CN103046108A - Electrolysis process used in ITO film cleaning - Google Patents
Electrolysis process used in ITO film cleaning Download PDFInfo
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- CN103046108A CN103046108A CN2012105673668A CN201210567366A CN103046108A CN 103046108 A CN103046108 A CN 103046108A CN 2012105673668 A CN2012105673668 A CN 2012105673668A CN 201210567366 A CN201210567366 A CN 201210567366A CN 103046108 A CN103046108 A CN 103046108A
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Abstract
The invention relates to an electrolysis process used in ITO (Indium Tin Oxide) film cleaning. The ITO film cleaning process comprises the following steps: placing a component in sulfuric acid electrolyte, and cleaning the ITO film by electrolyzation, wherein the component is an aluminum alloy component of which the surface is covered with the ITO film. In the process of dissolution of the ITO film, aluminum alloy is used as the anode in the sulfuric acid electrolyte to form a dense oxide film to protect parent metal of the component, so as to improve recycling service life of the component; and recovery of components of precious metal can be realized to avoid the loss in a traditional chemical recovery process.
Description
Technical field
The present invention relates to the ITO film, the particularly application of a kind of electrolysis process in the ITO film is cleaned.
Background technology
Tin indium oxide (ITO, perhaps tin-doped indium oxide) is a kind of indium (III family) oxide compound (In
2O
3) and tin (IV family) oxide compound (SnO
2) mixture, usually mass ratio is 90% In
2O
3, 10% SnO
2Usually the method for deposited by electron beam evaporation, physical vapor deposition or some sputter-deposition technologies deposits to the surface and obtains indium tin oxides film.
For cleaning of ITO film, usually adopt matting.At present conventional matting generally is that component (or being called accessory) directly is immersed in the acid solution and cleans, and acid solution itself has the corrosive wear of a great deal of to the component mother metal in the cleaning process, cleans to reach some amount, and it is relatively high that liquid medicine is carried out cost recovery.Another mode is to adopt high-pressure water cutter mode striping, can cause a large amount of recyclable ITO to run off.
Therefore, a kind of novel ITO film method of cleaning need to be developed in this area, avoids the corrosion of component and the loss of precious metal composition.
Summary of the invention
Purpose of the present invention just provides a kind of novel ITO film method of cleaning, electrochemical process is attached in the conventional ITO membrance chemistry wash clean process, to save cost and to improve the component life-span.
ITO film method of cleaning provided by the invention comprises component is placed sulfuric acid electrolyte, by electrolysis the ITO film is cleaned, and wherein, described component is covered with the component of the aluminum alloy material of ITO film for the surface.
According to the present invention, described sulfuric acid electrolyte is aqueous sulfuric acid, concentration range 120g/L～250g/L, 15～35 ℃ of temperature ranges.
According to the present invention, described electrolysis is take noble electrode as negative electrode, and take component as anode, the Area Ratio of negative electrode and positive electrode is 1:1～1:2, and voltage is 5～17V.
The electrolysis actual current is determined by the useful area of parts.
According to the present invention, described noble electrode is graphite, lead or titanium.
Among the present invention, so-called noble electrode refers to the material that do not dissolve as negative electrode under the electrolytic condition.
According to the present invention, described method also comprises the step of the component after the electrolysis being carried out aftertreatment, and described aftertreatment comprises: sandblast is molten penetrates.
The component that electrolytic cleaning is finished, post processing mode are same as the matting flow process substantially, and the floating ash in surface is removed in neutralization, according to the roughness demand, normally do sandblast and moltenly penetrate processing and get final product.
According to the present invention, described method also comprises the step of the sulfuric acid electrolyte after the electrolysis being carried out aftertreatment, and described aftertreatment comprises reclaims the In element in the sulfuric acid electrolyte.
In ITO film wash clean process, the ITO vitriolization wherein also can be mixed into aluminum ion, cupric ion etc., adopts graphite anode, titanium plate to do catholyte and reclaims metal In.
According to the present invention, the In constituent content reclaims the In element in the sulfuric acid electrolyte greater than 20g/L in described sulfuric acid electrolyte.
Method of the present invention, in the ITO film dissolution process, aluminium alloy forms dense oxidation film as anode the component mother metal is protected in sulfuric acid electrolyte, improves the life-span that component recycles.The present invention can also reclaim the precious metal composition, avoids the loss in the traditional chemical removal process.
In should be understood that within the scope of the present invention, above-mentioned each technical characterictic of the present invention and can making up mutually between specifically described each technical characterictic in below (eg embodiment), thus consist of new or preferred technical scheme.As space is limited, this tired stating no longer one by one.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used for explanation the present invention and be not used in and limit the scope of the invention.
Term
Tin indium oxide ITO
Tin indium oxide (ITO, perhaps tin-doped indium oxide) is a kind of indium (III family) oxide compound (In
2O
3) and tin (IV family) oxide compound (SnO
2) mixture, usually mass ratio is 90% In
2O
3, 10% SnO
2It is clear, colorless when film like.When bulk state, it is yellow partially grey.The main characteristic of tin indium oxide is its electricity conduction and optically transparent combination.
The indium tin oxide films the most normally method of deposited by electron beam evaporation, physical vapor deposition or some sputter-deposition technologies deposits to the surface, and using maximum is reactive magnetron sputtering method.Wherein, the ITO conducting film is method sputter transparent indium tin oxide (ITO) conductive film coating and the high-tech product that obtains through the high temperature anneal on transparent organic film material that adopts magnetron sputtering.
Embodiment 1
Present embodiment is take TFT(thin film transistor production unit) the color membrane production equipment substrate carrier of color film ITO Sputter(CF Carrier of the 6th generation) component carries out electrolytic cleaning as example
Component surface Direct precipitation ITO film after sandblast increases bulk processing during use, its upper and lower plates is aluminium matter; Aqueous sulfuric acid with 150g/L in the operation is done electrolytic solution, the titanium plate that the total area is 600 square decimeters (a kind of noble electrode that the present invention is used) is negative electrode, each upper lower aluminum sheet (totally 8, about 600 square decimeters of the total area) of 4 Carrier that loads is as anode; Processing temperature is controlled at 17 ± 2 ℃, and voltage is about 7V; Each electrolysis takes about 3 hours; Normally neutralize with the nitre fluoric acid after electrolytic cleaning is finished, and cleaning is finished in washing, sandblast etc.
Cleaning performance: the membranous cleaning of component surface ITO after the electrolytic cleaning is complete, and the whole slight loss of parts surface is the uniform loss shape; With the Measurement and analysis with groove test piece and actual component, the loss of electrolytic cleaning is at 10～15 microns (μ m).
Embodiment 2
Adopt the method for embodiment 1 to clean the ITO film, when In content is 22g/L in the electrolytic solution, reclaim
With 20dm
2The titanium plate do negative electrode, 20dm
2Graphite cake is anode, and room temperature condition voltage stabilizing 3V carries out electrolysis, the about 16A of actual current, and about 20 hours of electrolysis, cathode surface deposits thick indium, obtains indium metal after the refinement.
Embodiment 3-6
The method of embodiment 3-6 is substantially the same manner as Example 1, and difference is:
Embodiment 3: adopt the aqueous sulfuric acid of 225g/L to do electrolytic solution, the membranous cleaning of component surface ITO after the electrolytic cleaning is complete, and the whole slight loss of parts surface is the uniform loss shape; With the Measurement and analysis with groove test piece and actual component, the loss of electrolytic cleaning is at 10～15 microns (μ m).
Embodiment 4: the electrolysis processing temperature is 25 ± 2 ℃, and voltage is 15V, and the membranous cleaning of component surface ITO after the electrolytic cleaning is complete, and the whole slight loss of parts surface is the uniform loss shape; With the Measurement and analysis with groove test piece and actual component, the loss of electrolytic cleaning is at 15～25 microns (μ m).
Embodiment 5: load the upper lower aluminum sheet (totally 4, about 300 square decimeters of the total area) of 2 Carrier, the membranous cleaning of component surface ITO after the electrolytic cleaning is complete at every turn, and the whole slight loss of parts surface is the uniform loss shape; With the Measurement and analysis with groove test piece and actual component, the loss of electrolytic cleaning is at 8～12 microns (μ m).
Embodiment 6: as negative electrode, the membranous cleaning of component surface ITO after the electrolytic cleaning is complete with graphite, and the whole slight loss of parts surface is the uniform loss shape; With the Measurement and analysis with groove test piece and actual component, the loss of electrolytic cleaning is at 10～15 microns (μ m).
Cleaning performance: the membranous cleaning of component surface ITO after the electrolytic cleaning is complete, and the whole slight loss of parts surface is the uniform loss shape; With the Measurement and analysis with groove test piece and actual component, the loss of electrolytic cleaning is 8～12 microns (μ m) at 10～15um or lower.
Comparative Examples:
Comparative Examples adopts traditional acid cleaning process, and the component in the embodiment 1 use the 40%(volume ratio as processing object) the aqueous nitric acid immersion.After soaking about 1 hour, the membranous cleaning of surperficial ITO is complete, and the corrosion uneven phenomenon appears in aluminium sheet, and the loss of striping process aluminum mother plate is at 50～60 microns (μ m).
Method of the present invention is compared with traditional method, and in the ITO film dissolution process, aluminium alloy forms dense oxidation film as anode the component mother metal is protected in sulfuric acid electrolyte, improves the life-span that component recycles, and saves the treatment time.The present invention can also reclaim the precious metal composition, avoids the loss in the traditional chemical removal process.
All quote in this application as a reference at all documents that the present invention mentions, just as each piece document is quoted separately as a reference.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after having read above-mentioned teachings of the present invention, these equivalent form of values fall within the application's appended claims limited range equally.
Claims (8)
1. an ITO film method of cleaning is characterized in that, described method comprises component is placed sulfuric acid electrolyte, by electrolysis the ITO film is cleaned, and wherein, described component is covered with the component of the aluminum alloy material of ITO film for the surface.
2. the method for claim 1 is characterized in that, described sulfuric acid electrolyte is aqueous sulfuric acid, concentration range 120g/L～250g/L, and the electrolysis range of working temperature is 15～35 ℃.
3. the method for claim 1 is characterized in that, described electrolysis is take noble electrode as negative electrode, and take component as anode, the Area Ratio of negative electrode and positive electrode is 1:1～1:2, and voltage is 5～17V.
4. method as claimed in claim 3 is characterized in that, described noble electrode is graphite, lead or titanium.
5. the method for claim 1 is characterized in that, described method also comprises the step of the component after the electrolysis being carried out aftertreatment, and described aftertreatment comprises: sandblast is molten penetrates.
6. the method for claim 1 is characterized in that, described method also comprises the step of the sulfuric acid electrolyte after the electrolysis being carried out aftertreatment, and described aftertreatment comprises reclaims the In element in the sulfuric acid electrolyte.
7. method as claimed in claim 6 is characterized in that, adopts graphite as anode, and the titanium plate is as the In in the catholyte reclaim(ed) sulfuric acid electrolytic solution.
8. such as claim 6 or 7 described methods, it is characterized in that the In constituent content reclaims the In element in the sulfuric acid electrolyte greater than 20g/L in described sulfuric acid electrolyte.
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| CN201210567366.8A CN103046108B (en) | 2012-12-24 | 2012-12-24 | Application of the electrolysis process in ito film is cleaned |
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| CN201210567366.8A CN103046108B (en) | 2012-12-24 | 2012-12-24 | Application of the electrolysis process in ito film is cleaned |
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Citations (7)
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| JPS60186019A (en) * | 1984-03-05 | 1985-09-21 | Mitsubishi Electric Corp | Etching method of ito |
| CN1420184A (en) * | 2002-11-07 | 2003-05-28 | 长沙矿冶研究院 | Method for extracting refined indium from indium tin oxide waste material |
| JP2007033967A (en) * | 2005-07-28 | 2007-02-08 | Seiko Epson Corp | Manufacturing method of liquid crystal apparatus, liquid crystal apparatus and electronic device |
| JP2007056367A (en) * | 2005-07-29 | 2007-03-08 | Mitsubishi Materials Corp | Method for recovering indium from blast particle |
| CN101104883A (en) * | 2007-07-07 | 2008-01-16 | 王树楷 | Method for reclaiming indium and tin from ITO waste material by pickling-vulcanization deposition combined technique |
| CN101235508A (en) * | 2007-11-08 | 2008-08-06 | 韶关市锦源实业有限公司 | Method for preparing high-purity indium sulfate |
| CN101416283A (en) * | 2006-04-12 | 2009-04-22 | 日立造船株式会社 | Method of removing conductive metal oxide thin-film and apparatus thereof |
-
2012
- 2012-12-24 CN CN201210567366.8A patent/CN103046108B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60186019A (en) * | 1984-03-05 | 1985-09-21 | Mitsubishi Electric Corp | Etching method of ito |
| CN1420184A (en) * | 2002-11-07 | 2003-05-28 | 长沙矿冶研究院 | Method for extracting refined indium from indium tin oxide waste material |
| JP2007033967A (en) * | 2005-07-28 | 2007-02-08 | Seiko Epson Corp | Manufacturing method of liquid crystal apparatus, liquid crystal apparatus and electronic device |
| JP2007056367A (en) * | 2005-07-29 | 2007-03-08 | Mitsubishi Materials Corp | Method for recovering indium from blast particle |
| CN101416283A (en) * | 2006-04-12 | 2009-04-22 | 日立造船株式会社 | Method of removing conductive metal oxide thin-film and apparatus thereof |
| CN101104883A (en) * | 2007-07-07 | 2008-01-16 | 王树楷 | Method for reclaiming indium and tin from ITO waste material by pickling-vulcanization deposition combined technique |
| CN101235508A (en) * | 2007-11-08 | 2008-08-06 | 韶关市锦源实业有限公司 | Method for preparing high-purity indium sulfate |
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Effective date of registration: 20181213 Address after: 244000 Jinqiao Economic Development Zone, Tongling, Anhui Province Patentee after: Anhui Fule De Science and Technology Development Co., Ltd. Address before: No. 181 Shanlian Road, Baoshan City Industrial Park, Baoshan District, Shanghai, 2004 Patentee before: Shanghai Shenhe Thermo-magenetic Electronic Co., Ltd. |
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