CN101717645A - Etching plaster for metal and metal oxide transparent conducting layer and etching process - Google Patents
Etching plaster for metal and metal oxide transparent conducting layer and etching process Download PDFInfo
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- CN101717645A CN101717645A CN200910193983A CN200910193983A CN101717645A CN 101717645 A CN101717645 A CN 101717645A CN 200910193983 A CN200910193983 A CN 200910193983A CN 200910193983 A CN200910193983 A CN 200910193983A CN 101717645 A CN101717645 A CN 101717645A
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Abstract
The invention discloses an etching plaster for metal and metal oxide transparent conducting layers and an etching process, in the invention, lagging production processes, such as the use of organic solvents, strong acid etching and strong alkaline cleaning and the like, are not used any longer, instead, the etching plaster and the etching process which do not pollute the environment are used. The etching plaster comprises the following components in parts by weight: 0.1-20 parts of salt substance, 2-50 parts of non-volatile acid, 10-30 parts of aqueous high molecular polymer, 0.1-10 parts of dilute wetting dispersant, 0.1-5 parts of defoamer, 10-40 parts of thickening agent, 0.1-10 parts of bacteriostat and 2-30 parts of water. The invention simplifies the process flow, cancels acid and alkali soaking and the use of organic solvents, lowers the environmental protection cost, improves the etching quality of products, and has the effects of high efficiency, energy saving and environmental protection. The invention is widely applied to the fields of electron, semiconductors, fine chemistry industry and the like.
Description
Technical field
The present invention relates to a kind of etching paste, particularly a kind of transparent metal conductive layer or oxidic transparent conductive layers etching and etch process that is applied to fields such as electronics, semi-conductor and fine chemistry industry.
Background technology
The etching technics of present known sheet glass or the epipial conduction plated film of PVC is: silk-screen (acid-proof ink or protection glue) → dry → acid bubble (etching) → alkali bubble (ink removing) → cross clear water → pure water cleaning machine to clean.Promptly, it is coated on the conduction plated film by silk screen printing with acid-proof ink or protection glue according to the requirement of circuit board line pattern; Treat that it dries the back sheet glass or PVC mantle are immersed in the acid solution, the conduction plated film that is not covered by printing ink has been corroded, then be retained by the line pattern of acid-proof ink or the covering of protection glue; And then put into alkali lye and soak, remove acid-proof ink that covers on the line pattern or the purpose of protecting glue; Clean with clear water at last and dry.The main drawback of this technology is:
(1) organic solvent that uses in the technical process such as Tianna solution and strong acid and highly basic, the intense stimulus smell that is produced not only influences workers ' health, contaminate environment, and etching apparatus, acceleration equipment aging.
(2) technology is too complicated, the requirement harshness of each program, as: to the regulation and control of potential of hydrogen, restive.
Summary of the invention
Technical problem to be solved by this invention is to overcome the deficiencies in the prior art, provide a kind of removal with an organic solvent, the production technique that cancellation strong acid etching and highly basic cleaning etc. fall behind is used etching paste that is used for metal and metal oxide transparent conducting layer and etch process free from environmental pollution instead.
The technical scheme that etching paste adopted that the present invention is used for metal and metal oxide transparent conducting layer is: by weight, it is composed of the following components:
0.1～20 part of salts substances
2～50 parts of non-volatile acids
10～30 parts of aqueous polymers
0.1～10 part of dilution wetting dispersing agent
0.1～5 part of defoamer
10～40 parts of thickening materials
0.1～10 part of fungistat
2～30 parts in water
Described salts substances is made of metal ion and acid ion.
Described salts substances is iron(ic) chloride or iron protochloride or zinc chloride or cupric chloride or iron nitrate or cupric nitrate or Silver Nitrate.
Described non-volatile acid is at least a in oxalic acid, sulfuric acid, phosphoric acid, metaphosphoric acid, tetra-sodium, sulfonic acid, the carboxylic acid.
Described aqueous polymer is at least three kinds in aqueous polyurethane, polyvinyl alcohol, water-soluble epoxy resin, water soluble alkyd resin, polyoxyethylene glycol, treated starch, modified fibre resin, modified-cellulose ether, water soluble oils, modified rosin resin and the Sudan Gum-arabic.
Described dilution wetting dispersing agent is at least two kinds in Viscotrol C sulphate, poly-phosphate, silicate, polyacrylic acid derivative, the polyoxyethylene glycol alkyl ester.
Described thickening material has and is taken to few two kinds in colloidal state silicon, methylcellulose gum, carboxymethyl cellulose, Walocel MT 20.000PV, talcum powder, silicon dioxide powder, polyacrylic acid, the bentonite; Described fungistat is that benzene two is fine between TS-802 Biocidal algae-killing agent or SJ-304 Biocidal algae-killing agent or 2.4.5.6-tetrachloro.
The technical scheme that etch process adopted that the present invention is used for the etching paste of metal and metal oxide transparent conducting layer is: this etch process may further comprise the steps:
(a) etching step: described etching paste is coated on sheet glass or the epipial conduction plated film of PVC;
(b) normal temperature is placed or baking procedure: treat that described sheet glass or described PVC mantle normal temperature in the step (a) placed 5-30 minute, or described sheet glass or described PVC mantle toasted, the temperature of described sheet glass baking is 60 ℃～180 ℃, and the temperature of described PVC mantle baking is 60 ℃～130 ℃;
(c) soaking step: with described sheet glass in tap water or the pure water soaking step (b) or described PVC mantle;
(d) cleaning step: the described sheet glass in the step (c) or described PVC mantle are crossed cleaning machine with pure water spray, flush clean and air-dry.
Etched mode can or be soaked mark or silk screen printing or stencilization or impression or bat printing or ink jet printing are finished by spraying or spin coating in the described step (a).
Storing temperature in the described step (b) is 80 ℃～130 ℃.
The invention has the beneficial effects as follows: owing to the present invention includes etching step, normal temperature is placed or baking procedure, soaking step, cleaning step, remove with an organic solvent, the production technique that cancellation strong acid etching and highly basic cleaning etc. fall behind, use the environmentally friendly metal and the etching paste of metal oxide transparent conducting layer instead, save soda acid and soaked operation, avoided the damage of the conducting film that strong acid and highly basic in the immersion process keeps need, simplified technical process, remove the use of soda acid immersion and organic solvent from, so reduce the environmental protection cost, improved the etching quality of product, had efficient, energy-conservation, the effect of environmental protection.
The present invention can pass through variety of way: as spraying, spin coating, soak mark or be coated on the transparent conductive layer by methods such as silk screen printing, stencilization, impression, bat printing or ink jet printings, and according to electro-conductive material different as: tin indium oxide In
2O
3: Sn (ITO), the adulterated stannic oxide SnO of fluorine
2: F (FTO), the adulterated stannic oxide SnO of antimony
2: Sb (ATO), the adulterated zinc oxide ZnO:AI of aluminium (AZO), stannic acid cadmium CdSnO
3(CTO), the adulterated zinc oxide ZnO:In of indium (IZO), unadulterated stannic oxide (IV) (TO), unadulterated Indium sesquioxide (III) (IO), unadulterated zinc oxide (ZO) amorphous sial conductive layer etc.; select proportioning between the starting material and suitable temperature and time and finish etching; characteristics such as not only etch capabilities is strong for it, etching precision height, easy operation; the most key is save energy, enhances productivity and environment protection.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Embodiment
Embodiment one:
The prescription of etching paste of the present invention is: by weight, it is composed of the following components:
Iron(ic) chloride is got 0.1 part;
Sulfuric acid and oxalic acid are got 2 parts;
Aqueous polyurethane, polyvinyl alcohol, water-soluble epoxy resin are got 10 parts;
Viscotrol C sulphate, poly-phosphate are got 0.1 part;
Defoamer is that the SN-D468 defoamer that Japanese San Nopco produces is got 0.1 part;
Thickening material is that colloidal state silicon and methylcellulose gum are got 10 parts;
Fungistat is 0.1 part of a TS-802 Biocidal algae-killing agent;
Water is 30 parts; Above-mentioned raw materials is mixed with forms etching paste.
The etch process that the present invention is used for the etching paste of metal and metal oxide transparent conducting layer is:
As shown in Figure 1, described etching paste is imprinted on tin indium oxide In by silk screen printing
2O
3: on the conduction plated film of Sn (ITO), the silk screen mesh is the 100-380 order, the silk screen printing speed control is at 30cm/ about second, scraper speed will guarantee down the China ink amount, silk screen is made the back close inspection silk screen that finishes, prevent the defective of slipping through the net, cause the ITO conducting film to keep the damage of face, printing back normal temperature was placed 5-10 minute, soak about 5-20 minute (or soak to shorten soak time through ultrasonic bath) with tap water or pure water, etching reaction speed is accelerated with the lifting of temperature, and specific requirement can be done necessary adjustment according to producing needs, crosses cleaning machine at last and sprays with pure water, flush clean is also air-dry.
Embodiment two:
The prescription of etching paste of the present invention is: by weight, it is composed of the following components:
Iron protochloride is got 20 parts;
Sulfuric acid and pyrosulfuric acid are got 50 parts;
Water soluble alkyd resin, polyoxyethylene glycol, treated starch are got 30 parts;
Poly-phosphate, silicate, polyacrylic acid derivative are got 10 parts;
Defoamer is that the Bevaloid691 defoamer that the Bew-aloid of Britain produces is got 5 parts;
Thickening material is that carboxymethyl cellulose, Walocel MT 20.000PV are got 40 parts;
Fungistat is got 10 parts for the SJ-304 Biocidal algae-killing agent;
Water is 2 parts; Above-mentioned raw materials is mixed with forms etching paste.
The etch process that the present invention is used for the etching paste of metal and metal oxide transparent conducting layer is:
Described etching paste is imprinted on the adulterated stannic oxide SnO of fluorine by silk screen printing
2: on the conduction plated film of F (FTO), the silk screen mesh is the 100-380 order, the silk screen printing speed control is at 30cm/ about second, scraper speed will guarantee down the China ink amount, silk screen is made the back close inspection silk screen that finishes, prevent the defective of slipping through the net, cause the ITO conducting film to keep the damage of face, the printing back required to enter baking in 10-30 minute, storing temperature is 80-120 ℃, and 5-20 minute (or soak can shorten soak time through ultrasonic bath) soaked with tap water or pure water in baking back, and etching reaction speed is accelerated with the lifting of temperature, can do necessary adjustment according to producing needs, cross cleaning machine at last and spray with pure water, flush clean is also air-dry.Present embodiment is longer than the etching period of embodiment one.
Embodiment three:
The prescription of etching paste of the present invention is: by weight, it is composed of the following components:
Cupric chloride is got 10 parts;
Sulfonic acid, carboxylic acid are got 25 parts;
Modified-cellulose ether, water soluble oils, modified rosin resin and Sudan Gum-arabic are got 20 parts;
Silicate, polyacrylic acid derivative, polyoxyethylene glycol alkyl ester are got 5 parts;
Defoamer is that the Bevaloid691 defoamer that the Bew-aloid of Britain produces is got 3 parts;
Thickening material is that polyacrylic acid, organic bentonite and inorganic bentonite are got 25 parts;
To be that benzene two is fine between the 2.4.5.6-tetrachloro get 5 parts to fungistat;
Water is 20 parts; Above-mentioned raw materials is mixed with forms etching paste.
The difference of present embodiment and embodiment two is: material is a conducting film on glass, and storing temperature is 120-140 ℃, and etching period is 5-20 minute.
All the other are identical with embodiment two.
Embodiment four:
The prescription of etching paste of the present invention is: by weight, it is composed of the following components:
Iron nitrate is got 10 parts;
Metaphosphoric acid and oxalic acid are got 25 parts;
Polyoxyethylene glycol, treated starch, modified fibre resin, modified-cellulose ether, water soluble oils are got 20 parts;
Silicate, polyacrylic acid derivative are got 5 parts;
Defoamer is that high-carbon alcohol ester ester compound DSA-5 gets 3 parts;
Thickening material is that Walocel MT 20.000PV, talcum powder are got 25 parts;
Fungistat is got 5 parts for the SJ-304 Biocidal algae-killing agent;
Water is 30 parts; Above-mentioned raw materials is mixed with forms etching paste.
The difference of present embodiment and embodiment two is: material is that the film conductive layer spins in Japan, and storing temperature is 140-150 ℃, and etching period is 25-30 minute.
All the other are identical with embodiment two.
Embodiment five:
The prescription of etching paste of the present invention is: by weight, it is composed of the following components:
Iron nitrate is got 1 part;
Metaphosphoric acid is got 2 parts;
Polyoxyethylene glycol, treated starch, modified fibre resin, modified-cellulose ether, water soluble oils are got 10 parts;
Silicate, polyacrylic acid derivative are got 1 part;
Defoamer is that high-carbon alcohol ester ester compound DSA-5 gets 1 part;
Thickening material is that Walocel MT 20.000PV, talcum powder are got 10 parts;
Fungistat is got 2 parts for the SJ-304 Biocidal algae-killing agent;
Water is 20 parts; Above-mentioned raw materials is mixed with forms etching paste.
The difference of present embodiment and embodiment two is: material is the tindioxide conducting film, and storing temperature is 140-150 ℃, and etching period is 25-30 minute.
All the other are identical with embodiment two.
Embodiment six:
The prescription of etching paste of the present invention is: by weight, it is composed of the following components:
Iron nitrate is got 20 parts;
Metaphosphoric acid is got 50 parts;
Polyoxyethylene glycol, treated starch, modified fibre resin, modified-cellulose ether, water soluble oils are got 30 parts;
Silicate, polyacrylic acid derivative are got 10 parts;
Defoamer is that high-carbon alcohol ester ester compound DSA-5 gets 5 parts;
Thickening material is that Walocel MT 20.000PV, talcum powder are got 40 parts;
Fungistat is got 10 parts for the SJ-304 Biocidal algae-killing agent;
Water is 30 parts; Above-mentioned raw materials is mixed with forms etching paste.
Engraving method is with embodiment one.
The amount of etching period of the present invention and salts substances and non-volatile acid is inversely proportional to, according to the difference of conductive material, and etched asynchronism(-nization). Can select suitable temperature and time to finish etching according to conductive material. The characteristics such as not only etch capabilities is strong in the present invention, etching precision height, easy operation, the most key is energy savings, enhances productivity and environmental protection.
Claims (10)
1. be used for the etching paste of metal and metal oxide transparent conducting layer, it is characterized in that: by weight,
It is composed of the following components:
0.1～20 part of salts substances
2～50 parts of non-volatile acids
10～30 parts of aqueous polymers
0.1～10 part of dilution wetting dispersing agent
0.1～5 part of defoamer
10～40 parts of thickening materials
0.1～10 part of fungistat
2～30 parts in water
2. the etching paste that is used for metal and metal oxide transparent conducting layer according to claim 1 is characterized in that: described salts substances is made of metal ion and acid ion.
3. the etching paste that is used for metal and metal oxide transparent conducting layer according to claim 2 is characterized in that: described salts substances is iron(ic) chloride or iron protochloride or zinc chloride or cupric chloride or iron nitrate or cupric nitrate or Silver Nitrate.
4. the etching paste that is used for metal and metal oxide transparent conducting layer according to claim 1 is characterized in that: described non-volatile acid is at least a in oxalic acid, sulfuric acid, phosphoric acid, metaphosphoric acid, tetra-sodium, sulfonic acid, the carboxylic acid.
5. the etching paste that is used for metal and metal oxide transparent conducting layer according to claim 1 is characterized in that: described aqueous polymer is at least three kinds in aqueous polyurethane, polyvinyl alcohol, water-soluble epoxy resin, water soluble alkyd resin, polyoxyethylene glycol, treated starch, modified fibre resin, modified-cellulose ether, water soluble oils, modified rosin resin and the Sudan Gum-arabic.
6. the etching paste that is used for metal and metal oxide transparent conducting layer according to claim 1 is characterized in that: described dilution wetting dispersing agent is at least two kinds in Viscotrol C sulphate, poly-phosphate, silicate, polyacrylic acid derivative, the polyoxyethylene glycol alkyl ester.
7. the etching paste that is used for metal and metal oxide transparent conducting layer according to claim 1 is characterized in that: described thickening material has and is taken to few two kinds in colloidal state silicon, methylcellulose gum, carboxymethyl cellulose, Walocel MT 20.000PV, talcum powder, silicon dioxide powder, polyacrylic acid, the bentonite; Described fungistat is that benzene two is fine between TS-802 Biocidal algae-killing agent or SJ-304 Biocidal algae-killing agent or 2.4.5.6-tetrachloro.
8. one kind is utilized the described etch process that is used for the etching paste of metal and metal oxide transparent conducting layer of claim 1, and it is characterized in that: this etch process may further comprise the steps:
(a) etching step: described etching paste is coated on sheet glass or the epipial conduction plated film of PVC;
(b) normal temperature is placed or baking procedure: treat that described sheet glass or described PVC mantle normal temperature in the step (a) placed 5-30 minute, or described sheet glass or described PVC mantle toasted, the temperature of described sheet glass baking is 60 ℃～180 ℃, and the temperature of described PVC mantle baking is 60 ℃～130 ℃;
(c) soaking step: with described sheet glass in tap water or the pure water soaking step (b) or described PVC mantle;
(d) cleaning step: the described sheet glass in the step (c) or described PVC mantle are crossed cleaning machine with pure water spray, flush clean and air-dry.
9. the etch process that is used for the etching paste of metal and metal oxide transparent conducting layer according to claim 8 is characterized in that: etched mode can or be soaked mark or silk screen printing or stencilization or impression or bat printing or ink jet printing are finished by spraying or spin coating in the described step (a).
10. the etch process that is used for the etching paste of metal and metal oxide transparent conducting layer according to claim 8 is characterized in that: the storing temperature in the described step (b) is 80 ℃～130 ℃.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910193983A CN101717645A (en) | 2009-11-17 | 2009-11-17 | Etching plaster for metal and metal oxide transparent conducting layer and etching process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910193983A CN101717645A (en) | 2009-11-17 | 2009-11-17 | Etching plaster for metal and metal oxide transparent conducting layer and etching process |
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| CN101717645A true CN101717645A (en) | 2010-06-02 |
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| CN102127447A (en) * | 2009-12-30 | 2011-07-20 | 杜邦太阳能有限公司 | Morphology design of transparent conductive metal oxide films |
| CN102540608A (en) * | 2010-12-07 | 2012-07-04 | 比亚迪股份有限公司 | Flexible light-dimming stacking body and preparation method thereof |
| CN102902389A (en) * | 2011-07-27 | 2013-01-30 | 比亚迪股份有限公司 | Method for manufacturing touch sensor |
| CN103215592A (en) * | 2013-04-27 | 2013-07-24 | 苏州诺菲纳米科技有限公司 | Etching cream, applications of etching cream, and method for etching nano silver conductive material by utilizing etching cream |
| CN103508677A (en) * | 2013-09-24 | 2014-01-15 | 苏州诺维克光伏新材料有限公司 | Paste material and application thereof |
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| CN103980905A (en) * | 2014-05-07 | 2014-08-13 | 佛山市中山大学研究院 | Novel etching solution used in oxide material system, and etching method and application thereof |
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| CN102127447A (en) * | 2009-12-30 | 2011-07-20 | 杜邦太阳能有限公司 | Morphology design of transparent conductive metal oxide films |
| CN102540608A (en) * | 2010-12-07 | 2012-07-04 | 比亚迪股份有限公司 | Flexible light-dimming stacking body and preparation method thereof |
| CN102540608B (en) * | 2010-12-07 | 2016-03-02 | 比亚迪股份有限公司 | A kind of preparation method of flexible light modulation duplexer and flexible light modulation duplexer |
| CN102902389A (en) * | 2011-07-27 | 2013-01-30 | 比亚迪股份有限公司 | Method for manufacturing touch sensor |
| CN102902389B (en) * | 2011-07-27 | 2016-04-20 | 深圳市比亚迪电子部品件有限公司 | A kind of method for making of touch sensor |
| CN103215592B (en) * | 2013-04-27 | 2015-07-08 | 苏州诺菲纳米科技有限公司 | Etching cream, applications of etching cream, and method for etching nano silver conductive material by utilizing etching cream |
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| CN103593090A (en) * | 2013-11-30 | 2014-02-19 | 东莞市平波电子有限公司 | Manufacturing technology of touch module of GF2 double-face conducting thin film and silver elargol wiring structure |
| CN103980905A (en) * | 2014-05-07 | 2014-08-13 | 佛山市中山大学研究院 | Novel etching solution used in oxide material system, and etching method and application thereof |
| CN104765515A (en) * | 2015-03-12 | 2015-07-08 | 青岛元盛光电科技有限公司 | Manufacture technology for G1F structure capacitive type touch screen |
| WO2016203268A1 (en) * | 2015-06-19 | 2016-12-22 | Dst Innovations Limited | A method for making patterned conductive textiles |
| CN106283055A (en) * | 2016-08-31 | 2017-01-04 | 河源西普电子有限公司 | A kind of engraving method of printed panel |
| CN106433647B (en) * | 2016-09-19 | 2019-02-15 | 苏州诺菲纳米科技有限公司 | Etching paste and preparation method thereof based on nano-silver conductive film |
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| CN109722248A (en) * | 2018-01-03 | 2019-05-07 | 厦门蓝科电子科技有限公司 | A kind of etching paste and preparation method thereof |
| CN109358437A (en) * | 2018-09-12 | 2019-02-19 | 东莞通华液晶有限公司 | A kind of etch tool and technique applied to RTP |
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| CN112194255A (en) * | 2020-10-16 | 2021-01-08 | 中交天航港湾建设工程有限公司 | Ecological restoration method and device for eutrophic river water body |
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| CN113957717A (en) * | 2021-11-15 | 2022-01-21 | 安徽华烨特种材料有限公司 | Ultra-high molecular weight polyethylene fiber reinforced material and preparation method thereof |
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Application publication date: 20100602 |