CN102634758A - High-transmittivity vanadium-based multi-layer superlattice film and preparation method thereof - Google Patents
High-transmittivity vanadium-based multi-layer superlattice film and preparation method thereof Download PDFInfo
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- CN102634758A CN102634758A CN201210127760XA CN201210127760A CN102634758A CN 102634758 A CN102634758 A CN 102634758A CN 201210127760X A CN201210127760X A CN 201210127760XA CN 201210127760 A CN201210127760 A CN 201210127760A CN 102634758 A CN102634758 A CN 102634758A
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Abstract
The invention relates to a high-transmittivity vanadium-based multi-layer superlattice film and a preparation method of the high-transmittivity vanadium-based multi-layer superlattice film, belonging to the field of thin-film materials. The superlattice film is prepared by alternately depositing a VO2 film and a metal oxide film on a substrate. Compared with the prior art, the superlattice film and the preparation method have notable advantages that (1) the operation is simple, the process time is short and is easy to control, and the superlattice film is suitable for industrial production; (2) the thickness of the growing film can be accurately controlled; (3) the surface of the growing film is smooth, and the distribution is uniform; and (4) the transmittivity of the growing film is high, and the superlattice film is preferably applied to the fields such as intelligent windows, light storage, and photoelectricity consecration.
Description
Technical field
The invention belongs to the thin-film material field, be specifically related to high-transmission rate vanadium Quito layer superlattice film and preparation method thereof.
Background technology
VO
2It is a kind of thermochromic material.Along with the rising of temperature, vanadium dioxide is transformed into the hot metal phase mutually by cryogenic semiconductor, and crystalline structure is changed to the high temperature rutile structure by the low temperature monocline.Be accompanied by phase transformation, reversible mutation all can take place in many photoelectric characteristics such as its resistivity, specific refractory power, transsmissivity, and these superior performances make film in fields such as smart window, light storage, photoswitcs high using value arranged all.
In order to improve the optical characteristics of vanadium dioxide, some other elements that can mix also can more compound compounds, improve its chemicalstability, cover on the sensitive material, and it is high to play the effect of protective film, particularly visible light and near-infrared region transmitance.
Introduce vanadium dioxide film 70 surplus in piece Chinese patent, there have minority to introduce vanadium dioxide film to be adulterated, perhaps vanadium dioxide laminated film research.For example Chinese CN102241482A is equipped with vanadium dioxide film through the wet chemical solution legal system, again through prepare laminated film VO at colloidal sol-gel technique
2/ SiO
2, VO
2/ ZnO, VO
2/ ZrO
2Perhaps VO
2/ TiO
2For another example, Chinese patent CN101786798A introduces the preparation and the application thereof of vanadium-based multiple coating liquid and laminated film, realizes through the spin-coating method plated film.For aforesaid method, although equipment cost is low, these method process times are long, wayward; Grow to such an extent that film thickness is restive; Film crystal grain skewness, the surface is smooth inadequately.These shortcomings all have very big influence to performance, in large-scale commercial prodn, more will pay attention to the performance requriements of material.
Summary of the invention
The purpose of this invention is to provide a kind of process time short, be suitable for suitability for industrialized production, and product has that controllable thickness, crystal grain are evenly distributed, vanadium Quito layer superlattice film of high-transmission rate and preparation method thereof.
The technical scheme that realizes the object of the invention is: a kind of vanadium Quito layer superlattice film of high-transmission rate, described multilayer superlattice film are on substrate, alternately to deposit VO
2Film and metal oxide film, described MOX are one or more in Ti, W, Zn, Gr, Mo or the Cu oxide compound.
Above-mentioned superlattice film adopts pulsed laser deposition, laser molecular beam epitaxy method or magnetron sputtering method preparation.
Wherein, Pulsed laser deposition or laser molecular beam epitaxy method have identical preparation process; Concrete technology may further comprise the steps: substrate and target are installed as in the growth chamber; Utilize mechanical pump and molecular pump to be evacuated subsequently, it is 300 ℃ to 700 ℃ that the preceding underlayer temperature of deposition rises to, and oxygen partial pressure is adjusted to 10
-5Pa to 10
2Pa, regulating energy of lasers subsequently is 100 ~ 300mJ, frequency is at 5 ~ 10Hz; Being target as sputter 3-5 minute with the vanadium earlier, is target as sputter 3-5 minute with among mix other metal Ti, W, Zn, Gr, Mo or the Cu one or more again, alternating deposit Between 300 ℃ to 700 ℃, anneal after deposition finishes and obtained the multilayer superlattice film in 30-60 minute.
Among the preparation method of vanadium of the present invention Quito layer superlattice film, preparatory sputter is 3 ~ 5 minutes before the deposition superlattice film.
Prepare with magnetron sputtering method: put into substrate, regulate flow, the control substrate temperature is 300 ℃ to 700 ℃, air pressure: 0.001 ~ 50Pa, O
2Under the atmosphere, sputtering power is 100W-1500W, is target as sputter 3-5 minute with the vanadium earlier, is target as sputter 3-5 minute with among mix other metal Ti, W, Zn, Gr, Mo or the Cu one or more again, alternating deposit Between 300 ℃ to 700 ℃, anneal after deposition finishes and obtained the multilayer superlattice film in 30-60 minute.
Among the preparation method of vanadium of the present invention Quito layer superlattice film, substrate is SiO
2Perhaps Al
2O
3
Through the resulting vanadium of above-mentioned film growth mode Quito layer superlattice film thickness in 1 ~ 800 nanometer.
The present invention compared with prior art, its remarkable advantage is: (1) is simple to operate, the process time is short, is convenient to control, is suitable for suitability for industrialized production; (2) film thickness of growth can accurately be controlled; (3) film surface of growth is smooth, is evenly distributed; (4) the film transsmissivity of growth is high, can better be applied to fields such as smart window, light storage, photoswitc.
Description of drawings
Fig. 1 is the VO of the embodiment of the invention 1
2Film alternating temperature Raman spectrogram.
Fig. 2 is the VO of the embodiment of the invention 1
2The transmitted light spectrogram of film and vanadium Quito layer superlattice film.
Fig. 3 is the surface and the cross-section morphology figure of vanadium Quito layer superlattice film of the embodiment of the invention 1.
Fig. 4 is the interface element distribution plan of vanadium Quito layer superlattice film of the embodiment of the invention 1.
Embodiment
Below in conjunction with accompanying drawing the present invention is further described.
The film of gained of the present invention is described constitutional features such as Fig. 1 of film through Raman spectrometer; Surface and cross-section morphology such as Fig. 3 through field emission scanning electron microscope (SEM) viewing film; Observing interface element through energy dispersion X-ray spectrum (EDS) distributes like Fig. 4.Transsmissivity such as Fig. 2 through the spectrophotometer testing film.
Embodiment 1: at SiO
2Growth vanadium Quito layer superlattice film on the substrate.
(1) adopt the pulsed laser deposition growing film, concrete growth conditions is: with SiO
2Substrate and vanadium, titanium target are installed as in the growth chamber, utilize mechanical pump and molecular pump to be evacuated subsequently, and it is 300 ℃ that the preceding underlayer temperature of deposition rises to, and oxygen partial pressure is adjusted to 10
-5Pa, regulating energy of lasers subsequently is 100mJ, frequency is at 5Hz; Being target as sputter 3 minutes with the vanadium earlier, is target as sputter 3 minutes with doping metals Ti again, alternating deposit ...Between 300 ℃, anneal after deposition finishes and obtained the multilayer superlattice film in 30 minutes.
Comparative Examples: adopt the pure VO of pulsed laser deposition growth
2Film, concrete growth conditions is: with SiO
2Substrate and vanadium target are installed as in the growth chamber, utilize mechanical pump and molecular pump to be evacuated subsequently, and it is 300 ℃ that the preceding underlayer temperature of deposition rises to, and oxygen partial pressure is adjusted to 10
-5Pa, regulating energy of lasers subsequently is 100, frequency is 5; Deposit the before preparatory sputter of superlattice film 3 minutes, between 300 ℃, annealed 30 minutes after deposition finishes.
(1) adopt Raman spectrometer to prepare VO
2The constitutional features of film is analyzed, and obtains the alternating temperature Raman spectrogram like accompanying drawing 1.
(2) observe vanadium Quito layer superlattice film interface element through energy dispersion X-ray spectrum (EDS) and distribute shown in accompanying drawing 4, surface and the cross-section morphology of observing vanadium Quito layer superlattice film through field emission scanning electron microscope (SEM) are shown in accompanying drawing 3.Growing vanadium Quito layer superlattice film thickness is 400nm.
(3) VO
2Film and vanadium Quito layer superlattice film insulation mutually with the optical transmission rate curve of metallographic phase shown in accompanying drawing 2.The light wavelength scope is the visible wavelength of 400-850nm.VO
2Film is compared with vanadium Quito layer superlattice film, and is better to the optical transmission performance at the insulation phase time, lower in the transsmissivity in metallographic phase time, under the 750nm wavelength, the insulation of vanadium Quito layer superlattice film mutually and metallographic phase transsmissivity difference compare VO
2Film improves three times.
Embodiment 2: at Al
2O
3Growth vanadium Quito layer superlattice film on the substrate.
Adopt the pulsed laser deposition growing film, concrete growth conditions is: with Al
2O
3Substrate and vanadium, tungsten target material are installed as in the growth chamber, utilize mechanical pump and molecular pump to be evacuated subsequently, and it is 500 ℃ that the preceding underlayer temperature of deposition rises to, and oxygen partial pressure is adjusted to 10
-3Pa, regulating energy of lasers subsequently is 200mJ, frequency is at 7Hz; Being target as sputter 4 minutes with the vanadium earlier, is target as sputter 4 minutes with doping metals Ti again, alternating deposit ...After finishing, deposition between 500 ℃, annealed 50 minutes.Growing vanadium Quito layer superlattice film thickness is 500nm.All the other tests are with embodiment 1.
Embodiment 3: at SiO
2Growth vanadium Quito layer superlattice film on the substrate.
Adopt the pulsed laser deposition growing film, concrete growth conditions is: with SiO
2Substrate and vanadium, titanium, tungsten target material are installed as in the growth chamber, utilize mechanical pump and molecular pump to be evacuated subsequently, and it is 700 ℃ that the preceding underlayer temperature of deposition rises to, and oxygen partial pressure is adjusted to 10
-2Pa, regulating energy of lasers subsequently is 300mJ, frequency is at 10Hz; Being target as sputter 5 minutes with the vanadium earlier, is target as sputter 5 minutes with doping metals Ti again, is target as sputter 5 minutes with doping metals W again, alternating deposit ...After finishing, deposition between 700 ℃, annealed 60 minutes.Growing vanadium Quito layer superlattice film thickness is 800nm.All the other tests are with embodiment 1.
Embodiment 4: at SiO
2Growth vanadium Quito layer superlattice film on the substrate.
Adopt laser molecular beam epitaxy method growing film, concrete growth conditions is: with SiO
2Substrate and vanadium, titanium, copper target are installed as in the growth chamber, utilize mechanical pump and molecular pump to be evacuated subsequently, and it is 700 ℃ that the preceding underlayer temperature of deposition rises to, and oxygen partial pressure is adjusted to 10
-2Pa, regulating energy of lasers subsequently is 300mJ, frequency is at 10Hz; Being target as sputter 3 minutes with the vanadium earlier, is target as sputter 3 minutes with doping metals Ti again, is target as sputter 3 minutes with doping metals Cu again, alternating deposit ...After finishing, deposition between 700 ℃, annealed 60 minutes.Growing vanadium Quito layer superlattice film thickness is 600nm.All the other tests are with embodiment 1.
Embodiment 5: at Al
2O
3Growth vanadium Quito layer superlattice film on the substrate.
Adopt the magnetron sputtering method growing film, put into Al
2O
3Substrate is regulated flow, and the control substrate temperature is 300 ℃, air pressure: 2Pa, O
2Under the atmosphere, sputtering power is 500W, is target as sputter 3 minutes with the vanadium earlier, is target as sputter 3 minutes with doping metals W again, is target as sputter 3 minutes with doping metals Cu again, alternating deposit Deposition finishes the back 300 ℃ of annealing 30 minutes.Growing vanadium Quito layer superlattice film thickness is 600nm.All the other tests are with embodiment 1.
Embodiment 6: at Al
2O
3Growth vanadium Quito layer superlattice film on the substrate.
Adopt the magnetron sputtering method growing film, put into substrate, regulate flow, the control substrate temperature is 500 ℃, air pressure: 10Pa, O
2Under the atmosphere, sputtering power is 1000W, is target as sputter 4 minutes with the vanadium earlier, is target as sputter 4 minutes with doping metals Mo again, is target as sputter 4 minutes with doping metals Zn again, alternating deposit After finishing, deposition between 500 ℃, annealed 40 minutes.Growing vanadium Quito layer superlattice film thickness is 700nm.All the other tests are with embodiment 1.
Embodiment 7: at SiO
2Growth vanadium Quito layer superlattice film on the substrate.
Adopt the magnetron sputtering method growing film, put into substrate, regulate flow, the control substrate temperature is 700 ℃, air pressure: 20Pa, O
2Under the atmosphere, sputtering power is 1500W, is target as sputter 5 minutes with the vanadium earlier, is target as sputter 5 minutes with doping metals Mo again, is target as sputter 5 minutes with doping metals Gr again, alternating deposit After finishing, deposition between 700 ℃, annealed 60 minutes.Growing vanadium Quito layer superlattice film thickness is 800nm.All the other tests are with embodiment 1.
Claims (9)
1. vanadium Quito layer superlattice film of a high-transmission rate is characterized in that described multilayer superlattice film is on substrate, alternately to deposit VO
2Film and metal oxide film, described MOX are one or more in Ti, W, Zn, Gr, Mo or the Cu oxide compound.
2. vanadium Quito layer superlattice film of high-transmission rate according to claim 1 is characterized in that described substrate is SiO
2Perhaps Al
2O
3
3. vanadium Quito layer superlattice film of high-transmission rate according to claim 1 is characterized in that described multilayer superlattice film adopts pulsed laser deposition, laser molecular beam epitaxy method or magnetron sputtering method preparation.
4. the preparation method of vanadium Quito layer superlattice film of a high-transmission rate is characterized in that described preparation method is for alternately depositing VO on substrate
2Film and metal oxide film, described MOX are one or more in Ti, W, Zn, Gr, Mo or the Cu oxide compound.
5. the preparation method of vanadium Quito layer superlattice film of high-transmission rate according to claim 4 is characterized in that described substrate is SiO
2Perhaps Al
2O
3
6. the preparation method of vanadium Quito layer superlattice film of high-transmission rate according to claim 4 is characterized in that described preparation method comprises pulsed laser deposition, laser molecular beam epitaxy method or magnetron sputtering method.
7. according to the preparation method of vanadium Quito layer superlattice film of claim 4 or 6 described high-transmission rates; It is characterized in that the concrete technology that described pulsed laser deposition and laser molecular beam epitaxy legal system are equipped with the multilayer superlattice film is: substrate and target are installed as in the growth chamber; Utilize mechanical pump and molecular pump to be evacuated subsequently; It is 300 ℃ to 700 ℃ that the preceding underlayer temperature of deposition rises to, and oxygen partial pressure is adjusted to 10
-5Pa to 10
2Pa, regulating energy of lasers subsequently is 100 ~ 300mJ, frequency is at 5 ~ 10Hz; Being target as sputter 3-5 minute with the vanadium earlier, is target as sputter 3-5 minute with among mix other metal Ti, W, Zn, Gr, Mo or the Cu one or more again, alternating deposit Between 300 ℃ to 700 ℃, anneal after deposition finishes and obtained the multilayer superlattice film in 30-60 minute.
8. the preparation method of vanadium Quito layer superlattice film of high-transmission rate according to claim 7 is characterized in that the before preparatory sputter of deposition superlattice film 3 ~ 5 minutes.
9. according to the preparation method of vanadium Quito layer superlattice film of claim 4 or 6 described high-transmission rates; It is characterized in that the concrete technology that described magnetron sputtering method prepares the multilayer superlattice film is: put into substrate; Regulate flow; The control substrate temperature is 300 ℃ to 700 ℃, air pressure: 0.001 ~ 50Pa, O
2Under the atmosphere, sputtering power is 100W-1500W, is target as sputter 3-5 minute with the vanadium earlier, is target as sputter 3-5 minute with among mix other metal Ti, W, Zn, Gr, Mo or the Cu one or more again, alternating deposit After finishing, deposition between 300 ℃ to 700 ℃, annealed 30-60 minute.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105887016A (en) * | 2016-05-24 | 2016-08-24 | 中国科学技术大学 | Preparation method, product and application of flexible vanadium dioxide film |
| CN107210010A (en) * | 2015-01-26 | 2017-09-26 | 旭硝子株式会社 | Building glass plate and building glass structure with display device |
| CN110284125A (en) * | 2019-07-02 | 2019-09-27 | 电子科技大学 | A kind of adjustable vanadium dioxide laminated film of transmissivity and preparation method thereof |
| WO2021114136A1 (en) * | 2019-12-11 | 2021-06-17 | 深圳大学 | Method for preparing vanadium dioxide thin film |
| CN114394766A (en) * | 2022-01-24 | 2022-04-26 | 河南理工大学 | Novel VO2Preparation method and application of thermochromism-based composite film |
| CN114394765A (en) * | 2022-01-24 | 2022-04-26 | 河南理工大学 | VO2Thermochromic composite film and application thereof |
| CN115988956A (en) * | 2023-01-31 | 2023-04-18 | 北京大学 | Superlattice Mott phase change device with adjustable phase change temperature |
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| CN108807346B (en) * | 2018-06-28 | 2020-04-28 | 中国科学院微电子研究所 | Detector, thermistor, vanadium oxide film and manufacturing method thereof |
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| CN107210010A (en) * | 2015-01-26 | 2017-09-26 | 旭硝子株式会社 | Building glass plate and building glass structure with display device |
| CN105887016A (en) * | 2016-05-24 | 2016-08-24 | 中国科学技术大学 | Preparation method, product and application of flexible vanadium dioxide film |
| CN105887016B (en) * | 2016-05-24 | 2018-04-10 | 中国科学技术大学 | A kind of preparation method, product and the application of flexible vanadium dioxide film |
| CN110284125A (en) * | 2019-07-02 | 2019-09-27 | 电子科技大学 | A kind of adjustable vanadium dioxide laminated film of transmissivity and preparation method thereof |
| WO2021114136A1 (en) * | 2019-12-11 | 2021-06-17 | 深圳大学 | Method for preparing vanadium dioxide thin film |
| CN114394766A (en) * | 2022-01-24 | 2022-04-26 | 河南理工大学 | Novel VO2Preparation method and application of thermochromism-based composite film |
| CN114394765A (en) * | 2022-01-24 | 2022-04-26 | 河南理工大学 | VO2Thermochromic composite film and application thereof |
| CN114394766B (en) * | 2022-01-24 | 2023-09-26 | 河南理工大学 | Novel VO 2 Preparation method and application of base thermochromic composite film |
| CN114394765B (en) * | 2022-01-24 | 2023-09-26 | 河南理工大学 | VO 2 Base thermochromic composite film and application thereof |
| CN115988956A (en) * | 2023-01-31 | 2023-04-18 | 北京大学 | Superlattice Mott phase change device with adjustable phase change temperature |
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