CN104376895B - Transparent conductive film and its preparation method and application - Google Patents
Transparent conductive film and its preparation method and application Download PDFInfo
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- CN104376895B CN104376895B CN201410637665.3A CN201410637665A CN104376895B CN 104376895 B CN104376895 B CN 104376895B CN 201410637665 A CN201410637665 A CN 201410637665A CN 104376895 B CN104376895 B CN 104376895B
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Abstract
The invention discloses a kind of transparent conductive film and its preparation method and application, component and each constituent mass number are as follows: zinc acetate 10 ~ 20 parts, ethanolamine 3 ~ 8 parts, ethylene glycol monomethyl ether 10 ~ 30 parts, hexamethylenetetramine 8 ~ 12 parts, stannum oxide 10 ~ 15 parts, molybdenum oxide 2 ~ 6 parts, 1 ~ 5 part of aluminum, reinforcing agent 2 ~ 5 parts.Also include o-dichlorohenzene 0.3 ~ 1.6 part.Described reinforcing agent is carbon silica fibre.This transparent conductive film has good visible light permeability and electric conductivity, the mean transmissivity of the visible region of thin film is more than 85.0%, square resistance is less than 30/sq, it is expected to as clear bottom application of electrode among solaode, for carrying out the developmental research of solaode transparency electrode, there is definite meaning.
Description
Technical field
The invention belongs to solar cell conductive technology field of membrane materials, be specifically related to a kind of transparent conductive film and system thereof
Preparation Method and application.
Background technology
In today of society's high speed development, non-renewable resources constantly reduce, and find for this and tap a new source of energy into pendulum and exist
In the process of human development.It is well known that the use of non-renewable energy resources is often along with the pollution of ecological environment, this is also
It is mankind's difficult problems of having to go solve.Solar energy does not has any nonstaining property as a kind of green energy resource to environment, and
Its source is simple, it can be said that in the existence time limit of the mankind, it is inexhaustible.Solar energy is not only one
Secondary performance source, or clean energy resource, its aboundresources, generally exist, right without transporting, also can freely use, the most important thing is
Environment does not has any pollution.Solaode also because of the particularity of solar energy have not available for other generation modes many excellent
Point: without geographical restrictions, do not consume fuel, scale is changeable, motility is big, pollution-free, noiselessness, safe and reliable, build
Cycle is short, safeguard simply, have most the probability of large-scale application.So a lot of experts using solar energy as alternatively
The energy goes exploitation, it is desirable to the sun can be brought benefit to the mankind.Nowadays it is by sun electricity greatly that the solar energy used has
Pond conversion gets.Because solaode has sensing to light, it is possible to the luminous energy being radiated at its surface is converted to electric energy.Mesh
Before, under the effort of relevant expert, solaode is own through having moved towards commercialization and industrialization.
Transparent conductive film as the hearth electrode of organic solar batteries, and can provide the logical of radiant light entrance device
Road.The most commonly used of application is ITO electro-conductive glass.ITO is the mixture of indium oxide and tin-oxide.Generally, they
Mass fraction be respectively 90% and 10%.ITO thin film transmitance in oxide conductive film is the highest, and electric conductivity is best,
And easily in acid solution, etch trickle figure, therefore obtain a wide range of applications in photoelectric field.But due to
The indium of one of the essential element composition of ITO is the element of relative scarcity, so ITO is for the most high from the point of view of the demand of people
Expensive.In this sense, for photovoltaic cell and other photoelectric devices exploitation application other or novel electrically conducting transparent is thin
Film just seems necessary.Develop new transparent conductive film the research of the transparency electrode of polymer solar battery is had
Important meaning.Transparent conductive oxide (TCO) includes FTO, ITO, AZO etc., although be widely used in photoelectric device, but
It is that their resistivity is still insufficient to the low requirement meeting these practicality in some cases.
Summary of the invention
It is an object of the invention to provide a kind of transparent conductive film and its preparation method and application, this transparent conductive film has
There are good visible light permeability and electric conductivity.
To achieve these goals, the technological means that the present invention uses is:
A kind of transparent conductive film, component and each constituent mass number are as follows: zinc acetate 10 ~ 20 parts, ethanolamine 3 ~ 8 parts,
Ethylene glycol monomethyl ether 10 ~ 30 parts, hexamethylenetetramine 8 ~ 12 parts, stannum oxide 10 ~ 15 parts, molybdenum oxide 2 ~ 6 parts, 1 ~ 5 part of aluminum, strengthen
Agent 2 ~ 5 parts.
Also include o-dichlorohenzene 0.3 ~ 1.6 part.
Described reinforcing agent is carbon silica fibre.
Transparent conductive film, component and each constituent mass number are as follows: zinc acetate 12 ~ 18 parts, ethanolamine 4 ~ 6 parts, second two
Alcohol methyl ether 15 ~ 25 parts, hexamethylenetetramine 10 ~ 12 parts, stannum oxide 12 ~ 14 parts, molybdenum oxide 3 ~ 5 parts, 2 ~ 4 parts of aluminum, adjacent dichloro
Benzene 0.6 ~ 1.2 part, reinforcing agent 3 ~ 4 parts.
Transparent conductive film, component and each constituent mass number are as follows: zinc acetate 16 parts, ethanolamine 5 parts, ethylene glycol monomethyl ether
20 parts, hexamethylenetetramine 11 parts, stannum oxide 13 parts, molybdenum oxide 4 parts, 3 parts of aluminum, o-dichlorohenzene 0.9 part, reinforcing agent 3.5
Part.
The preparation method of described transparent conductive film, comprises the steps:
1) zinc acetate is joined in ethylene glycol monomethyl ether, is configured to solution, be subsequently adding ethanolamine, be heated to 50 ~ 80 DEG C,
High-speed stirred 2 ~ 4h, forms transparent colloid, stands 18 ~ 30h；
2) hexamethylenetetramine, stannum oxide, molybdenum oxide, aluminum, o-dichlorohenzene and reinforcing agent are added sequentially to step 1) obtain
To colloid in, stirring, be warming up to 500 ~ 800 DEG C, mutually melted infiltration, stir 10 ~ 20h, be exposed under ultraviolet light, ultraviolet light
Power is 800 ~ 1200W, and open-assembly time is 1 ~ 3h, obtains filmogen；
3) by step 2) filmogen that obtains uses sol evenning machine spin coating to transfer to, on solar battery glass substrate, obtain
Transparent conductive film.
Step 1) is heated to 65 DEG C, high-speed stirred 3h, form transparent colloid, stand 34h, the rotating speed of high-speed stirred is
12000rpm。
Step 2) in be warming up to 700 DEG C, mutually melted infiltration, stir 15h, be exposed under ultraviolet light, uv power is
1000W, open-assembly time is 2h.
In step 3), the rotating speed of sol evenning machine low speed is 800rpm, and high speed rotating speed is 4000rpm, keeps at a high speed 30s.
The application in preparing solaode transparency electrode of the described transparent conductive film.
Beneficial effect: a kind of transparent conductive film that the present invention provides and its preparation method and application, this electrically conducting transparent is thin
Film has good visible light permeability and electric conductivity, and the mean transmissivity of the visible region of thin film is more than 85.0%, square
Block resistance is less than 30/sq, is expected to as clear bottom application of electrode among solaode, transparent for carrying out solaode
The developmental research of electrode has definite meaning.
Detailed description of the invention
Embodiment 1
A kind of transparent conductive film, component and each constituent mass number are as follows: zinc acetate 10 parts, ethanolamine 3 parts, ethylene glycol
Methyl ether 10 parts, hexamethylenetetramine 8 parts, stannum oxide 10 parts, molybdenum oxide 2 parts, 1 part of aluminum, reinforcing agent carbon silica fibre 2 parts.
Preparation method, comprises the steps:
1) zinc acetate is joined in ethylene glycol monomethyl ether, be configured to solution, be subsequently adding ethanolamine, be heated to 65 DEG C, high
Speed stirring 3h, forms transparent colloid, stands 34h, and the rotating speed of high-speed stirred is 12000rpm；
2) hexamethylenetetramine, stannum oxide, molybdenum oxide, aluminum, o-dichlorohenzene and reinforcing agent are added sequentially to step 1) obtain
To colloid in, stirring, be warming up to 700 DEG C, mutually melted infiltration, stir 15h, be exposed under ultraviolet light, uv power is
1000W, open-assembly time is 2h, obtains filmogen；
3) by step 2) filmogen that obtains uses sol evenning machine spin coating to transfer to, on solar battery glass substrate, obtain
Transparent conductive film.The rotating speed of sol evenning machine low speed is 800rpm, and high speed rotating speed is 4000rpm, keeps at a high speed 30s.
Embodiment 2
A kind of transparent conductive film, component and each constituent mass number are as follows: zinc acetate 20 parts, ethanolamine 8 parts, ethylene glycol
Methyl ether 30 parts, hexamethylenetetramine 12 parts, stannum oxide 15 parts, molybdenum oxide 6 parts, 5 parts of aluminum, reinforcing agent carbon silica fibre 5 parts.
Preparation method, comprises the steps:
1) zinc acetate is joined in ethylene glycol monomethyl ether, be configured to solution, be subsequently adding ethanolamine, be heated to 65 DEG C, high
Speed stirring 3h, forms transparent colloid, stands 34h, and the rotating speed of high-speed stirred is 12000rpm；
2) hexamethylenetetramine, stannum oxide, molybdenum oxide, aluminum, o-dichlorohenzene and reinforcing agent are added sequentially to step 1) obtain
To colloid in, stirring, be warming up to 700 DEG C, mutually melted infiltration, stir 15h, be exposed under ultraviolet light, uv power is
1000W, open-assembly time is 2h, obtains filmogen；
3) by step 2) filmogen that obtains uses sol evenning machine spin coating to transfer to, on solar battery glass substrate, obtain
Transparent conductive film.The rotating speed of sol evenning machine low speed is 800rpm, and high speed rotating speed is 4000rpm, keeps at a high speed 30s.
Embodiment 3
A kind of transparent conductive film, component and each constituent mass number are as follows: zinc acetate 10 parts, ethanolamine 3 parts, ethylene glycol
Methyl ether 10 parts, hexamethylenetetramine 8 parts, stannum oxide 10 parts, molybdenum oxide 2 parts, 1 part of aluminum, o-dichlorohenzene 0.3 part, reinforcing agent
Carbon silica fibre 2 parts.
Preparation method, comprises the steps:
1) zinc acetate is joined in ethylene glycol monomethyl ether, be configured to solution, be subsequently adding ethanolamine, be heated to 65 DEG C, high
Speed stirring 3h, forms transparent colloid, stands 34h, and the rotating speed of high-speed stirred is 12000rpm；
2) hexamethylenetetramine, stannum oxide, molybdenum oxide, aluminum, o-dichlorohenzene and reinforcing agent are added sequentially to step 1) obtain
To colloid in, stirring, be warming up to 700 DEG C, mutually melted infiltration, stir 15h, be exposed under ultraviolet light, uv power is
1000W, open-assembly time is 2h, obtains filmogen；
3) by step 2) filmogen that obtains uses sol evenning machine spin coating to transfer to, on solar battery glass substrate, obtain
Transparent conductive film.The rotating speed of sol evenning machine low speed is 800rpm, and high speed rotating speed is 4000rpm, keeps at a high speed 30s.
Embodiment 4
A kind of transparent conductive film, component and each constituent mass number are as follows: zinc acetate 20 parts, ethanolamine 8 parts, ethylene glycol
Methyl ether 30 parts, hexamethylenetetramine 12 parts, stannum oxide 15 parts, molybdenum oxide 6 parts, 5 parts of aluminum, o-dichlorohenzene 1.6 parts, reinforcing agent
Carbon silica fibre 5 parts.
Preparation method, comprises the steps:
1) zinc acetate is joined in ethylene glycol monomethyl ether, be configured to solution, be subsequently adding ethanolamine, be heated to 65 DEG C, high
Speed stirring 3h, forms transparent colloid, stands 34h, and the rotating speed of high-speed stirred is 12000rpm；
2) hexamethylenetetramine, stannum oxide, molybdenum oxide, aluminum, o-dichlorohenzene and reinforcing agent are added sequentially to step 1) obtain
To colloid in, stirring, be warming up to 700 DEG C, mutually melted infiltration, stir 15h, be exposed under ultraviolet light, uv power is
1000W, open-assembly time is 2h, obtains filmogen；
3) by step 2) filmogen that obtains uses sol evenning machine spin coating to transfer to, on solar battery glass substrate, obtain
Transparent conductive film.The rotating speed of sol evenning machine low speed is 800rpm, and high speed rotating speed is 4000rpm, keeps at a high speed 30s.
Embodiment 5
Transparent conductive film, component and each constituent mass number are as follows: zinc acetate 12 parts, ethanolamine 4 parts, ethylene glycol monomethyl ether
15 parts, hexamethylenetetramine 10 parts, stannum oxide 12 parts, molybdenum oxide 3 parts, 2 parts of aluminum, o-dichlorohenzene 0.6 part, reinforcing agent carbon silicon
Fiber 3 parts.
Preparation method, comprises the steps:
1) zinc acetate is joined in ethylene glycol monomethyl ether, be configured to solution, be subsequently adding ethanolamine, be heated to 65 DEG C, high
Speed stirring 3h, forms transparent colloid, stands 34h, and the rotating speed of high-speed stirred is 12000rpm；
2) hexamethylenetetramine, stannum oxide, molybdenum oxide, aluminum, o-dichlorohenzene and reinforcing agent are added sequentially to step 1) obtain
To colloid in, stirring, be warming up to 700 DEG C, mutually melted infiltration, stir 15h, be exposed under ultraviolet light, uv power is
1000W, open-assembly time is 2h, obtains filmogen；
3) by step 2) filmogen that obtains uses sol evenning machine spin coating to transfer to, on solar battery glass substrate, obtain
Transparent conductive film.The rotating speed of sol evenning machine low speed is 800rpm, and high speed rotating speed is 4000rpm, keeps at a high speed 30s.
Embodiment 6
Transparent conductive film, component and each constituent mass number are as follows: zinc acetate 18 parts, ethanolamine 6 parts, ethylene glycol monomethyl ether
25 parts, hexamethylenetetramine 12 parts, stannum oxide 14 parts, molybdenum oxide 5 parts, 4 parts of aluminum, o-dichlorohenzene 1.2 parts, reinforcing agent carbon silicon
Fiber 4 parts.
Preparation method, comprises the steps:
1) zinc acetate is joined in ethylene glycol monomethyl ether, be configured to solution, be subsequently adding ethanolamine, be heated to 65 DEG C, high
Speed stirring 3h, forms transparent colloid, stands 34h, and the rotating speed of high-speed stirred is 12000rpm；
2) hexamethylenetetramine, stannum oxide, molybdenum oxide, aluminum, o-dichlorohenzene and reinforcing agent are added sequentially to step 1) obtain
To colloid in, stirring, be warming up to 700 DEG C, mutually melted infiltration, stir 15h, be exposed under ultraviolet light, uv power is
1000W, open-assembly time is 2h, obtains filmogen；
3) by step 2) filmogen that obtains uses sol evenning machine spin coating to transfer to, on solar battery glass substrate, obtain
Transparent conductive film.The rotating speed of sol evenning machine low speed is 800rpm, and high speed rotating speed is 4000rpm, keeps at a high speed 30s.
Embodiment 7
Transparent conductive film, component and each constituent mass number are as follows: zinc acetate 16 parts, ethanolamine 5 parts, ethylene glycol monomethyl ether
20 parts, hexamethylenetetramine 11 parts, stannum oxide 13 parts, molybdenum oxide 4 parts, 3 parts of aluminum, o-dichlorohenzene 0.9 part, reinforcing agent carbon silicon
Fiber 3.5 parts.
Preparation method, comprises the steps:
1) zinc acetate is joined in ethylene glycol monomethyl ether, be configured to solution, be subsequently adding ethanolamine, be heated to 65 DEG C, high
Speed stirring 3h, forms transparent colloid, stands 34h, and the rotating speed of high-speed stirred is 12000rpm；
2) hexamethylenetetramine, stannum oxide, molybdenum oxide, aluminum, o-dichlorohenzene and reinforcing agent are added sequentially to step 1) obtain
To colloid in, stirring, be warming up to 700 DEG C, mutually melted infiltration, stir 15h, be exposed under ultraviolet light, uv power is
1000W, open-assembly time is 2h, obtains filmogen；
3) by step 2) filmogen that obtains uses sol evenning machine spin coating to transfer to, on solar battery glass substrate, obtain
Transparent conductive film.The rotating speed of sol evenning machine low speed is 800rpm, and high speed rotating speed is 4000rpm, keeps at a high speed 30s.
300-800 nm saturating with ultraviolet-visible spectrometer (VarianCary 5000) test transparent conductive film
Penetrate spectrum, calculate the mean transmissivity of the visible region of thin film, electrical properties Ecopia HMS 3000 type Hall effect
Tester and SX1934 type four probe are measured, and the results are shown in Table 1.
Table 1:
| Transmitance/% | Square resistance/(/sq) | |
| Embodiment 1 | 85.0 | 30 |
| Embodiment 2 | 86.4 | 28 |
| Embodiment 3 | 92.3 | 20 |
| Embodiment 4 | 93.1 | 21 |
| Embodiment 5 | 96.5 | 15 |
| Embodiment 6 | 95.3 | 14 |
| Embodiment 7 | 97.8 | 11 |
Claims (10)
1. a transparent conductive film, it is characterised in that raw material components and each constituent mass number are as follows: zinc acetate 10 ~ 20 parts,
Ethanolamine 3 ~ 8 parts, ethylene glycol monomethyl ether 10 ~ 30 parts, hexamethylenetetramine 8 ~ 12 parts, stannum oxide 10 ~ 15 parts, molybdenum oxide 2 ~ 6 parts,
1 ~ 5 part of aluminum, reinforcing agent 2 ~ 5 parts；Zinc acetate is joined in ethylene glycol monomethyl ether, be configured to solution, be subsequently adding ethanolamine, add
Hot to 50 ~ 80 DEG C, high-speed stirred 2 ~ 4h, form transparent colloid, stand 34h；By hexamethylenetetramine, stannum oxide, molybdenum oxide,
Aluminum, o-dichlorohenzene and reinforcing agent are added sequentially in colloid obtained above, stirring, are warming up to 500 ~ 800 DEG C, mutually melt and ooze
Thoroughly, stirring 10 ~ 20h, be exposed under ultraviolet light, uv power is 800 ~ 1200W, and open-assembly time is 1 ~ 3h, filmogen；Will
The filmogen obtained uses sol evenning machine spin coating to transfer to, on solar battery glass substrate, obtain transparent conductive film.
Transparent conductive film the most according to claim 1, it is characterised in that: also include o-dichlorohenzene 0.3 ~ 1.6 part.
Transparent conductive film the most according to claim 1, it is characterised in that: described reinforcing agent is carbon silica fibre.
Transparent conductive film the most according to claim 2, it is characterised in that raw material components and each constituent mass number are as follows: vinegar
12 ~ 18 parts of zinc of acid, ethanolamine 4 ~ 6 parts, ethylene glycol monomethyl ether 15 ~ 25 parts, hexamethylenetetramine 10 ~ 12 parts, stannum oxide 12 ~ 14 parts,
Molybdenum oxide 3 ~ 5 parts, 2 ~ 4 parts of aluminum, o-dichlorohenzene 0.6 ~ 1.2 part, reinforcing agent 3 ~ 4 parts.
Transparent conductive film the most according to claim 4, it is characterised in that raw material components and each constituent mass number are as follows: vinegar
16 parts of zinc of acid, ethanolamine 5 parts, ethylene glycol monomethyl ether 20 parts, hexamethylenetetramine 11 parts, stannum oxide 13 parts, molybdenum oxide 4 parts, aluminum 3
Part, o-dichlorohenzene 0.9 part, reinforcing agent 3.5 parts.
6. the preparation method of transparent conductive film described in claim 1, it is characterised in that comprise the steps:
1) zinc acetate is joined in ethylene glycol monomethyl ether, be configured to solution, be subsequently adding ethanolamine, be heated to 50 ~ 80 DEG C, at a high speed
Stirring 2 ~ 4h, forms transparent colloid, stands 34h；
2) hexamethylenetetramine, stannum oxide, molybdenum oxide, aluminum, o-dichlorohenzene and reinforcing agent are added sequentially to what step 1) obtained
In colloid, stirring, it is warming up to 500 ~ 800 DEG C, the most melted infiltration, stir 10 ~ 20h, be exposed under ultraviolet light, uv power
Being 800 ~ 1200W, open-assembly time is 1 ~ 3h, filmogen；
3) by step 2) filmogen that obtains uses sol evenning machine spin coating to transfer to, on solar battery glass substrate, obtain transparent
Conductive film.
The preparation method of transparent conductive film the most according to claim 6, it is characterised in that: step 1) is heated to 65 DEG C,
High-speed stirred 3h, forms transparent colloid, stands 34h, and the rotating speed of high-speed stirred is 12000rpm.
The preparation method of transparent conductive film the most according to claim 6, it is characterised in that: step 2) in be warming up to 700 DEG C,
The most melted infiltration, stirs 15h, is exposed under ultraviolet light, and uv power is 1000W, and open-assembly time is 2h.
The preparation method of transparent conductive film the most according to claim 6, it is characterised in that: sol evenning machine low speed in step 3)
Rotating speed is 800rpm, and high speed rotating speed is 4000rpm, keeps at a high speed 30s.
10. the application in preparing solaode transparency electrode of the transparent conductive film described in claim 1.
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| JPWO2007142330A1 (en) * | 2006-06-08 | 2009-10-29 | 旭硝子株式会社 | Transparent conductive film, method for producing the same, and sputtering target used for the production thereof |
| KR100999501B1 (en) * | 2008-09-04 | 2010-12-09 | 한국전자통신연구원 | Method for Preparing Metal Doped Transparent Conductive Oxide Thin Film and Thin Film Transistor Using the Same |
| CN102447072A (en) * | 2010-10-12 | 2012-05-09 | 西安文景光电科技有限公司 | Organic electroluminescent device taking aluminum and molybdenum oxide blended thin film as anode |
| CN102442787B (en) * | 2011-09-23 | 2013-09-04 | 青岛海信电器股份有限公司 | Nano air-sensitive thin film and preparation method thereof |
| CN102593239B (en) * | 2011-10-11 | 2015-04-15 | 江苏大学 | Preparation method of latticed textured azo compound (AZO) transparent conductive membrane |
| CN102646759B (en) * | 2012-05-04 | 2015-05-27 | 深圳市科聚新材料有限公司 | Preparing method for transparent conductive oxide film |
| CN102903456B (en) * | 2012-10-17 | 2014-11-26 | 山东建筑大学 | Method for preparing triple-doped novel transparent conductive thin film |
| CN103681901B (en) * | 2013-11-25 | 2016-01-13 | 广州北峻工业材料有限公司 | A kind of blended metal oxide semiconductor solar cell and preparation method thereof |
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