CN109336045A - A kind of dynamic quickly regulates and controls the flexible device and its preparation method and application of infrared light transmittance - Google Patents
A kind of dynamic quickly regulates and controls the flexible device and its preparation method and application of infrared light transmittance Download PDFInfo
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- CN109336045A CN109336045A CN201811150903.2A CN201811150903A CN109336045A CN 109336045 A CN109336045 A CN 109336045A CN 201811150903 A CN201811150903 A CN 201811150903A CN 109336045 A CN109336045 A CN 109336045A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
- B81B3/00—Devices comprising flexible or deformable elements, e.g. comprising elastic tongues or membranes
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- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
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- B81C1/00349—Creating layers of material on a substrate
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- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00388—Etch mask forming
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- G—PHYSICS
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- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
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Abstract
The present invention relates to the flexible devices and its preparation method and application that a kind of dynamic quickly regulates and controls infrared light transmittance, belong to flexible device preparation technical field.Flexible device of the invention successively includes flexible substrate layer, phase-change material layers, graphene heating layer from bottom to up, wherein: the phase-change material is vanadium dioxide@polyurethane laminated film, two end electrodes are additionally provided between the phase-change material layers and graphene heating layer, two end electrodes are for being biased heating graphene；The graphene is laminated graphene, and the flexible substrate is polyethylene terephthalate (PET) film.Using graphene as heating layer, the MIT behavior of vanadium dioxide is creatively regulated and controled by graphene heating layer indirectly by the present invention, realizes the dynamic regulation to infrared light transmittance, flexible device fast response time produced by the present invention, response device time TOFFAnd TONMost short is respectively 5S and 2S, can be applied to preparation smart window product.
Description
Technical field
The invention belongs to flexible device preparation technical fields, and in particular to a kind of dynamic quickly regulates and controls infrared light transmittance
Flexible device and its preparation method and application.
Background technique
Global warming is the problem of whole mankind faces jointly.People explore new effective ways constantly to reduce weather
Variation endangers mankind's bring.The update of energy technology is getting faster, also closely coupled with expanding economy.Currently,
The effective solution method that people explore first is that energy conservation project.
Vanadium dioxide (VO2) it is a kind of excellent phase-change material, phase transition temperature is 68 DEG C, the variation of phase transformation front-end geometry
Lead to the reversible transition to infrared light from transmission to reflection, people are applied to according to this characteristic prepares intelligent temperature control film
Field.Due to its excellent electrology characteristic, which also can be applied to electronic device.
Vanadium dioxide structure is numerous, and M phase therein contains M1Phase and M2Two kinds of structures of phase, under normal circumstances not outer
Under the interference effect of bound pair vanadium dioxide, that vanadium dioxide is presented is the M in M phase at room temperature1Structure, M2Phase structure is
Due to caused by extraneous perturbation.
Graphene is one of highest material of known strength, while also having good toughness, and can be bent, graphene
Theoretical Young's modulus reach 1.0TPa, intrinsic tensile strength be 130GPa.And utilize the reduced graphene of hydrogen plasma modification
Also there is very high intensity, average modulus can be greater than 0.25TPa.On the other hand, graphene has that resistivity is low, saturation current
High, thermal coefficient height, unit area heating power is high, conducts heat the features such as fast, fever is uniform.Therefore, graphene is very suitable to answer
For heating film field.Based on this, the present invention selects heating layer of the graphene as infrared regulation device.
Microwave-hydrothermal method using microwave as heating tool, realizes the stirring on molecular level, overcomes conventional hydrothermal kettle
Heat non-uniform disadvantage, shorten the reaction time, improve working efficiency, have fast heating speed, homogeneous heating, without temperature gradient,
The advantages that without hysteresis effect.
PET film also known as high temperature resistance polyester film.It has excellent physical property, chemical property and dimensional stability, thoroughly
Bright property, recuperability can be widely applied to magnetic recording, photosensitive material, electronics, electric insulation, industrial film, package decoration, screen
The fields such as curtain protection, the protection of optical grade specular surface.
The present invention devises graphene/vanadium dioxide@polyurethane/PET device, is synthetically prepared dioxy using microwave-hydrothermal method
Change vanadium powder, graphene heating film controls the temperature of vanadium dioxide to realize the dynamic regulation to infrared light transmittance.Simultaneously
The present invention uses flexible substrate, is prepared for flexible device, extends the application range of the device.Device junction proposed by the invention
Structure is simple, low in cost, and manufacture craft is simple, and response device speed is fast, performance is stablized, and can be directly used for the product of smart window
Metaplasia produces.
Summary of the invention
The purpose of the present invention is to provide flexible device and its preparation sides that a kind of dynamic quickly regulates and controls infrared light transmittance
Method and application.The present invention is directed to generate heat to regulating and controlling M by laminated graphene1Phase VO2Metal-insulator phase transition (MIT) behavior,
Realize the dynamic regulation to infrared light transmittance.
In order to realize above-mentioned first purpose of the invention, the present invention adopts the following technical scheme:
A kind of dynamic quickly regulates and controls the flexible device of infrared light transmittance, and the device successively includes flexible liner from bottom to up
Bottom, phase-change material layers, graphene heating layer, in which: the phase-change material is vanadium dioxide@polyurethane laminated film, described
Two end electrodes are additionally provided between phase-change material layers and graphene heating layer, two end electrodes are for being biased heating graphene.
Further, above-mentioned technical proposal, the graphene are laminated graphene.
Further, above-mentioned technical proposal, the flexible substrate are polyethylene terephthalate (PET) film.
Another object of the present invention is to provide dynamics described above quickly to regulate and control the flexible device of infrared light transmittance
Preparation method, described method includes following steps:
(1) by M1Phase hypovanadic oxide (VO2) powder is added in appropriate dehydrated alcohol, be ultrasonically treated it is evenly dispersed after, then plus
Enter polyvinylpyrrolidone (PVP), stirring, centrifugation, washing, vacuum drying obtain modified M1Phase VO2Powder；
(2) the modification M for obtaining step (1)1Phase VO2Powder is distributed in acetone solvent, adds thermoplastic polyurethane
(TPU), after being dispersed with stirring uniformly, M is obtained1Phase VO2Suspension；
(3) dip coating method is utilized, polyethylene terephthalate (PET) substrate is infiltrated to step (2) and is obtained
M1Phase VO20.5~1h in suspension, the pull rate for controlling coating machine is 2~6cm/min, obtains VO2@TPU/PET is compound
Film；
(4) by VO made from step (3)2@TPU/PET laminated film is placed on mask plate, is placed in vacuum coating equipment, is opened
It opens vacuum pump to vacuumize, is lower than 10 to vacuum degree-4When Pa, heating Al particle prepares bar shaped Al electrode at laminated film both ends；
(5) it is shifted by wet process and laminated graphene is transferred to laminated film and electrode surface, obtained of the present invention
Dynamic regulation infrared light transmittance flexible device.
Further, the mass ratio of above-mentioned technical proposal, step (1) polyvinylpyrrolidone and vanadium dioxide is 3
~8:100.
Further, the mass ratio of above-mentioned technical proposal, step (2) thermoplastic polyurethane and vanadium dioxide be 40~
80:100.
Further, above-mentioned technical proposal, step (1) described M1Phase VO2Powder is with vanadic anhydride, and oxalic acid is raw material,
A phase hypovanadic oxide powder is first prepared using microwave-hydrothermal method, then by A phase hypovanadic oxide powder in argon atmosphere
It is made annealing treatment, obtains the M1Phase hypovanadic oxide powder.
Third object of the present invention is to provide the application of flexible device made from method described above, gained flexibility device
Part can be used for preparing smart window product.
The principle of the present invention is as follows:
The invention firstly uses microwave-hydrothermal methods to be synthetically prepared vanadium dioxide powder, then changes vanadium dioxide powder
Property, the flexible vanadium dioxide@polyurethane laminated film using PET as substrate is prepared by dip coating, then in laminated film table
Aluminium electrode is deposited in face both ends, and laminated graphene is finally transferred to laminated film surface, and graphene/titanium dioxide has been prepared in design
Vanadium@polyurethane/PET device.
The present invention is biased by the two end electrodes to device, and graphene film generates Joule heat, and heat is conducted to two
Vanadium oxide composite film causes the phase transformation of vanadium dioxide；The present invention can also control THIN COMPOSITE by adjusting the size being biased
The MIT transformation behavior of vanadium dioxide film in film, to realize the dynamic regulation to infrared light transmittance；In addition, device of the present invention
The good light permeability and thermal conductivity of graphene can also be used under conditions of not being biased in part, assists heating side by other
Heat is directly conducted to vanadium dioxide laminated film by formula (such as sunlight irradiation, hot environment etc.), and it is thin to cause vanadium dioxide
The transformation behavior of film, equally achievable regulation of the device to infrared light transmittance.
Compared with prior art, a kind of dynamic of the present invention quickly regulate and control infrared light transmittance flexible device and its
Preparation method and application have the following beneficial effects:
(1) present invention regulates and controls dioxy by graphene heating layer creatively using graphene as heating layer indirectly
Change the MIT behavior of vanadium, realizes the dynamic regulation to infrared light transmittance, flexible device fast response time produced by the present invention, device
Part response time TOFFAnd TONMost short is respectively 5S and 2S；
(2) currently available technology generallys use pulse laser deposition (PLD) method, prepared by magnetron sputtering (Sputter) method
What vanadium dioxide smart window was all made of is sapphire as substrate material, and the substrate material and vanadium dioxide stickiness are poor, shadow
Ring heat conduction efficiency.And the present invention uses PET as flexible substrate, vanadium dioxide laminated film has preferable in pet sheet face
Adhesiveness, therefore the device heat conduction efficiency of dynamic regulation infrared light transmittance produced by the present invention is high, moreover, prepared is soft
Property device can widen the application range of vanadium dioxide smart window；
(3) present invention prepares vanadium dioxide powder using microwave-hydrothermal method, can significantly shorten the reaction time, improves system
Standby production efficiency.
Detailed description of the invention
Fig. 1 is the structural schematic diagram for the flexible device that dynamic of the invention quickly regulates and controls infrared light transmittance；
Fig. 2 is the infrared light modulation effect comparison diagram of flexible device made from the embodiment of the present invention 1~3；
Fig. 3 is the speed of response figure of flexible device made from the embodiment of the present invention 1；
Fig. 4 is the speed of response figure of flexible device made from the embodiment of the present invention 2；
Fig. 5 is the speed of response figure of flexible device made from the embodiment of the present invention 3；
Fig. 6 is the process flow chart that four layer laminate graphene wet processes shift in the embodiment of the present invention 1.
Specific embodiment
It elaborates below to case study on implementation of the invention.The implementation case under the premise of technical solution of the present invention into
Row is implemented, and the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to following realities
Apply case.
The information for including according to the application, to those skilled in the art can be easily to essence of the invention
Really description carries out various changes, without departing from spirit and scope of the appended claims.It should be understood that the scope of the present invention is not
Process, property defined by being confined to or component, because these embodiments and other descriptions are just for the sake of schematic
Illustrate certain aspects of the present disclosure.In fact, this field or those skilled in the relevant art obviously can be to embodiment party of the present invention
The various changes that formula is made all cover within the scope of the appended claims.
It is not intended to limit the scope of the invention for a better understanding of the present invention, expression dosage used in this application,
All numbers of percentage and other numerical value, are understood to be modified with word " about " in all cases.Therefore,
Unless stated otherwise, otherwise digital parameters listed in specification and appended book are all approximations, may
It can be changed according to the difference for the desirable properties for attempting to obtain.Each digital parameters at least should be considered as according to being reported
Effective digital and obtained by the conventional method of rounding up.
M involved in the following each embodiments of the present invention1Phase hypovanadic oxide powder is all made of following methods and is prepared, described
Method includes the following steps:
(i) 0.182g vanadium pentoxide powder is weighed, is dissolved in 40mL 0.15M oxalic acid solution, is stirred at 70 DEG C
30min obtains blue-tinted transparent solution.
(ii) step (i) acquired solution is transferred in PPL (polyparaphenylene phenol) reaction kettle that volume is 100mL, is used
Microwave-hydrothermal method, in 800W power, synthetic reaction 4h at 5MPa pressure and 240 DEG C, reaction product obtains black after centrifuge washing
Color VO2(A) powder；
(iii) VO for obtaining step (ii)2(A) black powder is placed in alumina ceramic crucible, and horizontal true
It is made annealing treatment in empty tube furnace (GSL-1600x), annealing conditions: 500 DEG C, argon atmosphere (pressure is maintained at 0.03MPa),
60min is kept the temperature, M is obtained1Phase VO2Powder.
Embodiment 1
A kind of dynamic of the present embodiment quickly regulates and controls the flexible device of infrared light transmittance, and the device is from bottom to up successively
Including flexible substrate layer, phase-change material layers, graphene heating layer, in which: the phase-change material is that vanadium dioxide@polyurethane is compound
Film, is additionally provided with two end electrodes between the phase-change material layers and graphene heating layer, two end electrodes add for being biased
Hot graphene；The graphene is four layer laminate graphenes；The flexible substrate is polyethylene terephthalate (PET)
Film.
The present embodiment flexible device described above is prepared with the following method, includes the following steps:
(1) by 0.1g M1Phase VO2Powder is added in 30ml dehydrated alcohol, then ultrasonic treatment dispersion 30min is weighed
0.003g polyvinylpyrrolidone (PVP) is dispersed in above-mentioned dispersion liquid, mechanical stirring 5h, and centrifugation is washed with deionized 2
It is secondary, it is dried in vacuo under the conditions of 60 DEG C, obtains modified M1Phase VO2Powder.
(2) by modified M made from step (1)1Phase VO2Powder is scattered in 10ml acetone, adds 0.04g thermoplastic poly
Urethane (TPU), mechanical stirring 1d obtain M1Phase VO2Suspension.
(3) dip coaterd is utilized, in the suspension that 2cm*2cm*100 μm of PET substrate infiltration is obtained to step (2)
40min, the pull rate for controlling coating machine is 2cm/min, obtains VO2@TPU/PET laminated film.
(4) laminated film is placed on mask plate, is placed in vacuum coating equipment, and opened vacuum pump and vacuumize, to vacuum
Degree is 10-4When Pa or less, deposit to obtain bar shaped Al electrode at laminated film both ends by heating Al particle.
(5) using wet process shift four layer laminate graphenes, be finally prepared dynamic of the present invention quickly regulate and control it is red
The Graphene/VO of outer light transmission rate2@TPU/PET flexible device.
Fig. 6 is shown in using the specific implementation process that wet process shifts four layer laminate graphenes in above-mentioned steps (5), specific steps are such as
Under:
(a) the copper-based single-layer graphene of four same sizes (13mm*10mm*4mm) is sheared, number is A, B, C, D respectively；
(b) it coats polymethyl methacrylate (PMMA): being revolved on copper-based single-layer graphene (sample A) surface that number is A
Tu PMMA；
(c) it heating: thering is the sample A of PMMA to heat spin coating under air atmosphere, control heating temperature is 100~150 DEG C,
Heating time is 10~15min, attaches PMMA closely with graphene layer, is cooled to room temperature after heating；
(d) it polishes: the back side sample A of slightly being polished with sand paper；
(e) remove copper: by sample A be polished one down, be placed in the iron nitrate solution of 0.7M, control etching temperature be
40~60 DEG C, completely remove Cu；
(f) it cleans: with the PMMA/ graphene film obtained after deionized water etching 3 times to 5 times；
(g) it shifts: with numbering the copper-based single-layer graphene (backside of substrate has been polished with sand paper) for being B for PMMA/ graphene
Film is gently hauled out, and is picked up；
(h) dry: to be air-dried at room temperature；
(i) it coats PMMA: revolving Tu PMMA again on laminated graphene surface, control heating temperature is 100~150 DEG C, is added
The hot time is 10~15min, is cooled to room temperature after heating；
(j) it repeats step (b) and arrives step (h), be repeated 2 times, obtain the laminated graphene using D as bottom；
(k) it coats PMMA: revolving Tu PMMA by the laminated graphene surface of bottom of D；
(l) heat: control heating temperature is 100~150 DEG C, and heating time is 10~15min, is cooled to after heating
Room temperature；
(m) it polishes: sample D backside of substrate of slightly being polished with sand paper；
(n) remove copper: by sample D be polished one down, be placed in the iron nitrate solution of 0.7M, control etching temperature be
40~60 DEG C, completely remove Cu；
(o) it cleans: being cleaned 3 times to 5 times with deionized water.
(p) it shifts: laminated graphene gently being hauled out with the film that the present embodiment step (4) obtains, is picked up；
(q) dry: to be air-dried at room temperature；
(r) it heats: being heated after Tu PMMA is revolved on laminated graphene surface, control heating temperature is 100~150 DEG C, heating
Time is 10~15min, makes graphene film and target substrate tight adhesion, sample is naturally cooled to room after heating
Temperature reuses acetone soln and carries out slightly rinsing 3 to 5 removals residual PMMA to PMMA, dry under 40~50 DEG C of vacuum conditions
10~15min is successfully prepared the flexible device for quickly regulating and controlling infrared light transmittance with the dynamic that graphene makees functional layer.
Apply the voltage of 14V between the device electrode made from the present embodiment, the results showed that the device is to 2500nm wavelength
Infrared light transmittance modulation effect reaches 3%.Response device time TOFFAnd TONRespectively 15S and 10S, specific test result ginseng
See Fig. 2 and Fig. 3.
Embodiment 2
A kind of dynamic of the present embodiment quickly regulates and controls the flexible device of infrared light transmittance, and the device is from bottom to up successively
Including flexible substrate layer, phase-change material layers, graphene heating layer, in which: the phase-change material is that vanadium dioxide@polyurethane is compound
Film, is additionally provided with two end electrodes between the phase-change material layers and graphene heating layer, two end electrodes add for being biased
Hot graphene；The graphene is four layer laminate graphenes；The flexible substrate is polyethylene terephthalate (PET)
Film.
The present embodiment flexible device described above is prepared with the following method, includes the following steps:
(1) by 0.1g M1Phase VO2Powder is added in 30ml dehydrated alcohol, then ultrasonic treatment dispersion 30min is weighed
0.005g polyvinylpyrrolidone (PVP) is dispersed in above-mentioned dispersion liquid, mechanical stirring 5h, and centrifugation is washed with deionized 2
It is secondary, it is dried in vacuo under the conditions of 60 DEG C, obtains modified M1Phase VO2Powder.
(2) by modified M made from step (1)1Phase VO2Powder is scattered in 10ml acetone, adds 0.06g thermoplastic poly
Urethane (TPU), mechanical stirring 1d obtain M1Phase VO2Suspension.
(3) dip coaterd is utilized, in the suspension that 2cm*2cm*100 μm of PET substrate infiltration is obtained to step (2)
60min, the pull rate for controlling coating machine is 3cm/min, obtains VO2@TPU/PET laminated film.
(4) laminated film is placed on mask plate, is placed in vacuum coating equipment, and opened vacuum pump and vacuumize, to vacuum
Degree is 10-4When Pa or less, deposit to obtain bar shaped Al electrode at laminated film both ends by heating Al particle.
(5) four layer laminate graphenes are shifted using the identical method of embodiment 1, be finally prepared of the present invention dynamic
State quickly regulates and controls the Graphene/VO of infrared light transmittance2@TPU/PET flexible device.
Apply the voltage of 18V between the device electrode made from the present embodiment, the results showed that the device is to 2500nm wavelength
Infrared light transmittance modulation effect reaches 18%.Response device time TOFFAnd TONRespectively 5S and 3S, test result are shown in figure respectively
2 and Fig. 4.
Embodiment 3
A kind of dynamic of the present embodiment quickly regulates and controls the flexible device of infrared light transmittance, and the device is from bottom to up successively
Including flexible substrate layer, phase-change material layers, graphene heating layer, in which: the phase-change material is that vanadium dioxide@polyurethane is compound
Film, is additionally provided with two end electrodes between the phase-change material layers and graphene heating layer, two end electrodes add for being biased
Hot graphene；The graphene is four layer laminate graphenes；The flexible substrate is polyethylene terephthalate (PET)
Film.
The present embodiment flexible device described above is prepared with the following method, includes the following steps:
(1) by 0.1g M1Phase VO2Powder is added in 30ml dehydrated alcohol, then ultrasonic treatment dispersion 30min is weighed
0.008g polyvinylpyrrolidone (PVP) is dispersed in above-mentioned dispersion liquid, mechanical stirring 5h, and centrifugation is washed with deionized 2
It is secondary, it is dried in vacuo under the conditions of 60 DEG C, obtains modified M1Phase VO2Powder.
(2) by modified M made from step (1)1Phase VO2Powder is scattered in 40ml acetone, adds 0.08g thermoplastic poly
Urethane (TPU), mechanical stirring 1d obtain M1Phase VO2Suspension.
(3) dip coaterd is utilized, in the suspension that 2cm*2cm*100 μm of PET substrate infiltration is obtained to step (2)
35min, the pull rate for controlling coating machine is 5cm/min, obtains VO2@TPU/PET laminated film.
(4) laminated film is placed on mask plate, is placed in vacuum coating equipment, and opened vacuum pump and vacuumize, to vacuum
Degree is 10-4When Pa or less, deposit to obtain bar shaped Al electrode at laminated film both ends by heating Al particle.
(5) four layer laminate graphenes are shifted using using the identical method of embodiment 1, be finally prepared of the present invention
Dynamic quickly regulate and control the Graphene/VO of infrared light transmittance2@TPU/PET flexible device.
Apply the voltage of 21V between the device electrode made from the present embodiment, the results showed that the device is to 2500nm wavelength
Infrared light transmittance modulation effect reaches 29%.Response device time TOFFAnd TONRespectively 5S and 2S, test result are shown in figure respectively
2 and Fig. 5.
Embodiment 4
A kind of dynamic of the present embodiment quickly regulates and controls the flexible device of infrared light transmittance, and the device is from bottom to up successively
Including flexible substrate layer, phase-change material layers, graphene heating layer, in which: the phase-change material is that vanadium dioxide@polyurethane is compound
Film, is additionally provided with two end electrodes between the phase-change material layers and graphene heating layer, two end electrodes add for being biased
Hot graphene；The graphene is three layer laminate graphenes；The flexible substrate is polyethylene terephthalate (PET)
Film.
The present embodiment flexible device described above is prepared with the following method, includes the following steps:
(1) by 0.1g M1Phase VO2Powder is added in 30ml dehydrated alcohol, then ultrasonic treatment dispersion 30min is weighed
0.004g polyvinylpyrrolidone (PVP) is dispersed in above-mentioned dispersion liquid, mechanical stirring 5h, and centrifugation is washed with deionized 2
It is secondary, it is dried in vacuo under the conditions of 60 DEG C, obtains modified M1Phase VO2Powder.
(2) by modified M made from step (1)1Phase VO2Powder is scattered in 20ml acetone, adds 0.05g thermoplastic poly
Urethane (TPU), mechanical stirring 1d obtain M1Phase VO2Suspension.
(3) dip coaterd is utilized, in the suspension that 2cm*2cm*100 μm of PET substrate infiltration is obtained to step (2)
30min, the pull rate for controlling coating machine is 6cm/min, obtains VO2@TPU/PET laminated film.
(4) laminated film is placed on mask plate, is placed in vacuum coating equipment, and opened vacuum pump and vacuumize, to vacuum
Degree is 10-4When Pa or less, deposit to obtain bar shaped Al electrode at laminated film both ends by heating Al particle.
(5) three layer laminate graphenes are shifted using using the identical method of embodiment 1, be finally prepared of the present invention
Dynamic quickly regulate and control the Graphene/VO of infrared light transmittance2@TPU/PET flexible device.
Apply the voltage of 21V between the device electrode made from the present embodiment, the results showed that the device is to 2500nm wavelength
Infrared light transmittance modulation effect reaches 23%.Response device time TOFFAnd TONRespectively 5S and 3S.
Embodiment 5
A kind of dynamic of the present embodiment quickly regulates and controls the flexible device of infrared light transmittance, and the device is from bottom to up successively
Including flexible substrate layer, phase-change material layers, graphene heating layer, in which: the phase-change material is that vanadium dioxide@polyurethane is compound
Film, is additionally provided with two end electrodes between the phase-change material layers and graphene heating layer, two end electrodes add for being biased
Hot graphene；The graphene is five layer laminate graphenes；The flexible substrate is polyethylene terephthalate (PET)
Film.
The present embodiment flexible device described above is prepared with the following method, includes the following steps:
(1) by 0.1g M1Phase VO2Powder is added in 40ml dehydrated alcohol, then ultrasonic treatment dispersion 35min is weighed
0.007g polyvinylpyrrolidone (PVP) is dispersed in above-mentioned dispersion liquid, mechanical stirring 4h, and centrifugation is washed with deionized 2
It is secondary, it is dried in vacuo under the conditions of 60 DEG C, obtains modified M1Phase VO2Powder.
(2) by modified M made from step (1)1Phase VO2Powder is scattered in 20ml acetone, adds 0.05g thermoplastic poly
Urethane (TPU), mechanical stirring 1d obtain M1Phase VO2Suspension.
(3) dip coaterd is utilized, in the suspension that 2cm*2cm*100 μm of PET substrate infiltration is obtained to step (2)
45min, the pull rate for controlling coating machine is 4cm/min, obtains VO2@TPU/PET laminated film.
(4) laminated film is placed on mask plate, is placed in vacuum coating equipment, and opened vacuum pump and vacuumize, to vacuum
Degree is 10-4When Pa or less, deposit to obtain bar shaped Al electrode at laminated film both ends by heating Al particle.
(5) five layer laminate graphenes are shifted using using the identical method of embodiment 1, be finally prepared of the present invention
Dynamic quickly regulate and control the Graphene/VO of infrared light transmittance2@TPU/PET flexible device.
Apply the voltage of 21V between the device electrode made from the present embodiment, the results showed that the device is to 2500nm wavelength
Infrared light transmittance modulation effect reaches 25%.Response device time TOFFAnd TONRespectively 5S and 2S.
Embodiment 6
A kind of dynamic of the present embodiment quickly regulates and controls the flexible device of infrared light transmittance, and the device is from bottom to up successively
Including flexible substrate layer, phase-change material layers, graphene heating layer, in which: the phase-change material is that vanadium dioxide@polyurethane is compound
Film, is additionally provided with two end electrodes between the phase-change material layers and graphene heating layer, two end electrodes add for being biased
Hot graphene；The graphene is four layer laminate graphenes；The flexible substrate is polyethylene terephthalate (PET)
Film.
The present embodiment flexible device described above is prepared with the following method, includes the following steps:
(1) by 0.1g M1Phase VO2Powder is added in 40ml dehydrated alcohol, then ultrasonic treatment dispersion 35min is weighed
0.003g polyvinylpyrrolidone (PVP) is dispersed in above-mentioned dispersion liquid, mechanical stirring 4h, and centrifugation is washed with deionized 2
It is secondary, it is dried in vacuo under the conditions of 60 DEG C, obtains modified M1Phase VO2Powder.
(2) by modified M made from step (1)1Phase VO2Powder is scattered in 20ml acetone, adds 0.04g thermoplastic poly
Urethane (TPU), mechanical stirring 1d obtain M1Phase VO2Suspension.
(3) dip coaterd is utilized, in the suspension that 2cm*2cm*100 μm of PET substrate infiltration is obtained to step (2)
45min, the pull rate for controlling coating machine is 4cm/min, obtains VO2@TPU/PET laminated film.
(4) laminated film is placed on mask plate, is placed in vacuum coating equipment, and opened vacuum pump and vacuumize, to vacuum
Degree is 10-4When Pa or less, deposit to obtain bar shaped Al electrode at laminated film both ends by heating Al particle.
(5) four layer laminate graphenes are shifted using using the identical method of embodiment 1, be finally prepared of the present invention
Dynamic quickly regulate and control the Graphene/VO of infrared light transmittance2@TPU/PET flexible device.
Device made from the present embodiment is placed on miniature warm table, is heated to 90 DEG C from room temperature, the results showed that the device
29% is reached to 2500nm IR wavelengths transmitance modulation effect.
Claims (8)
1. the flexible device that a kind of dynamic quickly regulates and controls infrared light transmittance, it is characterised in that: the device is from bottom to up successively
Including flexible substrate layer, phase-change material layers, graphene heating layer, in which: the phase-change material is that vanadium dioxide@polyurethane is compound
Film, is additionally provided with two end electrodes between the phase-change material layers and graphene heating layer, two end electrodes add for being biased
Hot graphene.
2. the flexible device that dynamic according to claim 1 quickly regulates and controls infrared light transmittance, it is characterised in that: the stone
Black alkene is laminated graphene.
3. the flexible device that dynamic according to claim 2 quickly regulates and controls infrared light transmittance, it is characterised in that: described soft
Property substrate be polyethylene terephtalate film.
4. the preparation method that dynamic as claimed in claim 3 quickly regulates and controls the flexible device of infrared light transmittance, it is characterised in that:
Described method includes following steps:
(1) by M1Phase hypovanadic oxide VO2Powder is added in appropriate dehydrated alcohol, after ultrasonic treatment is evenly dispersed, adds poly- second
Alkene pyrrolidone PVP, stirring, centrifugation, washing, vacuum drying, obtains modified M1Phase VO2Powder；
(2) the modification M for obtaining step (1)1Phase VO2Powder is distributed in acetone solvent, is added thermoplastic polyurethane TPU, is stirred
It mixes after being uniformly dispersed, obtains M1Phase VO2Suspension；
(3) dip coating method is utilized, polyethylene terephtalate substrate is infiltrated to the M obtained to step (2)1Phase
VO20.5~1h in suspension, the pull rate for controlling coating machine is 2~6cm/min, obtains VO2@TPU/PET laminated film；
(4) by VO made from step (3)2@TPU/PET laminated film is placed on mask plate, is placed in vacuum coating equipment, is opened true
Empty pumping vacuum is lower than 10 to vacuum degree-4When Pa, heating Al particle prepares bar shaped Al electrode at laminated film both ends；
(5) it is shifted by wet process and laminated graphene is transferred to laminated film and electrode surface, obtained of the present invention dynamic
The flexible device of state regulation infrared light transmittance.
5. the preparation method of flexible device according to claim 4, it is characterised in that: step (1) described polyvinyl pyrrole
The mass ratio of alkanone and vanadium dioxide is 3~8:100.
6. the preparation method of flexible device according to claim 4, it is characterised in that: step (2) the thermoplastic poly ammonia
The mass ratio of ester and vanadium dioxide is 40~80:100.
7. the preparation method of flexible device according to claim 4, it is characterised in that: step (1) described M1Phase VO2Powder
It is with vanadic anhydride, oxalic acid is raw material, A phase hypovanadic oxide powder is first prepared using microwave-hydrothermal method, then by A phase two
Vanadium oxide powder is made annealing treatment in argon atmosphere, obtains the M1Phase hypovanadic oxide powder.
8. flexible device the answering in preparation smart window product that dynamic described in claim 1 quickly regulates and controls infrared light transmittance
With.
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