CN102693782A - Manufacturing method for cheap transparent conducting film - Google Patents
Manufacturing method for cheap transparent conducting film Download PDFInfo
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- CN102693782A CN102693782A CN201210168657XA CN201210168657A CN102693782A CN 102693782 A CN102693782 A CN 102693782A CN 201210168657X A CN201210168657X A CN 201210168657XA CN 201210168657 A CN201210168657 A CN 201210168657A CN 102693782 A CN102693782 A CN 102693782A
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- cheap
- base material
- film
- nesa coating
- manufacturing approach
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Abstract
A manufacturing method for a cheap transparent conducting film includes processing steps as the follows: preparing film coating solution, cleaning base material, coating film, electrode making, annealing and electrified aging formation. The manufacturing method is characterized in that the formula of the film coating solution is that the main material zinc acetate is 88g, dopant alchlor is 5g, high-temperature resistance stabilizer titanium chloride is 2g, high-temperature resistance stabilizer lead acetate is 4g, lead escape inhibitor manganous chloride is 1g, cosolvent acetic acid is suitable in proportion, and solvent distilled water is 500 to 1000g. The preparing steps of the film coating are as follows: A, using the acetic acid to acidize the distilled water, and covering for future use; B, weighing the titanium chloride according to the formula and covering for future use; C, weighing other components to be dissolved in the acidized distilled water, dripping slowly the titanium chloride solution to be sufficiently and uniformly mixed, and covering for future use; cleaning the base material; and carrying out film coating, electrode making and electrified aging formation of the base material. Compared with the existing transparent oxide conducting film, the cheap transparent conducting film has the advantages of cheap raw material, excellent cost performance and low cost, and is suitable for making the transparent conducting film.
Description
Technical field
The invention belongs to a kind of is the Ohmic resistance transparent conductive film of characteristic, particularly a kind of manufacturing approach of cheap nesa coating with material or material character.
Background technology
" transparent conductive oxide film " book introduction of publishing according to Higher Education Publishing House: the ZnO material has photoelectricity, piezoelectricity and characteristic such as ferroelectric, widely people's research over nearly 20 years concurrently.As a kind of piezoelectric, ZnO has bigger coupling coefficient, aspect photoelectric properties; Because of its response time fast; Sensing capability is strong, and is used to optical pickocff, after aluminium (Al) and gallium (Ga) doping; ZnO has good light transmission and conductivity, and the ZnO that mixes with lithium (Li) or magnesium (Mg) can be used as ferroelectric material.ZnO is applied in fields such as flat-panel monitor, solar cell and building glasses as a kind of multi-functional semi-conducting material.Problem is; The stability of these films in hot environment is at present no more than SnO
2And In
2O
3Doping system.
Data is introduced: the average content In of metal in the earth's crust: Sn: Zn is 0.1: 40: 132PPm.Consider the rich or poor of resource, sexual valence when market must find the honest and clean substitution material of a kind of property favorable rates as early as possible to the great demand of nesa coating, and the zno-based nesa coating is the most competitive undoubtedly.
Summary of the invention
The objective of the invention is to screen individual compound and make additive, a kind of succession advantage is provided, follow-up progress, the manufacturing approach of nesa coating cheap of fine quality, the stability of raising rete from the source to the problems referred to above.
The manufacturing approach of a kind of cheap nesa coating of the present invention comprises the aging setting process step of preparation coating liquid, cleaned base material, plated film, the system utmost point, annealing or energising, it is characterized in that:
(1) preparation coating liquid
1. coating liquid formulation weight ratio is:
2. the coating liquid preparation steps is:
A, with acetic acid with the distilled water acidifying, build subsequent use;
B, take by weighing titanium tetrachloride liquid, build subsequent use by prescription;
C, take by weighing zinc acetate, alchlor, lead acetate, manganous chloride, be dissolved in the distilled water of acidifying, stir down and slowly splashes into titanium tetrachloride liquid, stir, in the Plastic Drum with cover of packing into, build subsequent use by prescription;
(2) cleaned base material
Glass, pottery, carborundum class base material is placed vertically in the ultrasonic wave cleaning machine, cleans up with the running water polishing, wipes steam, puts into 120-150 ℃ of baking oven and dries, and builds subsequent use;
Micarex and the slim base material of mineral wool stationery are stained with a little wipes of alcohol dust, greasy dirt with absorbent cotton, put into 120-150 ℃ of baking oven and dry, and build subsequent use;
(3) plated film
Load onto clamping apparatus to the base material of cleaning-drying; Send in 600-650 ℃ the plated film stove; With removing the compressed air (pressure is 0.2-0.4MPa) of greasy dirt steam impurity, spray in the stove coating liquid and airborne oxygen and steam reaction with coating liquid is vaporific; The electrically conductive particles that generates is embedded in deposit film forming in the substrate surface lattice, forms the multifunctional transparent film of one deck photo and good thermal stability at substrate surface;
(CH
3COO)
2Zn·2H
2O+4O
2-Δ→ZnO+4CO
2↑+5H
2O↑
2AlCl
3·6H
2O -Δ→AI
2O
3+6HCl↑+3H
2O↑
TiCl
4+2H
2O -Δ→TiO
2+4HCl↑
(CH
3COO)
2Pb·3H
2O+4O
2-Δ→PbO+4CO
2↑+6H
2O↑
PbO+TiO
2 -Δ→PbTiO
3
The lead titanates that generates has low-k and high-curie temperature, can effectively improve the high-temperature stability of rete.
(4) the system utmost point
The brushing silver slurry in the appropriate location of nesa coating after 120-150 ℃ of oven dry, is sent in 600-650 ℃ the reduction furnace reductase 12 0-30 minute, treats that the silvery white that electrode is even compact is qualified.
(5) the aging typing of annealing or energising
Send into the electrically conducting transparent membrane component of system after extremely in 400-500 ℃ the annealing furnace logical N
2Annealing 5-10 divides swollen, or directly uses mechanical connection method extracting power supply cord, with the voltage that is higher than 1.25 times of work; Switched on 3-15 minute, and made the ordering of rete lattice, change the protoxide content in the rete; Improve carrier concentration, improve the conductivity and stability of rete.
The present invention compares with existing transparent oxide conducting film, has the following advantages: 1, and raw material are cheap, and the zinc content in the earth's crust is more than 1,000 times (1320 times) of steel, is 3.3 times of tin, and zinc resource is abundant, and material is easy to get, and has price advantage.2, cost performance is excellent, and the present invention makes principal crystalline phase with ZnO; Select alchlor to make dopant, screening titanium tetrachloride, lead acetate, manganous chloride are made additive, have both passed on photoelectricity, piezoelectricity and the ferroelectric characteristic of Zinc oxide film; Improved the thermal stability of rete again, cost performance is excellent.3, production cost is low, and the spraying thermal decomposition method has been successfully used to the large-area preparation zinc-oxide film; This method has easy and simple to handle, and is with low cost, is easy to advantages such as large tracts of land deposition; The cheap zinc acetate of modern employing replaces steel, tin to make major ingredient, uses through the distilled water instead of ethanol of acidifying with acetic acid and makes solvent, prevents to produce in the solution zinc hydroxide deposition effectively; Improve film quality, reduced production cost.The present invention is applicable to the manufacturing of nesa coating.
Embodiment
A kind of manufacturing approach of cheap nesa coating comprises the aging setting process step of preparation coating liquid, cleaned base material, plated film, the system utmost point, annealing or energising, it is characterized in that:
(1) preparation coating liquid
1. coating liquid recipe ingredient weight ratio:
2. coating liquid preparation steps:
A with the distilled water acidifying, builds subsequent use with acetic acid;
B takes by weighing four titanium oxide liquid by prescription, builds subsequent use;
C takes by weighing zinc acetate, alchlor, lead acetate, manganous chloride by prescription, is dissolved in the distilled water of acidifying, stirs down and slowly splashes into titanium tetrachloride liquid, stirs, and in the Plastic Drum with cover of packing into, builds subsequent use;
(2) cleaned base material
Glass, pottery, carborundum class base material is placed vertically in the ultrasonic wave cleaning machine, cleans up with the running water polishing, wipes steam, puts into 120-150 ℃ of baking oven and dries, and builds subsequent use;
Micarex and the slim base material of mineral wool stationery are stained with a little wipes of alcohol dust, greasy dirt with absorbent cotton, put into 120-150 ℃ of baking oven and dry, and build subsequent use;
(3) plated film
Load onto clamping apparatus to the base material of cleaning-drying; Send in 600-650 ℃ the plated film stove; With removing the compressed air (pressure is 0.2-0.4MPa) of greasy dirt steam impurity, spray in the stove coating liquid and airborne oxygen and steam reaction with coating liquid is vaporific; The electrically conductive particles that generates is embedded in deposit film forming in the substrate surface lattice, forms the multifunctional transparent film of one deck photo and good thermal stability at substrate surface;
(4) the system utmost point
The brushing silver slurry in the appropriate location of nesa coating after 120-150 ℃ of oven dry, is sent in 600-650 ℃ the reduction furnace reductase 12 0-30 minute, treats that the silvery white that electrode is even compact is qualified.
(5) the aging typing of annealing or energising
Send into the electrically conducting transparent membrane component of system after extremely in 400-500 ℃ the annealing furnace logical N
2Annealing 5-10 divides swollen, maybe should connect with mechanical connection method extracting power supply cord, with the voltage that is higher than 1.25 times of work; Switched on 3-15 minute, and made the ordering of rete lattice, change the protoxide content in the rete; Improve carrier concentration, improve the conductivity and stability of rete.
Claims (6)
1. the manufacturing approach of a cheap nesa coating comprises the aging setting process step of preparation coating liquid, cleaned base material, plated film, the system utmost point, annealing or energising, and it is characterized in that: said coating liquid formulation weight ratio is:
The coating liquid preparation steps is: A, with acetic acid with the distilled water acidifying, subsequent use; B, take by weighing titanium tetrachloride liquid by prescription, subsequent use; C, take by weighing zinc acetate, alchlor, lead acetate, manganous chloride, be dissolved in the distilled water of acidifying, stir down and slowly splashes into titanium tetrachloride liquid, stir by prescription, in the Plastic Drum with cover of packing into, subsequent use.
2. the manufacturing approach of a kind of cheap nesa coating as claimed in claim 1 is characterized in that, cleaned base material is glass; Pottery, carborundum class base material is placed vertically in the ultrasonic wave cleaning machine, cleans up with the running water polishing; Wipe steam, put into 120-150 ℃ of baking oven and dry, subsequent use; Micarex and the slim base material of mineral wool stationery, be stained with a little wipes of alcohol dust, greasy dirt with absorbent cotton, put into 120-150 ℃ of baking oven and dry, subsequent use.
3. the manufacturing approach of a kind of cheap nesa coating as claimed in claim 1 is characterized in that, plated film is to load onto clamping apparatus to the base material of cleaning-drying; Send in 600-650 ℃ the plated film stove; Spray in the stove coating liquid is vaporific with the compressed air of removing greasy dirt steam impurity, coating liquid and airborne oxygen and steam reaction, the electrically conductive particles of generation are embedded in the substrate surface lattice; The deposit film forming is at the multifunctional transparent film of substrate surface formation one deck photo and good thermal stability.
4. the manufacturing approach of a kind of cheap nesa coating as claimed in claim 1; It is characterized in that; The system utmost point is at the appropriate location of nesa coating brushing silver slurry; After 120-150 ℃ of oven dry, send in 600-650 ℃ the reduction furnace reductase 12 0-30 minute, treat that the silvery white that electrode is even compact is qualified.
5. the manufacturing approach of a kind of cheap nesa coating as claimed in claim 1 is characterized in that, annealing is to send into the electrically conducting transparent membrane component of system after extremely in 400-500 ℃ the annealing furnace logical N
2Annealing 5-10 divides swollen, makes the ordering of rete lattice.
6. the manufacturing approach of a kind of cheap nesa coating as claimed in claim 1 is characterized in that, the aging typing of energising is directly to use mechanical connection method extracting power supply cord, with the voltage that is higher than 1.25 times of work, switches on 3-15 minute, makes the ordering of rete lattice.
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| CN201210168657.XA CN102693782B (en) | 2012-05-29 | 2012-05-29 | Manufacturing method for cheap transparent conducting film |
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| CN102693782B CN102693782B (en) | 2014-07-30 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103757612A (en) * | 2013-05-30 | 2014-04-30 | 杨葆华 | Environmental protection multifunction electric conduction film manufacturing method |
| CN105239059A (en) * | 2014-07-13 | 2016-01-13 | 上海申航热能科技有限公司 | Preparation method for efficient environment-friendly electrothermal film |
| CN106686772A (en) * | 2016-12-12 | 2017-05-17 | 深圳市中和纳米技术开发有限公司 | Making method of high-temperature transparent electrothermal film |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005330337A (en) * | 2004-05-18 | 2005-12-02 | Sumitomo Metal Mining Co Ltd | Method for producing polyester resin composition containing optically functional microparticle, polyester resin composition containing optically functional microparticle, and polyester resin base containing optically functional microparticle |
| CN101660121A (en) * | 2009-09-15 | 2010-03-03 | 中国科学院上海硅酸盐研究所 | Cation-anion co-doping n-type zinc-oxide-base transparent conducting film and preparation method thereof |
| CN102065589A (en) * | 2010-12-27 | 2011-05-18 | 宁波高新区健坤电热技术有限公司 | Method for manufacturing high-temperature resistant transparent electric heating film |
| CN102311671A (en) * | 2011-08-30 | 2012-01-11 | 河南华美新材料科技有限公司 | AZO transparent conductive film paint, glass plated with the paint and preparation method thereof |
-
2012
- 2012-05-29 CN CN201210168657.XA patent/CN102693782B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005330337A (en) * | 2004-05-18 | 2005-12-02 | Sumitomo Metal Mining Co Ltd | Method for producing polyester resin composition containing optically functional microparticle, polyester resin composition containing optically functional microparticle, and polyester resin base containing optically functional microparticle |
| CN101660121A (en) * | 2009-09-15 | 2010-03-03 | 中国科学院上海硅酸盐研究所 | Cation-anion co-doping n-type zinc-oxide-base transparent conducting film and preparation method thereof |
| CN102065589A (en) * | 2010-12-27 | 2011-05-18 | 宁波高新区健坤电热技术有限公司 | Method for manufacturing high-temperature resistant transparent electric heating film |
| CN102311671A (en) * | 2011-08-30 | 2012-01-11 | 河南华美新材料科技有限公司 | AZO transparent conductive film paint, glass plated with the paint and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103757612A (en) * | 2013-05-30 | 2014-04-30 | 杨葆华 | Environmental protection multifunction electric conduction film manufacturing method |
| CN103757612B (en) * | 2013-05-30 | 2016-04-20 | 杨葆华 | The manufacture method of Environmental protection multifunction electric conduction film |
| CN105239059A (en) * | 2014-07-13 | 2016-01-13 | 上海申航热能科技有限公司 | Preparation method for efficient environment-friendly electrothermal film |
| CN106686772A (en) * | 2016-12-12 | 2017-05-17 | 深圳市中和纳米技术开发有限公司 | Making method of high-temperature transparent electrothermal film |
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| CN102693782B (en) | 2014-07-30 |
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