CN101037509A - Novel organic-inorganic hybrid transparent conductive film and preparation method thereof - Google Patents
Novel organic-inorganic hybrid transparent conductive film and preparation method thereof Download PDFInfo
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- CN101037509A CN101037509A CN 200610024694 CN200610024694A CN101037509A CN 101037509 A CN101037509 A CN 101037509A CN 200610024694 CN200610024694 CN 200610024694 CN 200610024694 A CN200610024694 A CN 200610024694A CN 101037509 A CN101037509 A CN 101037509A
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Abstract
The invention provides a flexible transparent conductive thin film and its preparing method, which using metal alcohol salt, organic polymer and so on as main raw material, preparing transparent PANI/ATO hybridization thin film by sol-gel method acted as electrode of flexible solar cell and conductive thin film of folding type display screen. Conductivity of the prepared transparent hybridization thin film reaches 10S/cm, visible light permeation ration reaches 85%, thickness is 200 nm, thin film is equal and compact, viscosity of immersing and coating liquid can keep stable for 25 days, finished product ratio of the preparing method is high, preparing period is shorter, and the preparing method is adapted for large-scale production.
Description
Technical field
The present invention relates to a kind of is main raw material with metal alkoxide and conductive polymers, and the utilization sol-gel method prepares the method for transparent hydridization conductive film.
Background technology
Nesa coating is a kind of crucial photoelectric material, with the high transmittance in its visible-range, infrared high reflectance and characteristic of semiconductor, be widely used in the aspect such as window, automotive window heat conduction glass of solar cell, indicating meter, gas sensor, antistatic coating and semiconductor/insulator/semi-conductor (SIS) heterojunction, modern opportunity of combat and cruise missile, as document: the novel electron thin-film material, Beijing Chemical Industry Press, 2002,408.
The preparation method of transparent conductive film has: sol-gel method, spray pyrolysis method, reactive magnetron sputtering method, chemical Vapor deposition process, electron-beam vapor deposition method, RF-reactively sputtered titanium method, biomimetic method etc.Wherein, sol-gel method is suitable for large-scale production owing to have advantages such as production cost is relatively low, plated film efficient height, good uniformity, especially is subjected to people to pay attention to widely, as document: material Leader, 2004,18 (3), 17-20.Of paramount importance is can prepare the uniform hybrid inorganic-organic materials of molecular level by sol-gel method, therefore is particularly suitable for preparing the organic and inorganic conductive film.But processing parameter has considerable influence for the structure and the performance of gained film in the sol-gel building-up process, needs accurately control.
Present In
2O
3: Sn (ITO), Sb:SnO
2(ATO), ZnO:Al inorganic oxide conductive films such as (ZAO) is widely used, as document: the Shandong science, 2005,18 (2), describe among the 46-49, the target preparation is comparatively ripe with film-forming process, has formed industrialization production.But they have shortcoming, such as the indium among the ITO severe toxicity are arranged, and are harmful in preparation and application; Film fragility is big, poor flexibility, can't combine with flexible substrates; Synthetic need comparatively high temps, it is first-class to be deposited on polymer base material.The conductive polymer polymkeric substance has polyaniline, Polythiophene, polypyrrole etc., as document: polymer material science and engineering, 2004,20 (1), described in the 210-213.Wherein as polyaniline (PANI) because of being easy to process and doping, flexibility is good, raw material cheaply is easy to get, have good environmental stability, often is used to prepare the conductive polymer film.But shortcomings such as also there is physical strength in the conductive polymer film and specific conductivity is lower, heat-resisting, chemical stability is not good.
Current development of science and technology is to the demands for higher performance of transparent conductive film.For example, conductive film on the folding display screen will have flexible, conductive film on the touch-screen needs wear resistance and solidity to corrosion preferably, the film that synthetic glass window surface is used for heating defrosting on the aircraft must combine firmly with the organic radical physical efficiency, but the conductive film of the organic or inorganic of single phase all can't satisfy this generic request fully.The organic and inorganic transparent conductive film combines organic and inorganic materials advantage separately, just might reach many-sided requirement, but this type of research is still few at present.Kim and Honma etc. have prepared phospho-wolframic acid (PWA)/hexadecane base TMA (TriMethylAmine) chlorine hybrid systems recently, and the specific conductivity of film in the time of 150 ℃ is 10
-2S/cm, as document: Solid State Ionics, 2005,176, described in the 47-552; Aparicio and Castro etc. have synthesized the film of (vinylbenzene-methacrylate) multipolymer/system on silicon with copolymerization method, and the specific conductivity in the time of 120 ℃ is 1Scm
-1, as document: SolidState Ionics, 2005,176, described in the 333-340.The deficiency of this class conductive film is that specific conductivity is all lower, and opaque.The difficult point of preparation organic-inorganic hybrid transparent conductive film mainly is to guarantee when improving specific conductivity that organic and inorganic thing forms homogeneous phase so that improve optical transmittance.
Summary of the invention
In order to overcome the shortcoming of above-mentioned single organic or inorganic film over-all properties difference, solve film and must close firm problem with the organic radical bear building-up, improve the specific conductivity and the visible light transmissivity of organic inorganic hybridization film, a kind of method for preparing novel organic-inorganic hybrid transparent conductive film is provided.
The object of the present invention is achieved like this:
A kind of novel organic-inorganic hybrid transparent conductive film is characterized in that, described organic-inorganic hybrid transparent conductive film comprises following component:
A: tin protochloride 50～80 weight parts;
B: doping agent 0～15 weight part;
C: conductive polymers 5～50 weight parts;
D: chemical additive 0.5～20 weight part
E: catalyzer 0.1-10 weight part;
Wherein: conductive polymers is that to be selected from molecular weight be a kind of in 1000～30000 polyaniline, Polythiophene, polypyrrole, poly-(right-penylene), polyphenyl thiophthene, poly-(2, the 5-pyridine); Doping agent is for being selected from butter of antimony, antimonous oxide, liquid hydrogen fluoride, Neutral ammonium fluoride; Chemical additive be in lithium perchlorate, Lithium Sulphate, copper sulfate, Silver Nitrate, superfine cupper powder, the super fine silver powder one or more; Catalyzer is for being selected from nitric acid, acetic acid, hydrochloric acid and the ammoniacal liquor one or more.
Polyaniline in the said components is a synthetic by the following method:
With Witco 1298 Soft Acid (DBSA): the ratio of aniline=4g/1ML, take by weighing the yellow oily Witco 1298 Soft Acid (DBSA) of purity 96% and the aniline liquid of purity 99.5%, earlier in above-mentioned Witco 1298 Soft Acid, add deionized water, evenly add above-mentioned aniline in the back with magnetic stirrer, form white emulsion, stir 30min～60min, aniline is uniformly dispersed, and the use ice bath, guarantee temperature＜5 ℃; Get a certain amount of ammonium persulphate (NH
4)
2S
2O
8(APS) be dissolved in the 100ml deionized water, be added drop-wise in the emulsion through 30min with dropping funnel; Stop to stir behind reaction 6～10h, add the trichloromethane liquid breakdown of emulsion of 100～150ml purity 99%, and the extraction polyaniline.Behind the standing demix, isolate the polyaniline extraction liquid with separating funnel, with deionized water repetitive scrubbing extraction liquid, and through as above leave standstill, the separatory process until washings pH value for neutral, make the trichloromethane volatilization in vacuum drying oven, obtaining cyan doping is Witco 1298 Soft Acid: the polyaniline powder of polyaniline=115%.
Wherein, ammonium persulphate (NH
4)
2S
2O
8The mol ratio of/Witco 1298 Soft Acid is 5.5%.
The present invention also provides a kind of method for preparing novel organic-inorganic hybrid transparent conductive film, and its spy is that described method comprises the following steps:
(1) by said ratio, A, B, C, D, E component are carried out thorough mixing, in the system that contains water and dehydrated alcohol, be hydrolyzed, polycondensation, temperature of reaction is 20～80 ℃, polyase 13 0 minute～12 hours obtains required hydridization dip-coating solution; Inferior solution was at room temperature left standstill 12 hours, get final product plated film;
(2) film preparation and thermal treatment
Polymer flake or slide glass are washed with water repeatedly, clean with ultrasonic oscillation then, the oven dry back is stand-by.The slide glass of clean dry is immersed in the hydridization solution of step (1) gained, leave standstill after 10～60 seconds and at the uniform velocity lift, the control rate of pulling is 0.2～5mm/s; The slide glass that will deposit film is then put into 50 ℃～100 ℃ baking ovens, and dry 30 minutes, cracking phenomena appearred in film surface when the high-temperature heat treatment to avoid.Be warming up to 200～300 degree thermal treatments again after 0.5～5 hour through the exsiccant film, remove organic solvent and impurity, obtain water white organic-inorganic hybrid film, last furnace cooling.
Wherein, the heat treated temperature rise rate of film is 1～3 ℃/min, and the control rate of pulling is preferably 1mm/s.
Beneficial effect: the specific conductivity of the transparent hydridization conductive film of the present invention's preparation reaches 10
1Scm
-1, visible light transmissivity reaches 85%, and thickness is 200nm, the film even compact; The viscosity of lotion can keep stable reaching in time of 25 days, be suitable for very much dipping process; Preparation method's yield rate height, preparation cycle are shorter, are suitable for mass production.
The present invention is described in detail below in conjunction with embodiment.
Embodiment 1:
(1) under the room temperature with pressed powder tin protochloride 20g, butter of antimony 1g, the polyaniline 9g of AG, the trichloromethane liquid 50ml of dehydrated alcohol 100ml, purity 99% and water 10ml thorough mixing add purity 95%～98% nitric acid 0.4ml again and stir, react.Be warming up to 80 ℃ of following polyase 13s 0 minute, mixing solutions at room temperature left standstill 12 hours, obtained required hydridization lotion, wherein contained polyaniline 50～150g in every liter of solution.
(2) slide glass with clean dry immerses in the hydridization solution, leaves standstill after 20 seconds at the uniform velocity to lift, and the control pull rate is 2mm/s.The slide glass that will deposit film is then put into 50 ℃ of baking ovens, and dry 30 minutes, cracking phenomena appearred in film surface when the high-temperature heat treatment to avoid.Be warming up to 250 ℃ of following thermal treatments 1 hour through the exsiccant film with 1 ℃/min, remove organic solvent and impurity, obtain water white organic-inorganic hybrid film, last furnace cooling.
Embodiment 2:
Preparation process is with embodiment 1, and with pressed powder tin protochloride 20g, butter of antimony 1g, Polythiophene 10g, dehydrated alcohol 100ml, trichloromethane liquid 50ml and water 20ml thorough mixing add nitric acid 0.4ml again and stir, react under the room temperature.Be warming up to 50 ℃ of following polymerizations 60 minutes, mixing solutions at room temperature left standstill 12 hours, obtained lotion.
(2) slide glass with clean dry immerses in the hydridization solution, leaves standstill after 20 seconds at the uniform velocity to lift, and the control pull rate is 5mm/s.The slide glass that will deposit film is then put into 80 ℃ of baking ovens, and dry 60 minutes, cracking phenomena appearred in film surface when the high-temperature heat treatment to avoid.Be warming up to 300 ℃ of following thermal treatments 4 hours through the exsiccant film with 1 ℃/min, remove organic solvent and impurity, obtain water white organic-inorganic hybrid film, last furnace cooling.
Embodiment 3:
Preparation process is with embodiment 1, and with pressed powder tin protochloride 20g, antimonous oxide 1.5g, polypyrrole 8g, dehydrated alcohol 100ml, trichloromethane liquid 50ml and water 15ml thorough mixing add nitric acid 0.6ml again and stir, react under the room temperature.Be warming up to 100 ℃ of following polymerizations 90 minutes, mixing solutions at room temperature leaves standstill 6h, obtains lotion.
(2) slide glass with clean dry immerses in the hydridization solution, leaves standstill after 10 seconds at the uniform velocity to lift, and the control pull rate is 6mm/s.The slide glass that will deposit film is then put into 100 ℃ of baking ovens, and dry 90 minutes, cracking phenomena appearred in film surface when the high-temperature heat treatment to avoid.Be warming up to 200 ℃ of following thermal treatments 2 hours through the exsiccant film with 1 ℃/min, remove organic solvent and impurity, obtain water white organic-inorganic hybrid film, last furnace cooling.
Embodiment 4:
Preparation process is with embodiment 1, under the room temperature with purity 99% hydrogen fluoride liquid 3g, pressed powder tin protochloride 20g, poly-(right-penylene) 9g, dehydrated alcohol 100ml, trichloromethane liquid 50ml and water 10ml thorough mixing add nitric acid 1ml again and stir, react, and other is constant.
Embodiment 5:
Preparation process is with embodiment 2, and with pressed powder tin protochloride 20g, Neutral ammonium fluoride 1g, polyphenyl thiophthene 10g, dehydrated alcohol 100ml, trichloromethane 50ml and water 10ml thorough mixing add nitric acid 0.8ml again and stir, react under the room temperature, and other is constant.
Embodiment 6:
Preparation process is with embodiment 3, and with pressed powder tin protochloride 20g, butter of antimony 1g, poly-(2, the 5-pyridine) 9g, dehydrated alcohol 100ml, trichloromethane 50ml and water 10ml thorough mixing add nitric acid 1ml again and stir, react under the room temperature, and other is constant.
Embodiment 7:
Preparation process is with embodiment 1, under the room temperature with pressed powder tin protochloride 20g, butter of antimony 1g, polyaniline 9g, lithium chlorate 2g, dehydrated alcohol 100ml, trichloromethane 50ml and water 10ml thorough mixing, the acetic acid 0.6ml that adds purity 99% again stirs, reacts, and other is constant.
Embodiment 8:
Preparation process is with embodiment 1, under the room temperature with pressed powder tin protochloride 20g, butter of antimony 1g, polyaniline 9g, Lithium Sulphate 1.5g, dehydrated alcohol 100ml, trichloromethane 50ml and water 10ml thorough mixing, adding volumetric concentration again is that 36% aqueous hydrochloric acid 0.9ml stirs, reacts, and other is constant.
Embodiment 9:
Preparation process is with embodiment 1, under the room temperature with pressed powder tin protochloride 20g, butter of antimony 1g, polyaniline 9g, copper sulfate 2g, dehydrated alcohol 100ml, trichloromethane 50ml and water 10ml thorough mixing, adding volumetric concentration again is that 25%～28% ammoniacal liquor 0.6ml stirs, reacts, and other is constant.
Embodiment 10:
Preparation process is with embodiment 1, under the room temperature with pressed powder tin protochloride 20g, butter of antimony 1g, polyaniline 9g, Silver Nitrate 2, dehydrated alcohol 100ml, trichloromethane 50ml and water 10ml thorough mixing add ammoniacal liquor 0.6ml again and stir, react, and other is constant.
Embodiment 11:
Preparation process is with embodiment 1, under the room temperature with pressed powder tin protochloride 20g, butter of antimony 1g, polyaniline 9g, superfine cupper powder 1g, dehydrated alcohol 100ml, trichloromethane 50ml and water 10ml thorough mixing add nitric acid 0.4ml again and stir, react, and other is constant.
Embodiment 12:
Preparation process is with embodiment 1, under the room temperature with pressed powder tin protochloride 20g, butter of antimony 1g, polyaniline 9g, super fine silver powder 2g, dehydrated alcohol 100ml, trichloromethane 50ml and water 10ml thorough mixing add nitric acid 0.4ml again and stir, react, and other is constant.
Embodiment 13:
Preparation process is with embodiment 1, under the room temperature with pressed powder tin protochloride 20g, butter of antimony 1g, polyaniline 9g, Lithium Sulphate 1.5, dehydrated alcohol 150ml, trichloromethane 50ml and water 10ml thorough mixing add nitric acid 0.4ml again and stir, react, and other is constant.
Embodiment 14:
Preparation process is with embodiment 1, under the room temperature with pressed powder tin protochloride 20g, butter of antimony 1g, polyaniline 9g, Lithium Sulphate 1.5g, dehydrated alcohol 80ml, trichloromethane 40ml and water 10ml thorough mixing add nitric acid 0.4ml again and stir, react, and other is constant.
Embodiment 15:
(1) food ingredient is with embodiment 1, and the slide glass of clean dry is immersed in the hydridization solution, leaves standstill after 20 seconds at the uniform velocity to lift, and the control pull rate is 5mm/s.The slide glass that will deposit film is then put into 80 ℃ of baking ovens, and dry 60 minutes, cracking phenomena appearred in film surface when the high-temperature heat treatment to avoid.Be warming up to 300 ℃ of following thermal treatments 1 hour through the exsiccant film with 3 ℃/min, remove organic solvent and impurity, obtain water white organic-inorganic hybrid film, last furnace cooling.
Claims (6)
1, a kind of novel organic-inorganic hybrid transparent conductive film is characterized in that, described organic-inorganic hybrid transparent conductive film comprises following component:
A: tin protochloride 50～80 weight parts;
B: doping agent 0～15 weight part;
C: conductive polymers 5～50 weight parts;
D: chemical additive 0.5～20 weight part
E: catalyzer 0.1-10 weight part;
Wherein: conductive polymers is that to be selected from molecular weight be a kind of in 1000～30000 polyaniline, Polythiophene, polypyrrole, poly-(right-penylene), polyphenyl thiophthene, poly-(2, the 5-pyridine); Doping agent is for being selected from butter of antimony, antimonous oxide, liquid hydrogen fluoride, Neutral ammonium fluoride; Chemical additive be in lithium perchlorate, Lithium Sulphate, copper sulfate, Silver Nitrate, superfine cupper powder, the super fine silver powder one or more; Catalyzer is for selecting in white nitric acid, acetic acid, hydrochloric acid and the ammoniacal liquor one or more.
2, novel organic-inorganic hybrid transparent conductive film as claimed in claim 1 is characterized in that, wherein said component polyaniline is a synthetic by the following method:
With Witco 1298 Soft Acid (DBSA): the ratio of aniline=4g/1ml, take by weighing the yellow oily Witco 1298 Soft Acid (DBSA) of purity 96% and the aniline liquid of purity 99.5%, earlier in above-mentioned Witco 1298 Soft Acid, add deionized water, evenly add above-mentioned aniline in the back with magnetic stirrer, form white emulsion, stir 30min～60min, aniline is uniformly dispersed, and the use ice bath, guarantee temperature＜5 ℃; Get a certain amount of ammonium persulphate (NH
4)
2S
2O
8Pressed powder is dissolved in the 100ml deionized water, is added drop-wise in the emulsion through 30min with dropping funnel; Stop to stir behind reaction 6～10h, add the trichloromethane liquid breakdown of emulsion of 100～150ml purity 99%, and the extraction polyaniline; Behind the standing demix, isolate the polyaniline extraction liquid with separating funnel, with deionized water repetitive scrubbing extraction liquid, and through as above leave standstill, the separatory process until washings pH value for neutral, make the trichloromethane volatilization in vacuum drying oven, obtaining cyan doping is Witco 1298 Soft Acid: the polyaniline powder of polyaniline=115%.
3, a kind of preparation method of novel organic-inorganic hybrid transparent conductive film as claimed in claim 1 is characterized in that, described method comprises the following steps:
(1) by the described proportioning of claim 1, A, B, C, D, E component are carried out thorough mixing, be hydrolyzed in the system that contains water and dehydrated alcohol, polycondensation, temperature of reaction is 20～80 ℃, polyase 13 0 minute～12 hours obtains required hydridization dip-coating solution; Inferior solution was at room temperature left standstill 12 hours, get final product plated film;
(2) film preparation and thermal treatment
Polymer flake or slide glass are washed with water repeatedly, clean with ultrasonic oscillation then, the oven dry back is stand-by.The slide glass of clean dry is immersed in the hydridization solution of step (1) gained, leave standstill after 10～60 seconds and at the uniform velocity lift, the control rate of pulling is 0.2～2mm/s; The slide glass that will deposit film is then put into 50 ℃～100 ℃ baking ovens, drying, and the film of drying is warming up to 200～300 degree again, after the thermal treatment 0.5～5 hour, remove organic solvent and impurity, obtain water white organic-inorganic hybrid film, last furnace cooling.
4, novel organic-inorganic hybrid transparent conductive film as claimed in claim 2 is characterized in that, when the polyaniline for preparing wherein, and ammonium persulphate (NH
4)
2S
2O
8The mol ratio of/Witco 1298 Soft Acid is 5.5%.
5, the preparation method of novel organic-inorganic hybrid transparent conductive film as claimed in claim 3 is characterized in that, the control rate of pulling is 1mm/s in the described step (2).
6, the preparation method of novel organic-inorganic hybrid transparent conductive film as claimed in claim 3 is characterized in that, the heat treated temperature rise rate of film is 1 ℃/min in step (2).
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101280106B (en) * | 2008-05-30 | 2010-06-02 | 昆明理工大学 | Preparation of magnetic conductive polyaniline nanometer composite material |
| CN101328314B (en) * | 2007-11-21 | 2010-11-17 | 华东理工大学 | Method for rapidly preparing Ag/PPy composite material |
| CN101976591A (en) * | 2010-08-31 | 2011-02-16 | 中国乐凯胶片集团公司 | Transparent conductive film |
| CN101550239B (en) * | 2009-05-12 | 2011-08-31 | 厦门大学 | Method of preparing polypyrrole micro-/nano-structure with super-hydrophilic |
| CN102282097A (en) * | 2008-10-23 | 2011-12-14 | 国立科学研究中心 | Fluorosulphates useful as electrode materials |
| CN103265699A (en) * | 2013-05-08 | 2013-08-28 | 上海纳米技术及应用国家工程研究中心有限公司 | Nanometer tin dioxide modified polyaniline nano-tube preparation method |
| CN104276601A (en) * | 2013-07-08 | 2015-01-14 | 三星显示有限公司 | Composition for tin oxide semiconductor and method of formation of tin oxide semiconductor thin film |
| CN106298066A (en) * | 2016-08-17 | 2017-01-04 | 梅庆波 | A kind of preparation method of flexible transparent conducting film |
| CN111562293A (en) * | 2020-05-03 | 2020-08-21 | 泰兴瑞深新材科技有限公司 | Preparation method of anti-interference photoelectrochemistry biomass sensor |
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| CN101328314B (en) * | 2007-11-21 | 2010-11-17 | 华东理工大学 | Method for rapidly preparing Ag/PPy composite material |
| CN101280106B (en) * | 2008-05-30 | 2010-06-02 | 昆明理工大学 | Preparation of magnetic conductive polyaniline nanometer composite material |
| CN102282097B (en) * | 2008-10-23 | 2015-04-29 | 国立科学研究中心 | Fluorosulphates useful as electrode materials |
| CN102282097A (en) * | 2008-10-23 | 2011-12-14 | 国立科学研究中心 | Fluorosulphates useful as electrode materials |
| CN101550239B (en) * | 2009-05-12 | 2011-08-31 | 厦门大学 | Method of preparing polypyrrole micro-/nano-structure with super-hydrophilic |
| CN101976591A (en) * | 2010-08-31 | 2011-02-16 | 中国乐凯胶片集团公司 | Transparent conductive film |
| CN101976591B (en) * | 2010-08-31 | 2012-07-25 | 中国乐凯胶片集团公司 | Transparent conductive film |
| CN103265699A (en) * | 2013-05-08 | 2013-08-28 | 上海纳米技术及应用国家工程研究中心有限公司 | Nanometer tin dioxide modified polyaniline nano-tube preparation method |
| CN103265699B (en) * | 2013-05-08 | 2015-11-18 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of nano-stannic oxide modifies the preparation method of polyaniline nanotube |
| CN104276601A (en) * | 2013-07-08 | 2015-01-14 | 三星显示有限公司 | Composition for tin oxide semiconductor and method of formation of tin oxide semiconductor thin film |
| CN106298066A (en) * | 2016-08-17 | 2017-01-04 | 梅庆波 | A kind of preparation method of flexible transparent conducting film |
| CN106298066B (en) * | 2016-08-17 | 2017-07-28 | 石狮市森科智能科技有限公司 | A kind of preparation method of flexible transparent conducting film |
| CN111562293A (en) * | 2020-05-03 | 2020-08-21 | 泰兴瑞深新材科技有限公司 | Preparation method of anti-interference photoelectrochemistry biomass sensor |
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