CN106057359B - A kind of preparation method of embedded more orientation metal nano wire transparent conductive films - Google Patents
A kind of preparation method of embedded more orientation metal nano wire transparent conductive films Download PDFInfo
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- CN106057359B CN106057359B CN201610567937.6A CN201610567937A CN106057359B CN 106057359 B CN106057359 B CN 106057359B CN 201610567937 A CN201610567937 A CN 201610567937A CN 106057359 B CN106057359 B CN 106057359B
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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
- H01B13/0013—Apparatus or processes specially adapted for manufacturing conductors or cables for embedding wires in plastic layers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
Abstract
The present invention discloses a kind of preparation method of embedded more orientation metal nano wire transparent conductive films, include the following steps, S1. metal nanometer line solution is added on temporary substrates, arrangement is oriented to metal nanometer line again, the temporary substrates are hydrophilic material, and S2. is surface modified temporary substrates so that temporary substrates become hydrophobicity from hydrophily, the modified substrate metal nano wire film in surface is obtained, S3. is embedded in stripping process：Metal nanometer line is embedded into solidification glue using solidification glue, and carries out the stripping between solidification glue and temporary substrates.The present invention by adjusting temporary substrates hydrophilic and hydrophobic, to obtain one with better conductivity, adhesion, flatness and stability embedded more orientation metal nano wire transparent conductive films.
Description
Technical field
The present invention relates to film conduction fields, more particularly, to a kind of embedded more orientation metal nano wire electrically conducting transparents
The preparation method of film.
Background technology
Transparent conductive film be it is a kind of having both highly conductive and visible light wave range high transparency characteristic basic photoelectric material, extensively
Applied to the photoelectric displays such as display, luminescent device, solar cell, sensor, flexible touch screen field, there is extensive quotient
Industry application prospect.Traditional transparent conductive film is based on indium tin oxide material, although the manufacture of the display photoelectricity based on this material
Technology is quite ripe, however since tin indium oxide contains exotic material, cause its cost higher；And indium tin oxide films
Flexibility it is very poor, it is impossible to be used in prepare flexible display, be extremely restricted in application aspect.Scientist is developed in recent years
It can be used for the conductive material that flexible and transparent is shown, including graphene, metal nanometer line/ball, carbon nanotube and organic polymer
Conductive material etc., wherein metal nanometer line due to have transparency is high, sheet resistance is small, it is cost-effective, can be achieved large area printing and
Base material selectable range extensively waits many advantages.Currently, in numerous metal nanometer lines, nano-silver thread is considered as most having
One of the material of traditional ito transparent electrode may be substituted.
In general, using the transparent conductive film of metal nanometer line material preparation, the nano wire on surface is random distribution
, nano wire distribution is uniform not to the utmost, or even there are some isolated nano wires, leads to the reduction of seepage flow efficiency, to weaken film light
Electrical property.The low problem of nano-silver thread film generally existing stability at present, is easy to fall off, causes electric conductivity in use
Drastically decline；General ameliorative way includes stabilizer, adhesive being added into Nano silver solution, or carry out surface to substrate
Processing increases the adhesion of nano-silver thread and substrate；Chinese patent application discloses 102481757 A of CN and describes a kind of water solubility
The nano-silver thread film of adhesive, improves the adhesion of film.Chinese patent discloses in 102481758 A of CN in nano-silver thread
Cellulose ester polymer is mixed into solution to improve the stability and adhesion of film.In addition to this, nano wire film surface is thick
Rugosity is also significantly larger than ito thin film, this will influence whether performance and the service life of device.Such as OLED, coarse anode will reduce
The external quantum efficiency of device, and make local organic material aging, to reduce service life and the stability of device.Chinese patent
Open 102522145 B of CN describe a kind of multi-layer nano silver wire laminated film to improve adhesion of thin film and stability, wrap
Include PEDOT:PSS and macromolecule adhesion promoting layer.But there is research to point out PEDOT:PSS can deteriorate the stability of AgNWs.Make
Transparent conductive film based on metal nanometer line pushes functionization to, needs a kind of processing procedure that can prepare while having high conductance
Embedded more orientation metal nano wire transparent conductive films of rate, high-adhesiveness, stability and low surface roughness.
Invention content
For the metal nanometer line transparent conductive film of conventional solution coating, there are electric conductivity, stability, adhesions and thick
Rough cosmetic issue, the present invention propose a kind of preparation method of orientation metal nanometer line embedded type laminated film.The present invention is due to adopting
With the metal nanometer line network being orientated, the conductivity of film can be improved, and due to inciting somebody to action under the premise of not influencing light transmittance
Metal nanometer line is partially submerged into substrate interior and forms laminated film so that there are three advantages for this film tool：Make metal nanometer line
Not easily to fall off, polymer wrapped enhances the oxidation resistance of metal nanometer line, Film roughness declines.Improve orientation metal
The stability of nano wire laminated film.
A kind of preparation method of embedded more orientation metal nano wire transparent conductive films further disclosed, including with
Lower step,
S1. the drop coating metal nanometer line solution on temporary substrates is oriented arrangement to metal nanometer line, and described faces
When substrate be hydrophilic material,
S2. temporary substrates are surface modified so that temporary substrates become hydrophobicity from hydrophily, obtain surface and change
Substrate-metal nanometer line laminated film after property,
S3. it is embedded in stripping process：Metal nanometer line is embedded into liquid curing glue, solidification glue is carried out after solidification and is faced
When substrate between stripping.
The temporary substrates are hard substrates or flexible substrate, and carry out hydrophily processing, institute to temporary substrates surface
The hydrophily stated handles preferred corona method, UV ozone method or surface grafting, more preferably UV ozone method.
The preferred soda-lime glass of the hard substrates；The flexible substrate, including but be not limited only to polyacrylate,
Such as polymethacrylates, polyacrylonitrile, polyvinyl alcohol；Polyesters such as polyethylene terephthalate, polycarbonate, are gathered
Mela mine-formaldehyde resin；Aromatic polymer, as polystyrene, polyimides, polyamic acid, polyetherimide, polyphenylene oxide, polyurethane,
Epoxy resin etc.；
The grafting is to connect hydroxyl.
Described aligning is realized by Meyer rubbing method.
Described being surface modified to the temporary substrates for being coated with nano wire specially modifies temporary substrates, institute
Decorative material is organo-silicon compound, and described organo-silicon compound one end carries hydrolyzable group, and the other end carries
Hydrophobic grouping.
The hydrolyzable group is-Cl ,-OCH3、 -OC2H5、 -OC2H4OCH3、 -OSi(CH3)3Or CH3COO-,
Preferably-Cl, the hydrophobic grouping are-CH3Or-CF3。
The insertion stripping process is that the modified substrate-metal nanowire thin-films in the surface that obtains to S2 cure
Glue is coated with, and nano silver-solidification glue laminated film that metal nanometer line is partially submerged into is formed by stripping after solidification.
The insertion stripping process be first solidification glue is coated in target substrate, then with S2 obtain surface it is modified
Substrate-metal nanowire thin-films fitting target substrate is removed from temporary substrates by curing schedule, obtain be orientated more
Metal nanometer line-polymer-target substrate laminated film.
The metal nanometer line is including but not limited to Au, Ag, Cu, Fe, Ni, Co or alloy nano metal wire and its mixes
Condensation material.
Embedded more orientation metal nano wire transparent conductive films made from a kind of above-mentioned preparation method are disclosed again, it is described
Transparent conductive film in metal nanometer line be multi-direction to align in the film layer that solidification glue is formed.
Compared with prior art, the invention has the advantages that：
1. the present invention is first, Meyer rod coating is used on temporary substrates, the metal nano of orientation is obtained after dry out solvent
Gauze network, repeats the above steps, you can obtains more orientation nano gauze networks；Then, it is received by being surface-treated the change of selectivity
The hydrophilic and hydrophobic of rice noodles-temporary substrates, keeps substrate hydrophobic and the hydrophilic and hydrophobic of nano-silver thread is uninfluenced；Finally, pass through coating
Solidification glue simultaneously cures, removes, and nano-silver thread is made to shift and be partially submerged into solidification glue, and orientation, Embedded metal is made
Nano wire transparent conductive film.
2. hydrophilic substrate is conducive to metal nanometer line being uniformly distributed in substrate surface, is conducive to nano wire and is formed
It aligns；And hydrophobic substrate is conducive to the stripping of solidification glue；Therefore the present invention is obtained by adjusting hydrophilic and hydrophobic
The embedded more orientation metal nano wire transparent conductive films aligned with more preferable effect.
It, can be in the feelings for not influencing light transmittance 3. the conductive network that used metal nanometer line is ordered into, feature are
Under condition, electric conductivity is improved.
4. metal nanometer line is finally fixed in a manner of partial embedding in the substrate, improve between nano wire and substrate
Stick, nano-silver thread is not easily to fall off, and has had both high conductivity.
5. metal nanometer line insertion polymer makes nano wire most surfaces and air insulated, nano wire is improved
Antioxygenic property.Polymer wrapped can also enhance adhesion, Bending Stability.
6. embedded more orientation metal nano wire transparent conductive films prepared by have both high conductivity, high transparency, height
Flexibility, stability and smooth surface, can be applied to flexible touch screen, solar cell, organic light emitting diode etc.
Photoelectric device.
Description of the drawings
Fig. 1 is that orientation nano silver wire network is coated on soda-lime glass.
Fig. 2 is double orientation nano-silver thread network.
Fig. 3 is water contact angle of the glass in HMDS before and after the processing
Fig. 4 is that nano-silver thread-glass is bonded with the PET for being coated with UV glue.
Fig. 5 is to carry out UV solidifications to glass-nano-silver thread-solidification glue-PET construction.
Fig. 6 is laminated film stripping process.
Fig. 7 is that the embedded composite conductive thin film schematic diagram of nano-silver thread and SEM scheme.
Specific implementation mode
The preferred embodiments of the present invention will be described in detail below in conjunction with the accompanying drawings, so that advantages and features of the invention are more
It is easily readily appreciated by one skilled in the art, to make apparent define to protection scope of the present invention.
1 temporary substrates hydroxylating of embodiment
Present case handles temporary substrates by hydroxylating, so that substrate surface hydrophily is enhanced, this is conducive to metal nanometer line
In being uniformly distributed for substrate surface, it is also beneficial to be formed and aligns.In addition, hydroxyl provides reaction subsequently to graft anti-stick group
Site；Used temporary substrates can be flexible substrate or rigid substrate；Used hydroxylating processing can passing through
Learn solution surface grafting or UV ozone facture etc..Two embodiments are provided individually below to be illustrated：
If used temporary substrates are polyethylene terephthalate flexible (PET).It, will by lifting infusion process
Its immerse APTES- toluene mixed solutions, APTES a concentration of 5wt%, dip time 10min, later with 2000 μm/s of speed from
APTES lifts out.Gained PET film contact angle becomes 40 ° from 70 °；100 degrees Celsius of baking processing is carried out to film, when
Between about 5 min, later UVO handle about 5 min, make substrate generate great amount of hydroxy group；The water contact angle of treated PET is dropped from 40 °
It is 5 ° or so.
If temporary substrates are pure soda-lime glass, acetone, ethyl alcohol, water is first used sequentially to distinguish ultrasound 15 minutes with removal
Surface organic matter, then several minutes are dried after being dried up with nitrogen gun, finally handled two minutes with UV ozone.Treated glass
It can be flooded profit completely, illustrate that glass shows rich in hydroxyl group.
The preparation of 2 double orientation nano-silver thread transparent membrane of embodiment
For one-dimensional metal nano wire, using micro- line on Meyer stick to the guiding function of nano wire during rod coating,
Realize the control being orientated to nano wire.Film is dried after single application, then carries out nano thread ordered coating next time again,
The orderly metal nanometer line of double orientation is can be obtained, uniform conductive network is formed.
Present case selects hydroxylated glass as temporary substrates, is prepared as metal nanometer line using nano-silver thread more
The orderly conductive film of layer.Used nano-silver thread average diameter is 34 nm, and length is 18 μm, and nano-silver thread is dispersed in ethyl alcohol
Solution, a concentration of 10 mg/ml.Nano-silver thread dispersion liquid is with anhydrous isopropyl alcohol according to 1：4 mass ratio mixing, ultrasound is after 2 minutes
Shake up dispersion.
Present case selects the Meyer stick of 12 μm of line footpath, about 10 μm of wet-film thickness after coating speed 5 cm/s. coatings.In order to
Alcohol solvent is volatilized, transfers substrates on 80 DEG C of hot plates and toasts about 2 minutes.This step is taking for curing nano silver wire
To making it not influenced by being coated with next time.A step coating is carried out after solidification, the direction that nano-silver thread is orientated can be by Meyer stick
It is coated with direction controlling.The direction of coating twice of present case is mutually perpendicular to.After second is coated with, transfers them to 80 DEG C of hot plates and carry out
Baking 2 minutes, the schematic diagram being coated with twice is as shown in Figure 1.
Fig. 2 illustrates the nano-silver thread conductive film that case 1 is coated with twice, it can be seen that there are two mainly take nano-silver thread
To two orientations are mutually perpendicular to.Nano-silver thread is oriented along central orientation in certain distribution, and central orientation is defined as Meyer here
The direction of rod coating.The square resistance average value of two layers of ordered nano silver wire of present case is 25 ohm/sq, than in identical face
The square resistance of random distribution nano-silver thread declines about 50% under density.
The 3 close and distant water process of selectivity of embodiment
Committed step of the present invention is to carry out selective modification to nano-silver thread-temporary substrates, i.e., is only carried out to modification substrate
Hydrophobic modification, without modifying nano-silver thread itself.
It is preferred that hexamethyldisilane is as decorative material.2 ml hexamethyldisilane solution are drawn, culture dish, juxtaposition are instilled
In closed baking oven, temperature is set as 70 DEG C；Above-mentioned ordered nano silver wire-hydroxylating glass is placed in superjacent.
In solution evaporation process, the imino group of hexamethyldisilane solution is reacted with the hydroxyl of glass surface, production
Raw trimethylsiloxy group group.In order to fully react, sedimentation time is set as 20 minutes.Pure nano-silver thread does not have hydroxyl, therefore not
Meeting and silane group, surface will not hydrophobizations.The step for purpose be in order to reduce the surface energy of glass substrate, to drop
Adhesion between low glass and solidification glue.
Surface energy can be characterized with water contact angle, and substrate surface can be smaller, and water is bigger in contact angle above.It is hydroxylated
Glass can be by deionized water complete wetting glass.It is handled after twenty minutes by HMDS, contact angle increases to 76 °.Such as Fig. 3 institutes
Show.
The performance of coating, the solidification, stripping and laminated film of 4 solidification glue of embodiment
The solidification glue used is ultraviolet for epoxy resin（UV）Solidification glue, using the Meyer stick of #6 um in target substrate PET
On be coated.Then the PET of solidification glue and above-mentioned ordered nano silver wire-glass by the close and distant water process of selectivity are coated with
Glass is bonded.（Fig. 4）
After coating optical power density be 15 mW/cm2UV lamp under expose 1 min, so that cross linking of epoxy resin is cured, it
100 ° of hot plates are used to toast 5 minutes afterwards, so far solidification glue is fully cured.（Fig. 5）
It is finally stripping technology.Solidification rear film structure is PET- solidification glues-ordered nano silver wire-glass.Pass through stripping
（Fig. 6）, become ordered nano silver wire-solidification glue-PET construction, nano-silver thread at this time is partially submerged into inside solidification glue（Fig. 7）.
In addition, in order to compare, we are prepared for pure nano-silver thread film on PET（AgNWs/PET）.In preparation process
In, nano-silver thread solution concentration is consistent with solution used in transfer method, is 2 mg/ml.Meyer stick thread pitch, rod coating speed with turn
Shifting method is identical.After being coated in PET film, it is transferred to 80 DEG C of hot plates and toasts 2 minutes.
Obtained film uses the square resistance of four probe method testing film, and corresponding light transmittance is using ultraviolet-visible point
Light photometer measurement takes wavelength 550nm to deserved light transmittance to quantify film light transmission.Film surface appearance, which is respectively adopted, to be swept
Electron microscope, atomic force microscope are retouched to observe, wherein surface roughness refers to r.m.s. roughness Rq.Adhesion is using wide
For the adhesion special test adhesive tape of 12.7cm（3M）To test.Stick the adhesive tape all more renewed, adhesive tape stripping and film every time
At 90 degree, test 10 times in total.Film antioxygenic property is tested using high temperature and humidity case, and temperature is 85 DEG C, relative humidity
85%, 7 days in total.Film bends test is bent 1000 times using self-control curved platform, 3 mm of bending curvature radius.Adhesion,
Before and after crooked test, high temperature and humidity test, its square resistance of four-point probe measurment is used respectively.
Table one：The silver wire of the orientation nano prepared by the embodiment of the present invention-solidification glue-PET film is listed to receive with commonly pure
Photoelectric properties, adhesion, resistance to song, high temperature and humidity, the surface roughness of rice silver wire/PET film.R in tableSIt is square resistance,
RS0It is initial square resistance.ΔR/RS0=(RS-RS0)/RS0
It can find that embedded more orientation metal nano wire transparent conductive films of the present invention are ensureing thoroughly by above table
In the case of light rate, electric conductivity, adhesion and antioxygenic property are increased substantially, while reducing the flatness of film.
Claims (11)
1. a kind of preparation method of embedded more orientation metal nano wire transparent conductive films, which is characterized in that including following step
Suddenly,
S1. metal nanometer line solution is added on temporary substrates, then arrangement, the interim lining are oriented to metal nanometer line
Bottom is hydrophilic material,
S2. temporary substrates are surface modified so that temporary substrates become hydrophobicity from hydrophily, and it is modified to obtain surface
Substrate-metal nanometer line laminated film, decorative material used are organo-silicon compound, organo-silicon compound one end band
There are hydrolyzable group, the other end to carry hydrophobic grouping,
S3. it is embedded in stripping process：Metal nanometer line is embedded into liquid curing glue, solidification glue and temporary substrates are carried out after solidification
Between stripping.
2. the preparation method of embedded more orientation metal nano wire transparent conductive films according to claim 1, feature
It is, the temporary substrates include hard substrates or flexible substrate, and carry out hydrophily processing to temporary substrates surface, described
Hydrophily processing be corona method, UV ozone method or surface grafting.
3. the preparation method of embedded more orientation metal nano wire transparent conductive films according to claim 2, feature
It is, hydrophily processing is UV ozone method.
4. the preparation method of embedded more orientation metal nano wire transparent conductive films according to claim 2, feature
It is, the hard substrates are soda-lime glass；The flexible substrate is polyacrylate, polyesters or aromatic series polymerization
Object, the polyacrylate are polymethacrylates, polyacrylonitrile or polyvinyl alcohol；The polyesters are poly- terephthaldehyde
Sour glycol ester, polycarbonate or polyoxymethylene resin；The aromatic polymer be polystyrene, polyimides, polyamic acid,
Polyetherimide, polyphenylene oxide, polyurethane or epoxy resin；The grafting is to connect hydroxyl.
5. the preparation method of embedded more orientation metal nano wire transparent conductive films according to claim 1, feature
It is, described aligning is realized by Meyer rubbing method.
6. the preparation method of embedded more orientation metal nano wire transparent conductive films according to claim 1, feature
It is, the hydrolyzable group is-Cl ,-OCH3、-OC2H5、-OC2H4OCH3、-OSi(CH3) 3 or CH3COO-, it is described
Hydrophobic grouping is-CH3Or-CF3。
7. the preparation method of embedded more orientation metal nano wire transparent conductive films according to claim 6, feature
It is, the hydrolyzable group is-Cl.
8. the preparation method of embedded more orientation metal nano wire transparent conductive films according to claim 1, feature
It is, the insertion stripping process is the modified substrate-metal nanowire thin-films progress solidification glue in the surface that obtains to S2
Coating forms more orientation metal nano wire-solidification glue laminated films that metal nanometer line is partially submerged into after solidification by stripping.
9. the preparation method of embedded more orientation metal nano wire transparent conductive films according to claim 1, feature
Be, the insertion stripping process be first solidification glue is coated in target substrate, then with S2 obtain surface it is modified
Target substrate is removed from temporary substrates by curing schedule, obtains the metals being orientated more by substrate-metal nanometer thin film fitting
Nano wire-solidification glue-target substrate laminated film.
10. the preparation method of embedded more orientation metal nano wire transparent conductive films according to claim 1, feature
It is, the metal nanometer line is Au, Ag, Cu, Fe, Ni, Co, alloy nano metal wire or its mixing material.
11. embedded more orientation metal nano wire electrically conducting transparents made from a kind of any preparation methods of claim 1-10
Film, which is characterized in that the metal nanometer line in embedded more orientation metal nano wire transparent conductive films is multi-party
To aligning in the film layer that solidification glue is formed.
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| CN106601382B (en) * | 2016-12-15 | 2018-06-29 | 华南理工大学 | A kind of preparation method of flexible transparent conducting film |
| CN106710451B (en) * | 2017-03-06 | 2019-08-06 | 京东方科技集团股份有限公司 | The support shaft production method and flexible display panels of flexible display panels |
| CN108074660B (en) * | 2017-12-14 | 2019-06-07 | 上海交通大学 | A kind of composite and flexible transparent conductive film and preparation method thereof |
| CN112074965A (en) * | 2018-03-16 | 2020-12-11 | 株式会社东芝 | Method and apparatus for manufacturing transparent electrode |
| CN109065724B (en) * | 2018-07-18 | 2020-02-04 | 河南大学 | Mo-titanium dioxide-AgNWs flexible perovskite solar cell and preparation method thereof |
| CN110021462B (en) | 2019-05-17 | 2020-05-05 | 青岛五维智造科技有限公司 | Manufacturing method and application of embedded metal grid flexible transparent electrode |
| CN110708406B (en) * | 2019-10-09 | 2021-05-18 | Oppo广东移动通信有限公司 | Shell, preparation method thereof and electronic equipment |
| CN112053800B (en) * | 2020-07-31 | 2022-07-01 | 山东大学 | Embedded high-temperature-resistant transparent conductive film, and preparation method and application thereof |
| CN114095681A (en) * | 2021-11-23 | 2022-02-25 | 深圳市华科创智技术有限公司 | Nano silver wire flexible touch screen television |
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| JP5169389B2 (en) * | 2007-04-19 | 2013-03-27 | 三菱マテリアル株式会社 | Method for manufacturing conductive reflective film |
| CN102087884A (en) * | 2009-12-08 | 2011-06-08 | 中国科学院福建物质结构研究所 | Flexible transparent conductive film based on organic polymers and silver nanowires and preparation method thereof |
| CN103700430B (en) * | 2013-12-25 | 2017-12-05 | 中山大学 | A kind of conductive film being distributed in order and its manufacture method |
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