CN107689264A - Transparent conductive film and preparation method, the preparation method of PDLC component - Google Patents
Transparent conductive film and preparation method, the preparation method of PDLC component Download PDFInfo
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- CN107689264A CN107689264A CN201710684095.7A CN201710684095A CN107689264A CN 107689264 A CN107689264 A CN 107689264A CN 201710684095 A CN201710684095 A CN 201710684095A CN 107689264 A CN107689264 A CN 107689264A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
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- G—PHYSICS
- G02—OPTICS
- 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
- G02F1/01—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 for the control of the intensity, phase, polarisation or colour
- G02F1/13—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 for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1334—Constructional arrangements; Manufacturing methods based on polymer dispersed liquid crystals, e.g. microencapsulated liquid crystals
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
Abstract
This application discloses a kind of preparation method of transparent conductive film, including：Flexible substrate is provided, and generates mask on flexible substrates, mask has crackle, and crackle is interconnected and forms aperiodicity network；Metal level and sull continuously are sequentially depositing in the gap of crackle, until the metal level and sull that are deposited in gap reach setting thickness；The mask in flexible substrate is removed, obtains the transparent conductive film of aperiodicity network.The transparent conductive film of the application has higher permeability, preferable electric conductivity and buckle resistance energy for visible ray.In addition, the application also proposes a kind of preparation method of PDLC component.
Description
Technical field
The application is related to transparent conductive film technical field, more particularly, to a kind of transparent conductive film, the electrically conducting transparent
The preparation method of film and the method that PDLC component is prepared using transparent conductive electrode.
Background technology
Transparent conductive film (Transparent Conductive Films, TCF) refers in visible light wave range (wavelength
380~780nm) possess high transmittance, while but also with the film of high conductivity, it is widely used in solar cell, display
The fields such as screen, touch-screen, antistatic coating, intelligent window and semiconductor.
Current transparent conductive film includes metal system, sull system (Transparent Conductive
Oxide, TCO) and compound film system etc., wherein, including In2O3、SnO2, ZnO and its doping system In2O3：Sn(ITO)、ZnO：
Sull system including Al (ZAO) has good electric property, and has certain buckle resistance energy, and is considered as
The Main System of following transparent conductive film.But when electric conductivity strengthens, inevitably decay it to the saturating of visible ray
Rate is crossed, the transparent conductive film prepared using such material can not often meet the requirement of high transmittance, high conductivity.
In order to improve the optical property of transparent conductive film, there is researcher to be prepared for metal nanowire thin-films, preparation process
Including：Nano silver wire solution is obtained by solution processing methods such as the hot method of alcohol or hydro-thermal methods, then using spin-coating method, Meyer rod coating
Liquid comprising nano wire is transferred in transparent substrates by the technique such as method or spraying process, and it is thin just to obtain corresponding metal nanometer line
Film.The metal nanometer line transparent conductive film prepared by the above method has superior photoelectric properties and buckle resistance energy, by
It is the good conductor of electricity in itself in silver, nano silver wire is applied to conductive layer, energy loss can be reduced；Incidence is less than using diameter
The nano silver wire of optical wavelength makes electrode, can not only increase the electrode current collecting area of solar cell, and can utilize light
Diffraction special efficacy, fully absorb luminous energy.But the performance of metal nanometer line transparent conductive film is by nano wire close in itself
Degree, length, electric conductivity influence outside, also influenceed by contact resistance, and the nano wire in substrate surface Arbitrary distribution is mutual
Between lack good connectivity, under such case, film its electric conductivity made using metal nanometer line can not obtain
Effectively improve.Based on this, it is necessary to which the preparation method of existing transparent conductive film is improved.
The content of the invention
The application technology to be solved is prepared transparent to propose a kind of method for preparing transparent conductive film using this method
Conductive film has preferable translucency and buckle resistance energy, while has preferable electric property.
In order to solve the above technical problems, according to the one side of the application, a kind of transparent conductive film, including flexible liner are proposed
Bottom and a plurality of grid lines being deposited in the flexible substrate, a plurality of grid lines form the transparent of aperiodicity network
Conductive electrode, every grid lines include more metal layers and multilevel oxide film, and the more metal layers and the multilayer
Thickness direction of the sull along the transparent conductive electrode distributes alternately successively.
Further, the width of every grid lines is 3-50 μm, and the more metal layers are included in every grid lines
Thickness is 5-50nm, and the thickness that the multilevel oxide film is included in every grid lines is 10-100nm.
According to the another aspect of the application, a kind of preparation method of transparent conductive film is proposed, is comprised the following steps：
Flexible substrate is provided, and mask is generated in the flexible substrate, the mask has aperiodicity crackle,
And the crackle is interconnected and forms aperiodicity network；
Metal level and sull continuously are sequentially depositing in the gap of the crackle, until the gold being deposited in gap
Category layer and sull reach setting thickness；
The mask in the flexible substrate is removed, obtains the transparent conductive film of aperiodicity network.
Further, the mask obtains by the following method：
Colloidal sol is mixed to form according to setting ratio using persursor material and diluent, obtains mask liquid；
Deposited using the mask liquid in the flexible substrate and form mask film；
The flexible substrate of deposition mas version film is dried in the case where imposing a condition, obtained with aperiodicity crackle
Mask.
Further, the persursor material is titanium dioxide or water soluble acrylic acid.
Further, the width of the crackle is 3-50 μm.
Further, the sull is included in zinc-oxide film, WO 3 film, titanium dioxide, ito thin film
At least one.
According to the another further aspect of the application, a kind of preparation method of PDLC component is proposed, including：
Flexible substrate is provided, transparent conductive electrode is formed in the flexible substrate, obtains transparent conductive film, it is described
Bright conductive electrode includes a plurality of grid lines, and a plurality of grid lines forms aperiodicity network, and every grid lines includes more
Layer metal level and multilevel oxide film, and the more metal layers and the multilevel oxide film are electric along the electrically conducting transparent
The thickness direction of pole distributes alternately successively；
By ultraviolet light polymerizable monomer mixture and with the nematic liquid crystal of its index matching according to mass ratio (1-2): 3
Between mix, and add silicon dioxide microsphere and be well mixed, form liquid crystal solution；
Between the liquid crystal solution is coated in into two layers of transparent conductive film, and using ultraviolet light to coated with liquid crystal
Two layers of transparent conductive film of solution carries out radiation treatment, forms PDLC component.
Further, transparent conductive electrode is formed in the flexible substrate includes：
Mask is generated in the flexible substrate, the mask has aperiodicity crackle, and the crackle is mutual
Connection forms aperiodicity network；
Metal level and sull continuously are sequentially depositing in the gap of the crackle, until the gold being deposited in gap
Category layer and sull reach setting thickness；
The mask in the flexible substrate is removed, the transparent of aperiodicity network is obtained in the flexible substrate
Conductive electrode.
Further, the ultraviolet light polymerisable monomer in the ultraviolet light polymerizable monomer mixture, which includes ultraviolet light, to gather
Close silane coupler monomer, polyethyleneglycol diacrylate, glycol dimethacrylate isobornyl thiocyanoacetate, acrylic acid -3,5,5- tri-
In the own ester of methyl, senecioate-oxylactone, BDO diacrylate, glycidyl acrylate class monomer at least
It is a kind of.
Compared with prior art, the application has the beneficial effect that：Transparent conductive film includes substrate and transparent conductive electrode,
Substrate is as light transmission part, and for transparent conductive electrode as current-carrying part, transparent conductive electrode includes a plurality of grid lines, and a plurality of net
Ruling forms aperiodicity network, and the space of grid is then used as the transmission path of light, and incident light can be from aperiodicity
By so as to obtain broader optical region transmitance, improving the optical property of transparent conductive film in grid；Every grid lines
The composite bed formed comprising metal level and sull, the conduction of film can be realized by the series parallel structure of compound grid
Property, the PDLC components prepared with transparent conductive film have preferable switch performance and the faster speed of response；Electrically conducting transparent is thin
The substrate of film uses flexible material, has good bend resistance characteristic.
Brief description of the drawings
The detailed description made by reading with reference to the following drawings to non-limiting example, other features of the application,
Objects and advantages will become more apparent upon.
Fig. 1 a are the preparation method flow chart of transparent conductive film；
If Fig. 1 b are to form the transparent conductive film with aperiodicity network according to the method shown in Fig. 1 a to illustrate
Figure；
Fig. 2 is the preparation method flow chart of PDLC component；
Fig. 3 is the mask indicative of local optical image that the embodiment of the application one is formed；
Fig. 4 a are mask structural representation of the surface covered with acrylate film of another embodiment generation of the application；
Fig. 4 b are that the mask shown in Fig. 4 a deposits the structural representation after composite bed；
Fig. 4 c are the transparent conductive electrode schematic diagram that Fig. 4 b remove the aperiodicity network formed after mask；
Fig. 5 is PDLC component structure diagrams prepared by the another embodiment of the application；
Fig. 6 is the optical property figure of the PDLC components described in Fig. 5；
Fig. 7 is optical property figure of the PDLC components under different voltages described in Fig. 5.
Embodiment
Illustrate presently filed embodiment below by way of particular specific embodiment, those skilled in the art can be by this explanation
Content disclosed by book will readily appreciate that the further advantage and effect of the application.The application can also pass through specific realities different in addition
The mode of applying is embodied or practiced, and every details can also be based on different viewpoints and application in this specification, without departing from this
Various modifications or alterations are carried out under the spirit of application.
Diagram provided in embodiments herein only illustrates the basic conception of the application in a schematic way.Therefore, scheme
The metal grill transparent conductive film relevant with the application is only shown in showing rather than is painted according to shape during actual implement and size
System, PDLC component (also known as intelligent window or switching device) is not limited to when actually implementing, also including solar energy
The fields such as battery, display screen, touch-screen, antistatic coating and semiconductor.
It can not meet preferable light transmission, electric conductivity simultaneously to solve the transparent conductive film of existing method preparation
The problem of with buckle resistance energy, present applicant proposes a kind of transparent conductive film, the transparent conductive film include flexible substrate and
A plurality of/the grid lines of deposition on flexible substrates, a plurality of grid lines are distributed in strip and form aperiodicity network
Transparent conductive electrode, every grid lines include more metal layers and multilevel oxide film.More metal layers and multilevel oxide
Film can distribute alternately to form composite construction successively along the thickness direction (above-below direction) of transparent conductive electrode, i.e.,：Electrically conducting transparent
Every grid lines of electrode sequentially consists of：The order of metal level-sull-metal level repeats to arrange.Further
Ground, the grid lines that metal level is formed with oxide film layer are interspersed, and form aperiodicity (compound) network.
Such as the preparation method schematic flow sheet of transparent conductive film that Fig. 1 a are the embodiment of the application one, including following step
Suddenly：
S101., flexible substrate is provided, and generates mask on flexible substrates, the mask has or formed (a plurality of) to split
Line, and crackle is interconnected and forms aperiodicity network.Mask used can be Lithographic template or self assembly template,
For crackle in long and narrow distribution or strip distribution, the width of crackle can be any number between 3-50 μm, adjacent to split in mask
Spacing between line can be any number between 200-400 μm, and the depth of crackle can be any number between 10-150nm.
In certain embodiments, the material as flexible substrate can be flexible glass or polymer, such as：Poly- terephthaldehyde
Sour glycol ester (PET), polybutylene terephthalate (PBT) (PBT), polystyrene ester, makrolon (PC), polymethyl
Sour methyl esters (PMMA), polyallyl esters (PE), polyimides (PI), polycyclic alkene (PNB), ENB resin or fluoropolymer
One or more in.
In certain embodiments, mask can be obtained by photolithography method：First, deposition mas mother matrix on flexible substrates
(as mask film)；Then, using photolithography method etching mask mother matrix, the mask with aperiodicity crackle is formed.
It should be noted that in photolithographic process, horizontal photoengraving density and longitudinal photoengraving density can be adjusted respectively, also can adjust
The path of photoengraving, so as to which etching forms acyclic crack pattern on flexible substrates.Exemplarily, the shape of reticle
It may include into process：Colloidal sol is mixed to form according to setting ratio using persursor material and diluent, obtains mask liquid；Utilize
Mask liquid deposits to form film in flexible substrate.
In further embodiments, mask is self assembly template, and the forming process of the self assembly template mainly includes：It is first
First, colloidal solid and solvent are mixed to form uniform and stable liquid dispersion system, and flexible substrates is tied up to using the liquid dispersion
Surface forms uniform film；Then, the gradual bunching after the volatilization of solvent of the colloidal solid in disperse system, in atmospheric pressure, table
Under the influence of the complicated factors such as face speed air flow, capillary force, intermolecular force, non-homogeneous stress is produced in film,
When the internal stress of certain reaches critical value, film just ftractures；Then, as solvent persistently volatilizees, non-homogeneous stress enters one
The aggregation of step, crackle start to spread；Finally, produce non-periodic distribution (random walk or random distribution) and connectedness is good
Crackle, be interconnected between neighboring cracks, form the mask with crackle grid or cleat network.
In certain embodiments, the colloidal solid for forming liquid dispersion system can be TiO 2 sol and aqueous acrylamide
Acid, dispersant/diluent can be one or more combinations of water, acetone, ethanol.The ratio of colloidal solid and disperse system can
To be 1: any number between (10-2).Further, metatitanic acid four can be selected by forming the precursor material of TiO 2 sol
(molecular formula is Ti (O-C to butyl ester4H9)4), its hydrolysis can produce titanium oxide colloid particle.Certainly, in tetrabutyl titanate hydrolysis
When can also add acetic acid (molecular formula CH3COOH chelating agent) is used as, wherein, the volume ratio of butyl titanate and ethanol can be set
Put 1: the volume ratio of any number between (2-4), acetic acid and ethanol may be provided at 1: any number between (5-10).
In certain embodiments, the colloidal solid for forming liquid dispersion system can also be high-molecular organic material, pass through by
High-molecular organic material is well mixed with diluent (or dispersant), you can obtains liquid dispersion system.High-molecular organic material can
To be (water-based) acrylic resin, epoxy resin etc., diluent can be water, ethanol, acetone and other organic solvent, organic polymer
Material is generally in a liquid state, and the volume ratio of high-molecular organic material and diluent can be 7：Any number between (1-3).It is logical
The concentration of colloidal solid in liquid dispersant is overregulated, may be such that the crackle being subsequently formed has different depth and/or depth.
S102. metal level and sull continuously are sequentially depositing in the gap of aperiodicity crackle, until in gap
Deposited metal level and sull reaches setting thickness.Exemplarily, can use vacuum evaporation, magnetron sputtering plating,
The methods of plasma coating, metal level and sull is set to be sequentially filled in the gap of aperiodicity crackle.Pass through company
Continuous is sequentially depositing metal level, sull, can in the short transverse in gap interior edge gap/thickness direction of flexible substrate
It is upper to form metal level and the composite bed of sull interleaved distribution.Further, it is filled in compound in crackle gap
Layer interconnection/connection, aperiodicity grid is formed, the aperiodicity grid includes a plurality of grid lines that composite bed is formed, often
Bar grid lines is corresponding with each crackle.
The depth of crackle arbitrary value between 15-150nm, the setting thickness for depositing composite bed can be between 5-150nm
Any number, preferred scope are arranged between 15-135nm, and the setting thickness can be thick with the film of formation crackle on mask
Spend identical or be close, the width for depositing composite bed can be any number between 3-50 μm, between deposited adjacent composite bed
Spacing can be any number between 200-400 μm.Further, the material for forming metal level can be the conductions such as copper, gold, silver
The preferable material of property, deposit thickness can be arbitrary value between 5-50nm, preferably 5-35nm；Sull includes zinc oxide
One or more combinations in film, WO 3 film, titanium dioxide, ito thin film etc., deposit thickness can be 10-
Arbitrary value between 100nm, such film have good light transmission.
S103. the mask in flexible substrate is removed, obtains the transparent conductive film of aperiodicity network, this is transparent
Conductive film includes multiple grid lines that the composite bed of flexible substrate and deposition on flexible substrates is formed, and multiple grid lines are mutual
Connect and be interspersed to form the transparent conductive electrode of aperiodicity grid.
Alternatively, the removal of mask can be achieved by the steps of：By deposited metal layer and the mask of sull
Version is placed in acetone and is ultrasonically treated, you can crackle mask is removed, so as to obtain metal level on flexible substrates and oxide is thin
The grid lines that film is formed, also referred to as conductive grid or grid.Certainly, the removal of mask also can be by applying outside machinery
Active force is realized.
It should be noted that the method for preparing transparent conductive film of above-mentioned aperiodicity network, between each step also
It may include other operations, those skilled in the art can enter line translation to said sequence and and without departing from the protection model of the application
Enclose.In some implementations, can first in the crackle of non-periodic distribution deposition oxide film, the then sull again
Upper deposited metal layer.
If Fig. 1 b are the transparent conductive film schematic diagram according to the method formation shown in Fig. 1 a.It is corresponding with step S101,1.
For flexible substrate 11；2. for the mask film of deposition, mask film 12 is located at the upper surface of flexible substrate 11；3. for non-
The mask of periodicity crackle, the centre of mask film 12 form multiple crackles 13, and crackle 13 is in long and narrow distribution and randomly arranges.
It is corresponding with step S102,4. to be sequentially depositing the mask of metal level and sull, deposited in the gap of crackle 13 multiple
Layer 14 is closed, the composite bed 14 includes the metal level and sull that multilayer distributes alternately, and the thickness of composite bed is less than or equal to
The depth in gap 13.It is corresponding with step S103,5. to remove the electrically conducting transparent with composite lattice that is formed after mask
Film, the flexible substrate 11 of the transparent conductive film form a plurality of grid lines being made up of composite bed 14, and multiple grid lines are mutual
Connection composition transparent conductive electrode.
According to the another aspect of the application, it is also proposed that one kind prepares PDLC using above-mentioned transparent conductive film
The method of component, comprises the following steps as shown in Figure 2：
S201., flexible substrate is provided, and forms the transparent conductive electrode of aperiodicity network on flexible substrates, is obtained
Take transparent conductive film, transparent conductive electrode includes a plurality of grid lines, and a plurality of grid lines forms aperiodicity network, every
Grid lines includes more metal layers and multilevel oxide film, and more metal layers and multilevel oxide film are electric along electrically conducting transparent
The thickness direction of pole distributes alternately successively.
In certain embodiments, the transparent conductive electrode for aperiodicity network being formed in flexible substrate can refer to accompanying drawing
1 flow.Further, PET may be selected as flexible substrate, and the metal level or oxide film layer deposited in flexible substrate
Width (width of wall scroll grid lines) or mesh width be any number between 3-50 μm, the spacing between adjacent mesh can be with
For any number between 200-400 μm, the thickness of wall scroll grid lines is arranged to arbitrary value between 15-150nm.
S202. by ultraviolet light polymerizable monomer mixture and with the nematic liquid crystal of its index matching according to mass ratio 1:
Mixed between 3-2: 3, and add silicon dioxide microsphere and be well mixed, form liquid crystal solution.Alternatively, ultraviolet light polymerisable monomer
Ultraviolet light polymerisable monomer in mixture can be ultraviolet photopolymerizable silane coupler monomer, polyethylene glycol diacrylate
Ester, glycol dimethacrylate isobornyl thiocyanoacetate, acrylic acid -3,5, the own ester of 5- trimethyls, senecioate-oxylactone, Isosorbide-5-Nitrae-fourth two
One or more kinds of combinations in alcohol diacrylate, glycidyl acrylate class monomer.Nematic phase liquid crystal material can be with
Select LC605, SLC1717, LCE7 etc..Silicon dioxide microsphere is used as sept, can adjust the mixing of ultraviolet light polymerisable monomer
The concentration of thing and nematic liquid crystal.
S203. by liquid crystal solution coated between two layers transparent conductive film, and using ultraviolet light to molten coated with liquid crystal
The transparent conductive film of liquid carries out radiation treatment 10-120min, forms PDLC PDLC components.Further, also
PDLC assembly surfaces are cleaned using organic solvents such as methanol, to remove impurity.It should be noted that liquid crystal solution
Practical coating transparent conductive electrode and another layer of transparent conductive film of layer of transparent conductive film transparent conductive electrode it
Between.
Embodiment one
Copper is selected as flexible substrate, colloidal solid selection TiO 2 sol, the material of deposited metal layer from PET,
The sull of formation is titanium deoxid film.In this embodiment, metal grill transparent conductive film preparation process includes：
S301. mask is generated in PET flexible substrates, the crackle of non-periodic distribution is formed on mask plate.First, will
Butyl titanate, the acetic acid as chelating agent and the ethanol as dispersant of titanium source or persursor material are provided with 2: 1: 6
Volume ratio mixes, and opening, which is placed in air, is stirred vigorously 1-2h, and tetrabutyl titanate hydrolysis can obtain the faint yellow of homogeneous transparent
TiO 2 sol；Then, TiO 2 sol is homogeneously disposed on PET substrate using spin coating method, so as in PET substrate shape
Thickness into titanium deoxid film, and film is about 20nm；Then, titanium dioxide coating film is spontaneously dried at ambient temperature
Flexible substrate, until film formed crackle.
If Fig. 3 is the mask indicative of local optical image that the embodiment of the present application is formed, in this embodiment, mask plate film
For titanium deoxid film, and the surface of titanium deoxid film film forms crackle, and crack width is about 3-50 μm, the depth of crackle
For 20nm, 80-200 μm is spaced about between neighboring cracks, is interconnected between neighboring cracks, and crackle is along non-regular shape
Extension, the pattern of this aperiodic distribution is it is possible to prevente effectively from due to optical property caused by moire or optical diffraction phenomenon
Decline.Further, in the present embodiment, using PET flexible materials as substrate, have the characteristics that flexible, in light weight, carry
The high buckle resistance energy for forming transparent conductive film.
S302. metal level and sull are continuously sequentially depositing on mask using magnetically controlled sputter method, the metal
Layer and sull are specifically deposited in crackle gap, and metal level and sull Multiple depositions can form composite bed.
In this embodiment, the material selection copper target of deposited metal layer, the material selection titanium dioxide of deposition oxide film
Titanium target material.The power setting of magnetron sputtering is 50W (watt), sputter gas Ar, gas flow 40sccm (gas streams per minute
Measure volume), sputtering time 2.5min, two targets divide different periods to sputter respectively, the metal level and oxygen obtained in crackle gap
The thickness for the composite bed that compound film is formed is about 15-20nm, and the complex metal layer in corresponding different crackle gaps can be connected with each other,
And the filling rate of copper is 12%.
S303. remove the mask in flexible substrate, obtain composite gridding transparent conductive electrode, transparent conductive electrode with it is soft
Property substrate collectively constitutes transparent conductive film.In this embodiment, mask is removed using the method for mechanical grinding, stayed on substrate
Under a plurality of grid lines that is formed by composite bed, a plurality of grid lines is interlaced, forms aperiodicity network.
The metal grill transparent conductive film of the present embodiment has good bend resistance special because substrate uses flexible material
Property；The substrate of the transparent conductive film of network/grid type is made as light transmission part, the composite bed of aperiodicity network
For current-carrying part, both are separate, so can realize the conduction of film by the series parallel structure of aperiodicity grid
Property, and the space of grid is then used as the transmission path of light, wavelength is that 300nm to 1600nm light can be from aperiodicity grid
In by so as to obtain broader optical region transmitance；Further, when the line width of the conductive electrode in aperiodicity grid
It is small arrive certain magnitude in the case of, due to optical diffraction, the thickness of composite bed will no longer affect film in aperiodicity grid
Translucency, the transparent conductive film being consequently formed can take into account optical property and electric property simultaneously.
Embodiment two
From PET as flexible substrate, the material for forming colloidal solid selects water soluble acrylic acid, the material of deposited metal layer
Selection is silver-colored (Ag), and the material for forming sull is zinc oxide (ZnO).Transparent conductive film preparation process includes：
S401., flexible substrate is provided, and acrylate film, natural air drying life are prepared using method of pulling up on flexible substrates
Into mask, there is acyclic crackle, and crackle is interconnected and forms aperiodicity network on the mask.
In this embodiment, first, 100mL water soluble acrylic acid is added into 25mL distilled water dilutings, and by after dilution
Solution is placed on Best-Effort request coating machine；Using adhesive tape by the clean sheet glass of flexible substrate conglutinate, substrate
Size is 4.5cm × 4.5cm, and both overlapping region areas are about 2.25cm2, meanwhile, the sheet glass other end is clipped in coating machine
On the clip of top, acrylic acid is coated uniformly on by substrate surface using the above method；Finally by the substrate after plated film in room temperature
20min is stood in lower so that aqueous acrylamide acid solution is thoroughly air-dried, and the crackle of non-periodic distribution is formed on mask, and non-
The crackle of periodic distribution is interconnected and forms aperiodicity network.
In this embodiment, filming parameter is set as follows：Dropping distance may be configured as 12cm；Decrease speed is 400 μm/s；
Impregnate 15s；Lifting number is repeated as twice, the lifting time is 5min.By above-mentioned lifting process, what is formed on substrate covers
The thickness of masterplate film is about 40nm.It is corresponding, the depth for the aperiodicity crackle that mask film exposure cracking is formed
Also about 40nm, width is about 20 μm, and is spaced about 200-400 μm between neighboring cracks.
S402. silver and zinc-oxide film are continuously sequentially depositing on mask using magnetically controlled sputter method, until in gap
Deposited Ag and ZnO film reaches setting thickness, and ZnO-Ag- so can be being formed in the gap of PET base upper surface
ZnO composite beds.
In the present embodiment, the material of deposited metal layer selects silver-colored target, the material selection zinc oxide target of deposition oxide film
Material.The parameter of magnetron sputtering is：Using 50W (watt) power splash-proofing sputtering metal silver and zinc-oxide film, sputter gas Ar, gas
Flow 40sccm (gas flow volume per minute), sputtering time 5min, two targets divide different periods to distinguish alternating sputtering,
Metal layer A g and the ZnO film composite bed to be formed that distributes alternately reach and set thickness as 40nm, and the filling rate of silver is 15%.
S403. the mask in flexible substrate is removed, forms the aperiodicity of silver and zinc oxide composition on flexible substrates
The transparent conductive electrode of network, flexible substrate collectively constitute transparent conductive film with transparent conductive electrode.In this embodiment
In, composite bed includes the Ag layers that distribute alternately and ZnO layer along its thickness direction, and removing after mask can shape on flexible substrates
The a plurality of grid lines formed into ZnO-Ag-ZnO, a plurality of interlaced formation nethike embrane of grid lines.It is pointed out that flexible liner
ZnO-Ag-ZnO grid lines on bottom may include multilayer, and be that ZnO layer-Ag layers repeat to distribute alternately.
Further, the substrate for depositing composite bed is placed in acetone soln and is supersound process 2h, acrylic acid can be removed,
And the grid lines being made up of composite bed in nethike embrane slot is left, the width of the width of grid lines and the crackle of non-periodic distribution
Quite, about 20 μm.So, the width of single grid lines is also accordingly 20 μm, and the width of different grid lines is about 200-
400μm。
If Fig. 4 a are mask structural representation of the surface covered with acrylate film that the embodiment of the present application generates.Propylene
Sour film forms separate subregion in PET (deposition has zinc-oxide film) exposure cracking, and adjacent subarea is formed between domain
Crackle, crackle is in random distribution and forms interlaced aperiodicity grid.
It is the structural representation after the mask deposition Ag and ZnO shown in Fig. 4 a, argent and zinc-oxide film such as Fig. 4 b
It is filled in the gap of crackle.If Fig. 4 c are that Fig. 4 b remove after mask that the composite gridding comprising Ag and ZnO that is formed is transparent to lead
Electrode schematic diagram, a plurality of grid lines that argent and zinc oxide are formed be in random distribution, and it is interlaced be distributed formed it is non-
Grid-structure.
In the present embodiment, based on the transparent conductive film of the aperiodicity grid making comprising Ag and ZnO, because light can
Passed through among from grid, have good transmitance in visible near-infrared wave band, improve the optical property of transparent conductive film.
Due to significantly improving transparent lead comprising Ag, its aperiodic structure grid formed in the composite bed of aperiodicity network
The electric property of conductive film, when as heating film, thermal resistance value can reach 228 DEG C of cm2/W, saturating higher than prepared by prior art
The thermal resistance value of bright conductive film, improve the thermal property of transparent conductive film.Further, the present embodiment is using PET as substrate
ZnO-Ag-ZnO nethike embranes/composite bed, by the designing impedance matching of ZnO film and Ag layers there is laminated film certain
Anti-reflection acts on, so as to reduce the transmissivity that the reflection of incident light improves electrode.
Embodiment three
Based on the transparent conductive film formed by above-described embodiment one or two, it can prepare to form PDLC
(PDLC) component.
In this embodiment, substrate is made, with ZnO-Ag-ZnO producing transparent conductive electrode shapes with PET in selection example two
Into transparent conductive film, and using the transparent conductive film prepare PDLC components.Preparation method comprises the following steps：
First, ultraviolet light polymerisable monomer or prepolymer selection ultra-violet curing optical cement (such as NOA 65), nematic liquid crystal
Material selection LC E7 (TNI=92.2 DEG C, Δ n=0.24, Δ ξ=13.0), by NOA 65 and LC E7 according to volume ratio 2: 3
Mixing, while add the silica SiO that average diameter is 20 μm2Microballoon is used as sept to control the thickness of PDLC devices.
Then, LC E7, NOA 65 and silica are sufficiently mixed into clear solution and drop coating is thin in two layers of electrically conducting transparent
Between film (PET makees substrate, with ZnO-Ag-ZnO producing transparent conductives electrode), and keep whole device clamp 5-10min, so as to from
Unnecessary mixture is replaced in device, obtains uniform pdlc film thickness.
Finally, it is 15mW/cm exposed to intensity by PDLC devices2UV light under 10min, solidify the matrix of NOA 65.Certainly,
The outer surface of methanol cleaning device also can use to complete the manufacture of PDLC devices.
As a comparison, the embodiment of the present application is also prepared for including the PDLC components of silver electrode, and preparation process is as follows：
First, there is provided PET flexible substrates, and mask is generated on PET, the mask has or formed aperiodicity to split
Line, and the crackle of non-periodic distribution is interconnected and forms aperiodicity network；
Then, deposit Ag in the gap of the crackle of non-periodic distribution, until the Ag being deposited in gap it is close or
Reach crackle upper surface；
Then, the mask on PET is removed, obtains the transparent conductive film with Ag networks；
Then, drop coating LC E7, NOA 65 and titanium dioxide between two layers of transparent conductive film with Ag networks
The solution that silicon is formed；Finally, treatment with ultraviolet light is carried out to said structure, obtains the PDLC components for including silver electrode.
As Fig. 5 be the embodiment of the present application the PDLC component structure diagrams for including ZnO-Ag-ZnO transparent conductive electrodes,
It is followed successively by from top to bottom：Composite bed (ZnO-Ag-ZnO transparent conductive electrodes), NOA 65, the LC of PET substrate, ZnO and Ag formation
E7 and SiO2PDLC, ZnO-Ag-ZnO transparent conductive electrodes and the PET substrate that microballoon is formed.
Such as the optical property that Fig. 6 is the PDLC components comprising ZnO-Ag-ZnO transparent conductive electrodes prepared as described in Figure 5
Figure, wherein abscissa represent the wavelength (unit nm) of incident light, and ordinate represents the transmitance (unit to incident light
For %).L1 represents transmitance testing result of the PET substrate to incident light, has to the incident light that wavelength is 300-1600nm and connects
Nearly 90% transmitance；L2 represents that the PDLC components comprising ZnO-Ag-ZnO transparent conductive electrodes are examined to the transmitance of incident light
Result is surveyed, there is 85% transmitance to the incident light that wavelength is 300-1600nm, and especially approached in 300-400nm transmitances
Transmitances of the PET to incident light (close to 88%)；L3 represents that the PDLC components comprising Ag electrodes detect to the transmitance of incident light
As a result, it is about 78% to the incident light transmission rate that wavelength is 300-1600nm.Therefore, included using prepared by the application method
The PDLC components of ZnO-Ag-ZnO transparent conductive electrodes have higher translucency.
If Fig. 7 is light of the PDLC components comprising ZnO-Ag-ZnO transparent conductive electrodes under different voltages shown in Fig. 5
Performance map is learned, wherein abscissa represents applied voltage (unit V, volt), and ordinate represents the transmitance (unit to incident light
For %), the wavelength of incident light is set as 400nm.M1 represents the PDLC components comprising ZnO-Ag-ZnO transparent conductive electrodes not
With, to the transmitance testing result of incident light, M2 represents that the PDLC components comprising silver electrode are examined to the transmitance of incident light under voltage
Survey result.It can be seen that from figure, when applied voltage is in 10-20V, two kinds of PDLC components are to the permeability of incident light all with voltage liter
Height, and both light transmissions approach；When applied voltage is gradually changed to 70V from 20V, ZnO-Ag-ZnO transparent conductive electrodes are included
PDLC components to the transmitance of incident light apparently higher than the latter.Further, when applied voltage is gradually changed to 100V from 70V
During change, the transmitance to incident light of two kinds of PDLC components tends towards stability, and includes ZnO-Ag-ZnO transparent conductive electrodes
PDLC components are stable 65% or so to the transmitance of incident light, and the PDLC components comprising silver electrode are to the transmission of incident light
Rate is only 50%.Therefore, the PDLC components of the transparent conductive electrode formed comprising composite bed prepared using the application method are existed
Equally there is preferable optical transmission under voltage effect.The component is used as the intelligent window of solar film battery, response speed
Degree is about 30s, has preferable switch performance and the faster speed of response compared with existing PDLC components.
The principle and its effect of the merely exemplary explanation the application of above-described embodiment, not for limitation the application, extra
Embodiment also falls into the scope of claims.In addition, although the application is described for particular implementation, originally
Art personnel to form and details it should be appreciated that can be changed, without departing from spirit and scope.
Any of the above is incorporated herein by reference interior file and is restricted, and is runed counter to so as not to include with clear and definite disclosure in text
Subject content.
Claims (10)
1. a kind of transparent conductive film, it is characterised in that including flexible substrate and a plurality of net being deposited in the flexible substrate
Ruling, a plurality of grid lines form the transparent conductive electrode of aperiodicity network, and every grid lines includes multiple layer metal
Layer and multilevel oxide film, and the more metal layers and thickness of the multilevel oxide film along the transparent conductive electrode
Degree direction distributes alternately successively.
2. transparent conductive film according to claim 1, it is characterised in that the width of every grid lines is 3-50 μm, and
The thickness comprising the more metal layers is 5-50nm in every grid lines, and it is thin to include the multilevel oxide in every grid lines
The thickness of film is 10-100nm.
3. a kind of preparation method of transparent conductive film, it is characterised in that comprise the following steps：
Flexible substrate is provided, and mask is generated in the flexible substrate, the mask has crackle, and the crackle phase
Intercommunicated formation aperiodicity network；
Metal level and sull continuously are sequentially depositing in the gap of the crackle, until the metal level being deposited in gap
Reach setting thickness with sull；
The mask in the flexible substrate is removed, obtains the transparent conductive film of aperiodicity network.
4. the preparation method of transparent conductive film according to claim 3, it is characterised in that the mask passes through as follows
Method obtains：
Colloidal sol is mixed to form according to setting ratio using persursor material and diluent, obtains mask liquid；
Deposited using the mask liquid in the flexible substrate and form mask film；
The flexible substrate of deposition mas version film is dried in the case where imposing a condition, obtains the mask with aperiodicity crackle
Version.
5. the preparation method of transparent conductive film according to claim 4, it is characterised in that the persursor material is two
Titanium oxide or water soluble acrylic acid.
6. the preparation method of transparent conductive film according to claim 4, it is characterised in that the width of the crackle is 3-
50μm。
7. the preparation method of transparent conductive film according to claim 3, it is characterised in that the sull includes
At least one of zinc-oxide film, WO 3 film, titanium dioxide, ito thin film.
8. a kind of preparation method of PDLC component, including：
Flexible substrate is provided, transparent conductive electrode is formed in the flexible substrate, obtains transparent conductive film, it is described transparent to lead
Electrode includes a plurality of grid lines, and a plurality of grid lines forms aperiodicity network, and every grid lines includes multilayer gold
Belong to layer and multilevel oxide film, and the more metal layers and the multilevel oxide film are along the transparent conductive electrode
Thickness direction distributes alternately successively；
By ultraviolet light polymerizable monomer mixture and with the nematic liquid crystal of its index matching according to mass ratio (1-2): between 3
Mixing, and add silicon dioxide microsphere and be well mixed, form liquid crystal solution；
Between the liquid crystal solution is coated in into two layers of transparent conductive film, and using ultraviolet light to coated with liquid crystal solution
Two layers of transparent conductive film carry out radiation treatment, formed PDLC component.
9. the preparation method of PDLC component according to claim 8, it is characterised in that in the flexible liner
Transparent conductive electrode is formed on bottom to be included：
Mask is generated in the flexible substrate, the mask has crackle, and the crackle is interconnected and forms non-week
Phase property network；
Metal level and sull continuously are sequentially depositing in the gap of the crackle, until the metal level being deposited in gap
Reach setting thickness with sull；
The mask in the flexible substrate is removed, the electrically conducting transparent of aperiodicity network is obtained in the flexible substrate
Electrode.
10. the preparation method of PDLC component according to claim 8, it is characterised in that the ultraviolet light
Ultraviolet light polymerisable monomer in polymerizable monomer mixture includes ultraviolet photopolymerizable silane coupler monomer, polyethylene glycol two
Acrylate, glycol dimethacrylate isobornyl thiocyanoacetate, acrylic acid -3,5, the own ester of 5- trimethyls, senecioate-oxylactone, 1,
At least one of 4- butanediol diacrylates, glycidyl acrylate class monomer.
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