CN104099563A - Method for preparing vanadium dioxide film by using magnetron sputtering process - Google Patents
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Abstract
A method for preparing a vanadium dioxide film by using a magnetron sputtering process comprises: taking metal vanadium as a target material, taking argon as a sputtering gas, and taking oxygen as a reaction gas, performing sputtering so as to form the vanadium dioxide film on a substrate, and specifically controlling the deposition temperature to be 300-500 DEG C, the deposition total pressure to be 0.5-2.0 Pa and the oxygen partial pressure to be 1-5%. The method helps to overcome the disadvantage that a conventional preparation technology for a vanadium oxide film is complex, and also the prepared vanadium oxide film is a vanadium dioxide film with adjustable phase-transition temperature.
Description
Technical field
The present invention relates to the preparation method of the adjustable vanadium dioxide pure phase film of a kind of transformation temperature, the mode by non-doping that specifically refers to adopts magnetron sputtering method to realize the adjustable vanadium dioxide pure phase membrane structure of a kind of transformation temperature, belongs to novel inorganic energy-saving material field.
Background technology
China's construction unit area energy consumption is 3 to 4 times of developed country.Building energy consumption accounts for the nearly 1/3 of energy overall consumption, not only causes the huge waste of the energy, is also the emphasis rich and influential family of greenhouse gas emission.Thermosteresis major part for building and heating refrigeration air-conditioner concentrates on the opening parts such as window and body of wall, the buildings outer walls such as roof.To the outer wall of buildings particularly window partly carry out the intelligent photo-thermal comprehensive regulation of low-carbon (LC), develop energy-efficient comfortable New Generation of Intelligent Energy Saving Windows, meet national strategy demand, there is important scientific value and application prospect, will make huge contribution to China's energy-saving and emission-reduction.The Energy Saving Windows of domestic and international market is mainly Low-E glass at present, and feature is to utilize coating structure to control to realize static photo-thermal adjusting.But this adjusting is not with seasonal variation or artificially need and change, cannot meet the demand of China's regional two-ways regulation cold in winter and hot in summer.Intelligent type energy saving glass can according to season environment or occupant need to carry out at any time photo-thermal regulation and control, reach energy-conservation comfortable object cool in summer and warm in winter.In various types of intelligent type energy saving glass, utilize the thermochromism energy-saving glass of material phase transformation characteristic research and development, simple in structure have outstanding advantages such as automatic photo-thermal two-ways regulation, is described as energy-conservation comfortable " window of dream " of future generation.
This thermochromic material is with vanadium dioxide (VO
2) material is representative, mainly utilizes its reversible transformation characteristic: in temperature, be elevated to after transformation temperature VO
2at the utmost point, in the short period of time, by monoclinic phase, change Tetragonal into.Follow phase transformation, VO
2infrared transmission is changed to low transmission by high transmission, but visible light permeability keeps substantially constant simultaneously, thereby can not cause obvious visually-clear to change.Meanwhile, VO
2base thermochromism glass is also that current structure is the simplest, the cheapest intelligent power saving glass of cost form, and transformation temperature can regulate by suitable technique and Composition Control, and application prospect is rather wide.
VO
2transformation temperature at 341K(68 ℃) during left and right, high transformation temperature has hindered VO greatly
2application, but up to the present, people also do not find a kind of practical way to produce the VO of the saturating contrast gradient of high light, low transformation temperature
2film meets the needs of commercial applications.For the effort that reduces transformation temperature, mainly concentrate on two aspects: one is the way of taking doping.Doping method is a kind ofly can effectively reduce VO
2the method of transformation temperature.In fact the process of doping is exactly a progressive failure VO
2the process of semi-conductor state stability.Its principle is to VO by dopant ion
2the replacement of middle oxonium ion or vanadium ion destroys V
+ 4-V
+ 4homopolarity combination.Along with V
+ 4-V
+ 4the minimizing of homopolarity combination, VO
2semiconductor phase-change obtain unstable, thereby also just make VO
2the transition temperature of metallic state-semi-conductor state is reduced.Obviously, dopant ion is to VO
2the replacement of intermediate ion can cause VO simultaneously
2the variation of crystalline network.The direct result of this variation is film the reducing in phase transformation front and back optics, electrology characteristic rangeability causing after doping.Therefore, in the process of doping, for concrete needs, also must select suitable impurity, to guarantee both can effectively to reduce transformation temperature, not make again VO
2phase transformation transition amplitude too little, this has just increased numerous and diverse degree of work greatly.Another is exactly in plain situation, to explore different thin film preparation processes.Research shows, the VO of extension
2transformation temperature is only 318K(45 ℃), be far smaller than the VO conventionally seeing
2transformation temperature (341K), and heat lag phenomenon also can become not obvious, this makes it become a kind of method that can relatively effectively reduce transformation temperature in non-doping situation.It is higher that yet epitaxial method requires substrate, generally will or have the Grown of certain specific orientation to obtain at monocrystalline, thereby limit VO
2the large-scale application of film.2002, Li etc. were by research nanometer VO
2the particle size of film, finds that grain size is about the VO of 8nm
2polycrystal film, the minimum 318K left and right of being down to of transformation temperature, this shows, VO
2the transformation temperature of film is also subject to the impact of crystal microscopic structure and stressed condition.Nearest research is found, at preparation VO
2in the process of film, the trace of oxygen partial pressure regulates can significantly change VO
2the transformation temperature of film, maximal regulated amplitude can reach 25 ℃, and can keep good phase transition performance.In addition, the change of depositing temperature (underlayer temperature), has also caused the variation of transformation temperature.Therefore study the rule that affects of the parameter trace regulation and control such as preparation temperature, oxygen partial pressure on film microstructure, for deep understanding VO
2the phase-change mechanism of film, finally obtains the high quality VO of non-impurity-doped low transformation temperature
2film, has important scientific meaning, and then promotes VO
2the practical development of thin-film device.
CN102912308A discloses a kind of low transformation temperature vanadium dioxide film preparation technology, it adopts direct current reaction magnetron sputtering technology and annealing technology to prepare the vanadium dioxide film of low transformation temperature, yet the scope narrower (36～42 ℃) regulating by the standby vanadium dioxide film transformation temperature of this legal system,, temperature changes (△ T
c) less, be only 6 ℃; In addition, this method also needs anneal to carry out modification to film.
Summary of the invention
The problem existing in the face of prior art, based on above-mentioned to energy-saving glass VO
2the general introduction of thin film study present situation, the object of this invention is to provide the adjustable VO of a kind of transformation temperature
2pure phase film and preparation method, adopt reaction magnetocontrol sputtering method, by explore different thin film preparation processes under the condition of non-doping, by controlling sputtering parameter, regulates and controls VO
2the microstructure composition of film reaches the object of effective adjusting transformation temperature.
The present invention adopts magnetron sputtering method to prepare VO
2film, adopts vanadium metal target, by strict control substrate (substrate) temperature, pass into the means such as oxygen content, carries out VO
2the trace of film composition is controlled, and prepares the single crystallization phases VO of anoxic or oxygen enrichment
2polycrystal film, realizes metal-insulator phase transition temperature variation and is not less than 30 ℃ of (△ T
c>=30 ℃).Whole technique is simple, adopts the mode of non-doping, and by sputtering pressure, the precision of oxygen partial pressure and microstructure is controlled, and regulates VO
2the component of film (V:O ratio), grain-size and void content etc., do not changing under the prerequisite of film thermocolour performance substantially, reaches regulation and control VO
2the object of thin film phase change temperature, the detrimentally affect that can effectively avoid doping to bring, is conducive to film to high-quality, high performance future development.At present, similar structures there is not yet report in all kinds of documents at home and abroad.
In the present invention, by described target is carried out sputter directly to form the adjustable vanadium dioxide film of transformation temperature on substrate without anneal.The present invention has not only overcome the shortcoming of in the past preparing the complicated process of preparation of vanadium oxide film, and the vanadium oxide film of preparation is the adjustable vanadium dioxide film of transformation temperature simultaneously.
Preferably, can control depositing temperature is 300～400 ℃.
Preferably, to can be purity be more than 99.99% non-doping high purity vanadium metal to described target.
Preferably, described oxygen purity can be more than 99.99%, and the purity of described argon gas can be 99.99%.
In the present invention, substrate can adopt and do not contain simple glass, silica glass, the sapphire of Na or be coated with layer of sin
xsi substrate.
In the present invention, can make the transformation temperature of vanadium dioxide film of preparation adjustable continuously between 55～90 ℃ by changing described depositing temperature.So strict control underlayer temperature, between 300～500 ℃ (preferably 300～400 ℃), by regulation and control various substrate, regulates VO
2the crystallization property of film, realizes the adjustable continuously of transformation temperature.
In the present invention, can make the transformation temperature of vanadium dioxide film of preparation adjustable continuously between 55～90 ℃ by changing described sputter total head again.Like this, preparation process is controlled different sputter total heads, film surface appearance is changed, thereby realize the adjustable continuously of transformation temperature.
In the present invention, can make the transformation temperature of vanadium dioxide film of preparation adjustable continuously between 55～90 ℃ by changing described oxygen partial pressure again.Like this, in preparation process, the argon-mixed middle oxygen argon ratio of oxygen is adjustable in micro-scope, thereby realizes precision control VO
2the object of the component of film (V:O ratio), realizes the adjustable continuously of transformation temperature.
Preferably, also can control back end vacuum is 1～5 * 10
-5pa, sputtering power is 50～100W, sputtering time is 100～200 minutes.
Accompanying drawing explanation
The vanadium dioxide film XRD diffractogram that Fig. 1 example of the present invention makes;
Fig. 2 illustrates the resistance temperature curve figure of sputter oxygen partial pressure on the impact of the transformation temperature of the vanadium dioxide film making;
Fig. 3 illustrates the resistance temperature curve figure of underlayer temperature on the impact of the transformation temperature of the vanadium dioxide film making;
Fig. 4 illustrates the resistance temperature curve figure of sputter total head on the impact of the transformation temperature of the vanadium dioxide film making;
Fig. 5 A～5C illustrates respectively the surface topography map of the vanadium dioxide film making under different sputter total heads.
Embodiment
With reference to Figure of description, and further illustrate with the following embodiments the present invention, should be understood that Figure of description and following embodiment are only for the present invention is described, and unrestricted the present invention.
The present invention, by explore different thin film preparation processes under the condition of non-doping, regulates and controls VO
2the microstructure composition of film reaches the object of effective adjusting transformation temperature.Described preparation method is mainly magnetron sputtering method and prepares VO
2film, adopts vanadium metal target, by strict control base reservoir temperature, pass into the means such as oxygen content, carries out VO
2the trace of film composition is controlled, and prepares the single crystallization phases VO of anoxic or oxygen enrichment
2polycrystal film, realizes metal-insulator phase transition temperature variation and is not less than 30 ℃ (△ Tc>=30 ℃).
Preparation method of the present invention, for the preparation method who adopts is magnetron sputtering method, adopts multifunctional magnetic control sputtering system, with vanadium metal target, vacuumizes, and controls underlayer temperature, passes into argon gas and oxygen and as sputter gas and reactant gases, prepares VO respectively
2film.Particularly, can adopt multifunctional magnetic control sputtering system, take high purity metal vanadium (purity: 99.99%) be target, 2～4 inches of target diameters, thickness 4～6mm, back end vacuum is 1～5 * 10
-5pa, underlayer temperature is 300～500 ℃, Ar airshed 30～50 mark condition milliliter per minutes (sccm), sputtering power is 20～100w, sputtering time 60～300min, oxygen flow 0.4～2sccm.
Substrate can be selected as not containing English glass, the sapphire of Na simple glass, stone or being coated with layer of sin
xsi substrate.For example adopt and be coated with layer of sin
xsi sheet as substrate, SiNx layer is mainly insulation layer, avoids the electric leakage of film in electrical testing.Substrate cleans through acetone, ethanol and deionized water standard ultrasound.
Vanadium metal target preferably adopts the vanadium metal of non-doping, and especially purity is more than 99.99% vanadium metal.The diameter of target can be 2～4 inches, and thickness can be 4～6mm.
In the present invention, strictly control underlayer temperature between 300～500 ℃, by regulation and control different deposition temperatures, regulate VO
2the crystallization property of film, realizes the adjustable continuously of transformation temperature.For example, referring to Fig. 3, it is illustrated under different deposition temperatures (underlayer temperature) condition VO under temperature condition
2resistance temperature loop line figure, within the scope of depositing temperature changes from 300～400 ℃, transformation temperature changes and can reach more than 20 ℃.
Before passing into sputter gas and reactant gases, the vacuum chamber of multifunctional magnetic control sputtering system is evacuated to 1～5 * 10
-5pa(back end vacuum).
Argon gas and oxygen as sputter gas and reactant gases preferably adopt by high-purity gas, for example, adopt purity to be more than 99.99% oxygen and argon gas respectively as reactant gases and sputter gas.
In the present invention, the total pressure (sputter total head) of controlling oxygen argon mixture gas in sputter procedure is 0.6～1.8Pa, can, by controlling the total pressure (sputter total head) of oxygen argon mixture gas in film preparation process, regulate VO
2the microtexture of film and surface topography, realize the adjustable continuously of transformation temperature.For example, referring to Fig. 5 A～5C, it illustrates respectively the surface topography map of the vanadium dioxide film making under different sputter total heads, the particle size that vanadium dioxide film prepared by visible this law forms is 10-200nm, and the gauge control of film is at the preferred 50～100nm of 10～500nm() in scope.
In the present invention, controlling the argon-mixed middle oxygen argon of oxygen in sputter procedure is 1～5% than (oxygen partial pressure), for example, adopt the argon stream amount of 40 mark condition milliliter per minutes (sccm), adopts the oxygen flow amount of 0.4～2sccm.More adjustable in micro-scope than (oxygen partial pressure) by the argon-mixed middle oxygen argon of oxygen in control film preparation process, thus realize precision control VO
2the object of the component of film (V:O ratio), realizes the adjustable continuously of transformation temperature.For example, referring to Fig. 2, it illustrates VO under different oxygen partial pressure conditions
2resistance temperature loop line figure, at oxygen partial pressure, change within the scope of 1%-5%, transformation temperature changes and can reach more than 30 ℃.
Referring to Fig. 1, the vanadium dioxide film XRD diffractogram that an example of the present invention makes, therefrom visible, vanadium dioxide film prepared by the present invention is pure phase (monocline M phase) polycrystalline vanadium dioxide, without other dephasign, exists.Referring to Fig. 2～4, the continuous regulation and control that the metal-insulator phase transition temperature of prepared film of the present invention can be between 55-90 ℃ according to mode of deposition and microtexture, before and after phase transformation, transmittance changes at 20%-60%, and resistivity can change 2-3 the order of magnitude.
The prepared thin film phase change temperature of the present invention is adjustable, low temperature visible light transmissivity is high, regulating power to sunlight is higher, not only can be applied to intelligent energy-saving coating, also can be applied to sun power temperature control unit, the fields such as micro optical switch device, thermistor, optical information storage, can be applied to thermochromism film, energy-conservation film, intelligent power saving glass curtain wall, temperature control unit (for example sun power temperature control unit) and energy-saving coating.For example, be applicable to directly manufacture energy-saving glass, also can, for existing simple glass is transformed, can also be applied to the reducing energy consumption on the surfaces such as existing building, car and boat.
The present invention is based on inorganic oxide based film material cheaply, by regulation and control preparation technology parameter, substantially do not changing under the prerequisite of film thermocolour performance, reach regulation and control VO
2the object of thin film phase change temperature, the detrimentally affect of effectively having avoided doping to bring, is conducive to film to high-quality, high performance future development.
Below further list some exemplary embodiments so that the present invention to be described better.Should understand; the above-mentioned embodiment that the present invention describes in detail; and following examples are only not used in and limit the scope of the invention for the present invention is described, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjust and all belong to protection scope of the present invention.Airshed, underlayer temperature, sputtering power and the sputtering time etc. of the substrate that following example is concrete, back end vacuum, sputter total head, oxygen and argon gas are only also examples in OK range,, those skilled in the art can do in suitable scope and be selected by explanation herein, and do not really want to be defined in the below concrete numerical value of example.
By regulating the oxygen partial pressure in sputter deposition process, obtain the VO of different transformation temperatures
2film
Select the Si sheet that is coated with layer of sin x as substrate, adopt vanadium metal target (purity: 99.99%), by magnetron sputtering method, pass into argon gas and oxygen is prepared VO
2film, thickness 50～100nm; By regulating the oxygen partial pressure in sputter deposition process, obtain the VO of different transformation temperatures
2film.
Embodiment 1
Substrate selects the Si sheet that is coated with layer of sin x as substrate, and SiNx layer is mainly insulation layer, avoids the electric leakage of film in electrical testing, through acetone, ethanol and deionized water standard ultrasound, cleans.Adopt multifunctional magnetic control sputtering system, take high purity metal vanadium (purity: 99.99%) be target, target 2 inches diameter, thickness 5mm, back end vacuum is 3 * 10
-5pa, depositing temperature is 400 ℃, Ar airshed 40 mark condition milliliter per minutes (sccm), sputtering power is 60w, sputtering time 150min, oxygen flow 0.4sccm(is that oxygen partial pressure is 1.0%), the particle size that makes vanadium dioxide film is 15nm, thickness is 70nm.
Embodiment 2
The basic step that repeats embodiment 1, that different is oxygen flow 0.6sccm, oxygen partial pressure is 1.5%,, the particle size that makes vanadium dioxide film is 18nm, thickness is 70nm.
Embodiment 3
The basic step that repeats embodiment 1, that different is oxygen flow 0.8sccm, and oxygen partial pressure is 2%, and the particle size that makes vanadium dioxide film is 20nm, and thickness is 70nm.
Embodiment 4
The basic step that repeats embodiment 1, that different is oxygen flow 2.0sccm, and oxygen partial pressure is 5%, and the particle size that makes vanadium dioxide film is 25nm, and thickness is 70nm.
Mutually as shown in Figure 1, film presents VO to the thin film crystallization of X-ray diffractometer analysis for tonneau (XRD) test implementation example 1 preparation
2simple crystallization phases, generates without dephasign.Referring to Fig. 2, the VO that under different oxygen partial pressure conditions, (embodiment 1～4) makes is shown
2the resistance temperature loop line figure of film, wherein, the VO of embodiment 1 preparation
2the transformation temperature of film is 48 ℃, the VO of embodiment 2 preparations
2the transformation temperature of film is 59 ℃, the VO of embodiment 3 preparations
2the transformation temperature of film is 71 ℃, the VO of embodiment 4 preparations
2the transformation temperature of film is 83 ℃.At oxygen partial pressure, change within the scope of 1%-5% as seen, transformation temperature changes and can reach more than 30 ℃.
By regulating the underlayer temperature in sputter deposition process, obtain the VO of different transformation temperatures
2film
Select and be coated with layer of sin
xsi sheet as substrate, adopt vanadium metal target (purity: 99.99%), by magnetron sputtering method, pass into argon gas and oxygen is prepared VO
2film, thickness 50～100nm; By regulating the sputtering sedimentation temperature (underlayer temperature) in deposition process, obtain the VO of different transformation temperatures
2film.
Embodiment 5
Substrate is selected and is coated with layer of sin
xsi sheet as substrate, SiN
xlayer is mainly insulation layer, avoids the electric leakage of film in electrical testing, through acetone, ethanol and deionized water standard ultrasound, cleans.Adopt multifunctional magnetic control sputtering system, take high purity metal vanadium (purity: 99.99%) be target, target 2 inches diameter, thickness 5mm, back end vacuum is 3 * 10
-5pa, depositing temperature is 300 ℃, Ar airshed 40 mark condition milliliter per minutes (sccm), sputtering power is 60w, sputtering time 150min, oxygen flow 1sccm,, the particle size that makes vanadium dioxide film is 16nm, thickness is 70nm.
Embodiment 6
The basic step that repeats embodiment 5, different is that depositing temperature is 350 ℃, and the particle size that makes vanadium dioxide film is 19nm, and thickness is 70nm.
Embodiment 7
The basic step that repeats embodiment 5, different is that depositing temperature is 400 ℃, and the particle size that makes vanadium dioxide film is 22nm, and thickness is 70nm.
Utilize X-ray diffractometer analysis (XRD) testing film crystallization phases to present VO
2simple crystallization phases, generates without dephasign.Fig. 3 is VO under different deposition temperatures condition
2resistance temperature loop line figure, wherein, the VO of embodiment 5 preparation
2the transformation temperature of film is 52 ℃, the VO of embodiment 6 preparations
2the transformation temperature of film is 61 ℃, the VO of embodiment 7 preparations
2the transformation temperature of film is 73 ℃, and within the scope of depositing temperature changes from 300-400 ℃, transformation temperature variation can reach more than 20 ℃ as seen.
By regulating the deposition total head in sputter deposition process, obtain the VO of different transformation temperatures
2film
Select healthy and free from worry vitreosil sheet glass as substrate, adopt vanadium metal target (purity: 99.99%), by magnetron sputtering method, pass into argon gas and oxygen is prepared VO
2film, thickness 50～100nm; By regulating the deposition total head in sputter deposition process, obtain the VO of different transformation temperatures
2film.
Embodiment 8
Substrate selects healthy and free from worry vitreosil sheet glass as substrate, through acetone, ethanol and deionized water standard ultrasound, cleans.Adopt multifunctional magnetic control sputtering system, take high purity metal vanadium (purity: 99.99%) be target, target 2 inches diameter, thickness 5mm, back end vacuum is 3 * 10
-5pa, depositing temperature is 450 ℃, Ar, O
2mixed gas flow 40 mark condition milliliter per minutes (sccm), oxygen partial pressure 2.5%, deposition total head is 0.6Pa, sputtering power is 50w, sputtering time 150min, the particle size that makes vanadium dioxide film is 40nm, thickness is 50nm.
Embodiment 9
The basic step that repeats embodiment 8, that different is Ar, O
2mixed gas flow is 45 mark condition milliliter per minutes (sccm), and sputter total head is 1.2Pa, and the particle size that makes vanadium dioxide film is 47nm, and thickness is 50nm.
Embodiment 10
The basic step that repeats embodiment 8, that different is Ar, O
2mixed gas flow 50 mark condition milliliter per minutes (sccm), sputter total head is 1.8Pa, and the particle size that makes vanadium dioxide film is 60nm, and thickness is 50nm.
Utilize X-ray diffractometer analysis (XRD) testing film crystallization phases to present VO
2simple crystallization phases, generates without dephasign. and referring to Fig. 4, it illustrates not VO under synsedimentary total head condition
2resistance temperature loop line figure, wherein, the VO of embodiment 8 preparation
2the transformation temperature of film is 71.7 ℃, the VO of embodiment 9 preparations
2the transformation temperature of film is 76.6 ℃, the VO of embodiment 10 preparations
2the transformation temperature of film is 81.8 ℃, changes within the scope of 0.6-1.8Pa as seen in deposition total head, and transformation temperature variation can reach more than 10 ℃.Referring to Fig. 5 A～5C, it illustrates under synsedimentary total head variation again, and film surface appearance changes, and when deposition pressure is respectively 0.6Pa, 1.2Pa, 1.8Pa, roughness of film is respectively 5.6nm, 6.2nm, 7.5nm.When deposition pressure is respectively 0.6Pa, 1.2Pa, 1.8Pa, low temperature visible light transmissivity is respectively 33.3%, 36.9%, 45.3%, and transformation temperature is respectively 71.7 ℃, 76.6 ℃, 81.8 ℃, and sunlight regulation rate is respectively 5.5%, 4.6%, 5.0%.Experimental result shows, with sputtering pressure, increases, and visible light transmissivity obviously increases, and transformation temperature raises to some extent, sunlight regulation rate substantially constant.When deposition pressure is respectively 0.6Pa, 1.2Pa, 1.8Pa, the refractive index n that is 614nm sunlight place at wavelength is respectively 2.94,2.85,2.63.
Industrial applicability: the prepared film of the present invention is expected to be widely used in intelligent energy-saving coating, sun power temperature control unit, the fields such as micro optical switch device, thermistor, optical information storage.Method provided by the invention, technique is simple, cost is low, yield is high, is applicable to scale production.
Claims (10)
1. a magnetron sputtering method is prepared the method for vanadium dioxide film, it is characterized in that, comprise: take vanadium metal as target, the argon gas of take carries out sputter to form vanadium dioxide film on substrate to described target as reactant gases as sputter gas and the oxygen of take, and wherein controlling depositing temperature and be 300～500 ℃, deposition total head is that 0.5～2.0Pa, oxygen partial pressure are 1～5%.
2. method according to claim 1, is characterized in that, by described target is carried out sputter directly to form the adjustable vanadium dioxide film of transformation temperature on substrate without anneal.
3. method according to claim 1 and 2, is characterized in that, controlling depositing temperature is 300～400 ℃.
4. according to the method described in any one in claim 1～3, it is characterized in that, described target is that purity is more than 99.99% non-doping high purity vanadium metal.
5. according to the method described in claim 1～4, it is characterized in that, described oxygen purity is more than 99.99%, and the purity of described argon gas is 99.99%.
6. according to the method described in any one in claim 1～5, it is characterized in that, described substrate is not for containing simple glass, silica glass, the sapphire of Na or being coated with layer of sin
xsi substrate.
7. according to the method described in any one in claim 1～6, it is characterized in that, by changing described depositing temperature, make the transformation temperature of vanadium dioxide film of preparation adjustable continuously between 55～90 ℃.
8. according to the method described in any one in claim 1～6, it is characterized in that, by changing described sputter total head, make the transformation temperature of vanadium dioxide film of preparation adjustable continuously between 55～90 ℃.
9. according to the method described in any one in claim 1～6, it is characterized in that, by changing described oxygen partial pressure, make the transformation temperature of vanadium dioxide film of preparation adjustable continuously between 55～90 ℃.
10. according to the method described in any one in claim 1～9, it is characterized in that, controlling back end vacuum is 1～5 * 10
-5pa, sputtering power is 50～100W, sputtering time is 100～200 minutes.
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| CN104914211A (en) * | 2015-04-10 | 2015-09-16 | 天津大学 | Preparation method of particle and short rod-like vanadium oxide film |
| CN105132877A (en) * | 2015-09-16 | 2015-12-09 | 深圳大学 | Low-temperature deposition method for vanadium dioxide thin film |
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| CN113564522A (en) * | 2021-08-04 | 2021-10-29 | 南京信息工程大学 | Vanadium dioxide thin film and preparation method and application thereof |
| CN117127153A (en) * | 2023-08-30 | 2023-11-28 | 无锡尚积半导体科技有限公司 | Vanadium dioxide film and preparation method thereof |
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| CN104914211A (en) * | 2015-04-10 | 2015-09-16 | 天津大学 | Preparation method of particle and short rod-like vanadium oxide film |
| WO2017045398A1 (en) * | 2015-09-16 | 2017-03-23 | 深圳大学 | Low-temperature deposition method for vanadium dioxide thin film |
| CN105132877A (en) * | 2015-09-16 | 2015-12-09 | 深圳大学 | Low-temperature deposition method for vanadium dioxide thin film |
| CN105256280A (en) * | 2015-11-24 | 2016-01-20 | 天津大学 | Method for regulating and controlling phase transition temperature of vanadium dioxide through fast heat treatment |
| CN105937019B (en) * | 2016-06-12 | 2019-06-11 | 中国科学院上海硅酸盐研究所 | A kind of VO of metallic element Mg doping2Film and preparation method thereof |
| CN105937019A (en) * | 2016-06-12 | 2016-09-14 | 中国科学院上海硅酸盐研究所 | VO2 thin film doped with metallic element Mg and preparation method thereof |
| CN108220897A (en) * | 2016-12-14 | 2018-06-29 | 中国科学院上海硅酸盐研究所 | The method of magnetron sputtering low temperature preparation vanadium dioxide film |
| CN110171931A (en) * | 2019-07-15 | 2019-08-27 | 吉林农业科技学院 | A kind of preparation method for mixing vanadium bilayer electro-allochromatic nickel oxide film |
| 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 |
| CN110791740B (en) * | 2019-12-02 | 2021-08-24 | 武汉理工大学 | Preparation method of high-performance ZIF-L/vanadium dioxide composite film |
| CN112921291A (en) * | 2021-01-26 | 2021-06-08 | 上海交通大学 | Preparation method of tungsten-doped vanadium dioxide thin film with adjustable phase-change temperature |
| CN113564522A (en) * | 2021-08-04 | 2021-10-29 | 南京信息工程大学 | Vanadium dioxide thin film and preparation method and application thereof |
| CN117127153A (en) * | 2023-08-30 | 2023-11-28 | 无锡尚积半导体科技有限公司 | Vanadium dioxide film and preparation method thereof |
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