CN106929906A - The method for removing transparent conductive oxide - Google Patents
The method for removing transparent conductive oxide Download PDFInfo
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- CN106929906A CN106929906A CN201511022922.3A CN201511022922A CN106929906A CN 106929906 A CN106929906 A CN 106929906A CN 201511022922 A CN201511022922 A CN 201511022922A CN 106929906 A CN106929906 A CN 106929906A
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- coating
- base material
- aqueous solution
- oxide
- oxide skin
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F1/00—Electrolytic cleaning, degreasing, pickling or descaling
- C25F1/02—Pickling; Descaling
- C25F1/04—Pickling; Descaling in solution
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- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
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- Photovoltaic Devices (AREA)
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Abstract
The present invention relates to a kind of method for removing transparent conductive oxide.Method from base material removal including transparent conducting oxide layer of the invention includes electrolysis step, base material is immersed in the aqueous solution in the electrolysis step, and oxide skin(coating) is conductively connected with direct voltage source or DC current source in the way of the oxide skin(coating) is worked as negative electrode.
Description
Technical field
Subject of the present invention is a kind of method for removing transparent conductive oxide, wherein, make use of electrochemical process.
Background technology
The layer example being made up of transparent conductive oxide (TCO) as used in thin-layer solar cell, Display Technique or
Using in building glass, to produce the electrode of printing opacity.These oxides are metal oxide (for example zinc oxide or oxidations
Tin), its can doped with other elements or with other element compounds.Such as known aluminum zinc oxide (AZO), tin indium oxide
(ITO), fluorine oxide tin (FTO) and antimony tin (ATO) and stannate (for example cadmium stannate).These layers can for example by heat
Solution, chemical vapor deposition, electrochemically or by sputtering as the close, layer of large area or as structured
Layer be applied on base material.Here, concept " base material " includes to deposit thereon the arbitrary material of transparent conductive oxide
And/or sequence of layer.For by sputtering generation oxide, concept " base material " thus for example also including so-called sputtering piece, it is used
Make framework or the mask as the structure for depositing restriction that script treats coating base material.
If depositing oxide skin(coating) by entire surface, then these oxide skin(coating)s are by laser cutting or by machinery afterwards
Processing (such as scribing, scribing) carry out structuring, for example described in document WO2008/147696A1 as.So
And these methods are only limitedly suitable for removing the large area of the layer for depositing, because they are quite time-consuming and high cost
's.Additionally, also can result in causing damage the base material under this layer during the technique.Oxide based on zinc oxide
Layer can also be removed by being etched with hydrochloric acid (HCl).However, the oxide skin(coating) based on tin oxide is (particularly when they adulterate
During with other elements) it is in chemistry metastable and therefore, it is difficult to carry out wet chemical etching.In document EP0230104
It is referred to：Structuring is carried out to tin oxide with silicon tetrachloride by reactive ion etching (RIE).Document US4752501 is described
A kind of method, deposits the tin compound (carboxylic acid tin compound) of less stable first wherein, and water-soluble by alkalescence
Liquid carries out structuring, wherein, structured layer is then converted into tin oxide by sintering process.
For the removal of oxide skin(coating) deposited on sputtering piece, used so far such as sandblasting, with other materials (for example
Dry ice) injection, and using grinding or wet chemical method (as etching), for example in document US2011/0281026A1 and document
As DE98/50600A1 is described.But these methods are troublesome and sometimes expensive, or in wet-chemical erosion
Corrosivity and poisonous chemicals are used in lithography.Additionally, residual contaminants are likely to remain on base material, particularly when the base material
During with rough surface.
The content of the invention
Thus task is, there is provided a kind of alternative solution for removing this oxide skin(coating), the program overcomes prior art
Defect, and particularly also can be used in the oxide skin(coating) based on tin oxide.
According to the present invention, the task is resolved by method according to claim 1.Advantageous approach mode exists
Disclosure is obtained in dependent claims.
Include electrolysis step from the method for base material removal including transparent conducting oxide layer, base material is immersed in the electrolysis step
To in the aqueous solution, and oxygen supply compound layer loading DC voltage or the direct current in the way of making oxide skin(coating) be worked as negative electrode
Stream.By the electric current for introducing in aqueous, reduction reaction is triggered on negative electrode, nascent hydron has been generated in the reduction reaction.
The nascent hydron of this only of short duration stabilization (is abbreviated as Hnasc) possess than molecular hydrogen (H2) reducing power higher.On the one hand, nascent hydron
Exist with atom form after just being formed, on the other hand, forming H2Soon afterwards, it is in energy excited state.Therefore,
Even chemically oxide also reacts with nascent hydron, wherein, oxide is reduced to institute
The metal for containing or the ion containing the metal.The metal or the ion for being generated are dissolved in the aqueous solution, or with aqueous solution institute
The material for containing reacts, so as to oxide is removed from the base material.
The method according to the invention thus includes：At least oxide skin(coating) and direct voltage source or DC current source conduction
The step of connection；The step of anode is connected with direct voltage source or DC current source；Base material and anode at least in part
It is immersed in the step in the aqueous solution；To base material and anode loading DC voltage and DC current the step of, during this period base material and
Anode is in the aqueous solution.If the base material is constructed from a material that be electrically conducting, oxide skin(coating) preferably passes through base material and direct voltage source
It is conductively connected with DC current source.The base material and/or anode need not be totally immersed in the aqueous solution during electrolysis step.So
And, only the region from the immersion aqueous solution removes oxide skin(coating).Additionally, oxide skin(coating) only also is removed from the region of following immersion, only
It is wanted not insulated with water-soluble liquid phase by non-conductive layer in the region.The base material and the anode are preferably immersed in the aqueous solution simultaneously
In, but can also immerse successively.
The various aqueous solution by electrolytically generated nascent hydron are used as the aqueous solution.That is, can also use in principle pure
Water.Advantageously however, the aqueous solution contains other things of the electrical conductivity that improve the aqueous solution and/or the formation for accelerating nascent hydron
Matter.Here, the solution environmental (alkalescence is acid) for being dissolved in the type of the material of water and thus generating is selected in an advantageous manner
It is selected as so that one or more material and/or anode of base material and/or other objects contacted with solution formation are not etched
(for example corroding).
The aqueous solution is preferably alkaline solution, and it further preferably can include sodium acid carbonate (NaHCO using coming from3)、
NaOH (NaOH), saleratus (KHCO3) and potassium hydroxide (KOH) group material.Other materials can also be used,
As sodium carbonate (Na2CO3) or lithium hydroxide (LiOH).The concentration of contained salt covers a wide scope (from 1g/L solution
To 100g/L solution).It is particularly preferred that mentioned salt concentration in the solution is between 5g/L solution and 80g/L solution.
The aqueous solution preferably has the concentration between 0.5% and 8%.
Electrolysis step is implemented preferably under room temperature (that is, at about 20 DEG C), but can also be (straight in the temperature for somewhat improving
To about 80 DEG C) under implement.The DC voltage or introduced DC current for being applied are advantageously located at following ranges, i.e. at this
Size adjusting in scope according to base material goes out in 0.15A/dm2And 25A/dm2Between current density.
The time (i.e. the time of applied voltage or electric current) of the step of for being electrolysed depends on oxide skin(coating) to be removed
Thickness and the current density for being reached.Preferably, electrolysis step is implemented only through the short time but with current density high.Electricity
The time for solving step is in the scope between 30 seconds and 15 minutes.
Advantageously, (that is, from after base material removal transparent conductive oxide) carries out neutralization step after electrolysis step
Suddenly, base material is inserted into neutralization solution in this step, the neutralization solution to the aqueous solution suitable for neutralizing.In other words：If
The aqueous solution is alkaline solution, then it is acid solution (acetic acid, citric acid or the hydrochloric acid that for example dilute) to neutralize solution, and when using sour
Property solution as the aqueous solution when, neutralize solution be alkaline solution.During solution is neutralized for being carried out to the aqueous solution residual on base material
With so as to prevent aqueous composition that further chemical reaction occurs.
It is preferred that carrying out cleaning step with cleaning agent after electrolysis step.It is particularly preferred that in the laggard of neutralization procedure
Row cleaning step, and cleaning step is used to remove the residual of the aqueous solution (and neutralizing solution when necessary), and removal through also
But the former transparent conductive oxide residue also sticked on base material.All suitable media can be used as cleaning
The aqueous solution or combination of agent, particularly preferred deionized water, and isopropanol or acetone or these materials.Secondarily,
Soft mechanism can also be carried out by sponge or hairbrush or by ultrasound, in order to also removal adhesion when necessary
Oxide particle on base material.Finally, the base material is preferably through drying.
As the anode of electrolysis step, the material from the group including platinum, carbon, iron, nickel, titanium and stainless steel is preferably used.
Advantageously, anode material is during electrolysis inert relative to the aqueous solution for being used, that is, it will not both enter solution simultaneously
Decompose, will not be reacted with the material from the aqueous solution again, or reacted with the oxygen formed on anode.Cause
And, electric current that is uniform, hardly being changed with the time can be produced in aqueous, because, on anode not
The layer of electric insulation can be formed.It is particularly preferred that anode is made up of iron or stainless steel because, they relative to
Other anode materials only have the overvoltage of very little in oxygen generating process.
The method according to the invention provides following possibilities, i.e. will be by transparent conductive oxide group with wet chemical method
Into layer removal, wherein can also for conventional wet chemical etching relative inertness oxide and be applied to coarse base material table
The oxide in face is removed fully and in depth.Particularly also oxide can be removed from the hole of thick substrate surface, from
And can realize going deep into base material the cleaning of hole.It is of course also possible to clean smooth base material table with the method according to the invention
Face.In addition can avoid using corrosive and poisonous chemicals and avoid damage to be located under oxide to be removed
Substrate surface.Relative to the method for the removal oxide skin(coating) of machinery, the method according to the invention is quick, accurate and cheap, and this is
Because oxide can also be removed from big surface.Thus other advantage is drawn, i.e. by the method according to the invention,
The metal component of removed oxide exists in the form of ion or salt in aqueous, and they can be then by water
The further treatment of solution and reclaim.Therefore can particularly reuse costliness and/or rare material (as tin Sn, indium
In)。
The method according to the invention can be used for removing the layer being made up of transparent conductive oxide by entire surface, or for only
Partly remove such layer.Here, part removal is preferably directed to be gone completely in a thickness direction from the transverse area for limiting
Except oxide skin(coating), and the transverse area covered by suitable covering layer or coating during the method is implemented at other is not
Removal oxide skin(coating).The process is in being comparable to make the technique of layer structure oxide in a lateral direction.In principle certainly also
Oxide skin(coating) can be partly removed in a thickness direction, and this and not exclusively removes oxygen equivalent to the thickness for reducing oxide skin(coating)
Compound layer.
Brief description of the drawings
Fig. 1 show in cross section a kind of system, within the system in order to remove the oxide skin(coating) 2 being deposited on base material 1
And base material 1 is immersed in the aqueous solution 3, and the base material plays negative electrode in DC circuit.
Fig. 2 shown as the sputtering piece 11 of base material, wherein, oxide skin(coating) 2 should be removed by entire surface.
Fig. 3 A show a kind of solar cell semi-finished product with stereogram, the oxide in the solar cell semi-finished product
Layer 2 should the structuring by electrochemical process.
Fig. 3 B show the cross section of solar cell semi-finished product along line A-A, through Fig. 3 A (in removal oxide
Before layer 2).
Fig. 3 C show the cross section for coming from Fig. 3 B (after oxide skin(coating) 2 is removed).
Specific embodiment
Fig. 1 shows a kind of system, and the base material 1 wherein with the including transparent conducting oxide layer 2 on base material is immersed
Enter in the aqueous solution 3.Oxide skin(coating) 2 is located at the surface of base material 1, and is covered at least in part.The aqueous solution 3 is located at container
In 4, the container has following sizes, and the size corresponds to the size of base material 1 and for necessary to implementation electrochemical process
Spacing and volume.Base material 1 is fastened on support 51, so that it is until height hsBe immersed in the aqueous solution 3.Height hsBelow
In also referred to as " immersion depth of base material ".Base material can be immersed in the aqueous solution by support 51, and by base material from solution
In take out again.Further, it is also possible to pass through the adjustment height of support 51 hs, and be changed when necessary during the method.
Oxide skin(coating) 2 and/or base material 1 are by electric lead 61 and direct voltage source or the electrodes conduct of DC current source 7
Connection.Another electrode of direct voltage source or DC current source 7 is conductively connected by electric conductor 62 with anode 8, and the anode relies on
Support 52 is immersed in the aqueous solution.
The electric connection of conductor 61 or 62 can also be integrated into support 51 or 52.
DC voltage and DC current are applied by the oxide skin(coating) 2 worked to anode 8 and as negative electrode, in the aqueous solution
Nascent hydron is generated in negative electrode in 3, it reacts with oxide skin(coating) 2 and dissolves it.Therefore in the NaOH using 0.1%
In the case of the aqueous solution, following reactional equation is obtained in negative electrode for the tin oxide as oxide skin(coating)：
2H2O+2e-→2Hnasc+2OH- (1)
SnO2+4Hnasc→Sn+2H2O (2),
Wherein, NaOH is used to provide alkaline medium, so as not to can corrode base material 1 and/or anode 8 and/or support 51,
52 and/or the material of electric conductor 61,62, and improve the electrical conductivity of solution.
It is not electrochemical with the connecting portion and support 51 itself of support 51 for electric connection or electric conductor 61 and base material 1
Learn the situation that technique or the aqueous solution 3 corrode, height hsCan also be the whole height of base material 1, so that the base material 1 or at least
Whole oxide skin(coating) 2 is immersed in the aqueous solution 3.If this is infeasible, and oxide skin(coating) 2 should also be as not having from base material 1
There is the region for being immersed in the aqueous solution 3 to be removed, then, the method is repeated quickly and easily as many times as required in the case where substrate location is changed, until
All regions that should remove oxide skin(coating) of base material are immersed in the aqueous solution 3 and undergo electrochemical treatments.
In order to test, the sputtering piece 11 (size is 6mm × 6mm, thickness 1mm) to being made of stainless steel is implemented according to this hair
Bright method.Fig. 2 shows the embodiment that in the method in accordance with the invention processes of such sputtering piece as base material 1, and this splashes
Penetrate piece and carry the oxide skin(coating) 2 (its thickness for carrying about 400 to 500nm) being deposited on by entire surface above it.In situation about showing
Under, oxide skin(coating) extends on the gamut of sputtering piece 11 on the surface of sputtering piece 11.However, the surface of sputtering piece 11
Can there was only certain area, or the other surface (for example sputtering the edge surface of piece 11) of sputtering piece 11 can also be oxidized
Nitride layer 2 is covered.In order to remove oxide skin(coating) 2, sputtering piece is immersed in 2% by the fixture as support 51 at room temperature
In sodium hydroxide solution 3, and with the voltage-drop loading 30s of about 10V, wherein, vehicle battery charger is used as direct voltage source
7.Measured electric current is 1.5A.Equally, stainless steel substrates (size：10cm × 10cm) it is used as anode 8, it is by being used as support 52
The second fixture be immersed in the aqueous solution.Electric conductor 61 and 62 is directly connected to conductive fixture.In the immersion region of sputtering piece 11,
Oxide skin(coating) 2 is completely removed under conditions of mentioned, wherein, base material itself does not weather.The surface of piece 11 is sputtered herein
(oxide skin(coating) 2 is initially applied to above it) be it is smooth or coarse be inessential.Even if rough surface can also
Fully erased oxide skin(coating) 2.
In the last of the method according to the invention, sputtering piece 11 washs 5s in 0.1% hydrochloric acid, is used to neutralize alkalescence molten
Liquid.Then, the cleaning step of each 5-10s is carried out with deionized water and with isopropanol, and is dried at room temperature for.
The other use example of the method according to the invention is shown in figure 3 a.Here, such as solar cell half
Finished product includes the glass baseplate 12 that is made up of float glass, and in order to experiment purpose have 10cm × 10cm size and
The thickness of 3.2mm.The oxide skin(coating) 2 in the whole face of cloth is applied with above-mentioned identical thickness range on the glass baseplate 12, it is being limited
The coated cap rock 9 in region covered.The coating 9 is designed as to be corroded by the component of the aqueous solution and nascent hydron, and because
The region of the oxide skin(coating) 2 that this protection is covered by it is not removed.The coating 9 is, for example, in semiconductor-and micro-system
Anti-corrosion body (Resist) common in technology, its thickness for carrying 100nm to 200nm.Therefore oxide skin(coating) 2 is only partially, also
Removed from glass baseplate 12 being uncovered the transverse area that layer 9 covered.Thus following possibilities are obtained, i.e. right
The structure that Ying Yu is constructed in coating 9 makes the structuring of oxide skin(coating) 2, and the base material without being pointed under it is impacted.
For the method condition of the structuring on glass baseplate 12 of oxide skin(coating) 2 substantially with the method condition phase for sputtering piece 11
Unanimously, just as reference to Figure 2.
It is unrestricted on the structure principle that can be generated in oxide skin(coating) 2.However, based on the bad of glass baseplate 12
Electrical conductivity should be noted that the region to be removed of oxide skin(coating) 2 is adjacent to oxide skin(coating) 2 and direct current at each method time point
The region that potential source or DC current source 7 are conductively connected.It is conductive material if located in the base material under oxide skin(coating) 2, then should
Limitation also disappears.
In figure 3b, show along in Fig. 3 A it is line A-A, through glass baseplate 12, oxide skin(coating) 2 and coating 9
Cross section (before oxide skin(coating) 2 is removed).The structure constructed in coating 9 has the width b of about 50nmd.And
Cross section same, after the transverse area removal oxide skin(coating) 2 covered from uncovered layer 9 is shown in fig. 3 c.
The spare area isotropically corroded in oxide skin(coating) 2 that the structure generated in oxide skin(coating) 2 passes through nascent hydron is somewhat
It is broader, and the width b with about 60nm0。
Description of reference numerals
1 base material
11 sputtering pieces
12 glass baseplates
2 oxide skin(coating)s
3 aqueous solution
4 containers
51st, 52 support
61st, 62 electric conductor
7 direct voltage sources or DC current source
8 anodes
9 coatings
hsThe immersion depth of base material
bdThe width of the structure in coating
boThe width of the structure in oxide skin(coating)
Claims (6)
1. it is a kind of from base material remove including transparent conducting oxide layer method, it is characterised in that methods described include electrolysis step,
Base material is immersed in the aqueous solution in the electrolysis step, and oxide skin(coating) and direct voltage source or DC current source so that
The oxide skin(coating) is obtained to be conductively connected as the mode that negative electrode works.
2. method according to claim 1, it is characterised in that the aqueous solution is alkaline solution.
3. method according to claim 2, it is characterised in that the aqueous solution contains from including sodium acid carbonate, hydrogen-oxygen
Change sodium, saleratus, the material of the group of potassium hydroxide.
4. the method according to any one of preceding claims, it is characterised in that neutralized after electrolysis step
Base material, is inserted neutralization solution, during the neutralization solution is suitable for carrying out the aqueous solution by step in the neutralization procedure
With.
5. the method according to any one of preceding claims, it is characterised in that cleaning agent is used after electrolysis step
Carry out cleaning step.
6. the method according to any one of preceding claims, it is characterised in that as the anode of electrolysis step, use
Material from the group including platinum, carbon, iron, nickel, titanium and stainless steel.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511022922.3A CN106929906A (en) | 2015-12-30 | 2015-12-30 | The method for removing transparent conductive oxide |
| PCT/CN2016/112112 WO2017114357A1 (en) | 2015-12-30 | 2016-12-26 | Method for removing transparent conductive oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511022922.3A CN106929906A (en) | 2015-12-30 | 2015-12-30 | The method for removing transparent conductive oxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106929906A true CN106929906A (en) | 2017-07-07 |
Family
ID=59224607
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201511022922.3A Pending CN106929906A (en) | 2015-12-30 | 2015-12-30 | The method for removing transparent conductive oxide |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN106929906A (en) |
| WO (1) | WO2017114357A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110319724A (en) * | 2019-07-03 | 2019-10-11 | 江西华度电子新材料有限公司 | A method of restoring liquid-sucking core capillary performance |
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|---|---|---|---|---|
| JPS52103333A (en) * | 1976-02-27 | 1977-08-30 | Kawasaki Steel Co | Method of fabricating tin plated steel plate |
| JPS62290900A (en) * | 1986-06-11 | 1987-12-17 | Oki Electric Ind Co Ltd | Method and apparatus for etching of transparent conductive film |
| CN1652912A (en) * | 2002-05-16 | 2005-08-10 | 松下电器产业株式会社 | Method and apparatus for releasing metal-resin joint |
| JP2008305910A (en) * | 2007-06-06 | 2008-12-18 | Hitachi Zosen Corp | Method and device for removing conductive metal-oxide thin film |
| CN102834552A (en) * | 2010-03-26 | 2012-12-19 | 法国原子能及替代能源委员会 | Method for etching conductive metal oxide layer using microelectrode |
| CN103422153A (en) * | 2013-08-22 | 2013-12-04 | 大连七色光太阳能科技开发有限公司 | Method for etching FTO (fluorine-doped tin oxide) conductive thin film |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5692080B2 (en) * | 2010-04-06 | 2015-04-01 | 新日鐵住金株式会社 | Manufacturing method of steel plate for container material with less environmental impact |
| CN102691093A (en) * | 2012-06-20 | 2012-09-26 | 哈尔滨工业大学 | Method for rapidly corroding and patterning indium tin oxide surface by using electrochemical technology |
| CN104419957A (en) * | 2013-09-04 | 2015-03-18 | 天津市大港镀锌厂 | Nickel electroplating assembly line pretreatment device |
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2015
- 2015-12-30 CN CN201511022922.3A patent/CN106929906A/en active Pending
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS52103333A (en) * | 1976-02-27 | 1977-08-30 | Kawasaki Steel Co | Method of fabricating tin plated steel plate |
| JPS62290900A (en) * | 1986-06-11 | 1987-12-17 | Oki Electric Ind Co Ltd | Method and apparatus for etching of transparent conductive film |
| CN1652912A (en) * | 2002-05-16 | 2005-08-10 | 松下电器产业株式会社 | Method and apparatus for releasing metal-resin joint |
| JP2008305910A (en) * | 2007-06-06 | 2008-12-18 | Hitachi Zosen Corp | Method and device for removing conductive metal-oxide thin film |
| CN102834552A (en) * | 2010-03-26 | 2012-12-19 | 法国原子能及替代能源委员会 | Method for etching conductive metal oxide layer using microelectrode |
| CN103422153A (en) * | 2013-08-22 | 2013-12-04 | 大连七色光太阳能科技开发有限公司 | Method for etching FTO (fluorine-doped tin oxide) conductive thin film |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110319724A (en) * | 2019-07-03 | 2019-10-11 | 江西华度电子新材料有限公司 | A method of restoring liquid-sucking core capillary performance |
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| WO2017114357A1 (en) | 2017-07-06 |
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Application publication date: 20170707 |