CN103757612B - The manufacture method of Environmental protection multifunction electric conduction film - Google Patents

The manufacture method of Environmental protection multifunction electric conduction film Download PDF

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CN103757612B
CN103757612B CN201310206271.8A CN201310206271A CN103757612B CN 103757612 B CN103757612 B CN 103757612B CN 201310206271 A CN201310206271 A CN 201310206271A CN 103757612 B CN103757612 B CN 103757612B
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film forming
water
film
acetate
environmental protection
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CN103757612A (en
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杨葆华
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Jilin Shengmin New Energy R&D Co.,Ltd.
Yang Baohua
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Abstract

A kind of manufacture method of Environmental protection multifunction electric conduction film, it is characterized in that, film forming liquid formula weight ratio is: zinc acetate two water 100g is major ingredient, aluminium acetate 47g is doping agent, manganese acetate four water 2.4g, neutralized verdigris one water 1.9g is for strengthening doping agent, and acetic acid is solubility promoter in right amount, and distilled water 100 ~ 500g is solvent.Its preparation process comprises: preparation film forming liquid, cleaned base material, pyrolysis film forming, pole processed lead-in wire, impact aging.Compared with prior art, its outstanding advantages is in the present invention: the present invention adopt zinc, aluminium, manganese, copper, acetate substitute conventional metal chloride prescription, environmental protection and energy saving.Conducting film of the present invention replaces tindioxide and Indium sesquioxide as principal crystalline phase using zinc oxide, replaces dehydrated alcohol make solvent with distilled water.With low-priced Dai Gui, raw material is easy to get, cheap.Can be used for piezoelectric, optical sensor, solar cell, the conducting film of military application and health care aspect.

Description

The manufacture method of Environmental protection multifunction electric conduction film
Technical field
The ohmic resistance conductive film that the present invention is is feature with material or material property, especially relates to a kind of manufacture method of environment protection type multifunctional conducting film.
Background technology
Metal conductive oxide material is the important member in semi-conductor family, and because it has good electrical property and energy-saving effect, recent decades, widely people paid close attention to.The unremitting effort of numerous scientific and technical personnel, technical progress is remarkable, Application Areas is constantly widened, particularly film-type planar electro-conductive material, and because its thermal response is fast, electric conversion efficiency is high, and energy-saving effect is remarkable, and in heating, be used widely in the aspects such as water-heater.
At present, conventional metal conductive oxide film mainly contains tindioxide, indium trioxide, zinc oxide and indium acid cadmium and doping system thereof.Mostly they are to adopt the muriate of respective metal to be dissolved in dehydrated alcohol, are formulated as film forming liquid, at high temperature form metal conductive oxide film through spray pyrolysis or other method, then the elementization that gone between through pole processed is produced.Problem is the ethanolic soln of these metal chlorides, and a large amount of chlorine produced in pyrolytic coating pyrolytic process and hydrogen chloride gas, cause severe contamination to air.Chlorination has rank smell, poisonous! In the air of general operation place, content must not more than 0.001mg/ liter, and the moisture in respiratory tract makes chlorination intense reaction generate hypochlorous acid and hydrochloric acid, the former extremely unstable, and then is decomposed into oxygen and hydrogenchloride.Hydrogenchloride is very easily water-soluble and generate hydrochloric acid.Hydrochloric acid is one of strong acid, has extremely strong corrodibility, can cause burn to skin, has pungency damage to respiratory system.
China has put into effect the regulation of " environmental protection right of veto by one vote " in recent years, describes in the importance of China environmental protection, urgency and national great attention.Walk the old road that developed country " pollutes, century-old improvement " for a year with it, not as beginning from myself, from source to power, doing everything possible and reducing or stop to pollute.
Summary of the invention
The object of the invention is the manufacture method proposing a kind of Environmental protection multifunction electric conduction film, in accordance with the old maxim of " enhance agricultural production and economize expenses ", from protection of the environment, the starting material prescription that the rich inexpensive pollution of candidate is little, reaching can be cost-saving, can treat again the object of environment kindly.
Technical scheme of the present invention is following realization, a kind of manufacture method of Environmental protection multifunction electric conduction film, and its film forming liquid formula weight ratio is:
A manufacture method for Environmental protection multifunction electric conduction film, its processing step comprises: preparation film forming liquid, cleaned base material, pyrolysis film forming, pole processed lead-in wire, impact aging, specifically:
1, preparation film forming liquid: first with acetic acid by distilled water acidifying, in case zinc salt hydrolysis; Take each component by formula again, slowly add zinc acetate two water, aluminium acetate, manganese acetate four water, neutralized verdigris one water under stirring successively, stirring to dissolving completely, building, for subsequent use.
2, cleaned base material: the hard temperature resistant substrate tap water such as glass, pottery, silicon carbide, enamel are cleaned, wipes steam, dry, dust-proof, for subsequent use; Slim temperature resistant substrate is as mica, and mineral wool cloth etc., wipe clean with alcohol swab if desired.
3, pyrolysis masking: base material dry and comfortable for cleaning is loaded onto clamping apparatus, film forming stove is pushed along track, at 250 ~ 300 DEG C, ultra low volume spray (namely utilize special equipment and shower nozzle, make the droplet of ejection be less than 100 microns) is adopted to spray in stove by the atomization of film forming liquid, pass through series of chemical, generate corresponding metal conductive oxide particulate, sedimentation embeds in substrate surface lattice, and long-pending generate take zinc oxide as the conductive doped film of principal crystalline phase.
(CH 3COO) 2Zn·2H 2O+4O 2=ZnO+4CO 2+5H 2O
2(CH 3COO) 3Al+12O 2=Al 2O 3+12CO 2+9H 2O
2(CH 3COO) 2Mn·4H 2O+9O 2=2MnO 2+8CO 2+14H 2O
(CH 3COO) 2Cu·H 2O+4O 2=CuO+4CO 2+4H 2O
CuO+MnO 2=CuMnO 3
National standard method is good semiconductor material, is entrained in zinc oxide crystalline phase, improves capacitive character and the stability of rete.
4, pole processed lead-in wire: according to product needed, coat conductive silver paste in the appropriate location of rete, after about 100 DEG C oven dry, to send in 250 ~ 300 DEG C of reduction furnaces reductase 12 0 ~ 30 minute, cause electrode to be even compact, smooth silvery white is qualified.
5, impact aging: from electrode extraction electrode line, with the voltage higher than operating voltage 1 ~ 25 times with each second for after interval break-make 10 ~ 20 times, logical 3 ~ 10 minutes continuously, make rete Ordering lattice, allow the product of defectiveness fully expose problem simultaneously, screen out in time, to guarantee quality product.
Advantage of the present invention: 1; decreasing pollution; kind treatment environment; the present invention adopt zinc, aluminium, manganese, copper, acetate substitute conventional metal chloride prescription; stopped obnoxious flavour chlorine and hydrogenchloride in reactor off-gas, the substitute is oxygen, the animals and plants such as carbonic acid gas and aqueous vapor survive necessary beneficial gas; to decreasing pollution, protection of the environment plays a role.2, raw material is easy to get, low price, has data introduction: " metal average content indium in the earth's crust: tin: zinc is 0.1: 40: 132ppm ", and conducting film of the present invention replaces tindioxide and Indium sesquioxide as principal crystalline phase using zinc oxide, replace dehydrated alcohol with distilled water and make solvent.With how for few, with low-priced Dai Gui, not only raw material is easy to get, and price advantage is obvious.3, enhance agricultural production and economize expenses, reduce energy consumption, the present invention adopts ultra low volume spray film forming, does not economize because thing is rich, and not thrifty because of inexpensive, medication is few, and effect is fast, and number of dropouts is little, meets the old maxim of " enhance agricultural production and economize expenses ".Film-forming temperature, not as good as the half of prior art, greatly reduces film forming energy consumption.4, performance is various, is widely used, and zinc oxide electro-conductive material has optical, electrical, piezoelectricity and the characteristic such as ferroelectric.As a kind of piezoelectric, zinc oxide percentage coupling is comparatively large, and mutual synergistic effect, can strengthen its task performance, is widely used in modern electronic technology, acousto-optic and Radio Physics molecular engineering techniques.In photoconductive property, because its induction force is strong, response is fast and be used to optical sensor; The doping of aluminium improves the light transmission of rete, electroconductibility and stability and be used to solar cell, flat-panel monitor and heating glass etc., and the doping of national standard method, enhances electric conductivity and the stability of rete; 90% infrared reflectance, has widened the application in military application and health care.As the inexpensive multi-functional semiconductor material of one, zinc chloride conducting film and doping system thereof have wide Prospect of R & D.
Embodiment
A manufacture method for Environmental protection multifunction electric conduction film, its film forming liquid formula weight ratio is:
A manufacture method for Environmental protection multifunction electric conduction film, its processing step comprises: preparation film forming liquid, cleaned base material, pyrolysis film forming, pole processed lead-in wire, impact aging, specifically:
1, preparation film forming liquid: first with acetic acid by distilled water acidifying, in case zinc salt hydrolysis; Take each component by formula again, slowly add zinc acetate two water, aluminium acetate, manganese acetate four water, neutralized verdigris one water under stirring successively, stirring to dissolving completely, building, for subsequent use.
2, cleaned base material: the hard temperature resistant substrate tap water such as glass, pottery, silicon carbide, enamel are cleaned, wipes steam, dry, dust-proof, for subsequent use; Slim temperature resistant substrate is as mica, and mineral wool cloth etc., wipe clean with alcohol swab if desired.
3, pyrolysis masking: base material dry and comfortable for cleaning is loaded onto clamping apparatus, film forming stove is pushed along track, at 250 ~ 300 DEG C, ultra low volume spray (namely utilize special equipment and shower nozzle, make the droplet of ejection be less than 100 microns) is adopted to spray in stove by the atomization of film forming liquid, pass through series of chemical, generate corresponding metal conductive oxide particulate, sedimentation embeds in substrate surface lattice, and long-pending generate take zinc oxide as the conductive doped film of principal crystalline phase.
4, pole processed lead-in wire: according to product needed, coat conductive silver paste in the appropriate location of rete, after about 100 DEG C oven dry, to send in 250 ~ 300 DEG C of reduction furnaces reductase 12 0 ~ 30 minute, cause electrode to be even compact, smooth silvery white is qualified.
5, impact aging: from electrode extraction electrode line, with the voltage higher than operating voltage 1 ~ 25 times with each second for after interval break-make 10 ~ 20 times, logical 3 ~ 10 minutes continuously, make rete Ordering lattice, allow the product of defectiveness fully expose problem simultaneously, screen out in time, to guarantee quality product.

Claims (2)

1. a manufacture method for Environmental protection multifunction electric conduction film, is characterized in that film forming liquid formula weight ratio is:
2. the manufacture method of a kind of Environmental protection multifunction electric conduction film as claimed in claim 1, is characterized in that processing step comprises: preparation film forming liquid, cleaned base material, pyrolysis film forming, pole processed lead-in wire, impact aging, specifically:
Preparation film forming liquid: first with acetic acid by distilled water acidifying, in case zinc salt hydrolysis; Take each component by formula again, slowly add zinc acetate two water, aluminium acetate, manganese acetate four water, neutralized verdigris one water under stirring successively, stirring to dissolving completely, building, for subsequent use;
Cleaned base material: glass, pottery, silicon carbide, enamel hard temperature resistant substrate tap water are cleaned, wipes steam, dry, dust-proof, for subsequent use; The mica of slim temperature resistant substrate, mineral wool cloth, wipes clean with alcohol swab;
Pyrolysis masking: base material dry and comfortable for cleaning is loaded onto clamping apparatus, film forming stove is pushed along track, at 250 ~ 300 DEG C, ultra low volume spray is adopted to spray in stove by the atomization of film forming liquid, pass through series of chemical, generate corresponding metal conductive oxide particulate, sedimentation embeds in substrate surface lattice, and long-pending generate take zinc oxide as the conductive doped film of principal crystalline phase;
Pole processed lead-in wire: coat conductive silver paste in the appropriate location of rete, after drying at 100 DEG C, to send in 250 ~ 300 DEG C of reduction furnaces reductase 12 0 ~ 30 minute, cause electrode to be even compact, smooth silvery white is qualified;
Impact aging: from electrode extraction electrode line, with the voltage higher than operating voltage 1 ~ 25 times with each second for after interval break-make 10 ~ 20 times, logical 3 ~ 10 minutes continuously, make rete Ordering lattice, to guarantee quality product.
CN201310206271.8A 2013-05-30 2013-05-30 The manufacture method of Environmental protection multifunction electric conduction film Active CN103757612B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102291860A (en) * 2011-04-25 2011-12-21 马秀芝 Method for manufacturing automatic temperature-limiting oxide electric-heating film
CN102491742A (en) * 2011-11-17 2012-06-13 上海大学 Method and apparatus for preparing manganese and copper co-doped ZnO diluted magnetic semiconductor material
CN102693782A (en) * 2012-05-29 2012-09-26 姜家福 Manufacturing method for cheap transparent conducting film
CN102923758A (en) * 2012-11-27 2013-02-13 中国科学院广州能源研究所 Preparation method of highly-aluminium-doped zinc oxide nano-powder

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030207093A1 (en) * 2001-12-03 2003-11-06 Toshio Tsuji Transparent conductive layer forming method, transparent conductive layer formed by the method, and material comprising the layer
JP5773354B2 (en) * 2011-02-22 2015-09-02 国立研究開発法人産業技術総合研究所 Method for producing transparent conductive film and transparent conductive film
JP5943318B2 (en) * 2011-07-29 2016-07-05 国立大学法人島根大学 Method for making transparent conductive film

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102291860A (en) * 2011-04-25 2011-12-21 马秀芝 Method for manufacturing automatic temperature-limiting oxide electric-heating film
CN102491742A (en) * 2011-11-17 2012-06-13 上海大学 Method and apparatus for preparing manganese and copper co-doped ZnO diluted magnetic semiconductor material
CN102693782A (en) * 2012-05-29 2012-09-26 姜家福 Manufacturing method for cheap transparent conducting film
CN102923758A (en) * 2012-11-27 2013-02-13 中国科学院广州能源研究所 Preparation method of highly-aluminium-doped zinc oxide nano-powder

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
"铜掺杂氧化锌薄膜的阻变特性";董清臣等;《电子元件与材料》;20110531;第30卷(第5期);第18-19页 *

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