CN103046108B - Application of the electrolysis process in ito film is cleaned - Google Patents
Application of the electrolysis process in ito film is cleaned Download PDFInfo
- Publication number
- CN103046108B CN103046108B CN201210567366.8A CN201210567366A CN103046108B CN 103046108 B CN103046108 B CN 103046108B CN 201210567366 A CN201210567366 A CN 201210567366A CN 103046108 B CN103046108 B CN 103046108B
- Authority
- CN
- China
- Prior art keywords
- component
- sulfuric acid
- ito film
- acid electrolyte
- electrolysis
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Physical Vapour Deposition (AREA)
- Electrolytic Production Of Metals (AREA)
Abstract
The present invention relates to application of the electrolysis process in ito film is cleaned, component is placed in sulfuric acid electrolyte, is cleaned ito film by electrolysis, wherein, the component is covered with the component of the aluminum alloy material of ito film for surface.In ito film course of dissolution, aluminium alloy forms dense oxidation film in sulfuric acid electrolyte as anode and component mother metal is protected, and improves the life-span that component is recycled, and noble metal component can be reclaimed, it is to avoid the loss in traditional chemical removal process.
Description
Technical field
The present invention relates to ito film, application of more particularly to a kind of electrolysis process in ito film is cleaned.
Background technology
Tin indium oxide (ITO, or tin-doped indium oxide) is a kind of indium（III）Oxide (In2O3) and tin（IV races）Oxidation
Thing (SnO2) mixture, usual mass ratio be 90% In2O3, 10% SnO2.Generally deposited by electron beam evaporation, physical vapour deposition (PVD),
Or the method for some sputter-deposition technologies deposits to surface and obtains indium oxide tin film.
For cleaning for ito film, generally using Chemical cleaning.Conventional Chemical cleaning is usually by component at present（Or claim
For accessory）Clean in being immersed directly in acid solution, in cleaning process, acid solution there are considerable amount of corrosion losses in itself to component mother metal, clearly
Wash and reach certain amount, cost recovery is carried out to liquid medicine of a relatively high.Another mode is gone using high-pressure water knife mode
Film, can cause substantial amounts of recyclable ITO to be lost in.
Therefore, this area needs a kind of new ito film method of cleaning of exploitation, it is to avoid to the corrosion of component and noble metal into
The loss for dividing.
The content of the invention
It is an object of the invention to provide a kind of new ito film method of cleaning, electrochemical process is attached to conventional
In ito film chemistry wash clean process, with cost-effective and improve the component life-span.
The ito film method of cleaning that the present invention is provided, including component is placed in sulfuric acid electrolyte, by being electrolysed ito film
Clean, wherein, the component is covered with the component of the aluminum alloy material of ito film for surface.
According to the present invention, the sulfuric acid electrolyte be aqueous sulfuric acid, concentration range 120g/L～250g/L, temperature range
15～35 DEG C.
According to the present invention, with inert electrode as negative electrode, with component as anode, negative electrode with the area ratio of anode is for the electrolysis
1:1～1:2, voltage is 5～17V.
Electrolysis actual current is determined by the effective area of part.
According to the present invention, the inert electrode is graphite, lead or titanium.
In the present invention, so-called inert electrode is referred to for there is no the material for dissolving as negative electrode under electrolytic condition.
According to the present invention, methods described also includes the step of post-processing to the component after electrolysis, the post processing bag
Include：Sandblasting is molten to penetrate.
The component that electrolytic cleaned is completed, post processing mode are same as Chemical cleaning flow process substantially, and neutralization removes the floating ash in surface, root
According to roughness demand, normally do sandblasting and molten penetrate process.
According to the present invention, methods described also includes the step of post-processing to the sulfuric acid electrolyte after electrolysis, it is described after
Process includes reclaiming the In elements in sulfuric acid electrolyte.
In ito film wash clean process, ITO vitriolizations, wherein can also it is miscellaneous enter aluminium ion, copper ion etc., using graphite sun
Pole, titanium plate are done catholyte and reclaim metal In.
It is according to the present invention, when in the sulfuric acid electrolyte, In constituent contents are more than 20g/L, first to the In in sulfuric acid electrolyte
Element is reclaimed.
The method of the present invention, in ito film course of dissolution, aluminium alloy forms dense oxide in sulfuric acid electrolyte as anode
Film is protected to component mother metal, improves the life-span that component is recycled.The present invention can also be reclaimed to noble metal component, kept away
Exempt from the loss in traditional chemical removal process.
It should be understood that within the scope of the present invention, above-mentioned each technical characteristic of the present invention and have in below (eg embodiment)
Can be combined with each other between each technical characteristic of body description, so as to constitute new or preferred technical scheme.As space is limited, exist
This no longer tires out one by one states.
Specific embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limit the scope of the present invention.
Term
Tin indium oxide ITO
Tin indium oxide (ITO, or tin-doped indium oxide) is a kind of indium（III）Oxide (In2O3) and tin（IV races）Oxidation
Thing (SnO2) mixture, usual mass ratio be 90% In2O3, 10% SnO2.It is clear, colorless in film-form.In bulk
During state, it is in yellow grey partially.The main characteristic of tin indium oxide is that its electricity is conducted and optically transparent combination.
Indium tin oxide films are most often deposited by electron beam evaporation, physical vapour deposition (PVD) or some sputter-deposition technologies
Method deposits to surface, using it is most be reactive magnetron sputtering method.Wherein, ITO conducting films are the methods using magnetron sputtering
The height that transparent indium tin oxide (ITO) conductive film coating Jing the high temperature anneals are obtained is sputtered on transparent organic film material
Technical products.
Embodiment 1
The present embodiment is with TFT（Thin film transistor (TFT) production equipment）The color film ITO Sputter of the 6th generation（CF
Carrier coloured silk membrane production equipment substrate carriers）Electrolytic cleaned is carried out as a example by component
Component surface Direct precipitation ito film Jing after sandblasting increases bulk processing during use, its upper and lower plates is aluminum；In operation with
The aqueous sulfuric acid of 150g/L does electrolyte, the titanium plate that 600 square decimeters of the gross area（A kind of inert electrode used by the present invention）
For negative electrode, the upper lower aluminum sheet of 4 pieces of Carrier is loaded every time（Totally 8 pieces, about 600 square decimeters of the gross area）As anode；Operation temperature
At 17 ± 2 DEG C, voltage is in 7V or so for degree control；Electrolysis every time takes about 3 hours；Normally entered with nitre fluoric acid after the completion of electrolytic cleaned
Row neutralization, and wash, sandblasting etc. completes cleaning.
Cleaning performance：Component surface ito film matter cleaning after electrolytic cleaned is complete, the overall slight loss of parts surface, is in
Uniform loss shape；To analyze with groove test piece and the measurement of actual component, the loss of electrolytic cleaned is at 10～15 microns（μm）.
Embodiment 2
Using the method cleaning ito film of embodiment 1, when in electrolyte, In contents are 22g/L, reclaimed
With 20dm2Titanium plate be negative electrode, 20dm2Graphite cake is anode, and room temperature condition voltage stabilizing 3V is electrolysed, actual current
About 16A, is electrolysed about 20 hours, and cathode surface deposits thick indium, and indium metal is obtained after refinement.
Embodiment 3-6
The method of embodiment 3-6 is substantially the same manner as Example 1, and difference is：
Embodiment 3：Electrolyte is done using the aqueous sulfuric acid of 225g/L, the component surface ito film matter after electrolytic cleaned is clear
Wash complete, the overall slight loss of parts surface, in uniform loss shape；To analyze with groove test piece and the measurement of actual component, electrolysis
The loss of cleaning is at 10～15 microns（μm）.
Embodiment 4：Electrolysis processing temperature is 25 ± 2 DEG C, and voltage is 15V, and the component surface ito film matter after electrolytic cleaned is clear
Wash complete, the overall slight loss of parts surface, in uniform loss shape；To analyze with groove test piece and the measurement of actual component, electrolysis
The loss of cleaning is at 15～25 microns（μm）.
Embodiment 5：The upper lower aluminum sheet of 2 pieces of Carrier is loaded every time（Totally 4 pieces, about 300 square decimeters of the gross area）, electrolysis
Component surface ito film matter cleaning after cleaning is complete, the overall slight loss of parts surface, in uniform loss shape；With with groove test piece
And the measurement analysis of actual component, the loss of electrolytic cleaned is at 8～12 microns（μm）.
Embodiment 6：Using graphite as negative electrode, the component surface ito film matter cleaning after electrolytic cleaned is complete, and parts surface is whole
Body is slightly lost, in uniform loss shape；To analyze with groove test piece and the measurement of actual component, the loss of electrolytic cleaned is 10～15
Micron（μm）.
Cleaning performance：Component surface ito film matter cleaning after electrolytic cleaned is complete, the overall slight loss of parts surface, is in
Uniform loss shape；To analyze with groove test piece and the measurement of actual component, the loss of electrolytic cleaned, in 10～15um or lower, is 8
～12 microns（μm）.
Comparative example：
Comparative example adopts traditional acid cleaning process, with the component in embodiment 1 as process object, uses 40%（Volume ratio）'s
Aqueous solution of nitric acid soaks.After immersion about 1 hour, surface ito film matter cleaning is complete, and corrosion uneven phenomenon, striping mistake occurs in aluminium sheet
The loss of journey aluminum mother plate is at 50～60 microns（μm）.
, compared with conventional method, in ito film course of dissolution, aluminium alloy is as anode in sulfuric acid electrolyte for the method for the present invention
Middle formation dense oxidation film is protected to component mother metal, is improved the life-span that component is recycled, and is saved process time.This
It is bright noble metal component to be reclaimed, it is to avoid the loss in traditional chemical removal process.
The all documents referred in the present invention are all incorporated as reference in this application, independent just as each document
It is incorporated as with reference to such.In addition, it is to be understood that after the above-mentioned instruction content for having read the present invention, those skilled in the art can
To make various changes or modifications to the present invention, these equivalent form of values equally fall within the model limited by the application appended claims
Enclose.
Claims (5)
1. a kind of ito film method of cleaning, it is characterised in that methods described includes component is placed in sulfuric acid electrolyte, by electricity
Ito film is cleaned by solution, wherein, the component is covered with the component of the aluminum alloy material of ito film for surface；The sulfuric acid electrolyte is
Aqueous sulfuric acid, concentration range 120g/L～250g/L, electrolysis range of working temperature are 15～35 DEG C；The electrolysis is with inertia electricity
Extremely negative electrode, with component as anode, negative electrode is 1 with the area ratio of anode:1～1:2, voltage is 5～17V；The inert electrode
For graphite, lead or titanium.
2. the method for claim 1, it is characterised in that methods described also includes post-processing the component after electrolysis
The step of, the post processing includes：Sandblasting is molten to penetrate.
3. the method for claim 1, it is characterised in that methods described also includes carrying out the sulfuric acid electrolyte after electrolysis
The step of post processing, the post processing, include reclaiming the In elements in sulfuric acid electrolyte.
4. method as claimed in claim 3, it is characterised in that using graphite as anode, titanium plate is reclaimed as catholyte
In in sulfuric acid electrolyte.
5. the method as described in claim 3 or 4, it is characterised in that when In constituent contents are more than in the sulfuric acid electrolyte
20g/L, reclaims to the In elements in sulfuric acid electrolyte.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210567366.8A CN103046108B (en) | 2012-12-24 | 2012-12-24 | Application of the electrolysis process in ito film is cleaned |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210567366.8A CN103046108B (en) | 2012-12-24 | 2012-12-24 | Application of the electrolysis process in ito film is cleaned |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103046108A CN103046108A (en) | 2013-04-17 |
| CN103046108B true CN103046108B (en) | 2017-03-29 |
Family
ID=48058963
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210567366.8A Active CN103046108B (en) | 2012-12-24 | 2012-12-24 | Application of the electrolysis process in ito film is cleaned |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103046108B (en) |
Citations (6)
| 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 |
| 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 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007056367A (en) * | 2005-07-29 | 2007-03-08 | Mitsubishi Materials Corp | Method for recovering indium from blast particle |
-
2012
- 2012-12-24 CN CN201210567366.8A patent/CN103046108B/en active Active
Patent Citations (6)
| 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 |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103046108A (en) | 2013-04-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Fashu et al. | Influence of electrodeposition conditions on the microstructure and corrosion resistance of Zn–Ni alloy coatings from a deep eutectic solvent | |
| CN101528989B (en) | Method for collection of valuable metal from ITO scrap | |
| CN101528988B (en) | Method for collection of valuable metal from ITO scrap | |
| CN101528986B (en) | Method for collection of valuable metal from ITO scrap | |
| CN101528984B (en) | Method for collection of valuable metal from ITO scrap | |
| CN101528983A (en) | Method for collection of valuable metal from ITO scrap | |
| Leong et al. | Electrochemistry of tin in the 1-ethyl-3-methylimidazolium dicyanamide room temperature ionic liquid | |
| CA2859936C (en) | Anode for oxygen generation and manufacturing method for the same | |
| US10774433B2 (en) | Electrochemical recycling of lead-based materials | |
| BR112016011396B1 (en) | DEVICES AND METHOD FOR RECYCLING WITHOUT FUSER OF LEAD ACID BATTERIES. | |
| US3926751A (en) | Method of electrowinning metals | |
| CN100595578C (en) | Method for preparing platinum nano-perforated electrode by evaporation deposition | |
| CN103334132A (en) | Method for preparing aluminum-magnesium alloy membrane through electro-deposition at room temperature | |
| CN106835193B (en) | A kind of Pb bases/3D-PbO2/MeOx composite anodes and preparation method thereof | |
| CN103046108B (en) | Application of the electrolysis process in ito film is cleaned | |
| He et al. | Physicochemical characterization of PbO2 coatings electrosynthesized from a methanesulfonate electrolytic solution | |
| CA2859941A1 (en) | Anode for oxygen generation and manufacturing method for the same | |
| Abood et al. | Morphology of electrodeposited aluminium metal from aluminium chloride-urea room temperature ionic liquid (RTIL) at variable parameters | |
| JP6100525B2 (en) | Method for recovering metal or alloy from scrap of high purity metal or alloy | |
| Liu et al. | Preparation and electrochemical performance of the stainless steel/α-PbO2-ZrO2/β-PbO2-ZrO2-CNT composite anode | |
| CN113913868B (en) | Ionic liquid electrolyte, 6N ultrapure aluminum obtained by ionic liquid electrolyte and preparation method of ionic liquid electrolyte | |
| CN101122028A (en) | Method for preparing metal oxide anode used for protecting reinforced concrete cathode | |
| Haarberg et al. | Electrodeposition of Lead from Chloride Melts | |
| JP2019044221A (en) | Operation method of copper electrorefining | |
| Cao et al. | A Study of Molybdenum Coatings Underpotential Preparation in an Ionic Liquid System |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
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. |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20200611 Address after: 244000 Jinqiao Economic Development Zone, Tongling, Anhui, Tongling Patentee after: Anhui fullerde Technology Development Co., Ltd Address before: 244000 Jinqiao Economic Development Zone, Tongling, Anhui Patentee before: ANHUI FULEDE TECHNOLOGY DEVELOPMENT Co.,Ltd. |