CN108179394A - A kind of method for improving vanadium dioxide phase time-varying amplitude by regulating and controlling sputtering power - Google Patents
A kind of method for improving vanadium dioxide phase time-varying amplitude by regulating and controlling sputtering power Download PDFInfo
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- CN108179394A CN108179394A CN201810123782.6A CN201810123782A CN108179394A CN 108179394 A CN108179394 A CN 108179394A CN 201810123782 A CN201810123782 A CN 201810123782A CN 108179394 A CN108179394 A CN 108179394A
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- vanadium
- vanadium dioxide
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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
-
- 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
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
-
- 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
Abstract
The invention discloses a kind of methods for improving vanadium dioxide phase time-varying amplitude by regulating and controlling sputtering power, vanadium dioxide film is prepared in a manner that rapid thermal annealing is combined magnetron sputtering, vanadium metal film is prepared by the way of magnetron sputtering, sputtering power is using the multiple parameters between 40 160W in sputtering process, while in order to achieve the purpose that film thickness is identical, sputtering time is adjusted according to power parameter, Quick Oxidation annealing is then carried out in quick anneal oven.By the deposition of film and the preparative separation of vanadium dioxide in whole preparation process, reduce the technological requirement of preparation and regulation and control, in addition, the setting of more power parameters plays the role of regulating and controlling vanadium metal film microstructure in sputtering process, and then achievees the purpose that regulation and control and improve vanadium dioxide phase time-varying amplitude.The present invention studies the phase-change characteristic of prepared vanadium dioxide film using four-point probe, and it is simple to design a kind of preparation process, easily controllable, and can regulate and control and improve VO2The method of phase time-varying amplitude.
Description
Technical field
The present invention relates to a kind of methods for improving vanadium dioxide phase time-varying amplitude, and in particular to one kind is by regulating and controlling sputtering power
The method for improving vanadium dioxide phase time-varying amplitude.
Background technology
In life, the continuous service of hvac equipment is to maintain to build one of comfortable essential condition, but these
The operation of equipment is along with a large amount of energy consumption.Some researches show that China building energy consumption accounts for the 27% of social total energy consumption
Left and right.In building energy consumption, the energy consumption of windowpane accounts for the 40%~50% of whole building energy consumptions, therefore the energy saving of window is building
Key problems-solving is needed in energy saving.In order to reduce loss of the long-time service to the energy of hvac equipment, with VO2To have
The smart window of effect controlled material is come into being.Vanadium dioxide (VO2) it is a kind of solid-state thermochromic material, VO2Film is in thermal drivers
Down have semiconductor-metal phase-change characteristic, before phase change after, infrared light region optical transmittance occur invertibity mutation.Under low temperature,
VO2It is the semiconductor phase with monocline;Become the metal phase with cubic rutile structure during high temperature.After before phase change
Light, electrical property have a greater change, this makes it have extraordinary development prospect in fields such as smart windows.When temperature is less than phase alternating temperature
When spending, vanadium dioxide film is higher in infrared region transmissivity, and when temperature is higher than phase transition temperature, vanadium dioxide film is infrared
Region reflectivity is higher, so as to reach selectively absorption or reflected solar radiation.It is, when indoor temperature is low, titanium dioxide
Vanadium film is got in by infrared light, improves indoor temperature;When temperature is increased to certain temperature, vanadium dioxide film drops automatically
The transmitance of low infrared light, indoor temperature then continuously decrease;It is automatic again after temperature drops to certain value to improve to the saturating of infrared light
Cross rate.
In order to obtain better using effect, the characteristic that smart window should have sun optical modulation amplitude high.With higher phase
The vanadium dioxide film of time-varying amplitude, the transmissivity knots modification of infrared band light is big, therefore phase time-varying amplitude is for improving sunlight
Modulation amplitude plays an important role.VO2The preparation of film usually utilizes the side for the reaction magnetocontrol sputtering that oxygen is passed through in sputtering process
Method, at present domestic and international researcher be devoted to mostly by regulate and control reaction magnetocontrol sputtering parameter improve VO2Thin film phase change amplitude.To the greatest extent
Pipe can effectively regulate and control VO in reactive sputtering process by the regulation and control of sputtering parameter2Phase time-varying amplitude, but the tune of the parameter
Section needs high equipment and process conditions, this is to VO2The complexity and stability of phase time-varying amplitude regulation and control cause very big shadow
It rings.VO is prepared with reaction magnetocontrol sputtering2Film is compared, using magnetron sputtering with the mode that rapid thermal annealing is combined be also prepare
VO2One of thin film manner, requirement of this method to equipment and process conditions is low, prepares and stablizes, is easy to a wide range of industrial production,
And the sputtering power by adjusting in vanadium metal thin film sputtering process can be with Effective Regulation VO2Phase time-varying amplitude, to improve phase luffing
Degree.But rarely have to the research of this preparation method realized by changing the sputtering power of vanadium metal film to VO at present2Phase luffing
Spend the report of regulation and control.
Invention content
In order to solve the problems in the existing technology, the present invention provides a kind of by regulating and controlling sputtering power raising titanium dioxide
The method of vanadium phase time-varying amplitude overcomes traditional reaction magnetocontrol sputtering regulation and control VO in the prior art2Phase time-varying amplitude needs very high technique will
The problem of asking.
The technical scheme is that:A kind of method for improving vanadium dioxide phase time-varying amplitude by regulating and controlling sputtering power, packet
Include following steps:
(1) cleaning of sapphire substrates:
Sapphire sheet is sequentially placed into deionized water, acetone and absolute ethyl alcohol and is cleaned by ultrasonic, removes surface
Inorganic and organic impurities;It is washed with deionized water only, is finally put into sapphire substrate spare in absolute ethyl alcohol again;
(2) preparation of vanadium metal film:
Clean sapphire substrates are placed in the vacuum chamber of III type ultrahigh vacuum facing-target magnetron sputtering system coating machines of DPS-, are used
The vanadium metal that quality purity is 99.99% is 99.999% argon gas as working gas, background using quality purity as target
Vacuum degree 4.0 × 10-4Pa, substrate does not heat in sputtering process, argon gas flow 48mL/min, and sputtering operating air pressure is
2Pa, sputtering power 40-160W, sputtering time 4.5min-20min deposit vanadium film on surface;
(3) preparation of vanadium dioxide film:
Vanadium metal film made from step (2) is positioned over progress Quick Oxidation thermal annealing in quick anneal oven;Quick oxygen
Change in thermal annealing process, the change rule of in-furnace temperature is divided into heat up, keeping the temperature, cool down three phases, what when thermal oxide was passed through
Gas is high purity oxygen gas, and gas flow is fixed as 7slpm when heating up and keeping the temperature, remaining phase gas flow is fixed as 1slpm, protects
Temperature is 450-480 DEG C, and heating rate is determined by setting holding temperature and heating-up time.
Step (3) heating rate is 50 DEG C/s, heating-up time 9s, soaking time 70-110s, temperature fall time 90s.
The sputtering power of step (2) the vanadium metal film preparation uses multiple power parameters between 40-160W, simultaneously
In order to achieve the purpose that film thickness is identical, sputtering time is adjusted according to power parameter.Sputtering power is 40,50,60,70,80,
100th, 120, sputtering time corresponding to 160W be followed successively by 20,18.5,16,14.5,12.5,10,4.5min.
Beneficial effects of the present invention are:
1) it is easy to steadily prepare vanadium dioxide film, and the method for regulating and controlling vanadium dioxide film phase time-varying amplitude is more simple
Single, preparation time is short, and required process conditions are low, easily controllable.
2) first splash-proofing sputtering metal vanadium film, then carries out thermal annealing oxidation again, similar to practical process of factory production, is suitble to big
Volume industrial produces.
The present invention prepares vanadium metal film by the way of magnetron sputtering, and Quick Oxidation is then carried out in quick anneal oven
Annealing, by the deposition of film and the preparative separation of vanadium dioxide in whole preparation process, the technique for reducing preparation and regulation and control
It is required that and the phase-change characteristic of prepared vanadium dioxide film is studied using four-point probe, devise a kind of prepare
Process is simple, easily controllable, and can regulate and control and improve VO2The method of phase time-varying amplitude.
Description of the drawings
Fig. 1 is the vanadium dioxide film that is prepared of the different vanadium metal film of sputtering power under identical annealing conditions
Resistance transformation curve;Figure A, B, C, D correspond to sputtering power as 50W, 60W, 70W, 80W respectively;
Fig. 2 be sputtering power be respectively 50,60,70, the obtained titanium dioxide of the vanadium film of 80W under identical annealing conditions
The phase time-varying amplitude of vanadium film;
Fig. 3 is the vanadium dioxide film that the different vanadium metal film of sputtering power is prepared under identical annealing conditions
Resistance transformation curve;Figure A, B, C correspond to sputtering power as 40W, 80W, 160W respectively;
Fig. 4 be sputtering power be respectively 40,80, the vanadium metal film of 160W be prepared under identical annealing conditions two
The resistance phase time-varying amplitude of vanadium oxide film.
Specific embodiment
The present invention is described in further detail below in conjunction with the accompanying drawings.
The raw materials used in the present invention uses commercially available material.
Embodiment 1
1) sapphire cleans
Sapphire used is the sapphire of double polishings of (001) crystal face bought on the market, size 1cm*1cm.It will
Sapphire sheet, which is sequentially placed into deionized water, acetone and absolute ethyl alcohol, to be cleaned by ultrasonic, and every scavenging period is 20 points
Clock removes the inorganic and organic impurities on surface;It is washed with deionized water only, is finally put into sapphire substrate standby in absolute ethyl alcohol again
With.2) preparation of vanadium metal film
Clean sapphire substrates are placed in the vacuum chamber of III type ultrahigh vacuum facing-target magnetron sputtering system coating machines of DPS-, are used
The vanadium metal that quality purity is 99.99% is 99.999% argon gas as working gas, background using quality purity as target
Vacuum degree 4.0 × 10-4Pa, substrate does not heat in sputtering process, argon gas flow 48mL/min, and sputtering operating air pressure is
2Pa, sputtering power 50,60,70,80W, to ensure that vanadium metal film has same thickness, sputtering corresponding with sputtering power
Time is followed successively by 18.5,16,14.5,12.5min, the vanadium metal film thickness being prepared is about 90nm.
3) preparation of vanadium dioxide film
The vanadium metal film that 4 thickness that step 2) obtains are 90nm is positioned in quick anneal oven and carries out quick oxygen
Change thermal annealing.Set annealing temperature be 450 DEG C, heating rate be 50 DEG C/min, soaking time 110s, temperature fall time 90s,
Oxygen is passed through as reaction gas, the quality purity of oxygen is 99.99%, and oxygen flow is 7slpm when heating up and keeping the temperature, and is cooled down
When oxygen flow be 1slpm.Measured transformation curve is as shown in Figure 1, we choose 28 DEG C in temperature-rise period of film resistor
As the room temperature film resistance before phase transformation, 90 DEG C in temperature-rise period of film resistor is chosen as the high temperature film after phase transformation
Resistance, room temperature film resistance and the ratio of high temperature film resistance change amplitude for resistance, for weighing vanadium dioxide film phase transformation
Front and rear phase time-varying amplitude, sputtering power is respectively 50,60,70, the phase time-varying amplitude of the sample of 80W be respectively 7.2,20.5,15.0,
2.8, as shown in Figure 2.
Embodiment 2:
1) sapphire cleans
Sapphire used is the sapphire of double polishings of (001) crystal face bought on the market, size 1cm*1cm.It will
Sapphire sheet, which is sequentially placed into deionized water, acetone and absolute ethyl alcohol, to be cleaned by ultrasonic, and every scavenging period is 20 points
Clock removes the inorganic and organic impurities on surface;It is washed with deionized water only, is finally put into sapphire substrate standby in absolute ethyl alcohol again
With.2) preparation of vanadium metal film
Clean sapphire substrates are placed in the vacuum chamber of III type ultrahigh vacuum facing-target magnetron sputtering system coating machines of DPS-, are used
The vanadium metal that quality purity is 99.99% is 99.999% argon gas as working gas, background using quality purity as target
Vacuum degree 4.0 × 10-4Pa, substrate does not heat in sputtering process, argon gas flow 48mL/min, and sputtering operating air pressure is
2Pa, sputtering power 40,80,160W, to ensure that vanadium metal film has same thickness, during sputtering corresponding with sputtering power
Between be followed successively by 20,12.5,4.5min, the vanadium metal film thickness being prepared is about 90nm.
3) preparation of vanadium dioxide film
The vanadium metal film that 3 thickness that step 2) obtains are 90nm is positioned in quick anneal oven and carries out quick oxygen
Change thermal annealing.Set annealing temperature be 480 DEG C, heating rate be 50 DEG C/min, soaking time 70s, temperature fall time 90s,
Oxygen is passed through as reaction gas, the quality purity of oxygen is 99.99%, and oxygen flow is 7slpm when heating up and keeping the temperature, and is cooled down
When oxygen flow be 1slpm.Measured transformation curve is as shown in figure 3, we choose 40 DEG C in temperature-rise period of film resistor
As the room temperature film resistance before phase transformation, 80 DEG C in temperature-rise period of film resistor is chosen as the high temperature film after phase transformation
Resistance, room temperature film resistance and the ratio of high temperature film resistance change amplitude for resistance, for weighing vanadium dioxide film phase transformation
Front and rear phase time-varying amplitude, sputtering power is respectively 40,80, the phase time-varying amplitude of the sample of 160W be respectively 68.5,178.2,32.3,
As shown in Figure 4.
By above-mentioned two embodiment it is found that the method for the present invention during vanadium dioxide film is prepared by adjusting metal
The sputtering power of vanadium film has achieved the purpose that regulate and control and has improved vanadium dioxide film phase time-varying amplitude, and simple for process, repeats
Property it is high, have certain positive effect to the improvement of the preparation method of smart window.
Although above in conjunction with attached drawing, invention has been described, and the invention is not limited in above-mentioned specific implementations
Mode, above-mentioned specific embodiment is only schematical, is not restricted, those of ordinary skill in the art are at this
Under the enlightenment of invention, present inventive concept and scope of the claimed protection are not being departed from, many shapes can also be made
Formula, within these are all belonged to the scope of protection of the present invention.
Claims (4)
- A kind of 1. method for improving vanadium dioxide phase time-varying amplitude by regulating and controlling sputtering power, which is characterized in that include the following steps:(1) cleaning of sapphire substrates:Sapphire sheet is sequentially placed into deionized water, acetone and absolute ethyl alcohol and is cleaned by ultrasonic, removes the inorganic of surface And organic impurities;It is washed with deionized water only, is finally put into sapphire substrate spare in absolute ethyl alcohol again;(2) preparation of vanadium metal film:Clean sapphire substrates are placed in the vacuum chamber of III type ultrahigh vacuum facing-target magnetron sputtering system coating machines of DPS-, using quality The vanadium metal that purity is 99.99% is 99.999% argon gas as working gas, base vacuum using quality purity as target Degree 4.0 × 10-4Pa, substrate does not heat in sputtering process, argon gas flow 48mL/min, and sputtering operating air pressure is 2Pa, is splashed Power is penetrated as 40-160W, sputtering time 4.5min-20min, vanadium film is deposited on surface;(3) preparation of vanadium dioxide film:Vanadium metal film made from step (2) is positioned over progress Quick Oxidation thermal annealing in quick anneal oven;Quick Oxidation heat In annealing process, the change rule of in-furnace temperature is divided into heat up, keeping the temperature, cool down three phases, the gas that when thermal oxide is passed through For high purity oxygen gas, gas flow is fixed as 7slpm when heating up and keeping the temperature, remaining phase gas flow is fixed as 1slpm, heat preservation temperature It is 450-480 DEG C to spend, and heating rate is determined by setting holding temperature and heating-up time.
- 2. the method for improving vanadium dioxide phase time-varying amplitude by regulating and controlling sputtering power according to claim 1, which is characterized in that Step (3) heating rate is 50 DEG C/s, heating-up time 9s, soaking time 70-110s, temperature fall time 90s.
- 3. the method for improving vanadium dioxide phase time-varying amplitude by regulating and controlling sputtering power according to claim 1, which is characterized in that The sputtering power of step (2) the vanadium metal film preparation uses multiple power parameters between 40-160W, while in order to reach The identical purpose of film thickness adjusts sputtering time according to power parameter.
- 4. the method for improving vanadium dioxide phase time-varying amplitude by regulating and controlling sputtering power according to claim 3, which is characterized in that Sputtering power is 40,50,60,70,80,100,120, sputtering time corresponding to 160W be followed successively by 20,18.5,16,14.5, 12.5、10、4.5min。
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Cited By (6)
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CN109182974A (en) * | 2018-10-09 | 2019-01-11 | 天津大学 | A method of vanadium oxide film is prepared by two one-step rapid thermal anneals |
CN109402581A (en) * | 2018-10-17 | 2019-03-01 | 天津大学 | The method for improving vanadium dioxide film visible light transmittance is etched using dilute sulfuric acid |
CN109487338A (en) * | 2018-12-24 | 2019-03-19 | 东华大学 | A kind of preparation method of monocrystalline vanadium dioxide film |
CN110331366A (en) * | 2019-07-31 | 2019-10-15 | 武汉理工大学 | A kind of preparation method of hypovanadic oxide-based composite film |
CN114059032A (en) * | 2021-11-18 | 2022-02-18 | 吉林大学 | Preparation method of vanadium dioxide film |
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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CN109182974A (en) * | 2018-10-09 | 2019-01-11 | 天津大学 | A method of vanadium oxide film is prepared by two one-step rapid thermal anneals |
CN109402581A (en) * | 2018-10-17 | 2019-03-01 | 天津大学 | The method for improving vanadium dioxide film visible light transmittance is etched using dilute sulfuric acid |
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CN114059032A (en) * | 2021-11-18 | 2022-02-18 | 吉林大学 | Preparation method of vanadium dioxide film |
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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Application publication date: 20180619 |