteeing that vanadium dioxide is a certain amount of simultaneously, this significantly increases the visible light transmittance of film, and sunlight modulation efficiency also slightly improves, and has broad application prospects.
Description
Technical field
The invention belongs to field of material technology, and in particular to a kind of preparation method of hypovanadic oxide-based composite film.
Background technique
With the rapid development of our country's economy, the consumption of the energy is also increasing, and has thus also caused atmosphere pollution etc.
Problem, how energy-saving and emission-reduction become current hot topic.According to statistics, China's building unit area energy consumption is more significantly larger than
The specific energy consumption of developed country, building is mainly reflected in daylighting, heating and refrigeration etc..For these problems, in the market
It is proposed low-E glass, its main feature is that adding plating thin film to reflect infrared light largely on glass, to make interior
Temperature reduces, and achievees the effect that summer energy-saving.But this low-E glass is unable to satisfy China's bidirectional modulation need cold in winter and hot in summer
It asks, and intelligent glass can reach cool in summer and warm in winter according to the variation of Various Seasonal temperature, to indoor carry out photo-thermal regulation
Effect.This intelligent glass is the thin-film material by adding plating to have thermochromic properties on glass, easy to operate,
Advantage of lower cost has broad application prospects in energy-saving glass field.
Vanadium dioxide was widely studied in recent years as a kind of thermochromic material, and this material is in certain temperature
Reversible phase transformation can occur down, vanadium dioxide can be changed into cubic rutile by monoclinic phase in a short time when temperature increases
Phase, before phase change after, huge change occurs for the infrared light transmittance of vanadium dioxide, changed from high transmittance to low transmission, but
Visible light transmittance does not change substantially, and the phase transition temperature of vanadium dioxide is lower with respect to other thermochromic materials, blocky
Its phase transition temperature of vanadium dioxide material be 68 DEG C.In conjunction with these performance characteristics, vanadium dioxide is in intelligent glass using upper tool
There is apparent advantage.
There are many kinds of the methods for preparing vanadium dioxide film, mainly includes magnetron sputtering method, sol-gal process, pulse laser
Sedimentation and ion beam sputtering etc., in the preparation method of these films, magnetron sputtering is fine and close due to the film of its preparation
It is even, reproducible, preparation process is simple, and be adapted to large-scale industrial production, and be widely studied.
Currently, using the vanadium dioxide film of magnetron sputtering method preparation in the premise for meeting certain sunlight modulation efficiency
Under, visible light transmittance is all universal relatively low, and phase transition temperature is also higher, greatly differs from each other with its application requirement.
Summary of the invention
It is an object of that present invention to provide a kind of sunlight modulation efficiency is preferable, and the two of visible light transmittance with higher
The preparation method of vanadium oxide based coextruded film.
In order to achieve the above objectives, as follows using technical solution:
A kind of preparation method of hypovanadic oxide-based composite film, comprising the following steps:
1) with vanadium metal target and zinc-oxide ceramic target sputtering target material, argon gas is reaction gas, is deposited on quartz glass
To the vanadium film mixed with zinc oxide；
2) gained is put into annealing in annealing furnace mixed with the vanadium film of zinc oxide and obtains hypovanadic oxide-based composite film.
According to the above scheme, vanadium metal target purity used in step 1 is 99.99wt%, zinc-oxide ceramic target purity used
For 99.99wt%.
According to the above scheme, the purity of argon gas used in step 1 is 99.9wt%.
According to the above scheme, step 1 control back end vacuum is 1 × 10-3-3×10-3Pa, the power of sputtering are 65-85W, gold
The time for belonging to the sputtering of vanadium target is 15-18min, and the sputtering time of zinc-oxide ceramic target is 2-6min.
According to the above scheme, the temperature that step 1 deposits is room temperature, and the operating air pressure of deposition is 0.1-1.0Pa.
According to the above scheme, step 2 annealing process is divided into heating, heat preservation and cooling three phases；Annealing furnace is taken out when annealing
For vacuum to 1000-1500Pa, the temperature of annealing is set as 400-500 DEG C, and the heating rate of annealing is 5-10 DEG C/min, when heat preservation
Between be 30-90min, after heat preservation, furnace chamber slowly cools to room temperature under the action of cooling water.
Hypovanadic oxide-based composite film preparation method provided by the invention, at a certain temperature can be with oxygen using vanadium metal
Change zinc reaction and generates Zinc vanadate, and Zinc vanadate is that a kind of stability is good, it is seen that the high substance of light transmission rate.Preparing vanadium dioxide
The higher hypovanadic oxide-based composite film of visible light transmittance can be generated by the zinc oxide of incorporation part during film,
And the sunlight modulation efficiency of this film is also higher, meets certain use demand.
There is no particular limitation for requirement of the present invention for substrate, since vanadium dioxide thermochromic thin film is generally used for glass
On glass, the preferred glass of the present invention is as substrate, and since attachment of the quartz glass to film is preferable, and in subsequent annealing process
It will not make to introduce other impurity in film, therefore use quartz glass as substrate in the present invention.
The invention has the benefit that
(1) it does not need to heat chip bench in magnetron sputtering process of the present invention, sputtering process is simple, and will system
The standby vanadium film mixed with zinc oxide is separately handled with hypovanadic oxide-based composite film process is prepared, so that preparation process is easier to manipulate,
Subsequent annealing process is easy to operate, does not need to be passed through other gases, meets the requirement of large-scale production.
(2) there is vanadic acid on the basis of guaranteeing that vanadium dioxide is a certain amount of in hypovanadic oxide-based composite film prepared by the present invention
Zinc generates, this significantly increases the visible light transmittance of film, and sunlight modulation efficiency also slightly improves, and has wide
Application prospect.
Detailed description of the invention
Fig. 1: the XRD diffraction pattern of hypovanadic oxide-based composite film prepared by embodiment 1.
Fig. 2: hypovanadic oxide-based composite film room temperature and high temperature transmitted light spectrogram prepared by embodiment 1.
Fig. 3: the XRD diffraction pattern of hypovanadic oxide-based composite film prepared by embodiment 2.
Fig. 4: hypovanadic oxide-based composite film room temperature and high temperature transmitted light spectrogram prepared by embodiment 2.
Specific embodiment
Following embodiment further illustrates technical solution of the present invention, but not as limiting the scope of the invention.
It is as follows that the present invention uses double target magnetic control sputterings to prepare hypovanadic oxide-based composite film process:
(1) cleaning of quartz glass substrate
Quartz glass is first cleaned with detergent, then is successively cleaned by ultrasonic with distilled water and dehydrated alcohol, is finally put
Enter sealed in dehydrated alcohol it is spare.
(2) the vanadium film preparation of zinc oxide is mixed
By cleaned quartz glass substrate as in magnetron sputtering vacuum chamber, using quality purity 99.99% vanadium and
Zinc oxide is as target, and using the argon gas that quality purity is 99.9% as working gas, background vacuum is 1 × 10-3-3×10-3Pa, substrate is room temperature in sputtering process, and the flux of argon gas is 100-200sccm, and sputtering operating air pressure is 0.1-1.0Pa,
Vanadium target is identical with the sputtering power of zinc oxide target, and the sputtering time of vanadium target is 15-18min and uninterrupted, oxidation in sputtering process
Zinc target is using interruption sputtering.
(3) preparation of hypovanadic oxide-based composite film
It is made annealing treatment being put into annealing furnace mixed with the vanadium film of zinc oxide, temperature change rule is divided into liter in annealing furnace
Temperature, heat preservation and cooling three phases.Annealing furnace is evacuated to 1000-1500Pa when annealing, the temperature of annealing is set as 400-
500 DEG C, the heating rate of annealing is 5-10 DEG C/min, and the soaking time of annealing is 30-90min, and after heat preservation, furnace chamber is cold
But room temperature is slowly cooled under the action of water.
Step 1 distilled water is identical with the dehydrated alcohol ultrasonic cleaning time.
To keep the film of sputtering more uniform in step 2, glass substrate platform slowly rotates in sputtering process；Vanadium target uses
Magnetically controlled DC sputtering, zinc oxide target use rf magnetron sputtering.
Embodiment 1
Hypovanadic oxide-based composite film is prepared in quartz glass substrate on piece, the specific steps are as follows:
(1) glass substrate is cleaned, process is as follows: first being cleaned with detergent to glass surface, distilled water is then added
It is cleaned by ultrasonic 20min, is finally putting into dehydrated alcohol and is cleaned by ultrasonic 20min, then cleaned sheet glass is put into dehydrated alcohol
Middle sealing is spare.
(2) the vanadium film mixed with zinc oxide is prepared on above-mentioned substrate using direct current and rf magnetron sputtering, by quartzy glass
The drying of glass substrate, is fixed on chip bench with adhesive tape resistant to high temperature, is put into magnetron sputtering operating room, it is (pure to be put into vanadium metal target
99.99%) then degree is evacuated to 3.0 with molecular pump essence first with mechanical pumping low vacuum with zinc oxide (purity 99.99%) target
×10-3Pa is passed through reaction gas argon gas (purity 99.9%), until intracavitary stable gas pressure in 0.5Pa, keeps stablizing.Vanadium metal
Target uses magnetically controlled DC sputtering, and zinc oxide target uses rf magnetron sputtering.Set the sputtering power of direct current and rf magnetron sputtering
It is 65W.The sputtering time of vanadium target is 16min and uninterrupted, zinc oxide target interruption sputtering 2min in sputtering process, and is existed respectively
Vanadium target starts simultaneously to sputter when sputtering 1.75min, 5.75min, 9.75min, 13.75min, stops after sputtering 0.5min every time
Only sputter.
(3) the vanadium film for mixing zinc oxide for obtaining sputtering closes fire door, annealing furnace is evacuated to as in annealing furnace
1000Pa, the temperature of annealing are set as 450 DEG C, and the heating rate of annealing is 10 DEG C/min, and the soaking time of annealing is 50min,
After heat preservation, furnace chamber takes out sample in furnace when slowly cooling to 70 DEG C or less under the action of cooling water.
(4) know that the ingredient of the film is mainly the compound of vanadium dioxide and Zinc vanadate by XRD spectrum in Fig. 1.It is right
Sample carries out high/low temperature transmission measurement, it can be seen that and the infrared light transmittance of hypovanadic oxide-based composite film is higher when room temperature,
When temperature rises to higher than thin film phase change temperature, the infrared light transmittance of hypovanadic oxide-based composite film is reduced.Wherein, this two
The visible light transmittance of vanadium oxide based coextruded film is 38.9%, and sunlight modulation efficiency is 11.8%, high/low temperature transmitance figure
Spectrum is as shown in Figure 2.
Embodiment 2
Hypovanadic oxide-based composite film is prepared in quartz glass substrate on piece, the specific steps are as follows:
(1) glass substrate is cleaned, process is as follows: first being cleaned with detergent to glass surface, distilled water is then added
It is cleaned by ultrasonic 20min, is finally putting into dehydrated alcohol and is cleaned by ultrasonic 20min, then cleaned sheet glass is put into dehydrated alcohol
Middle sealing is spare.
(2) the vanadium film mixed with zinc oxide is prepared on above-mentioned substrate using direct current and rf magnetron sputtering, by quartzy glass
The drying of glass substrate, is fixed on chip bench with adhesive tape resistant to high temperature, is put into magnetron sputtering operating room, it is (pure to be put into vanadium metal target
99.99%) then degree is evacuated to 1.0 with molecular pump essence first with mechanical pumping low vacuum with zinc oxide (purity 99.99%) target
×10-3Pa is passed through reaction gas argon gas (purity 99.9%), until intracavitary stable gas pressure in 0.1Pa, keeps stablizing.Vanadium metal
Target uses magnetically controlled DC sputtering, and zinc oxide target uses rf magnetron sputtering.Set the sputtering power of direct current and rf magnetron sputtering
It is 75W.The sputtering time of vanadium target is 16min and uninterrupted, zinc oxide target interruption sputtering 4min in sputtering process, and is existed respectively
Vanadium target starts simultaneously to sputter when sputtering 1.5min, 5.5min, 9.5min, 13.5min, stops splashing after sputtering 1min every time
It penetrates.
(3) the vanadium film for mixing zinc oxide for obtaining sputtering closes fire door, annealing furnace is evacuated to as in annealing furnace
1500Pa, the temperature of annealing are set as 400 DEG C, and the heating rate of annealing is 10 DEG C/min, and the soaking time of annealing is 70min,
After heat preservation, furnace chamber takes out sample in furnace when slowly cooling to 70 DEG C or less under the action of cooling water.
(4) know that the ingredient of the film is mainly the compound of vanadium dioxide and Zinc vanadate by XRD spectrum in Fig. 3.It is right
Sample carries out high/low temperature transmission measurement, it can be seen that and the infrared light transmittance of hypovanadic oxide-based composite film is higher when room temperature,
When temperature rises to higher than thin film phase change temperature, the infrared light transmittance of hypovanadic oxide-based composite film is reduced.Wherein, this two
The visible light transmittance of vanadium oxide based coextruded film is 48.7%, and sunlight modulation efficiency is 12.2%, high/low temperature transmitance figure
Spectrum is as shown in Figure 4.
Claims (6)
1. a kind of preparation method of hypovanadic oxide-based composite film, it is characterised in that the following steps are included:
1) with vanadium metal target and zinc-oxide ceramic target sputtering target material, argon gas is reaction gas, deposits and is mixed on quartz glass
There is the vanadium film of zinc oxide；
2) gained is put into annealing in annealing furnace mixed with the vanadium film of zinc oxide and obtains hypovanadic oxide-based composite film.
2. the preparation method of hypovanadic oxide-based composite film as described in claim 1, it is characterised in that vanadium metal used in step 1
Target purity is 99.99wt%, and zinc-oxide ceramic target purity used is 99.99wt%.
3. the preparation method of hypovanadic oxide-based composite film as described in claim 1, it is characterised in that argon gas used in step 1
Purity is 99.9wt%.
4. the preparation method of hypovanadic oxide-based composite film as described in claim 1, it is characterised in that step 1 controls back end vacuum
It is 1 × 10-3-3×10-3Pa, the power of sputtering are 65-85W, and the time of vanadium metal target sputtering is 15-18min, zinc oxide ceramics
The sputtering time of target is 2-6min.
5. the preparation method of hypovanadic oxide-based composite film as described in claim 1, it is characterised in that step 1 deposit temperature be
Room temperature, the operating air pressure of deposition are 0.1-1.0Pa.
6. the preparation method of hypovanadic oxide-based composite film as described in claim 1, it is characterised in that step 2 annealing process is divided into
Heating, heat preservation and cooling three phases；Annealing furnace is evacuated to 1000-1500Pa when annealing, the temperature of annealing is set as
400-500 DEG C, the heating rate of annealing is 5-10 DEG C/min, and soaking time 30-90min, after heat preservation, furnace chamber is in cooling
Room temperature is slowly cooled under the action of water.
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Cited By (3)
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| CN110791740A (en) * | 2019-12-02 | 2020-02-14 | 武汉理工大学 | Preparation method of high-performance ZIF-L/vanadium dioxide composite film |
| CN111334771A (en) * | 2020-04-24 | 2020-06-26 | 中国科学院兰州化学物理研究所 | Electrochromic film and preparation method and application thereof |
| CN112981347A (en) * | 2021-02-10 | 2021-06-18 | 武汉理工大学 | Preparation method of acid-treated vanadium dioxide film |
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| CN112981347B (en) * | 2021-02-10 | 2022-08-05 | 武汉理工大学 | Preparation method of acid-treated vanadium dioxide film |
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