CN106563632A - Low-temperature preparation method of metal nanowire transparent conducting thin film - Google Patents
Low-temperature preparation method of metal nanowire transparent conducting thin film Download PDFInfo
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- CN106563632A CN106563632A CN201610944618.2A CN201610944618A CN106563632A CN 106563632 A CN106563632 A CN 106563632A CN 201610944618 A CN201610944618 A CN 201610944618A CN 106563632 A CN106563632 A CN 106563632A
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- nanometer line
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/02—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to macromolecular substances, e.g. rubber
- B05D7/04—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to macromolecular substances, e.g. rubber to surfaces of films or sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2203/00—Other substrates
- B05D2203/30—Other inorganic substrates, e.g. ceramics, silicon
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Abstract
The invention discloses a low-temperature preparation method of a metal nanowire transparent conducting thin film which is ultralow in roughness and high in conductivity. The method comprises the steps of preparing a transparent flexible buffer layer of a certain thickness on the surface of a substrate; uniformly laying and extending metal nanowires onto the flexible buffer layer; and after low-temperature drying is completed, completely welding the metal nanowires to one another through a method of conducting normal-temperature pressurization on the metal nanowires, so that after inter-wire contact resistance is basically eliminated, the thin film ultrahigh in conductivity is obtained. Meanwhile, the metal nanowires are embedded into the flexible buffer layer, so that surface roughness of the thin film is greatly lowered. The method is convenient to operate and capable of being used for large-scale production. The whole procedure is implemented in a low-temperature environment, and the effect of applying the transparent conducting thin film to a flexible high polymer substrate which is not resistant to high temperature is achieved; and meanwhile, the thin film is ultralow in surface roughness, ultrahigh in conductivity and high in light transmittance and can be applied to the photoelectric fields such as organic light emitting diodes, sensors and solar cells as an electrode.
Description
Technical field
The present invention relates to conductive film preparation field, specially a kind of low temperature preparation has ultralow roughness high conductivity
The method of metal nanometer line transparent conductive film.
Background technology
Transparent conductive film is one of indispensable part of electronics and IT products, it is now widely used with ITO as generation
The metal-oxide film of table because its complicated process of preparation, high cost, it is non-flexible the problems such as meet with application development bottleneck.It is suitable
Electronic product flexibility, lightening, portability development trend are answered, for the research of transparent conductive film new material becomes heat
Point.
Material at present with development potentiality is numerous, and wherein metal nanometer line is because its electric conductivity is high, transparency is good, do not choose base
Bottom, is applicable to the extensive attention that the advantages such as large area production have obtained industry.But from the point of view of current research situation, based on metal
The transparent conductive film of nano wire still has problems to need to solve.One is contact resistance problem, welds incomplete between nano wire,
Have a strong impact on film overall conductivity；Two is big, high for the surface roughness requirements organic light-emitting diodes of surface roughness
Application difficult in the middle of the devices such as pipe；Three is weak with the associativity of substrate, is easily stripped off, totally unfavorable in the middle of practical application.
For problem above, many solutions are suggested.To solve the problems, such as contact resistance between line, conducting medium is added,
What such as Chinese patent CN104810079A was reported wraps up film forming by nano silver wire with conducting polymer, while improving film
Electric conductivity and the associativity with substrate, but fail to realize being welded between line, surface roughness certainly will be caused excessive；And for example, with polymerization
Thing transfer method solves the problems, such as surface roughness, and what such as Chinese patent CN102270524A was reported will by way of pressurized, heated
Nano silver wire conductive network is embedded in thermoplastic transparent polymer surfaces, but contact resistance is big between nano wire, affects film entirety
Electric conductivity；For another example, one layer of polysaccharose substance of covering on metal nanowire thin-films of Chinese patent CN104934094A reports, increases
The adhesiveness of strong nano wire and substrate, but because polysaccharose substance it is non-conductive, therefore the relatively simple gold of the overall electric conductivity of laminated film
Certainly will decrease for category nano wire film.In addition, it is contemplated that the transparent conductive film based on metal nanometer line is soft in future
Application in the middle of property device, its substrate is mostly the polymeric material of non-refractory, seeks one kind and can cross to solve at low ambient temperatures
Certainly the method for the problems referred to above is extremely urgent.
Therefore, those skilled in the art is devoted to developing a kind of preparation at low temperature and with ultralow roughness high connductivity
The method of the metal nanometer line transparent conductive film of property.
The content of the invention
In view of deficiency of the prior art, the technical problem to be solved in the present invention is to provide one kind and can grasp at low temperature
The metal nanometer line electrically conducting transparent that work, electric conductivity are high, roughness is low and substrate associativity is good, light transmittance is high and simple to operate is thin
The preparation method of film.
For achieving the above object, the invention provides a kind of low temperature preparation method of metal nanometer line transparent conductive film,
Comprise the following steps：
Step 1, prepare one in the spin-coated method of substrate surface or spraying process or knife coating that clean up or dipping-pulling method
Determine the supple buffer layer precursor thin-film of thickness, solidification and low temperature drying；
Step 2, by the spin-coated method of metal nanometer line suspension or spraying process or knife coating or dipping-pulling method described soft
Property cushion surface prepare metal nanowire thin-films, then rinsing drying, repeat this step can prepare multiple layer metal nano wire
Film；
Step 3, at normal temperatures to film surface apply pressure, keep a period of time after discharge, metal can be prepared
Nano wire is transparent to lead film.
Further, the supple buffer layer includes polymer, polymeric dielectric and surfactant.
Further, the polymer is polyvinyl alcohol, polyvinylpyrrolidone, polyvinyl butyral resin, poly- methyl-prop
It is e pioic acid methyl ester, polyethylene terephthalate, PEN, phenolic resin, epoxy resin, polyurethane, poly-
One kind in dimethyl siloxane, polyethylene, polypropylene, polyvinyl chloride；
The polymer dielectric be polychloride diallyl dimethyl amine-acrylamide, polyacrylate, alginate,
It is polyvinyl sulfonate, poly- to the one kind in vinylbenzenesulfonic acid salt, polyallylamine hydrochlorides；
The surfactant is polyoxyalkylenated primary, secondary, tertiary fatty amine salt, with amine root, quaternary amine root, imidazoles and triazine
Heterocyclic surfactant, and polyacrylic acid, polystyrolsulfon acid, polyvinyl sulfonic acid, polymethylacrylic acid, polyethylene phosphorus
One kind in acid, and carboxylate, sulfuric acid, sulfonate and phosphate ester salt.
Further, the supple buffer layer thickness is 50-600nm.
Further, the metal nanometer line includes nano silver wire, copper nano-wire and nanowires of gold, metal nanometer line it is outstanding
Turbid liquid is among one or more solvent that above-mentioned metal nanometer line is dispersed in deionized water, ethanol, ethylene glycol, acetone.
Further, the applying pressure is 0.5MPa-50MPa, and the retention time is 10s-60min.
Further, the substrate is hard base or flexible base board；The hard substrate be simple glass, quartz glass or
One kind in lucite；The flexible base board is polydimethylsiloxanefilm film layer (PDMS), PET
Film layer (PET), PEN film layer (PEN), polymethyl methacrylate film layer (PMMA) or poly- inclined
One kind in dichloroethylene film layer (PVDC).
Further, the number of times of repeat step 2 is 1-20 time.
Further, the turbid liquid concentration of the metal nanometer line is 0.01mg/ml-10mg/ml.
Further, the temperature of the drying is 30-100 DEG C, and drying time is 1-100min.
As shown in figure 1, the present invention adopts laminated film technology, add in substrate and metal nanowire thin-films interlayer flexible slow
Layer is rushed, realizes being welded between nano wire by room temperature pressurization, reduce contact resistance, and the embedded supple buffer layer of metal nanometer line is worked as
In, so that metal nanometer line has huge lifting, Neng Gouman with the associativity of substrate while substantially reducing surface roughness
The lightening development need of sufficient electronic device flexibility.
Beneficial effects of the present invention are as described below：
1st, low temperature preparation of the invention has the side of the metal nanometer line transparent conductive film of ultralow roughness high conductivity
Method, by using laminated film technology, as shown in Fig. 2 adding supple buffer layer in substrate and metal nanowire thin-films interlayer, leading to
Cross room temperature pressurization to realize being welded between nano wire, and make in the middle of the embedded supple buffer layer of metal nanometer line, ensureing the same of light transmittance
Shi Youxiao reduces contact resistance (as shown in Figure 3) between metal nanometer line, and roughness of film, lifts metal nanometer line and base
The binding ability of plate such that it is able to alternative metals oxide electrode material, is applied in the middle of the making of photoelectric device.
2nd, the preparation method process is simple, ambient operation, preparation condition is easily controlled, and substrate is not required, repeats
Property it is high, disclosure satisfy that the lightening development need of flexibility, be applicable to large-scale production, potential promotion metal nanometer line
Application development in the middle of the photoelectric devices such as Organic Light Emitting Diode (OLED), sensor, solar cell.
The technique effect of the design, concrete structure and generation of the present invention is described further below with reference to accompanying drawing, with
It is fully understood from the purpose of the present invention, feature and effect.
Description of the drawings
Fig. 1 is the structural representation of the metal nanometer line transparent conductive film of a preferred embodiment of the present invention；
Fig. 2 be the SEM side in supple buffer layer and metal nanometer line laminated film before and after pressurization and
Sectional drawing；
Fig. 3 is in supple buffer layer and light transmittance and sheet resistance change curve of the metal nanometer line laminated film before and after pressurization
Figure.
Specific embodiment
In order to preferably illustrate the present invention, the present invention is specifically described below by embodiment, but the present invention's is interior
With following examples are not limited solely to, it is nonessential that those skilled in the art makes some according to the content of the invention described above
Modifications and adaptations, belong to protection scope of the present invention.
Embodiment 1：
Step one, pet substrate deionized water, ethanol, isopropanol are cleaned by ultrasonic repeatedly, and are processed with oxygen plasma
20 minutes, dried with nitrogen；Polyvinylalcohol solids particle heating stirring is dissolved in into water and is made into the solution that concentration is 10mg/ml,
Adopt spraying process pet substrate surface prepare thickness for 150nm transparent membrane, 60 DEG C drying 20min；
Step 2, metal silver nanowires are dispersed in the middle of ethanol prepare 3mg/ml metal silver nanowires it is suspended
Liquid, is sprayed at polyvinyl alcohol film surface, and 75 DEG C of drying 20min, repeat this step 5 time after rinsing, obtains multiple layer metal silver and receives
Rice noodles film；
Step 3, the laminated film surface room temperature prepared in step 2 apply the pressure of 5MPa, after keeping 10min
Release, obtains the metal silver nanowires transparent conductive film of ultralow roughness high conductivity.
Embodiment 2：
Step one, glass substrate deionized water, ethanol, isopropanol are cleaned by ultrasonic repeatedly, and are used at oxygen plasma
Reason 20 minutes, is dried with nitrogen；Polyvinylpyrrolidone is dissolved in into water and is made into the solution that concentration is 8mg/ml, using spin-coating method
The transparent membrane that thickness is 200nm, 70 DEG C of drying 15min are prepared in glass baseplate surface；
Step 2, metal silver nanowires are dispersed in the middle of isopropanol prepare 5mg/ml metal silver nanowires it is suspended
Liquid, is sprayed at polyvinylpyrrolidone film surface, and 70 DEG C of drying 15min, repeat this step 3 time after rinsing, obtains multilayer gold
Category nano silver wire film；
Step 3, the laminated film surface room temperature prepared in step 2 apply the pressure of 7MPa, after keeping 5min
Release, obtains the metal silver nanowires transparent conductive film of ultralow roughness high conductivity.
Embodiment 3：
Step one, pmma substrate deionized water, ethanol, isopropanol are cleaned by ultrasonic repeatedly, and use oxygen plasma
Body is processed 20 minutes, is dried with nitrogen；Sodium Polyacrylate is dissolved in into water and is made into the solution that concentration is 5mg/ml, using spraying process
The transparent membrane that thickness is 100nm, 60 DEG C of drying 20min are prepared on pmma substrate surface；
Step 2, Nano line of metal copper is dispersed in the middle of ethanol prepare 5mg/ml Nano line of metal copper it is suspended
Liquid, is spun on Sodium Polyacrylate film surface, and 75 DEG C of drying 20min, repeat this step 4 time after rinsing, obtain multiple layer metal copper
Nano wire film；
Step 3, the laminated film surface room temperature prepared in step 2 apply the pressure of 10MPa, keep 20min it
After discharge, obtain the Nano line of metal copper transparent conductive film of ultralow roughness high conductivity.
Embodiment 4：
Step one, PEN substrate deionized waters, ethanol, isopropanol are cleaned by ultrasonic, and are processed with oxygen plasma repeatedly
20 minutes, dried with nitrogen；Sodium alginate is dissolved in into water and is made into the solution that concentration is 2mg/ml, using knife coating in PEN bases
Plate surface prepares the transparent membrane that thickness is 400nm, after bivalent metal ion solidification, 70 DEG C of drying 15min；
Step 2, Nano line of metal copper is dispersed in the middle of ethanol prepare 10mg/ml Nano line of metal copper it is suspended
Liquid, is sprayed at ALG sodium film surface, and 70 DEG C of drying 20min, repeat this step 3 time after rinsing, obtain multiple layer metal copper
Nano wire film；
Step 3, the laminated film surface room temperature prepared in step 2 apply the pressure of 30MPa, after keeping 5min
Release, obtains the Nano line of metal copper transparent conductive film of ultralow roughness high conductivity.
Embodiment 5：
Step one, PDMS substrate deionized water, ethanol, isopropanol are cleaned by ultrasonic repeatedly, and are used at oxygen plasma
Reason 20 minutes, is dried with nitrogen；Lauryl sodium sulfate is dissolved in into water and is made into the solution that concentration is 5mg/ml, using spraying process
The transparent membrane that thickness is 500nm, 60 DEG C of drying 20min are prepared on PDMS substrate surface；
Step 2, metal nanowires of gold is dispersed in the middle of isopropanol prepare 3mg/ml metal nanowires of gold it is suspended
Liquid, is sprayed at lauryl sodium sulfate film surface, and 70 DEG C of drying 20min, repeat this step 5 time after rinsing, obtains multilayer gold
Category nanowires of gold film；
Step 3, the laminated film surface room temperature prepared in step 2 apply the pressure of 50MPa, after keeping 3min
Release, obtains the metal nanowires of gold transparent conductive film of ultralow roughness high conductivity.
The preferred embodiment of the present invention described in detail above.It should be appreciated that the ordinary skill of this area is without the need for wound
The property made work just can make many modifications and variations with design of the invention.Therefore, all technical staff in the art
Pass through the available technology of logical analysis, reasoning, or a limited experiment on the basis of existing technology under this invention's idea
Scheme, all should be in the protection domain being defined in the patent claims.
Claims (10)
1. a kind of low temperature preparation method of metal nanometer line transparent conductive film, it is characterised in that comprise the following steps：
Step 1, prepare in the spin-coated method of substrate surface or spraying process or knife coating that clean up or dipping-pulling method it is certain thick
The supple buffer layer precursor thin-film of degree, solidification and low temperature drying；
Step 2, by the spin-coated method of metal nanometer line suspension or spraying process or knife coating or dipping-pulling method described flexible slow
The surface for rushing layer prepares metal nanowire thin-films, then rinsing drying, and repeating this step can prepare multiple layer metal nano wire film；
Step 3, at normal temperatures to film surface apply pressure, keep a period of time after discharge, metal nano can be prepared
Line transparent conductive film.
2. the low temperature preparation method of metal nanometer line transparent conductive film as claimed in claim 1, it is characterised in that described soft
Property cushion include polymer, polymeric dielectric and surfactant.
3. the low temperature preparation method of metal nanometer line transparent conductive film as claimed in claim 2, it is characterised in that described poly-
Compound is polyvinyl alcohol, polyvinylpyrrolidone, polyvinyl butyral resin, polymethyl methacrylate, poly terephthalic acid second
Diol ester, PEN, phenolic resin, epoxy resin, polyurethane, dimethyl silicone polymer, polyethylene, poly- third
One kind in alkene, polyvinyl chloride；
The polymer dielectric is polychloride diallyl dimethyl amine-acrylamide, polyacrylate, alginate, poly- second
It is alkene sulfonate, poly- to the one kind in vinylbenzenesulfonic acid salt, polyallylamine hydrochlorides；
The surfactant is polyoxyalkylenated primary, secondary, tertiary fatty amine salt, with the miscellaneous of amine root, quaternary amine root, imidazoles and triazine
Ring class surfactant, and polyacrylic acid, polystyrolsulfon acid, polyvinyl sulfonic acid, polymethylacrylic acid, polyvinyl, with
And the one kind in carboxylate, sulfuric acid, sulfonate and phosphate ester salt.
4. the low temperature preparation method of metal nanometer line transparent conductive film as claimed in claim 1, it is characterised in that described soft
Property buffer layer thickness be 50-600nm.
5. the low temperature preparation method of metal nanometer line transparent conductive film as claimed in claim 1, it is characterised in that the gold
Category nano wire includes nano silver wire, copper nano-wire and nanowires of gold, and the suspension of metal nanometer line is above-mentioned metal nanometer line point
Among being dispersed in one or more solvent in deionized water, ethanol, ethylene glycol, acetone.
6. the low temperature preparation method of metal nanometer line transparent conductive film as claimed in claim 1, it is characterised in that described to apply
Plus pressure is 0.5MPa-50MPa, the retention time is 10s-60min.
7. the low temperature preparation method of metal nanometer line transparent conductive film as claimed in claim 1, it is characterised in that the base
Plate is hard base or flexible base board；The hard substrate is the one kind in simple glass, quartz glass or lucite；It is described soft
Property substrate is polydimethylsiloxanefilm film layer (PDMS), polyethylene terephthalate thin film layer (PET), poly- naphthalenedicarboxylic acid second
In terephthalate films layer (PEN), polymethyl methacrylate film layer (PMMA) or polyvinylidene chloride film layer (PVDC)
It is a kind of.
8. the low temperature preparation method of metal nanometer line transparent conductive film as claimed in claim 1, it is characterised in that repeat to walk
Rapid 2 number of times is 1-20 time.
9. the low temperature preparation method of metal nanometer line transparent conductive film as claimed in claim 1, it is characterised in that the gold
The turbid liquid concentration of category nano wire is 0.01mg/ml-10mg/ml.
10. the low temperature preparation method of metal nanometer line transparent conductive film as claimed in claim 1, it is characterised in that described
The temperature of drying is 30-100 DEG C, and drying time is 1-100min.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108777915A (en) * | 2017-05-30 | 2018-11-09 | 杨军 | The effective production process of highly conductive single layer and multilayer circuit of the connection without drilling |
| CN109298045A (en) * | 2018-10-23 | 2019-02-01 | 大连大学 | A kind of silver nanowires based on PDMS/nanogold combination electrode and preparation method thereof |
| CN109415811A (en) * | 2016-08-19 | 2019-03-01 | 富士胶片株式会社 | Laminar substrate, conductive membrane, touch panel sensor, touch panel are plated by coating formation composition, by coating, band |
| CN109559843A (en) * | 2018-11-23 | 2019-04-02 | 合肥京东方光电科技有限公司 | Transparent flexible electrode film, production method and transparent flexible electrode |
| CN110783025A (en) * | 2019-09-27 | 2020-02-11 | 江苏科技大学海洋装备研究院 | Oxidation-resistant conductive copper nanowire film and preparation method and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109415811A (en) * | 2016-08-19 | 2019-03-01 | 富士胶片株式会社 | Laminar substrate, conductive membrane, touch panel sensor, touch panel are plated by coating formation composition, by coating, band |
| CN108777915A (en) * | 2017-05-30 | 2018-11-09 | 杨军 | The effective production process of highly conductive single layer and multilayer circuit of the connection without drilling |
| CN109298045A (en) * | 2018-10-23 | 2019-02-01 | 大连大学 | A kind of silver nanowires based on PDMS/nanogold combination electrode and preparation method thereof |
| CN109559843A (en) * | 2018-11-23 | 2019-04-02 | 合肥京东方光电科技有限公司 | Transparent flexible electrode film, production method and transparent flexible electrode |
| CN110783025A (en) * | 2019-09-27 | 2020-02-11 | 江苏科技大学海洋装备研究院 | Oxidation-resistant conductive copper nanowire film and preparation method and application thereof |
| CN110783025B (en) * | 2019-09-27 | 2021-03-12 | 江苏科技大学海洋装备研究院 | Oxidation-resistant conductive copper nanowire film and preparation method and application thereof |
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