CN106601339A - Method for preparing silver nanowire and alginate composite transparent conductive film - Google Patents
Method for preparing silver nanowire and alginate composite transparent conductive film Download PDFInfo
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- CN106601339A CN106601339A CN201611187017.8A CN201611187017A CN106601339A CN 106601339 A CN106601339 A CN 106601339A CN 201611187017 A CN201611187017 A CN 201611187017A CN 106601339 A CN106601339 A CN 106601339A
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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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- 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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- H—ELECTRICITY
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
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Abstract
The invention discloses a method for preparing an ultralow-roughness silver nanowire and alginate composite flexible transparent conductive film. Silver nanowires are spread on a thin sodium alginate layer by use of a composite film technology, the silver nanowires are welded into a high-conductivity nanowire network by means of pressurization, and the nanowire network is embedded into the thin sodium alginate layer. Then, the composite film is treated using calcium chloride solution. On one hand, cross-linking gelation of sodium alginate is achieved, and the silver nanowire network is firmly adhered to a substrate. On the other hand, the chloride ions in the calcium chloride solution can repair cracks and other damage to the silver nanowires under high pressure, and thus, a composite film structure with ultralow surface roughness and high conductivity is obtained. The method makes full use of the cross-linking effect of the calcium ions in the calcium chloride aqueous solution on sodium alginate and the micro repair effect of the chloride ions on the silver nanowires. The overall preparation process is carried out at room temperature. The method is suitable for preparing a flexible transparent conductive film on a polymer flexible substrate.
Description
Technical field
The present invention relates to transparent conductive film field, more particularly to one kind prepares nano silver wire and alginate composite transparent
The method of conductive film.
Background technology
Most of filrn photovoltaic devices, such as solar cell, Organic Light Emitting Diode etc., are used mostly sputtering gold
Category sull is used as its transparent electrode material.For now, the most widely used is based on tin indium oxide (ITO)
Transparent conductive film, but its defect gradually exposes during current use, such as complicated process of preparation, raw material are rare, fragility
Big not bending, and to reach preferable light transmittance and electric conductivity, technological temperature need to be controlled at 300-400 DEG C, nothing
Method is applied to the flexible polymer substrate of non-refractory.Therefore, sputtered metal oxide electrode does not adapt to future electronic product
Lightening, portability, the development trend of flexibility, find its alternative materials extremely urgent.
Study hotspot materials numerous at present, such as in the middle of nano silver wire, CNT, Graphene, conducting polymer, silver
Nano wire because of its electric conductivity height, good transparency, advantage of lower cost, be applicable to enjoy pass many advantages, such as large area is produced
Note.But photoelectric device is being applied to, especially during ultra-thin photoelectric device, still there are many problems to need to solve.First it is that line is indirect
Resistance of getting an electric shock is larger, and the mode for more effectively lifting conductance conventional at present has the modes such as high annealing, laser welding, hot pressing,
But high-temperature process is not suitable for the polymer flexibility substrate of non-refractory；The welding manner meeting of the mechanical pressure loading that normal temperature is adopted
Cause nano silver wire surface crackle or directly fracture occur, have a strong impact on the electric conductivity of nano wire film.Furthermore, prepare at present
The universal surface roughness of nano silver wire film for obtaining is excessive, and the stacking part between nano silver wire forms projection, is being applied to device
Easily it is short-circuited when in the middle of part and punctures.Additionally, the adhesion between nano silver wire and substrate is very weak, in the face of bending, stretch
Shi Jiyi is stripped off with substrate, and the durability for device in the middle of practical application is totally unfavorable.
For the problem that nano silver wire presently, there are, many solutions are suggested.Such as patent application CN102993995
With in CN102270524 using mechanical pressurization by nano silver wire and polymer composite membrane-forming, the method can be to a great extent
Surface roughness is solved the problems, such as, but have ignored damage of the mechanical pressure to nanowire surface, easily cause conductive film performance
It is unstable.For another example, patent application CN104810079 and CN103617830 are well mixed nano silver wire with polymer, alginic acid
Film forming afterwards, it is intended to thin film surface planarization is made while increasing nano wire with substrate adhesion, reduces surface roughness, but such
Polymer is covered in single nano silver wire surface, hinders the fusion between nano wire, very big to the overall Conductivity of film.
And for example, patent application CN103440907 is disclosed by the way that nano silver wire is combined with cellulose nano-fibrous, is prepared
Combined the transparent conductive film that preferably can be used for flexible base board with substrate, but the method fail to realize it is complete between nano silver wire
Welding, has tremendous influence to the overall electric conductivity of film, causes its square resistance in K Ω/sq orders of magnitude, fails to meet actual
Using electrical conductivity demand.And for example, patent application CN104934094 is covered in nano silver wire surface using polysaccharide, for increasing
The associativity of nano wire and substrate, the contact resistance for reducing between nano silver wire, but therefore class covering is non-conductive, therefore by bag
The mode such as wrap up in or cover and have a strong impact on the nano silver wire network electric conductivity of itself.Also such as, patent application CN103730194 is by silver
Nano wire is compounded to form multi-layer film structure with AZO, prepares the laminated film suitable for flexible base board, but its preparation technology is multiple
It is miscellaneous, and fail to solve the problems, such as that roughness of film is excessive.
Therefore, those skilled in the art is devoted to developing one kind to prepare nano silver wire and alginate composite transparent conductive
The method of film, using normal temperature technique, with the spy such as high conductivity, high transmission rate, strongly adherent, deflection, roughness be extremely low
Point.
The content of the invention
In view of the drawbacks described above of prior art, the technical problem to be solved is how to prepare one at normal temperatures
Transparent conductive film is planted, with strongly adherent and low roughness.
For achieving the above object, the invention provides one kind prepares nano silver wire and alginate compound transparent electricity conductive film
Method, comprise the following steps：
Step 1, sodium alginate is scattered in deionized water, heated stirring, that filtration prepares sodium alginate is water-soluble
Liquid, on poly-naphthalene dicarboxylic acid glycol ester ilm substrate surface alginate films layer is prepared, standby after air drying；
Step 2, the nano silver wire film that nano silver wire alcohol dispersion liquid is prepared a layer in alginate films layer surface,
Drying；
Step 3, the pressure for applying constant intensity uniform to film surface, discharge after being kept for a period of time；
Step 4, the laminated film of step 3 gained is soaked in calcium chloride water, is taken out after a period of time, rinsing is dry
It is dry.
Further, in step 1 and step 2, the preparation side of the alginate films and the nano silver wire film
Method is spin-coating method or knife coating or spraying process.
Further, in step 3, repeat step 3 after drying, obtains multilayer nano silver wire film, and number of repetition is 1-
25 times, the concentration of nano silver wire suspension is 0.01mg/ml-15mg/ml.
Further, in step 3, the pressure is 0.5MPa-50MPa.
Further, in step 2, the retention time of the pressure is 10s-60min..
Further, in step 4, the concentration of the calcium chloride water is 1mg/ml-5g/ml, and soak time is
10s-30min。
Further, the nano silver wire diameter is between 50nm-200nm,.
Further, the nano silver wire is fully or partially embedded in alginic acid salt deposit and forms damascene structures.
Further, the concentration of the sodium alginate aqueous solution be 0.5g/ml-2g/ml, the sodium alginate layer for preparing
Thickness in 50nm-300nm.
Beneficial effects of the present invention are as follows：
1st, the nano silver wire with ultralow roughness and alginate composite and flexible transparent conductive film in the present invention
Preparation flow is carried out at normal temperatures completely, is applicable to thermally sensitive polymer flexibility substrate.By applying mechanical pressure
The welding completely between metal nano is realized, the contact resistance between nano wire is reduced, it is ensured that the overall electric conductivity of film；Simultaneously will
In the middle of nano silver wire internet startup disk alginate thin layer, roughness of film is greatly reduced.
2nd, nano silver wire and alginate laminated film are processed using calcium chloride solution, on the one hand coagulates sodium alginate cross-linking
Glue, by composite construction and substrate strong bonded, on the other hand, the chlorion in solution acts on nano silver wire surface, to machinery
The damage on nano silver wire surface in high-pressure process is repaired, and further improves the overall electric conductivity of film.
3rd, the preparation method process is simple, normal-temperature operation, and preparation condition are easily controlled, and substrate is not required, repeat
Property it is high, disclosure satisfy that future device flexibility, lightening growth requirement, be applicable to large-scale production, it is very potential
Promote application and development of the nano silver wire in the middle of the photoelectric devices such as solar cell, sensor and Organic Light Emitting Diode.
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 nano silver wire-alginate structure of transparent conductive film schematic diagram of a preferred embodiment of the present invention；
Fig. 2 be machinery pressure force load after nano silver wire surface there is crackle schematic diagram；
Fig. 3 is that the chlorion in calcium chloride solution crackle occurs and carries out reparation schematic diagram to nano silver wire surface；
Fig. 4 is that the chlorion in calcium chloride solution completes schematic diagram to nano silver wire face crack reparation；
Fig. 5 is mechanical pressure before processing laminated film surface topography electromicroscopic photograph；
Fig. 6 is laminated film surface topography electromicroscopic photograph after mechanical pressure is processed；
Fig. 7 is laminated film surface topography electromicroscopic photograph after calcium chloride solution is processed；
Fig. 8 is mechanical pressure before processing nano silver wire structural representation；
Fig. 9 is nano silver wire structural representation after mechanical pressure is processed；
Figure 10 is nano silver wire structural representation after calcium chloride solution is processed；
Laminated film light transmittance curve figure after Figure 11 is after mechanical pressure before processing and calcium chloride solution is processed.
Specific embodiment
In order to preferably explain the present invention, the present invention is specifically described below by embodiment, but the present invention's is interior
Appearance is not only limited to following examples, and those skilled in the art makes some and nonessential changes according to the content of the invention described above
Enter and adjust, belong to protection scope of the present invention.
As shown in figure 1, transparent conductive film of the present invention includes nano silver wire, alginate film layer and substrate,
Following four embodiments of its preparation method：
Embodiment 1：
Step one, sodium alginate is scattered in deionized water, heated stirring, filtration prepare concentration for 0.5g/
The sodium alginate aqueous solution of ml, prepares the sodium alginate that thickness is 200nm thin in the spin-coated method of PEN substrate surfaces for cleaning up
Film layer, it is standby after air drying；
Step 2, the Yin Na that the spin-coated method of nano silver wire alcohol dispersion liquid is prepared a layer in alginate films layer surface
Rice noodles film, afterwards rinsing drying repeats this step 3 time and 3 layers of nano silver wire film is obtained；
The pressure of step 3, applying 10MPa uniform to film surface, keeps being discharged after 10min；
Step 4, the laminated film obtained by step 3 is soaked in concentration be 1g/ml calcium chloride water in, after 5min
Take out rinsing drying, you can prepare nano silver wire and alginate composite and flexible transparent conductive film.
Embodiment 2：
Step one, sodium alginate is scattered in deionized water, heated stirring, filtration prepare concentration for 1g/ml
Sodium alginate aqueous solution, the PEN substrate surface Jing knife coatings for cleaning up prepare thickness be 150nm alginate films
Layer, it is standby after air drying；
Step 2, the Yin Na that the spin-coated method of nano silver wire alcohol dispersion liquid is prepared a layer in alginate films layer surface
Rice noodles film, afterwards rinsing drying repeats this step 5 time and 5 layers of nano silver wire film is obtained；
The pressure of step 3, applying 8MPa uniform to film surface, keeps being discharged after 15min；
Step 4, the laminated film obtained by step 3 is soaked in concentration be 50mg/ml calcium chloride water in, 3min
Rinsing drying is taken out afterwards, you can prepare nano silver wire and alginate composite and flexible transparent conductive film.
Embodiment 3：
Step one, sodium alginate is scattered in deionized water, heated stirring, filtration prepare concentration for 0.1g/
The sodium alginate aqueous solution of ml, prepares the sodium alginate that thickness is 100nm thin in the PEN substrate surface Jing spraying processes for cleaning up
Film layer, it is standby after air drying；
Step 2, the Yin Na that the spin-coated method of nano silver wire alcohol dispersion liquid is prepared a layer in alginate films layer surface
Rice noodles film, afterwards rinsing drying repeats this step 4 time and 4 layers of nano silver wire film is obtained；
The pressure of step 3, applying 8MPa uniform to film surface, keeps being discharged after 8min；
Step 4, the laminated film obtained by step 3 is soaked in concentration be 2g/ml calcium chloride water in, after 1min
Take out rinsing drying, you can prepare nano silver wire and alginate composite and flexible transparent conductive film.
Embodiment 4：
Step one, sodium alginate is scattered in deionized water, heated stirring, filtration prepare concentration for 0.3g/
The sodium alginate aqueous solution of ml, the PEN substrate surfaces for cleaning up it is impregnated-czochralski method prepare thickness be 300nm marine alga
Sour sodium film layer, it is standby after air drying；
Step 2, the Yin Na that the spin-coated method of nano silver wire alcohol dispersion liquid is prepared a layer in alginate films layer surface
Rice noodles film, afterwards rinsing drying repeats this step 6 time and multilayer nano silver wire film is obtained；
The pressure of step 3, applying 15MPa uniform to film surface, keeps being discharged after 5min；
Step 4, the laminated film obtained by step 3 is soaked in concentration be 3g/ml calcium chloride water in, after 2min
Take out rinsing drying, you can prepare nano silver wire and alginate composite and flexible transparent conductive film.
The present invention adopts laminated film technology, and using mechanical pressure the welding completely between nano silver wire is realized, reduces contact
Resistance, while by the middle of nano silver wire internet startup disk alginate film, greatly reducing surface roughness.Using calcium chloride
Solution processes laminated film and alginate is crosslinked, fixed nano silver wire-alginate composite construction, while the chlorine in solution
Ion repairs the damaged structure of crackle on nano silver wire surface etc. under mechanical pressure, the nano silver wire surface and nano wire after process
Between pad it is smooth complete, the overall electric conductivity of laminated film before calcium chloride solution process compared with improving one times.
Fig. 2, Fig. 3 and Fig. 4 describe the process that the chlorion in calcium chloride solution repairs nano silver wire, machine in wherein Fig. 2
There is crackle in nano silver wire surface after the loading of tool pressure, and the chlorion in Fig. 3 in calcium chloride solution occurs to nano silver wire surface
Crackle is repaired, the nano silver wire surface state after the completion of repairing in Fig. 4.
Fig. 5 is that electromicroscopic photograph is retouched in the surface sweeping of the interlaced arrangement of nano silver wire before the mechanical pressure of loading, and Fig. 8 is Fig. 5 phases
Corresponding schematic perspective view；Fig. 6 is that electromicroscopic photograph is retouched in the surface sweeping that nano silver wire is mutually extruded after the mechanical pressure of loading, and Fig. 9 is
There is obvious crackle in Fig. 6 corresponding schematic perspective view, the junction for describing nano silver wire；Fig. 7 is to use calcium chloride solution
Electromicroscopic photograph is retouched in the surface sweeping that the nano silver wire for processing mutually merges, and Figure 10 is the corresponding schematic perspective views of Fig. 7；
The comparison of different light penetrations in the case of above-mentioned three kinds as shown in figure 11, loads the silver nanoparticle before mechanical pressure
The transmitance such as strigula of line-alginate laminated film (sheet resistance is 59.8 Ω/sq) is described, and loads the Yin Na after mechanical pressure
The transmitance such as line of dots of rice noodles-alginate laminated film (sheet resistance is 5.3 Ω/sq) is described, and adds calcium chloride solution to process
And strictly according to the facts line drawing is painted to load the transmitance of nano silver wire-alginate laminated film (sheet resistance be 2.3 Ω/sq) of mechanical pressure.
Load as seen from Figure 11 and repaired using calcium chloride solution after mechanical pressure, now but conductive film sheet resistance is greatly reduced light
Transmitance is not significantly lost.
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 method for preparing nano silver wire and alginate compound transparent electricity conductive film, it is characterised in that including following step
Suddenly：
Step 1, sodium alginate is scattered in deionized water, heated stirring, filtration prepare sodium alginate aqueous solution,
Poly-naphthalene dicarboxylic acid glycol ester ilm substrate surface prepares alginate films layer, standby after air drying；
Step 2, the nano silver wire film that nano silver wire alcohol dispersion liquid is prepared a layer in alginate films layer surface, dry
It is dry；
Step 3, the pressure for applying constant intensity uniform to film surface, discharge after being kept for a period of time；
Step 4, by step 3 gained laminated film be soaked in calcium chloride water, a period of time after take out, rinse drying.
2. the method for preparing nano silver wire and alginate compound transparent electricity conductive film as claimed in claim 1, its feature exists
In in step 1 and step 2, the preparation method of the alginate films and the nano silver wire film is spin-coating method or scrapes
Coating or spraying process.
3. the method for preparing nano silver wire and alginate compound transparent electricity conductive film as claimed in claim 1, its feature exists
In in step 3, repeat step 3 after drying obtain multilayer nano silver wire film, and number of repetition is 1-25 time, and nano silver wire hangs
The concentration of turbid liquid is 0.01mg/ml-15mg/ml.
4. the method for preparing nano silver wire and alginate compound transparent electricity conductive film as claimed in claim 1, its feature exists
In in step 3, the pressure is 0.5MPa-50MPa.
5. the method for preparing nano silver wire and alginate compound transparent electricity conductive film as claimed in claim 1, its feature exists
In in step 2, the retention time of the pressure is 10s-60min..
6. the method for preparing nano silver wire and alginate compound transparent electricity conductive film as claimed in claim 1, its feature exists
In in step 4, the concentration of the calcium chloride water is 1mg/ml-5g/ml, and soak time is 10s-30min.
7. the method for preparing nano silver wire and alginate compound transparent electricity conductive film as claimed in claim 1, its feature exists
In, the nano silver wire diameter between 50nm-200nm,.
8. the method for preparing nano silver wire and alginate compound transparent electricity conductive film as claimed in claim 1, its feature exists
In the nano silver wire is fully or partially embedded in alginic acid salt deposit and forms damascene structures.
9. the method for preparing nano silver wire and alginate compound transparent electricity conductive film as claimed in claim 1, its feature exists
In the concentration of the sodium alginate aqueous solution is 0.5g/ml-2g/ml, and the thickness of the sodium alginate layer for preparing is in 50nm-
300nm。
10. the nano silver wire for preparing such as claim 1-9 any one methods described is transparent with alginate composite and flexible to lead
Conductive film and its application in the electrodes.
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| CN201611187017.8A CN106601339A (en) | 2016-12-20 | 2016-12-20 | Method for preparing silver nanowire and alginate composite transparent conductive film |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110283347A (en) * | 2019-05-08 | 2019-09-27 | 广东石油化工学院 | A kind of elasticity electromagnetic shielding film and preparation method thereof |
| CN111057414A (en) * | 2019-12-30 | 2020-04-24 | 浙江工业大学 | Crosslinkable chemically-sinterable strong-adhesion silver nanowire conductive ink and conductive film prepared from same |
| WO2020224496A1 (en) * | 2019-05-08 | 2020-11-12 | 广东石油化工学院 | Synergistically enhanced electromagnetic shielding film and preparation method therefor |
| CN114112133A (en) * | 2021-11-23 | 2022-03-01 | 厦门大学 | Flexible photon pressure sensor, preparation method and application thereof |
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| CN104934094A (en) * | 2015-05-27 | 2015-09-23 | 复旦大学 | Metal nanowire composite transparent conductive film, preparation method and application thereof |
| CN106041115A (en) * | 2016-05-26 | 2016-10-26 | 华南理工大学 | Sodium alga acid/silver nanowire sol and preparation method thereof |
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| JP2009252437A (en) * | 2008-04-03 | 2009-10-29 | Konica Minolta Holdings Inc | Transparent conductive film |
| CN103606420A (en) * | 2013-11-08 | 2014-02-26 | 复旦大学 | Method for preparing metal conductive film |
| CN103762011A (en) * | 2014-01-16 | 2014-04-30 | 中国科学院青岛生物能源与过程研究所 | Transparent conducting thin film based on sodium alga acid and preparation method of transparent conducting thin film |
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| CN110283347A (en) * | 2019-05-08 | 2019-09-27 | 广东石油化工学院 | A kind of elasticity electromagnetic shielding film and preparation method thereof |
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| CN110283347B (en) * | 2019-05-08 | 2022-02-01 | 广东石油化工学院 | Elastic electromagnetic shielding film and preparation method thereof |
| CN111057414A (en) * | 2019-12-30 | 2020-04-24 | 浙江工业大学 | Crosslinkable chemically-sinterable strong-adhesion silver nanowire conductive ink and conductive film prepared from same |
| CN114112133A (en) * | 2021-11-23 | 2022-03-01 | 厦门大学 | Flexible photon pressure sensor, preparation method and application thereof |
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