CN109524173A - A kind of chitosan transparent conductive film and preparation method based on silver nanowires network - Google Patents
A kind of chitosan transparent conductive film and preparation method based on silver nanowires network Download PDFInfo
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- CN109524173A CN109524173A CN201811370513.6A CN201811370513A CN109524173A CN 109524173 A CN109524173 A CN 109524173A CN 201811370513 A CN201811370513 A CN 201811370513A CN 109524173 A CN109524173 A CN 109524173A
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- chitosan
- silver nanowires
- transparent conductive
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- conductive film
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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
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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
- H01B13/30—Drying; Impregnating
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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
Abstract
The invention discloses a kind of chitosan transparent conductive films and preparation method based on silver nanowires network, and using thio chitosan as basal layer, for silver nanowires as conductive layer, preparation step includes: that (1) prepares dialdehyde chitosan；(2) thio chitosan is prepared；(3) in silicon chip surface spin coating silver nanowires；(4) thio chitosan solution is slowly dropped to silver nanowires silicon wafer film surface, it is gently removed after air-drying from silicon chip surface, the chitosan transparent conductive film with excellent light transmission, electric conductivity, adhesion property, biodegradability, mechanical performance and anti-fatigue performance can be obtained.
Description
Technical field
The present invention relates to a kind of chitosan transparent conductive films and preparation method based on silver nanowires network, belong to photoelectricity material
Material field.
Background technique
Transparent conductive film refers to the thin of in visible-range light transmittance with higher and excellent electric conductivity
Membrane material, it is the important composition of numerous photoelectric devices including solar battery, light emitting diode, liquid crystal display etc.
Part.Current most commonly used transparent conductive film is tin indium oxide (ITO).But due to ITO it is fragile, it is frangible, lack it is flexible,
The disadvantages of expensive, does not adapt to the demand of flexible photoelectric device.Graphene, carbon nanotube, metal nanometer line and conductive height
Molecule is all used to replace ITO preparation flexible transparent electrode.The AgNWs being wherein prepared in solution both may be implemented to advise greatly
The roll-to-roll coating of mould becomes but also with the photoelectric properties for the ITO that can compare and replaces ITO most potential material (Liu Ping, Zeng Bao
Blueness, Wang Yaxiong, the preparation of Wang Jianghao nano wire transparent conductive film and application [J] material Leader in the opto-electronic device,
2017,31(07):6-18；In progress [J] of Duan Shasha, Zhang Ling, Li Chunzhong silver nanowires base flexible conducting material
State's Advances in Materials, 2016,35 (07): 545-551+544).
The flexible substrate material of common transparent conductive film has polyimides PI, polyethylene naphthalate PEN, gathers
The chemical fibres such as ethylene glycol terephthalate PET, but the generally existing poor biocompatibility of these base materials, environment are dirty
The disadvantages of contaminating, be difficult to degrade.Chitin is a kind of natural organic high-molecular polysaccharide, is distributed widely in the first such as nature shrimp, crab, insect
In the crust of shell guiding principle animal, fungi and the cell wall of plant.Is accounted in the natural organic high-molecular substance of reserves on earth
Two, it is only second to cellulose.Chitosan is the product after chitin deacetylation, is a kind of linear macromolecule, contains a large amount of trips
From-NH2。
Have at present many silver nanowires/chitosan films document report (Wang Lisha be based on silver nano material and shell
Biosensor research [D] the Zhejiang University of glycan composite membrane, 2014；The graphene of Lai Wenwei mechanical stripping preparation is to shell
Influence [D] the Harbin University of Science and Technology of glycan laminated film electric conductivity, 2016；Gong Yaming, pile text, Li Dong, Zhang Chao, Jiang Yu
Multiply chitosan/cellulose acetate/silver nanowires compound preparation and bacteriostasis property probe into [J] industry and scientific and technological forum,
2015,14(24):39+42；RSC Advances, 2016, 6, 47552；Applied Physics Express,2017,
10(6):065002；Analytical Methods, 2016,8 (8): 1806-1812).
Thio chitosan is a kind of important chitosan derivatives.Chinese invention patent CN201710258288.6 is disclosed
A kind of silver-sulphur covalent bond enhancing silver wire and thio chitosan composite material and preparation method, will be dispersed in deionized water
In silver wire and thio chitosan solution uniformly mixed by concussion, be built into self-supporting nano-silver thread-using self assembly is sprayed
Thio chitosan composite membrane.Its tensile stress and Young's modulus are respectively 248MPa and 32GPa, are pure thio chitosan films
3.9 and 11.7 times, while its tensile stress is far longer than nano-silver thread-chitosan film 165MPa, block-like metallic silver
170MPa, other most of nanocrystal enhancing chitosans and nano-silver thread organic matter composite membrane.In addition, nano-silver thread-sulfydryl
Chitosan complex film possesses good fatigue resistance.In the future, silver-sulphur covalent bond enhancing nano-silver thread-thio chitosan is compound
Film can help to manufacture other high performance composite membranes.Show covalent bond huge advantage (Nano Research, 2018,
11 (1): 410-419).
However the esterification or sulfydryl of current most document utilization thioacetic acid analog derivatives and chitosan hydroxyl
Chloroacetic chloride and the amidation process of amino of chitosan prepare thio chitosan.Common sulfhydryl modified dose has thioacetic acid, N- second
(Chinese Journal of New Drugs, 2007 (16): 1250-1254 such as acyl-L-cysteine, cysteine, thioglycolic acid；Agricultural science and technology with
Equipment, 2012 (12): 8-10；Ion exchange and absorption, 2010,26 (05): 475-480).Chinese invention patent
CN201710258288.6 is the thio chitosan being modified using N-acetyl-L-cysteine to chitosan.But
It is that above-mentioned reaction process answers strict control pH value, the excessively high air of pH value can be too low to make chitosan by sulfhydryl oxidase at disulfide bond
The activity of upper amino reduces, to cause sulfhydryl content in thio chitosan too low.In addition, the preparation side of conventional thio chitosan
Method also needs to activate using carbodiimides and N- hydroxyl sulfoacid base succimide, and reaction step is cumbersome.
Summary of the invention
In view of the above deficiencies, the present invention provides a kind of systems of chitosan transparent conductive film based on silver nanowires network
Preparation Method.
The technical scheme is that: (1) 2% acetic acid solution is dissolved the chitosan in, ultrasound is uniformly
Afterwards, the sodium metaperiodate of 1-10g/L is added, is protected from light 30-100min at 40-80 DEG C, is cleaned repeatedly with deionized water, dries
Dialdehyde chitosan is prepared.(2) above-mentioned dialdehyde chitosan is dissolved in 2% acetic acid solution, is configured to mass fraction 1-10%'s
Dialdehyde chitosan solution, is then slowly added into 2-MEA, and the mass ratio of the 2-MEA and dialdehyde chitosan is
0.5-2,50-80 DEG C of magnetic agitations are cleaned repeatedly for 24 hours, with deionized water, and thio chitosan is prepared in drying.(3) silver is received
Rice noodles are configured to the alcohol dispersion liquid of mass fraction 0.1-5%, then in polished silicon slice surface spin coating silver nanowires, the spin coating
Speed 2000-5000r/min, spin-coating time 10-60s.(4) above-mentioned thio chitosan is dissolved in 2% acetic acid solution, is configured to
Then the thio chitosan solution of mass fraction 1-10% is slowly dropped to silver nanowires silicon wafer film surface, from silicon wafer after air-drying
Surface is gently removed, and the chitosan transparent conductive film based on silver nanowires network can be obtained.
The present invention has the advantages that (1) avoids the esterification using thioacetic acid analog derivative and chitosan hydroxyl
Or the amidation process of mercaptoacetyl chlorine and amino of chitosan, pass through dialdehyde chitosan macromolecular surface aldehyde radical and 2-MEA
Thio chitosan is prepared in the schiff base reaction of molecular surface amino, and reaction step is simple, can operate, reaction condition is mild.
(2) by the coordination of sulfydryl and silver nanowires, obtain that there is excellent light transmission, electric conductivity, adhesion property, biology
The chitosan transparent conductive film of degradation property, mechanical performance and anti-fatigue performance.
Specific embodiment
The invention will be further elucidated with reference to specific embodiments.
Embodiment 1:(1) dissolve the chitosan in 2% acetic acid solution, ultrasound uniformly after, the sodium metaperiodate of 1g/L is added,
It is protected from light 100min at 40 DEG C, is cleaned repeatedly with deionized water, dialdehyde chitosan is prepared in drying.It (2) will be above-mentioned double
Aldehyde chitosan is dissolved in 2% acetic acid solution, is configured to the dialdehyde chitosan solution of mass fraction 1%, is then slowly added into 2- sulfydryl
Ethamine, the mass ratio of the 2-MEA and dialdehyde chitosan be 0.5,50 DEG C of magnetic agitations for 24 hours, it is repeatedly clear with deionized water
It washes, thio chitosan is prepared in drying.(3) silver nanowires is configured to the alcohol dispersion liquid of mass fraction 1%, is then being thrown
Light silicon chip surface spin coating silver nanowires, the spin speed 2000r/min, spin-coating time 60s.(4) by above-mentioned thio chitosan
It is dissolved in 2% acetic acid solution, the thio chitosan solution of mass fraction 1% is configured to, is then slowly dropped to silver nanowires silicon wafer
Film surface is gently removed from silicon chip surface after air-drying, the chitosan transparent conductive thin based on silver nanowires network can be obtained
Film.
Embodiment 2:(1) dissolve the chitosan in 2% acetic acid solution, ultrasound uniformly after, the sodium metaperiodate of 5g/L is added,
It is protected from light 60min at 60 DEG C, is cleaned repeatedly with deionized water, dialdehyde chitosan is prepared in drying.(2) by above-mentioned dialdehyde
Chitosan is dissolved in 2% acetic acid solution, is configured to the dialdehyde chitosan solution of mass fraction 5%, is then slowly added into 2- sulfydryl second
The mass ratio of amine, the 2-MEA and dialdehyde chitosan for 24 hours, is cleaned repeatedly for 1,60 DEG C of magnetic agitations with deionized water,
Thio chitosan is prepared in drying.(3) silver nanowires is configured to the alcohol dispersion liquid of mass fraction 2%, then in polishing silicon
Piece surface spin coating silver nanowires, the spin speed 3000r/min, spin-coating time 30s.(4) above-mentioned thio chitosan is dissolved in
2% acetic acid solution is configured to the thio chitosan solution of mass fraction 5%, is then slowly dropped to silver nanowires silicon wafer film
Surface gently removes from silicon chip surface after air-drying, the chitosan transparent conductive film based on silver nanowires network can be obtained.
Embodiment 3:(1) dissolve the chitosan in 2% acetic acid solution, ultrasound uniformly after, the sodium metaperiodate of 10g/L is added,
It is protected from light 30min at 80 DEG C, is cleaned repeatedly with deionized water, dialdehyde chitosan is prepared in drying.(2) by above-mentioned dialdehyde shell
Glycan is dissolved in 2% acetic acid solution, is configured to the dialdehyde chitosan solution of mass fraction 10%, is then slowly added into 2- sulfydryl second
The mass ratio of amine, the 2-MEA and dialdehyde chitosan for 24 hours, is cleaned repeatedly for 2,80 DEG C of magnetic agitations with deionized water,
Thio chitosan is prepared in drying.(3) silver nanowires is configured to the alcohol dispersion liquid of mass fraction 5%, then in polishing silicon
Piece surface spin coating silver nanowires, the spin speed 5000r/min, spin-coating time 10s.(4) above-mentioned thio chitosan is dissolved in
2% acetic acid solution is configured to the thio chitosan solution of mass fraction 10%, is then slowly dropped to silver nanowires silicon wafer film
Surface gently removes from silicon chip surface after air-drying, the chitosan transparent conductive film based on silver nanowires network can be obtained.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention.For those of ordinary skill in the art, may be used also on the basis of the above description
To make other variations or changes in different ways.Here all embodiments can not be exhaustive.It is all to belong to this hair
Bright technical solution changes and variations that derived from are still in the scope of protection of the present invention.
Claims (3)
1. a kind of chitosan transparent conductive film based on silver nanowires network, which is characterized in that using thio chitosan as base
Bottom, silver nanowires is as conductive layer.
2. a kind of preparation method of chitosan transparent conductive film based on silver nanowires network according to claim 1,
It is characterized in that, preparation step includes:
(1) it dissolves the chitosan in 2% acetic acid solution and the sodium metaperiodate of 1-10g/L is added, at 40-80 DEG C after ultrasound is uniform
Under be protected from light 30-100min, cleaned repeatedly with deionized water, drying dialdehyde chitosan is prepared；
(2) above-mentioned dialdehyde chitosan is dissolved in 2% acetic acid solution, is configured to the dialdehyde chitosan solution of mass fraction 1-10%,
It is then slowly added into 2-MEA, the mass ratio of the 2-MEA and dialdehyde chitosan is 0.5-2,50-80 DEG C of magnetic force
Stirring for 24 hours, is cleaned repeatedly with deionized water, and thio chitosan is prepared in drying；
(3) silver nanowires is configured to the alcohol dispersion liquid of mass fraction 0.1-5%, is then received in polished silicon slice surface spin coating silver
Rice noodles, the spin speed 2000-5000r/min, spin-coating time 10-60s；
(4) above-mentioned thio chitosan is dissolved in 2% acetic acid solution, is configured to the thio chitosan solution of mass fraction 1-10%,
Then it is slowly dropped to silver nanowires silicon wafer film surface, is gently removed after air-drying from silicon chip surface, be can be obtained and received based on silver
The chitosan transparent conductive film of nanowire network.
3. a kind of chitosan transparent conductive film based on silver nanowires network obtained by claim 2 preparation method.
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Cited By (2)
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| CN111048235A (en) * | 2019-11-25 | 2020-04-21 | 陈开兵 | Flexible transparent conductive thin film based on graphene/silver nanowire/chitosan |
| CN112863766A (en) * | 2021-01-12 | 2021-05-28 | 山东大学 | Method for preparing coffee ring conductive film based on silicon substrate and application |
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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 |
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| CN108148798A (en) * | 2016-12-05 | 2018-06-12 | 中国科学院大连化学物理研究所 | A kind of preparation method of electrical-conductive nanometer silver wire patterned film |
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Cited By (2)
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Application publication date: 20190326 |