CN106756840A - A kind of high-temperature flexible transparent conductive film and preparation method and application - Google Patents
A kind of high-temperature flexible transparent conductive film and preparation method and application Download PDFInfo
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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
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- 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
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- 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
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- 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
- C23C14/08—Oxides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/083—Oxides of refractory metals or yttrium
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
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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
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
Abstract
The invention discloses a kind of high-temperature flexible transparent conductive film and preparation method and application, the high-temperature flexible transparent conductive film, including：High-temperature flexible transparent substrates, and it is deposited on the transparency conducting layer in the high-temperature flexible transparent substrates.High-temperature flexible transparent conductive film of the present invention can high temperature resistant, thermal coefficient of expansion is low, surfacing, transparency are high, photoelectric properties are stable, and its manufacturing process is simple, with low cost.
Description
Technical field
The present invention relates to transparent conductive material technical field, more particularly to a kind of high-temperature flexible transparent conductive film and its
Preparation method and application.
Background technology
Transparent conductive material be it is a kind of can a kind of conductive material with high transmittance in visible-range again.It is transparent
Conductive material has a wide range of applications as a kind of important functional material in optical electrical son industry, and it can be used as FPD
The transparency electrode of device and solar cell；The antifrost antifogging of visible observation is done in terms of automobile, aircraft, freezer and instrument and meter
Film；Using its good electromagnetic shielding action, for computer floor, radar shielding protection etc..What is prepared on hard glass is saturating
Bright conductive material has reached preparation and application level higher.Although the transparent conductive material prepared on organic flexible matrix has
It is flexible, lightweight, portable, be easy to large area production etc. particular advantages, but due to the narrower original of its operating temperature range
Cause, result in the limitation of its application.So, the present invention proposes the system of high-temperature flexible transparent conductive film on this basis
Standby technology, it is provided simultaneously with the advantage and resistant to elevated temperatures feature of organic flexible matrix, is expected to developing transparent conductive film in high temperature
The application in Technology of Flexibility field.
ITO, AZO and sandwich structure that in common organic flexible substrate prepared by (PET, PI etc.)（oxide/
metal/oxide, OMO）Deng transparent conductive material electric conductivity and translucency preferably, but have can not for organic flexible base material
The defect for overcoming：Adhesion between non-refractory, substrate and material is poor and linear heat of between base material and conductive layer is swollen
Swollen coefficient has very big difference.Patent " possesses preparation method of flexible transparent conductive film of high thermal stability and products thereof "
By the use of the fluorine-containing polyimide film layer after solidification as substrate, there is certain heat-resisting quantity, but technique used is complex, prepares
Difficulty is higher.Although glass and metal foil can overcome the above defect, the former belongs to hard material, bending radius compared with
Greatly, the latter's translucency is poor.Therefore, technically just in the urgent need to developing a kind of novel fire resistant, low thermal coefficient of expansion, rough surface
Spend small, transparency flexible conductive substrates material high.
The content of the invention
In view of above-mentioned the deficiencies in the prior art, it is an object of the invention to provide a kind of high-temperature flexible transparent conductive film
And preparation method and application, so as to solve that existing flexible and transparent conductive material non-refractory, thermal coefficient of expansion be high, surface is thick
The problem that rugosity is big, transparency is low.
Technical scheme is as follows：
A kind of high-temperature flexible transparent conductive film, including：High-temperature flexible transparent substrates, and it is deposited on the high-temperature flexible
Transparency conducting layer in transparent substrates.
Described high-temperature flexible transparent conductive film, wherein, the high-temperature flexible transparent substrates are mica sheet（Comprising
Muscovite, Fluororystal mica）.
Described high-temperature flexible transparent conductive film, wherein, the transparency conducting layer is transparent conductive material, described
Bright conductive material includes SnO2Film, Sb2O3Film, ZnO film, CdO films, ito thin film, AZO films, FTO films, NTO are thin
Film, Sandwich film, nano-silver thread, Graphene, metal grill, CNT.
Described high-temperature flexible transparent conductive film, wherein, the thickness of the high-temperature flexible transparent substrates is 4 ~ 100
µm。
Described high-temperature flexible transparent conductive film, wherein, the thickness of the transparency conducting layer is 25 ~ 500 nm.
A kind of preparation method of high-temperature flexible transparent conductive film as described above, including step：
A, by target be arranged on magnetic control sputtering device radio frequency cathode target groove in, high-temperature flexible transparent substrates are put into substrate
Frame, in the media disk in substrate frame insertion sputtering chamber, adjustment the distance between target and substrate are 40 ~ 80 mm；
B, to sputtering chamber be evacuated, make sputtering chamber vacuum be less than 1.0 × 10-3After Pa, to argon gas is filled with sputtering chamber, adjust
Rate of air sucked in required, the gas pressure intensity for making sputtering chamber is 0.1 ~ 5 Pa；
C, the radio-frequency power supply for opening target, target correspondence position sputtering sedimentation transparency conducting layer is gone to by substrate, obtains high temperature resistant
Flexible transparent conductive film.
The preparation method of another high-temperature flexible transparent conductive film as described above, including step：
A, by target be arranged on pulse laser deposition apptss chamber in, adjustment target-substrate distance be 40 ~ 80 mm；Then it is high temperature resistant is soft
Property transparent substrates are fixed on substrate holder, are attached in chamber, then cavity is vacuumized, make vacuum in chamber be maintained at 5 ×
10-5 Pa ~5×10-4Between Pa；
B, light path is adjusted, starts excimer laser, made on the target in laser beam focus to chamber, deposit transparency conducting layer,
Obtain conductive film base material；
C, the conductive film base material for obtaining step B are annealed, and obtain high-temperature flexible transparent conductive film.
Described high-temperature flexible transparent conductive film method, wherein, in the step C, to being passed through high purity oxygen gas in chamber,
Inflation and the rate of air sucked in required of oxygen are adjusted, the oxygen pressure in cavity is maintained at 5 × 10-4~5×101Pa, the conduction that step B is obtained
Film substrate is heated to 100 ~ 600 DEG C and carries out in-situ annealing, is incubated 20 ~ 40 min.
Described high-temperature flexible transparent conductive film method, wherein, in the step C, the conductive thin that step B is obtained
Film base material takes out, and is positioned in tube furnace, is annealed at 100 ~ 600 DEG C, is incubated 10 ~ 60 min.
A kind of application of high-temperature flexible transparent conductive film, should by above-described high-temperature flexible transparent conductive film
In for photoelectric device, as the matrix or the electricity of flexible perovskite solar cell of high-temperature flexible transparent membrane heater
Pole material.
Beneficial effect：The invention provides a kind of high-temperature flexible transparent conductive film and preparation method and application, institute
High-temperature flexible transparent conductive film is stated, including：High-temperature flexible transparent substrates, and it is deposited on the transparent base of the high-temperature flexible
Transparency conducting layer on bottom.High-temperature flexible transparent conductive film of the present invention can high temperature resistant, thermal coefficient of expansion is low, surfacing,
Transparency is high, photoelectric properties are stable, and its manufacturing process is simple, with low cost.
Brief description of the drawings
Fig. 1 is the general flow chart of high-temperature flexible transparent conductive film method specific implementation of the present invention.
Fig. 2 is the high-temperature flexible transparent membrane heater prepared using high-temperature flexible transparent membrane of the present invention
Structural representation.
Fig. 3 is the structural representation of the perovskite solar cell prepared using high-temperature flexible transparent membrane of the present invention
Figure.
Specific embodiment
The present invention provides a kind of high-temperature flexible transparent conductive film and preparation method and application, to make mesh of the invention
, technical scheme and effect it is clearer, clear and definite, the present invention is described in more detail below.It should be appreciated that described herein
Specific embodiment be only used to explain the present invention, be not intended to limit the present invention.
The present invention provides a kind of high-temperature flexible transparent conductive film, as shown in figure 1, including：The transparent base of high-temperature flexible
Bottom 1, and it is deposited on the transparency conducting layer 2 in the high-temperature flexible transparent substrates 1.
Further, in the embodiment of the present invention, the high-temperature flexible transparent substrates 1 are mica sheet（Mica）, comprising white
Mica, Fluororystal mica.Mica of the present invention is a kind of rock-forming mineral, and hexagonal form of flake crystal, with low cost, nothing is presented
It is malicious, free from environmental pollution.Mica sheet stratiform cleavage is very complete, and after carrying out splitting, there is glass on surface up to atomically flating
Gloss, thin slice has elasticity, and translucency is good.Mica sheet can high temperature resistant（600 DEG C of ＞）, translucency and flexible subtracting with thickness
Small and gradually increase, thermal coefficient of expansion is small, after substrate heating or annealing are carried out to it, its microstructure and photoelectric properties
Can get a promotion, surfacing, photoelectric properties stabilization（It is basically unchanged after mechanical bend for several times）, tied between substrate
Close firm.
Further, in the embodiment of the present invention, the transparency conducting layer 2 can be different transparent conductive materials, its bag
Include but be not limited to In, the oxide and its composite multi-component sull of Sb, Zn and Cd, such as SnO2Film（Tin ash is thin
Film）、Sb2O3Film（Antimony oxide film）, ZnO film（Zinc-oxide film）, CdO films（Cadmium oxide）, ito thin film
（Indium tin oxide films）, AZO films（Al-Doped ZnO film）, FTO films（The SnO of doping fluorine2Film）, NTO films（Nb mixes
Miscellaneous TiO2Film）；It also includes Sandwich film（OMO）, nano-silver thread, Graphene, metal grill, CNT
（CNTs）.
Wherein, the Graphene includes single-layer graphene and multi-layer graphene, and Sandwich film includes oxide half
The Sandwich film that conductor/metal/oxide semiconductor is constituted（Such as ITO/Ag/ITO）, oxide semiconductor/oxidation
The Sandwich film that thing semiconductor/oxide semiconductor is constituted（Such as ZAO/ITO/ZAO）.
Further, in the embodiment of the present invention, the thickness of the high-temperature flexible transparent substrates is 4 ~ 100 μm.
Further, in the embodiment of the present invention, the thickness of the transparency conducting layer is 25 ~ 500 nm；Preferably 100 nm.
Further, the deposition process that transparency conducting layer 2 is deposited in high-temperature flexible transparent substrates 1 is had various, is wrapped
Include：Pulsed laser deposition（PLD, L-MBE）, magnetron sputtering method, sol-gel process（Sol-gel）, chemical vapour deposition technique
（CVD）Deng.
The preparation method of the one of which high-temperature flexible transparent conductive film that the present invention is provided, it is in high-temperature flexible
High-temperature flexible transparent conductive film, including step are prepared using magnetron sputtering deposition method in transparent substrates：
S110, by target be arranged on magnetic control sputtering device radio frequency cathode target groove in, high-temperature flexible transparent substrates are put into base
Horse, in the media disk in substrate frame insertion sputtering chamber, adjustment the distance between target and substrate are 40 ~ 80 mm；
During specific implementation, can be by the oxide target material of purity 99.99wt% in the sputtering chamber of magnetic control sputtering device
In the radio frequency cathode target groove of individual water-cooled, the flexible and transparent substrate mica by thickness after stripping for 8-50 μm is put into substrate frame, base
In media disk in horse insertion sputtering chamber, adjustment the distance between target and substrate are 40-80 mm.
S210, to sputtering chamber be evacuated, make sputtering chamber vacuum be less than 1.0 × 10-3After Pa, to being filled with argon in sputtering chamber
Gas, adjusts rate of air sucked in required, and the gas pressure intensity for making sputtering chamber is 0.1 ~ 5 Pa；
During specific implementation, sputtering chamber and gas pipeline are evacuated, the base vacuum of sputtering chamber is less than 1.0 × 10-3Pa, backward
The argon gas that purity is 99.99% is filled with sputtering chamber, rate of air sucked in required is adjusted, the gas pressure intensity for making sputtering chamber is 0.1-5 Pa.
S310, the radio-frequency power supply for opening target, target correspondence position sputtering sedimentation transparency conducting layer is gone to by substrate, is obtained
High-temperature flexible transparent conductive film；
During specific implementation, the radio-frequency power supply of oxide target material is opened, after after radio frequency glow discharge stabilization, flexible substrates are turned into will target
Material correspondence position carries out sputtering sedimentation transparent conductive film, and the thickness in film deposition process is supervised by the thickness of observing and controlling sputter equipment
Control instrument monitor in real time.
The preparation method of another high-temperature flexible transparent conductive film that the present invention is provided, it is saturating in high-temperature flexible
High-temperature flexible transparent conductive film, including step are prepared using pulsed laser deposition in bright substrate：
S120, by target be arranged on pulse laser deposition apptss chamber in, adjustment target-substrate distance be 40 ~ 80 mm；Then by high temperature resistant
Flexible and transparent substrate is fixed on substrate holder, is attached in chamber, then cavity is vacuumized, and vacuum in chamber is maintained at 5
×10-5 Pa ~5×10-4Between Pa；
During specific implementation, the oxide target material of 99.99wt% can be arranged in the chamber of pulse laser deposition apptss, adjust target
Cardinal distance is 40-80 mm；Mica sheet is carried out into mechanical stripping, makes its thickness for 8-50 μm, be fixed on substrate holder, installed
To chamber；Cavity is vacuumized, the atmospheric pressure in chamber is maintained at 5 × 10-5 Pa ~5×10-4 Between Pa.
S220, light path is adjusted, start excimer laser, made on the target in laser beam focus to chamber, deposited transparent
Conductive layer, obtains conductive film base material；
During specific implementation, light path is adjusted, start excimer laser（Frequency is 2-10 Hz, and laser intensity is 200-300
mJ）, make on the target in laser beam focus to chamber, start to deposit transparency conducting layer, transparency conducting layer thickness is 25-500 nm.
S320, the conductive film base material for obtaining step B are annealed, and obtain high-temperature flexible transparent conductive film.
Further, in the step S320, the conductive film base material that step S220 is obtained annealed wherein one
Planting method for optimizing is：To high purity oxygen gas are passed through in chamber, inflation and the rate of air sucked in required of oxygen are adjusted, the oxygen pressure in cavity is maintained at 5
×10-4~5×101Pa, the conductive film base material that step B is obtained is heated to 100 ~ 600 DEG C and carries out in-situ annealing, and insulation 20 ~
40 min；
During specific implementation, high purity oxygen gas can be poured in backward chamber after deposition, adjust inflation and the rate of air sucked in required of oxygen, made
Oxygen pressure in cavity is maintained at 5 × 10-4~5×101Pa, substrate is heated, and temperature carries out in-situ annealing for 100-600 DEG C, is protected
The warm time is 30 min.
Further, in the step S320, the another kind that the conductive film base material that step S220 is obtained is annealed
Method for optimizing is：The conductive film base material that step S220 is obtained takes out, and is positioned in tube furnace, is annealed at 100 ~ 600 DEG C,
10 ~ 60 min of insulation；
During specific implementation, base material can be taken out after deposition, be placed on being annealed at 100-600 DEG C in tube furnace, insulation
Time is 10-60 min.
Further, can be 6 × 10 with vacuum in control chamber body as the preferred embodiment of the invention-5 Pa, target-substrate distance
Be 50 mm, annealing temperature is 500 DEG C, the high-temperature flexible transparent conductive film for obtaining, its square resistance be 10-800 Ω/
, visible ray average transmittance are higher than 80%, and material structure and photoelectric properties are stable, are firmly combined with base material.
Present invention also offers a kind of application of high-temperature flexible transparent conductive film, by above-described high-temperature flexible
Transparent conductive film is applied in photoelectric device, used as the matrix or flexible perovskite of high-temperature flexible transparent membrane heater
The electrode material of solar cell.
The present invention utilizes the resistant to elevated temperatures feature of high-temperature flexible transparent conductive film, solves conventional flex film heating
Device operating temperature range is narrower, and the relatively low problem of conventional flex perovskite solar cell photoelectric transformation efficiency, to reach
Its purpose applied in above two photoelectric device.
The good high-temperature flexible transparent conductive film of the photoelectric properties prepared using above preferred embodiment, very
It is adapted to prepare high-temperature flexible transparent membrane heater and flexible perovskite solar cell.It is thin with existing flexible and transparent
Film heater is compared, and the high-temperature flexible transparent membrane prepared using high-temperature flexible transparent conductive film of the present invention is heated
The operating temperature range of device（30~600℃）Have and significantly widen, while the thermal response time also greatly shortens；It is soft with existing
Property perovskite solar cell compare, using high-temperature flexible transparent conductive film of the present invention prepare flexible perovskite too
Positive energy battery, can use high temperature preparation technology, and electricity conversion be obviously improved.
High-temperature flexible transparent conductive film of the present invention is done in detail with the specific embodiment of different transparency conducting layers below
Explanation：
Embodiment 1：Transparency conducting layer is 100 nm ITO
It is 15 μm of mica sheet that high-temperature flexible transparent substrates use thickness, directly carries out mechanical stripping, is not required to cleaning；By purity
For the commodity ITO target of 99.99wt% is arranged in the chamber of impulse laser deposition system, it is bonded on substrate holder with double faced adhesive tape
（Normal temperature is deposited）, it is attached in chamber, adjustment target-substrate distance is 50 mm；Cavity is evacuated, the pressure in chamber is remained 1.0 × 10-4 Pa；Light path is adjusted, starts excimer laser, made on the target in laser beam focus to chamber, deposition is started at room temperature
Film, film thickness is 100 nm；After deposition, high purity oxygen gas, modulation inflation and rate of air sucked in required are filled with backward chamber, make cavity
Gas pressure intensity is 10 Pa, and base material is heated into temperature for 500 DEG C carry out in-situ annealing, and soaking time is 30 min；Treat that temperature drops
After room temperature, conductive film base material is taken out；The square resistance of resulting high-temperature flexible transparent conductive film be 80 Ω/,
Visible ray average transmittance is 86%.Membrane structure and photoelectric properties stabilization, are firmly combined with mica sheet substrate.
Embodiment 2：Transparency conducting layer is 200 nm ITO
Preparation technology is basic with described in case study on implementation 1, except that the ito thin film thickness of deposition is 200 nm.Resulting
The square resistance of high-temperature flexible transparent conductive film is 40 Ω/, visible ray average transmittance is 83%.Membrane structure and light
Electric performance stablity, is firmly combined with mica sheet substrate.
Embodiment 3：Transparency conducting layer is 50 nm ITO
Preparation technology is basic with described in case study on implementation 1, except that the ito thin film thickness of deposition is 50 nm.Resulting is resistance to
The square resistance of high temperature flexible transparent conductive film is 300 Ω/, visible ray average transmittance is 88%.Membrane structure and light
Electric performance stablity, is firmly combined with mica sheet substrate.
Embodiment 4：Transparency conducting layer is 100 nm ITO
Preparation technology is basic with described in case study on implementation 1, except that the annealing temperature of the ito thin film of deposition is 400 DEG C.Gained
The square resistance of the high-temperature flexible transparent conductive film for arriving is 200 Ω/, visible ray average transmittance is 85%.Film knot
Structure and photoelectric properties stabilization, are firmly combined with mica sheet substrate.
Embodiment 5：Transparency conducting layer is 100 nm AZO
It is 15 μm of mica sheet that high-temperature flexible transparent substrates use thickness, directly carries out mechanical stripping, is not required to cleaning；By purity
The AZO targets of 99.99wt% are arranged in the radio frequency cathode target groove of a water-cooled in the sputtering chamber of magnetic control sputtering device, will be shelled
Substrate frame is put into from the flexible and transparent substrate mica that rear thickness is 15 μm, in the media disk in substrate frame insertion sputtering chamber, is adjusted
The distance between whole target and substrate are 40-80 mm；Sputtering chamber and gas pipeline are evacuated, the base vacuum for making sputtering chamber is
1.0×10-4 Pa, is filled with the argon gas that purity is 99.99% in backward sputtering chamber, adjust rate of air sucked in required, makes the gas pressure intensity of sputtering chamber
It is 1 Pa；The radio-frequency power supply of AZO targets is opened, after after radio frequency glow discharge stabilization, flexible substrates target correspondence position is gone into
The AZO transparent conductive film that sputtering sedimentation thickness is 100 nm is carried out, the thickness in film deposition process is by observing and controlling sputter equipment
Thickness monitoring instrument monitor in real time.The square resistance of resulting high-temperature flexible transparent conductive film is 56 Ω/, average
Visible light transmittance rate is 86%.Membrane structure and photoelectric properties stabilization, are firmly combined with mica sheet substrate.
Embodiment 6：Transparency conducting layer is 100 nm FTO (F:SnO2)
Preparation technology is basic with described in embodiment 1, except that target is changed into FTO, resulting high-temperature flexible is transparent
The square resistance of conductive film is 20 Ω/（F doping concentrations are 15%）, visible ray average transmittance be 84%（F doping concentrations
It is 6%）.Membrane structure and photoelectric properties stabilization, are firmly combined with mica sheet substrate.
Embodiment 7：Transparency conducting layer is 100 nm NTO（Nb:TiO2）
Preparation technology is basic with described in embodiment 1, except that target is changed into NTO, resulting high-temperature flexible is transparent
The square resistance of conductive film is 80 Ω/（Nb doping concentrations are 10%）, visible ray average transmittance be 80%（Nb doping is dense
Spend is 4%）.Membrane structure and photoelectric properties stabilization, are firmly combined with mica sheet substrate.
Embodiment 8：Transparency conducting layer is ITO（50 nm）/Ag（15 nm）/ITO（50 nm）
It is 15 μm of mica sheet that high-temperature flexible transparent substrates use thickness, directly carries out mechanical stripping, is not required to cleaning；By purity
For the commodity ITO target and Ag targets of 99.99wt% are arranged in the chamber of impulse laser deposition system, base material is glued using elargol
It is attached on substrate holder, is attached in chamber, adjustment target-substrate distance is 50 mm；Start to vacuumize cavity, make the atmospheric pressure in chamber
It is maintained at 1.0 × 10 by force-4Pa or so；Light path is adjusted, starts excimer laser, make the ITO targets in laser beam focus to chamber
On material, deposition film is started at room temperature, film thickness is 50 nm；After deposition, high purity oxygen gas are filled with backward chamber, modulated
Inflation and rate of air sucked in required, make the gas pressure intensity of cavity for 10 Pa, and base material is heated into temperature for 500 DEG C carry out in-situ annealing, are incubated
After 30 min, turn off oxygen valve；After room temperature is down to, the target location in adjustment chamber is again started up excimer laser, makes to swash
Light beam is focused on the Ag targets in chamber, and deposition film is started at room temperature, and film thickness is 15 nm；Finally chamber is adjusted again
Interior target location, repeats the preparation technology of above-mentioned ito thin film, and the ito thin film that a layer thickness is 50 nm, deposition are deposited again
Later, high purity oxygen gas, modulation inflation and rate of air sucked in required are filled with backward chamber, make the gas pressure intensity of cavity for 10 Pa, substrate is heated
In-situ annealing is carried out for 500 DEG C to temperature, after 30 min of insulation, turns off oxygen valve；After temperature is reduced to room temperature, conductive thin is taken out
Film base material.The square resistance of resulting high-temperature flexible transparent conductive film is 30 Ω/, visible ray average transmittance is
67%.Membrane structure and photoelectric properties stabilization, are firmly combined with mica sheet substrate.
Embodiment 9：Transparency conducting layer is AZO（30 nm）/Ag（15 nm）/AZO（30 nm）
Preparation technology is basic with described in embodiment 8, except that ITO target is changed to AZO targets, and it is thin in deposition AZO
It is 200 DEG C that underlayer temperature is kept during film, and oxygen pressure is 0.5 Pa, the side of resulting high-temperature flexible transparent conductive film
Block resistance is 2 Ω/, visible ray average transmittance is 75%.Membrane structure and photoelectric properties stabilization, are combined with mica sheet substrate
Firmly.
Embodiment 10：Transparency conducting layer is single-layer graphene
It is 15 μm of mica sheet that high-temperature flexible transparent substrates use thickness, directly carries out mechanical stripping, is not required to cleaning；Directly use
Be transferred to single-layer graphene on Cu paper tinsels on mica sheet by transfer method；The square of resulting high-temperature flexible transparent conductive film
Resistance is 450 Ω/, visible ray average transmittance is 92%.Membrane structure and photoelectric properties stabilization, are combined with mica sheet substrate
Firmly.
Embodiment 11：Transparency conducting layer is multi-layer graphene（15 layers）
Preparation technology is with described in embodiment 10, except that transfer multi-layer graphene (15 layers).Resulting high-temperature flexible
The square resistance of transparent conductive film is 130 Ω/, visible ray average transmittance is 86%.Membrane structure and photoelectric properties are steady
It is fixed, it is firmly combined with mica sheet substrate.
Embodiment 12：Transparency conducting layer is nano-silver thread
It is 15 μm of mica sheet that high-temperature flexible transparent substrates use thickness, directly carries out mechanical stripping, is not required to cleaning；By suction filtration
Good AgNWs-MCE films front is attached on mica sheet, and then hot press heats 100 DEG C, is that 0.5MPa is pressed 20 minutes with pressure；With
55 DEG C of acetone steams dry 4 minutes it is fully transparent to MCE films, be then placed in being soaked 15 minutes in acetone soln, MCE films is completely molten
Solution.The square resistance of resulting high-temperature flexible transparent conductive film is 60 Ω/, visible ray average transmittance is 85%.It is thin
Membrane structure and photoelectric properties stabilization, are firmly combined with mica sheet substrate.
Embodiment 13：Transparency conducting layer is metal grill
It is 15 μm of mica sheet that high-temperature flexible transparent substrates use thickness, directly carries out mechanical stripping, is not required to cleaning；Using sharp
Light sinters Ag particle inks and the method that unsintered Ag inks are washed away is prepared into two-dimensional metallic on flexible substrate mica sheet
Grid transparent conductive film, the line width of metal grill is 15 um, and transmitance is 85%, and square resistance is less than 30 Ω/.Film knot
Structure and photoelectric properties stabilization, are firmly combined with mica sheet substrate.Directly write with Argent grain ink and prepare metal grill, metal wire
A width of 5 μm, 280 nm high, line center spacing its transmitance highest at 400 μm, is 94%.Anneal 2 h at 300 DEG C, can obtain
Conductive metal grill is obtained, resistivity is 3.64 × 10-5Ω ﹒ cm.Membrane structure and photoelectric properties stabilization, with mica sheet
Substrate is firmly combined with.
Embodiment 14：Transparency conducting layer is CNT（CNTs）
It is 15 μm of mica sheet that high-temperature flexible transparent substrates use thickness, directly carries out mechanical stripping, is not required to cleaning；With 12
Sodium alkyl sulfonate (SDS) disperses CNTs, CNTs is uniformly deposited on filter membrane by the method for vacuum filtration then and forms thin
Film, washes away SDS, is finally transferred to the film of formation and CNT-TCFs is obtained in transparent substrates；Then to Arc carbon pipes be made it is thin
Adulterate thionyl chloride in film（SOCl2）The conductance that film can be obviously improved improves about 2.4 times, and to the translucidus of film almost
Without influence；Resistivity can finally be obtained for 160 Ω/, light transmittance is 87% high-temperature flexible transparent conductive film.It is thin
Membrane structure and photoelectric properties stabilization, are firmly combined with mica sheet substrate.
Application with specific embodiment to high-temperature flexible transparent conductive film of the present invention in the opto-electronic device below is done in detail
Describe in detail bright：
Embodiment 15：High-temperature flexible transparent membrane heater (ITO is conductive exothermal material)
Using above preferred embodiment prepare high-temperature flexible transparent membrane prepare thin film heater, structure as shown in Fig. 2
The direction of arrow is heating direction wherein in figure, at the two ends of the transparent conductive film 10 for preparing by depositing or coating a gold
Category band 20（Au, Ag, Cu etc.）, then draw two wires simultaneously respectively on two metal tapes, two wires are accessed
Keithley2400 digital sourcemeters, form a DC channel, and fixed DC voltage is applied to conductive material using digital sourcemeter,
It is set generate heat.The maximum heating temperature of resulting high-temperature flexible transparent membrane heater is apparently higher than existing substrate（Example
Such as glass, PET）The thin film heater of preparation and thermal response time is shorter, therefore greatly widened flexible, thin film heater
Operating temperature range, and greatly shorten thermal response time.
Embodiment 16：High-temperature flexible transparent membrane heater (AZO is conductive exothermal material)
Preparation technology is with described in embodiment 15, except that the conductive layer of thin film heater is changed to AZO films, it is resulting
High-temperature flexible transparent membrane heater has equally also significantly widened the operating temperature range of flexible, thin film heater, and greatly
Shorten thermal response time.
Case study on implementation 17：Flexible perovskite solar cell (with ITO/ Mica as electrode)
The high-temperature flexible transparent conductive film prepared using above preferred embodiment prepares perovskite solar cell, structure
As shown in figure 3, including mica sheet 41, ito thin film 42, TiO successively from bottom to up2Electron transfer layer 43, calcium titanium ore bed 44, hole
Transport layer 45, back electrode（Au）46；Wherein TiO2Electron transfer layer is prepared using PLD techniques, calcium titanium ore bed（CH3NH3PbI3- xClx）, hole transmission layer prepared using Sol-gel techniques；The I-V characteristic of battery is measured using the source tables of Keithley 2400,
Solar simulator is Newport 69911, and its power is 300W.The photoelectric conversion of the flexible perovskite solar cell for obtaining
Efficiency is 9.67%.
Case study on implementation 18：Flexible perovskite solar cell (with AZO/ Mica as electrode)
Preparation technology is with described in embodiment 17, except that battery hearth electrode is changed to AZO, the flexible perovskite sun for obtaining
The electricity conversion of energy battery is 13.73%.
High-temperature flexible transparent conductive film of the present invention is compared compared with transparent conductive material, with advantages below：This hair
The high-temperature flexible transparent substrates of bright use can high temperature resistant, manufacturing process is simple, with low cost, nontoxic, free from environmental pollution, made
Into high-temperature flexible transparent conductive film electric conductivity and optical transmittance it is high, thickness evenness is good, surfacing, photo electric
Can be stable, it is firmly combined with base material.
The present invention using the high-temperature flexible transparent conductive film as high-temperature flexible transparent membrane heater matrix
And the electrode material of flexible perovskite solar cell, prepare the flexibility that operating temperature range is big, the thermal response time is short saturating
Bright thin film heater, while passing through high-temperature technology（>450℃）Efficient flexible solar battery is prepared, is soft high temperature resistant
Property transparent membrane heater and flexible solar battery development new path is provided.
In sum, the invention provides a kind of high-temperature flexible transparent conductive film and preparation method and application, institute
High-temperature flexible transparent conductive film is stated, including：High-temperature flexible transparent substrates, and it is deposited on the transparent base of the high-temperature flexible
Transparency conducting layer on bottom.High-temperature flexible transparent conductive film of the present invention can high temperature resistant, thermal coefficient of expansion is low, surfacing,
Transparency is high, photoelectric properties are stable, and its manufacturing process is simple, with low cost.
It should be appreciated that application of the invention is not limited to above-mentioned citing, and for those of ordinary skills, can
To be improved according to the above description or converted, all these modifications and variations should all belong to the guarantor of appended claims of the present invention
Shield scope.
Claims (10)
1. a kind of high-temperature flexible transparent conductive film, it is characterised in that including：High-temperature flexible transparent substrates, and be deposited on
Transparency conducting layer in the high-temperature flexible transparent substrates.
2. high-temperature flexible transparent conductive film according to claim 1, it is characterised in that the high-temperature flexible is transparent
Substrate is mica sheet.
3. high-temperature flexible transparent conductive film according to claim 1, it is characterised in that the transparency conducting layer is
Bright conductive material, the transparent conductive material includes SnO2Film, Sb2O3Film, ZnO film, CdO films, ito thin film, AZO
Film, FTO films, NTO films, Sandwich film, nano-silver thread, Graphene, metal grill, CNT.
4. high-temperature flexible transparent conductive film according to claim 1, it is characterised in that the high-temperature flexible is transparent
The thickness of substrate is 4 ~ 100 μm.
5. high-temperature flexible transparent conductive film according to claim 1, it is characterised in that the thickness of the transparency conducting layer
It is 25 ~ 500 nm to spend.
6. a kind of preparation method of high-temperature flexible transparent conductive film as claimed in claim 1, it is characterised in that including step
Suddenly：
A, by target be arranged on magnetic control sputtering device radio frequency cathode target groove in, high-temperature flexible transparent substrates are put into substrate
Frame, in the media disk in substrate frame insertion sputtering chamber, adjustment the distance between target and substrate are 40 ~ 80 mm；
B, to sputtering chamber be evacuated, make sputtering chamber vacuum be less than 1.0 × 10-3 After Pa, to argon gas is filled with sputtering chamber, adjust
Rate of air sucked in required, the gas pressure intensity for making sputtering chamber is 0.1 ~ 5 Pa；
C, the radio-frequency power supply for opening target, target correspondence position sputtering sedimentation transparency conducting layer is gone to by substrate, obtains high temperature resistant
Flexible transparent conductive film.
7. a kind of preparation method of high-temperature flexible transparent conductive film as claimed in claim 1, it is characterised in that including step
Suddenly：
A, by target be arranged on pulse laser deposition apptss chamber in, adjustment target-substrate distance be 40 ~ 80 mm；Then it is high temperature resistant is soft
Property transparent substrates are fixed on substrate holder, are attached in chamber, then cavity is vacuumized, make vacuum in chamber be maintained at 5 ×
10-5 Pa ~5×10-4 Between Pa；
B, light path is adjusted, starts excimer laser, made on the target in laser beam focus to chamber, deposit transparency conducting layer,
Obtain conductive film base material；
C, the conductive film base material for obtaining step B are annealed, and obtain high-temperature flexible transparent conductive film.
8. high-temperature flexible transparent conductive film method according to claim 7, it is characterised in that in the step C, to
High purity oxygen gas are passed through in chamber, inflation and the rate of air sucked in required of oxygen is adjusted, the oxygen pressure in cavity is maintained at 5 × 10-4~5×101 Pa,
The conductive film base material that step B is obtained is heated to 100 ~ 600 DEG C and carries out in-situ annealing, is incubated 20 ~ 40 min.
9. high-temperature flexible transparent conductive film method according to claim 7, it is characterised in that in the step C, will
The conductive film base material that step B is obtained takes out, and is positioned in tube furnace, is annealed at 100 ~ 600 DEG C, is incubated 10 ~ 60 min.
10. a kind of application of high-temperature flexible transparent conductive film, it is characterised in that by high temperature resistant as claimed in claim 1
Flexible transparent conductive film is applied in photoelectric device, used as the matrix or flexible calcium of high-temperature flexible transparent membrane heater
The electrode material of titanium ore solar cell.
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