CN107507675A - A kind of preparation method of tin oxide conductive film - Google Patents
A kind of preparation method of tin oxide conductive film Download PDFInfo
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- CN107507675A CN107507675A CN201710697625.1A CN201710697625A CN107507675A CN 107507675 A CN107507675 A CN 107507675A CN 201710697625 A CN201710697625 A CN 201710697625A CN 107507675 A CN107507675 A CN 107507675A
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- deionized water
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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
- H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/1208—Oxides, e.g. ceramics
- C23C18/1216—Metal oxides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1254—Sol or sol-gel processing
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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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Abstract
The invention discloses a kind of preparation method of tin oxide conductive film, the present invention efficiently solves oxidic transparent conductive film and flexible polyester substrate matching is bad, and tack is poor, the critical problem easily fallen off, the present invention, redox graphene/SnO is prepared by in-situ chemical route2Composite granule, finally by processes such as spin coating and heat treatments on matrix, acquisition translucency is good, the high compound transparent electricity conductive film of conductance.
Description
Technical field
The present invention relates to conductive material field, and in particular to a kind of preparation method of tin oxide conductive film.
Background technology
Transparent conductive film be it is a kind of have both highly conductive and visible light wave range high transparency characteristic basic photoelectric material, extensively
Applied to the photoelectric display such as display, luminescent device, solar cell, sensor, flexible touch screen field, there is extensive business
Industry application prospect.
DSSC forms by light anode, dyestuff, electrolyte and to the part of electrode four.Wherein, light anode
All it is transparent conducting glass with the base material to electrode.At present, conventional transparency conducting layer is mainly tin indium oxide（ITO）With
The tin oxide of Fluorin doped（FTO）.FTO is the transparent conductive film for realizing industrialized production earliest, and preparation technology is simple, ripe,
But conductance is relatively low compared with ITO, ITO is the transparent conductive film having the call in the market, and photoelectric properties are very
It is outstanding, but indium can pollute to environment, and it is expensive, in addition, also there is the shortcomings that non-refractory in ITO, so as to limit
The development and application of dye sensitization of solar.Transparency conducting layer is also extensively used for organic solar batteries, Ca-Ti ore type
Solar cell and quantum dot sensitized solar cell etc..
Graphene-based and graphene doping transparent conductive film can improve the electric conductivity of film, while reduce and be produced into
This.But the graphene either prepared using chemical vapour deposition technique or oxidation-reduction method, due to graphene lacking in itself
Sunken and graphene film interlayer resistance all limits the electric conductivity of transparent graphene conductive film.Simultaneously as the oxygen dried
Graphite alkene is difficult to be uniformly dispersed, and makes the preparation of graphene also inapplicable and large-scale industrial production.
Through being retrieved to prior art, most of technologies are that the ink prepared using all kinds of conductive materials is coated with or is sprayed on
Flexible transparent conductive film, transparent conductive film prepared by such technology, although with preferably thin are prepared into flexible substrates
Film adhesive force, but optical transmittance and electric conductivity still have it is to be hoisted.
The content of the invention
The present invention provides a kind of preparation method of tin oxide conductive film, and the present invention efficiently solves oxidic transparent conduction
Film and flexible polyester substrate matching are bad, and tack is poor, and the critical problem easily fallen off, the present invention passes through original position
Chemical method prepares redox graphene/SnO2Composite granule, finally obtained on matrix by processes such as spin coating and heat treatments
It is good to obtain translucency, the high compound transparent electricity conductive film of conductance.
To achieve these goals, the invention provides a kind of preparation method of tin oxide conductive film, this method to include
Following steps：
（1）Plasma surface treatment is carried out to polyester base
Flexible polyester substrate is put into the deionized water containing certain abluent, in deionized water ultrasonic 10-15min；So
Afterwards, the positive and negative of flexible polyester substrate is scrubbed to remove the dirt of substrate surface and oil one by one with soft clean hairbrush
Dirt, afterwards, substrate is rinsed repeatedly with deionized water, untill substrate non-foam；Then, flexible polyester is put into ethanol and surpassed
Sound 10-15min, to remove the organic matter of substrate surface, afterwards, rinse substrate repeatedly with deionized water 4-6 times；Then, will be soft
Property polyester base carry out deionized water ultrasound 25-30mins, then, the deionized water after ultrasound in container is poured out, added new
Deionized water；Finally, the flexible polyester of cleaning is taken out one by one from deionized water and is laid on the large size culture dish of cleaning,
Put into together in the cleaning oven that temperature is 55-60 DEG C and carry out baking 24-30h；
Cleaning, dried flexible polyester substrate are put into the cavity of magnetron sputter, close all valves of magnetron sputter
Door, window, the sputtering baffle plate immediately below all targets, are vacuumized to cavity, to 3 × 10-4-5×10-4pa；
Reverse sputtering baffle plate is rotated to the surface of flexible polyester substrate, is passed through argon gas and oxygen, adjusts polyester base and backwash
The spacing of baffle plate is penetrated, sets corresponding argon oxygen ratio, overall gas flow, operating air pressure, sputtering power and corona treatment
Time, reverse sputtering corona treatment is carried out to flexible polyester substrate surface；
（2）Prepare conductive colloidal sol
Graphene oxide is distributed to stirring in deionized water and obtains the body of mixture one, the graphene oxide and deionized water
Product is than being 1:20-50；By SnCl2·2H2O is added to stirring in methanol and obtains mixture two, the SnCl2·2H2O and methanol
Mass ratio be 1:10-20；A certain amount of mixture two is slowly added in mixture A, meanwhile, according to the matter of additive and methanol
Amount is than being 1:50-100 adds additive, and persistently stirring 2-4h after being 8-10 with ammoniacal liquor regulation mixed solution pH obtains mixture
Three；Mixture three is transferred in 150ml reactors, reacted at 160-180 DEG C a period of time, centrifugation, is gone back after drying
Former graphene oxide/SnO2Composite granule；
According to redox graphene/SnO2The mass ratio of composite granule and ethanol is 1:150-200 mixes both, meanwhile,
It is 1 according to the mass ratio of organic bond and ethanol:20-40 adds organic bond, is obtained after stirring 30 min according to reduction
Graphene oxide/SnO2Conductive colloidal sol；
（3）By conductive colloidal sol, prepare zinc oxide in the above-mentioned polyester base after Surface Treatment with Plasma using spin-coating method and coagulate
Glue film, zinc oxide gel film will be obtained in atmosphere, 10-20min is dried under the conditions of 100-105 DEG C；Then in atmosphere,
10-20min is heat-treated under the conditions of 450-500 DEG C, obtains zinc-oxide film.
Preferably, in step（1）In, the technique of plasma treatment is：Polyester base and the spacing of reverse sputtering baffle plate are 35-
40mm；Argon oxygen ratio is 5:1-6:1；Oxygen and purity of argon are 99.99%；Total gas couette is 20-25sccm；Work gas
Press as 0.4-0.6pa；Sputtering power is 25-45W；Plasma treatment time is 70-90s.
Embodiment
Embodiment one
Flexible polyester substrate is put into the deionized water containing certain abluent, in deionized water ultrasonic 10min；Then,
The positive and negative of flexible polyester substrate is scrubbed to remove the dirt of substrate surface and greasy dirt one by one with soft clean hairbrush,
Afterwards, substrate is rinsed repeatedly with deionized water, untill substrate non-foam；Then, flexible polyester is put into ethanol ultrasonic
10min, to remove the organic matter of substrate surface, afterwards, rinse substrate repeatedly with deionized water 4 times；Then, by flexible polyester base
Bottom carries out deionized water ultrasound 25mins, and then, the deionized water after ultrasound in container is poured out, adds new deionized water；
Finally, the flexible polyester of cleaning is taken out one by one from deionized water and be laid on the large size culture dish of cleaning, put temperature into together
Spend in the cleaning oven for 55 DEG C and carry out baking 24h.
Cleaning, dried flexible polyester substrate are put into the cavity of magnetron sputter, close the institute of magnetron sputter
There are valve, window, the sputtering baffle plate immediately below all targets, cavity is vacuumized, to 3 × 10-4。
Reverse sputtering baffle plate is rotated to the surface of flexible polyester substrate, is passed through argon gas and oxygen, regulation polyester base with
The spacing of reverse sputtering baffle plate, set corresponding argon oxygen ratio, overall gas flow, operating air pressure, sputtering power and plasma
Processing time, reverse sputtering corona treatment is carried out to flexible polyester substrate surface.The technique of plasma treatment is：Polyester base
Spacing with reverse sputtering baffle plate is 35mm；Argon oxygen ratio is 5:1；Oxygen and purity of argon are 99.99%；Total gas couette is
20sccm；Operating air pressure is 0.4pa；Sputtering power is 25W；Plasma treatment time is 70s.
Graphene oxide is distributed to stirring in deionized water and obtains mixture one, the graphene oxide and deionized water
Volume ratio be 1:20；By SnCl2·2H2O is added to stirring in methanol and obtains mixture two, the SnCl2·2H2O and methanol
Mass ratio be 1:10；A certain amount of mixture two is slowly added in mixture A, meanwhile, according to the quality of additive and methanol
Than for 1:50 add additive, and persistently stirring 2h after being 8-10 with ammoniacal liquor regulation mixed solution pH obtains mixture three；Will mixing
Thing three is transferred in 150ml reactors, at 160 DEG C react a period of time, centrifugation, dry after obtain redox graphene/
SnO2Composite granule.
According to redox graphene/SnO2The mass ratio of composite granule and ethanol is 1:150-200 mixes both, together
When, it is 1 according to the mass ratio of organic bond and ethanol:20-40 adds organic bond, is obtained after stirring 30 min according to also
Former graphene oxide/SnO2Conductive colloidal sol.
By conductive colloidal sol, prepare zinc oxide in the above-mentioned polyester base after Surface Treatment with Plasma using spin-coating method and coagulate
Glue film, zinc oxide gel film will be obtained in atmosphere, 1min is dried under the conditions of 100 DEG C；Then in atmosphere, 450 DEG C of bars
10min is heat-treated under part, obtains zinc-oxide film.
Embodiment two
Flexible polyester substrate is put into the deionized water containing certain abluent, in deionized water ultrasonic 15min；Then,
The positive and negative of flexible polyester substrate is scrubbed to remove the dirt of substrate surface and greasy dirt one by one with soft clean hairbrush,
Afterwards, substrate is rinsed repeatedly with deionized water, untill substrate non-foam；Then, flexible polyester is put into ethanol ultrasonic
15min, to remove the organic matter of substrate surface, afterwards, rinse substrate repeatedly with deionized water 6 times；Then, by flexible polyester base
Bottom carries out deionized water ultrasound 30mins, and then, the deionized water after ultrasound in container is poured out, adds new deionized water；
Finally, the flexible polyester of cleaning is taken out one by one from deionized water and be laid on the large size culture dish of cleaning, put temperature into together
Spend in the cleaning oven for 60 DEG C and carry out baking 30h.
Cleaning, dried flexible polyester substrate are put into the cavity of magnetron sputter, close the institute of magnetron sputter
There are valve, window, the sputtering baffle plate immediately below all targets, cavity is vacuumized, to 5 × 10-4pa。
Reverse sputtering baffle plate is rotated to the surface of flexible polyester substrate, is passed through argon gas and oxygen, regulation polyester base with
The spacing of reverse sputtering baffle plate, set corresponding argon oxygen ratio, overall gas flow, operating air pressure, sputtering power and plasma
Processing time, reverse sputtering corona treatment is carried out to flexible polyester substrate surface.The technique of plasma treatment is：Polyester base
Spacing with reverse sputtering baffle plate is 40mm；Argon oxygen ratio is 6:1；Oxygen and purity of argon are 99.99%；Total gas couette is
25sccm；Operating air pressure is 0.6pa；Sputtering power is 45W；Plasma treatment time is 90s.
Graphene oxide is distributed to stirring in deionized water and obtains mixture one, the graphene oxide and deionized water
Volume ratio be 1: 50；By SnCl2·2H2O is added to stirring in methanol and obtains mixture two, the SnCl2·2H2O and first
The mass ratio of alcohol is 1:20；A certain amount of mixture two is slowly added in mixture A, meanwhile, according to the matter of additive and methanol
Amount is than being 1:100 add additive, and persistently stirring 4h after being 8-10 with ammoniacal liquor regulation mixed solution pH obtains mixture three；Will be mixed
Compound three is transferred in 150ml reactors, is reacted at 180 DEG C a period of time, centrifugation, reduction-oxidation graphite is obtained after drying
Alkene/SnO2Composite granule.
According to redox graphene/SnO2The mass ratio of composite granule and ethanol is 1:200 mix both, meanwhile,
It is 1 according to the mass ratio of organic bond and ethanol:40 add organic bond, are obtained after stirring 30 min according to reduction-oxidation
Graphene/SnO2Conductive colloidal sol.
By conductive colloidal sol, prepare zinc oxide in the above-mentioned polyester base after Surface Treatment with Plasma using spin-coating method and coagulate
Glue film, zinc oxide gel film will be obtained in atmosphere, 20min is dried under the conditions of 105 DEG C；Then in atmosphere, 500 DEG C of bars
20min is heat-treated under part, obtains zinc-oxide film.
It is described above, only it is presently preferred embodiments of the present invention, any restrictions is not done to the present invention, it is every according to invention skill
Any simple modification, change and the equivalent structure change that art is substantially made to above example, still fall within the technology of the present invention
In the protection domain of scheme.
Claims (2)
1. a kind of preparation method of tin oxide conductive film, this method comprise the following steps：
（1）Plasma surface treatment is carried out to polyester base
Flexible polyester substrate is put into the deionized water containing certain abluent, in deionized water ultrasonic 10-15min；So
Afterwards, the positive and negative of flexible polyester substrate is scrubbed to remove the dirt of substrate surface and oil one by one with soft clean hairbrush
Dirt, afterwards, substrate is rinsed repeatedly with deionized water, untill substrate non-foam；Then, flexible polyester is put into ethanol and surpassed
Sound 10-15min, to remove the organic matter of substrate surface, afterwards, rinse substrate repeatedly with deionized water 4-6 times；Then, will be soft
Property polyester base carry out deionized water ultrasound 25-30mins, then, the deionized water after ultrasound in container is poured out, added new
Deionized water；Finally, the flexible polyester of cleaning is taken out one by one from deionized water and is laid on the large size culture dish of cleaning,
Put into together in the cleaning oven that temperature is 55-60 DEG C and carry out baking 24-30h；
Cleaning, dried flexible polyester substrate are put into the cavity of magnetron sputter, close all valves of magnetron sputter
Door, window, the sputtering baffle plate immediately below all targets, are vacuumized to cavity, to 3 × 10-4-5×10-4pa；
Reverse sputtering baffle plate is rotated to the surface of flexible polyester substrate, is passed through argon gas and oxygen, adjusts polyester base and backwash
The spacing of baffle plate is penetrated, sets corresponding argon oxygen ratio, overall gas flow, operating air pressure, sputtering power and corona treatment
Time, reverse sputtering corona treatment is carried out to flexible polyester substrate surface；
（2）Prepare conductive colloidal sol
Graphene oxide is distributed to stirring in deionized water and obtains the body of mixture one, the graphene oxide and deionized water
Product is than being 1:20-50；By SnCl2·2H2O is added to stirring in methanol and obtains mixture two, the SnCl2·2H2O and methanol
Mass ratio be 1:10-20；A certain amount of mixture two is slowly added in mixture A, meanwhile, according to the matter of additive and methanol
Amount is than being 1:50-100 adds additive, and persistently stirring 2-4h after being 8-10 with ammoniacal liquor regulation mixed solution pH obtains mixture
Three；Mixture three is transferred in 150ml reactors, reacted at 160-180 DEG C a period of time, centrifugation, is gone back after drying
Former graphene oxide/SnO2Composite granule；
According to redox graphene/SnO2The mass ratio of composite granule and ethanol is 1:150-200 mixes both, meanwhile, press
It is 1 according to the mass ratio of organic bond and ethanol:20-40 adds organic bond, is obtained after stirring 30 min according to oxygen reduction
Graphite alkene/SnO2Conductive colloidal sol；
（3）By conductive colloidal sol, prepare zinc oxide in the above-mentioned polyester base after Surface Treatment with Plasma using spin-coating method and coagulate
Glue film, zinc oxide gel film will be obtained in atmosphere, 10-20min is dried under the conditions of 100-105 DEG C；Then in atmosphere,
10-20min is heat-treated under the conditions of 450-500 DEG C, obtains zinc-oxide film.
2. the method as described in claim 1, it is characterised in that in step（1）In, the technique of plasma treatment is：Polyester base
Bottom and the spacing of reverse sputtering baffle plate are 35-40mm；Argon oxygen ratio is 5:1-6:1；Oxygen and purity of argon are 99.99%；Always
Gas flow is 20-25sccm；Operating air pressure is 0.4-0.6pa；Sputtering power is 25-45W；Plasma treatment time is
70-90s。
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109727702A (en) * | 2018-12-12 | 2019-05-07 | 华南理工大学 | A kind of zirconium doped tin oxide transparent conductive film and preparation method thereof |
| CN110660926A (en) * | 2018-06-28 | 2020-01-07 | Tcl集团股份有限公司 | Novel transparent conductive film and preparation method and application thereof |
| CN110931657A (en) * | 2019-12-06 | 2020-03-27 | 中国乐凯集团有限公司 | Flexible composite substrate for perovskite thin-film solar cell and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105039910A (en) * | 2015-08-14 | 2015-11-11 | 陕西煤业化工技术研究院有限责任公司 | Flexible transparent conducting thin film |
| CN106920598A (en) * | 2017-03-12 | 2017-07-04 | 苏州南尔材料科技有限公司 | A kind of method for preparing tin oxide conductive film on a silicon substrate |
-
2017
- 2017-08-15 CN CN201710697625.1A patent/CN107507675A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105039910A (en) * | 2015-08-14 | 2015-11-11 | 陕西煤业化工技术研究院有限责任公司 | Flexible transparent conducting thin film |
| CN106920598A (en) * | 2017-03-12 | 2017-07-04 | 苏州南尔材料科技有限公司 | A kind of method for preparing tin oxide conductive film on a silicon substrate |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110660926A (en) * | 2018-06-28 | 2020-01-07 | Tcl集团股份有限公司 | Novel transparent conductive film and preparation method and application thereof |
| CN109727702A (en) * | 2018-12-12 | 2019-05-07 | 华南理工大学 | A kind of zirconium doped tin oxide transparent conductive film and preparation method thereof |
| CN110931657A (en) * | 2019-12-06 | 2020-03-27 | 中国乐凯集团有限公司 | Flexible composite substrate for perovskite thin-film solar cell and preparation method thereof |
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Application publication date: 20171222 |
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