CN106701085A - ITO (Indium Tin Oxide) reworking etching solution and preparation method of ITO reworking etching solution - Google Patents
ITO (Indium Tin Oxide) reworking etching solution and preparation method of ITO reworking etching solution Download PDFInfo
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- CN106701085A CN106701085A CN201611231750.5A CN201611231750A CN106701085A CN 106701085 A CN106701085 A CN 106701085A CN 201611231750 A CN201611231750 A CN 201611231750A CN 106701085 A CN106701085 A CN 106701085A
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- etching solution
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K13/00—Etching, surface-brightening or pickling compositions
- C09K13/04—Etching, surface-brightening or pickling compositions containing an inorganic acid
- C09K13/06—Etching, surface-brightening or pickling compositions containing an inorganic acid with organic material
Abstract
The invention relates to an ITO (Indium Tin Oxide) reworking etching solution and a preparation method of the ITO reworking etching solution. The etching solution is prepared from ferric trichloride, sulfuric acid, an additive, a surfactant and pure water, wherein the additive is thiourea and a derivative thereof or an imidazoline derivative; the surfactant is a sodium linear alkyl benzene sulfonate, ammonium salt or ethanolamine salt anionic surfactant. The preparation method of the ITO reworking etching solution comprises the following steps: dissolving the ferric trichloride into the high-purity water according to a ratio and adding a solution into a mixing kettle; then adding the sulfuric acid, the additive and the surfactant in sequence; after stirring and circulating, carrying out micro-filtration to obtain the formula product. The etching solution has stable component performances and a rapid etching speed, and can be used for rapidly removing an ITO film layer on the surface of a substrate in a production process; the added additive is used for effectively protecting a (metal) film layer in the production process of a lower layer from being corroded; the added surfactant can be used for effectively improving the wetting property of the etching solution and residues of ITO are reduced; the preparation method is simple and raw materials are cheap and easy to obtain; the industrial production cost can be more effectively reduced and the production efficiency is improved.
Description
Technical field
The present invention relates to a kind of wet etching composition for removing surface ito film layer in basal plate making process and its preparation side
Method.More particularly it relates to be used to prepare the indium tin oxide of LCD, FED, PDP, OLED/PLED display/screen etc.
(ITO) etching solution composition in the etching of doing over again of conducting film and preparation method thereof.
Background technology
Indium tin oxide (ITO) conducting film has translucency good, and resistivity is low, and high-temperature stability is good and prepares processing technology
Simple many advantages, such as, LCD, FED, PDP, OLED/PLED display/screen etc. is prepared so as to be widely used in, in production technology mistake
Cheng Zhong, indium tin oxide (ITO) layer is typically deposited in substrate surface by methods such as magnetron sputterings and formed, and works as indium tin oxide
(ITO) when layer does not reach technological requirement or defect occurs, it is necessary to remove ITO layer, ito thin film sputtering is re-started heavy
Product.
At present in PROCESS FOR TREATMENT, typically the etching of indium tin oxide (ITO) layer is gone using chemical method such as chloroazotic acid method all
Remove, or the method removal for passing through physical grinding, however, chloroazotic acid etching method etching process is acutely, its hydrochloric acid and nitric acid are volatile,
Environment and equipment are made a big impact, meanwhile, etching process is difficult to control, and corrosion is had to lower metal；Physical grinding method
Grinding metacoxal plate thickness is difficult to control, and sliver is easily caused during simultaneous grinding, causes bigger loss.
In existing patented technology, the method that patent CN201510937453.1 discloses removal substrate surface ITO, specially
To have the substrate of ITO to be placed in immersion in acid solution carries out pickling, and will be placed in alkali lye after pickling metacoxal plate removing surface acid solution
Row alkali cleaning, its acid solution composition by weight is 20%~25% hydrochloric acid, 30%~35% acetic acid and remaining water, its alkali lye group
Divide by weight 8%~10% alkali, 15%~20% nonionic surfactant and remaining water, above-mentioned processing method
In, handling process is relatively complicated, and efficiency is low, is unfavorable for treatment of largely doing over again, and lower floor's processing procedure (metal) film layer can be produced rotten
Erosion.
The content of the invention
Based on this, the invention reside in overcome the above process shortcoming with it is not enough, develop a kind of handling process it is simple, to environment and
Equipment is friendly, corrosion-free to lower floor's processing procedure (metal) film layer and substrate surface indium that substrate breaking is not resulted in processing procedure
The etching solution of doing over again of tin-oxide (ITO) layer.
The present invention second aims to overcome that existing ITO does over again and processes the deficiency of etching liquid preparing process, and design is a kind of
Simple ITO does over again etching liquid and preparation method thereof.
The technical solution adopted for the present invention to solve the technical problems is：
A kind of ITO does over again etching solution, and the etching solution is by ferric trichloride, sulfuric acid, additive, surfactant and pure water group
Into the additive is thiourea process or imidazolidine derivatives, and surfactant is cloudy sodium n-alkylbenzenesulfonate salt
Ionic surface active agent, ammonium salt anion surfactant or ethanolamine salt anion surfactant.
Preferably, the weight percent content of the etching solution each component is as follows：10~25% ferric trichloride, 5~
20% sulfuric acid, 0.01~1% additive, 0.01~0.1% surfactant, balance of pure water.
Preferably, the ferric trichloride, sulfuric acid raw material are respectively the ferric chloride (FeCl36H2O) of mass fraction 99.5% and 50% electricity
Sub- level sulfuric acid.
Preferably, the additive is any several combination in thiourea process and imidazolidine derivatives.
Preferably, the LABS ammonium salt anion surfactant is pelopon A, ammonium
One kind in salt and ethanolamine salt.
A kind of ITO does over again the preparation method of etching solution, and the preparation method comprises the following steps：
1) ferric trichloride is dissolved in high purity water in proportion, and is added in mixing kettle；
2) under conditions of being stirred continuously, electronic-grade sulfuric acid, and circulation stirring 30min are proportionally added into；
3) under conditions of being stirred continuously, additive, surfactant, and circulation stirring 6h are proportionally added into；
4) after mixing liquid is filtered by 0.1 μm of filter, obtain the ITO and do over again etching solution.
The present invention compared with prior art, the advantage is that：First, it is thiocarbamide through the additive of addition of the present invention
And its derivative or imidazolidine derivatives, it effectively plays a protective role to lower floor's processing procedure (metal) film layer, overcomes other
ITO does over again and produces the shortcoming of corrosion in etching solution processing procedure to lower metal；The surfactant of addition is linear alkylbenzene (LAB)
Sulfonate sodium, ammonium salt or ethanolamine salt anion surfactant, it effectively increases etching solution wellability, reduces etching
ITO residuals afterwards.Secondly, the etching solution of doing over again can regulate and control indium tin and aoxidize by adjusting the content proportioning of ferric trichloride and sulfuric acid
The etch-rate of thing (ITO), disclosure satisfy that the removal etching of indium tin oxide (ITO) layer of different thickness is required, range of application
Extensively.Finally, each component used by the etching solution compared with conventional aqua regia system etching solution, more stablize, and volatility is very by its component
It is smaller, this considerably increases the security of etching solution；Compared with prior art, its preparation process is simple, treatment of being done over again to substrate
Speed is fast, efficiency high, is adapted to extensive treatment of doing over again.Each component raw material is nontoxic simultaneously, environmentally friendly, pollution-free.
Brief description of the drawings
Fig. 1 is surface ITO residual condition top view of the embodiment 2 after etching process.
Fig. 2 is the top view of lower metal corrosion condition of the embodiment 2 after etching process.
Fig. 3 is the profile of lower metal corrosion condition of the embodiment 2 after etching process.
Fig. 4 is the vertical view of lower metal corrosion condition of the comparative example 3 after etching process.
Fig. 5 is the profile of lower metal corrosion condition of the comparative example 3 after etching process.
Fig. 6 is surface ITO residual condition top view of the comparative example 4 after etching process.
Specific embodiment
Below by specific embodiment, and with reference to accompanying drawing, technical scheme is described in further detail.
The present invention proposes that a kind of ITO does over again etching solution and preparation method thereof, and the etching formula of liquid is 10~25% trichlorine
Change iron, 5~20% sulfuric acid, 0.01~1% additive, 0.01~0.1% surfactant and surplus pure water.The etching
Liquid has many advantages, such as, implements to enter line justification to the etching solution component effect with reference to specific.
Implementation：The ITO is done over again the implementation of etching solution, and indium tin oxide (ITO) base plate glass is cut into
Fritter, under 40 DEG C of constant temperature, is etched with the etching solution for preparing, and etching is rushed base plate glass piece with high purity water after terminating
Wash and dried up with high pure nitrogen.
Etching fiducial time confirms：Before and after etching starts, determine ito glass surface using universal meter and fix point-to-point transmission
Resistance, glass surface still has resistance after etching, then increase etching period, until etching after determine resistance be shown as infinite
Greatly, then it is assumed that glass surface ito film has been etched to not
Continuous film layer is possible to determine when the sample has been completely etched, and now shortens etching period and is etched measure resistance again, currently
There is display resistance value to be shown as the adjacent secondary of infinity with measure resistance value after etching next time after secondary etching
When etching period interval was less than 2 seconds, on the basis of confirming that the measure resistance value is infinitely great etching period
Time.
Residual and corrosion condition observation：After the completion of etching, seen by SEM (SEM)
Examine ITO conducting film remaining residue situations and lower floor's processing procedure (metal) film layer corrosion condition.
Etch-rate determines：ITO etch-rates are determined by the ratio of thickness and said reference time.
Etching result:Etch residue situation evaluation of result standard is shown in Table 1, and lower metal is corroded after etching
Situation evaluation criterion be shown in Table 2, ITO do over again the composition of etching solution embodiment and comparative example, etch-rate,
Residual condition and corrosion condition are as shown in table 3 after etching.
Table 1 remains evaluation criterion
| Opinion rating | Residual evaluation criterion |
| A | Noresidue |
| B | Micro- residual |
| C | Moderate is remained |
| D | Serious residual |
| E | Remain completely |
The corrosion evaluation standard of table 2
| Evaluation criterion | Corrosion evaluation standard |
| Have | Corrosion |
| Nothing | It is corrosion-free |
Residual and lower floor's corrosion condition after the liquid etching composition of table 3, etch-rate and etching
Note：In table " " represent formula in do not add corresponding this kind of component." sodium salt " refers to dodecane in surfactant column
Base benzene sulfonic acid sodium salt salt anionic surfactant, " ammonium salt " refers to DBSA ammonium salt anion surfactant, " ethanol
Amine salt " refers to DBSA ethanolamine salt anion surfactant.
Embodiment 1：
ITO in the present embodiment does over again etching solution, and its component includes by weight percentage:25% ferric trichloride,
20% sulfuric acid, 0.4% additive diethyl thiourea, 0.01% surfactant sodium dodecyl base benzene sulfonic acid sodium salt and surplus
Pure water.
ITO in the present embodiment does over again the preparation method of etching solution, comprises the following steps：
1) ferric trichloride is dissolved in high purity water in proportion, and is added in mixing kettle；
2) under conditions of being stirred continuously, electronic-grade sulfuric acid, and circulation stirring 30min are proportionally added into；
3) under conditions of being stirred continuously, additive, surfactant, and circulation stirring 6h are proportionally added into；
4) after mixing liquid is filtered by 0.1 μm of filter, obtain the ITO and do over again etching solution.
Embodiment 2：
ITO in the present embodiment does over again etching solution, and its component includes by weight percentage:22% ferric trichloride,
18% sulfuric acid, 0.1% additive dimethyl sulfourea, 0.05% surfactant sodium dodecyl base benzene sulfonic acid ammonium salt and surplus
Pure water.
ITO in the present embodiment does over again the preparation method of etching solution, comprises the following steps：
1) ferric trichloride is dissolved in high purity water in proportion, and is added in mixing kettle；
2) under conditions of being stirred continuously, electronic-grade sulfuric acid, and circulation stirring 30min are proportionally added into；
3) under conditions of being stirred continuously, additive, surfactant, and circulation stirring 6h are proportionally added into；
4) after mixing liquid is filtered by 0.1 μm of filter, obtain the ITO and do over again etching solution.
Embodiment 3：
ITO in the present embodiment does over again etching solution, and its component includes by weight percentage:16% ferric trichloride,
12% sulfuric acid, 0.01% additive benzimidazole, 0.08% surfactant sodium dodecyl base benzene sulfonic acid ethanolamine salt and
Surplus pure water.
ITO in the present embodiment does over again the preparation method of etching solution, comprises the following steps：
1) ferric trichloride is dissolved in high purity water in proportion, and is added in mixing kettle；
2) under conditions of being stirred continuously, electronic-grade sulfuric acid, and circulation stirring 30min are proportionally added into；
3) under conditions of being stirred continuously, additive, surfactant, and circulation stirring 6h are proportionally added into；
4) after mixing liquid is filtered by 0.1 μm of filter, obtain the ITO and do over again etching solution.
Embodiment 4：
ITO in the present embodiment does over again etching solution, and its component includes by weight percentage:10% ferric trichloride, 5%
Sulfuric acid, 1.0% additive di-isopropyl thiourea, 0.1% surfactant sodium dodecyl base benzene sulfonic acid ammonium salt and surplus be pure
Water.
ITO in the present embodiment does over again the preparation method of etching solution, comprises the following steps：
1) ferric trichloride is dissolved in high purity water in proportion, and is added in mixing kettle；
2) under conditions of being stirred continuously, electronic-grade sulfuric acid, and circulation stirring 30min are proportionally added into；
3) under conditions of being stirred continuously, additive, surfactant, and circulation stirring 6h are proportionally added into；
4) after mixing liquid is filtered by 0.1 μm of filter, obtain the ITO and do over again etching solution.
Embodiment 5：
ITO in the present embodiment does over again etching solution, and its component includes by weight percentage:25% ferric trichloride, 5%
Sulfuric acid, 0.05% additive diphenyl-imidazole, 0.02% surfactant sodium dodecyl base benzene sulfonic acid ethanolamine salt and remaining
Amount pure water.
ITO in the present embodiment does over again the preparation method of etching solution, comprises the following steps：
1) ferric trichloride is dissolved in high purity water in proportion, and is added in mixing kettle；
2) under conditions of being stirred continuously, electronic-grade sulfuric acid, and circulation stirring 30min are proportionally added into；
3) under conditions of being stirred continuously, additive, surfactant, and circulation stirring 6h are proportionally added into；
4) after mixing liquid is filtered by 0.1 μm of filter, obtain the ITO and do over again etching solution.
Embodiment 6：
ITO in the present embodiment does over again etching solution, and its component includes by weight percentage:20% ferric trichloride,
10% sulfuric acid, 0.2% additive tolylthiourea, 0.04% surfactant sodium dodecyl base benzene sulfonic acid sodium salt and surplus
Pure water.
ITO in the present embodiment does over again the preparation method of etching solution, comprises the following steps：
1) ferric trichloride is dissolved in high purity water in proportion, and is added in mixing kettle；
2) under conditions of being stirred continuously, electronic-grade sulfuric acid, and circulation stirring 30min are proportionally added into；
3) under conditions of being stirred continuously, additive, surfactant, and circulation stirring 6h are proportionally added into；
4) after mixing liquid is filtered by 0.1 μm of filter, obtain the ITO and do over again etching solution.
Embodiment 7：
ITO in the present embodiment does over again etching solution, and its component includes by weight percentage:15% ferric trichloride,
13% sulfuric acid, 0.8% additive 1- phenyl -4-methylimidazole, 0.01% surfactant sodium dodecyl base ammonium benzene sulfonate
Salt and surplus pure water.
ITO in the present embodiment does over again the preparation method of etching solution, comprises the following steps：
1) ferric trichloride is dissolved in high purity water in proportion, and is added in mixing kettle；
2) under conditions of being stirred continuously, electronic-grade sulfuric acid, and circulation stirring 30min are proportionally added into；
3) under conditions of being stirred continuously, additive, surfactant, and circulation stirring 6h are proportionally added into；
4) after mixing liquid is filtered by 0.1 μm of filter, obtain the ITO and do over again etching solution.
Embodiment 8：
ITO in the present embodiment does over again etching solution, and its component includes by weight percentage:10% ferric trichloride,
18% sulfuric acid, 0.09% additive-treated oil acidic group imidazoles, 0.09% surfactant sodium dodecyl base benzene sulfonic acid sodium salt and remaining
Amount pure water.
ITO in the present embodiment does over again the preparation method of etching solution, comprises the following steps：
1) ferric trichloride is dissolved in high purity water in proportion, and is added in mixing kettle；
2) under conditions of being stirred continuously, electronic-grade sulfuric acid, and circulation stirring 30min are proportionally added into；
3) under conditions of being stirred continuously, additive, surfactant, and circulation stirring 6h are proportionally added into；
4) after mixing liquid is filtered by 0.1 μm of filter, obtain the ITO and do over again etching solution.
Embodiment 9：
ITO in the present embodiment does over again etching solution, and its component includes by weight percentage:10% ferric trichloride,
20% sulfuric acid, 0.6% additive allylthiourea, 0.06% surfactant sodium dodecyl base benzene sulfonic acid ethanolamine salt and
Surplus pure water.
ITO in the present embodiment does over again the preparation method of etching solution, comprises the following steps：
1) ferric trichloride is dissolved in high purity water in proportion, and is added in mixing kettle；
2) under conditions of being stirred continuously, electronic-grade sulfuric acid, and circulation stirring 30min are proportionally added into；
3) under conditions of being stirred continuously, additive, surfactant, and circulation stirring 6h are proportionally added into；
4) after mixing liquid is filtered by 0.1 μm of filter, obtain the ITO and do over again etching solution.
Comparative example 1：
ITO in this comparative example does over again etching solution, and its component includes by weight percentage:18% sulfuric acid, 0.1%
Additive dimethyl sulfourea, 0.05% surfactant sodium dodecyl base benzene sulfonic acid ammonium salt and surplus pure water.
ITO in this comparative example does over again the preparation method of etching solution, comprises the following steps：
1) ferric trichloride is dissolved in high purity water in proportion, and is added in mixing kettle；
2) under conditions of being stirred continuously, electronic-grade sulfuric acid, and circulation stirring 30min are proportionally added into；
3) under conditions of being stirred continuously, additive, surfactant, and circulation stirring 6h are proportionally added into；
4) after mixing liquid is filtered by 0.1 μm of filter, obtain the ITO and do over again etching solution.
Comparative example 2：
ITO in this comparative example does over again etching solution, and its component includes by weight percentage:22% ferric trichloride,
0.1% additive dimethyl sulfourea, 0.05% surfactant sodium dodecyl base benzene sulfonic acid ammonium salt and surplus pure water.
ITO in this comparative example does over again the preparation method of etching solution, comprises the following steps：
1) ferric trichloride is dissolved in high purity water in proportion, and is added in mixing kettle；
2) under conditions of being stirred continuously, electronic-grade sulfuric acid, and circulation stirring 30min are proportionally added into；
3) under conditions of being stirred continuously, additive, surfactant, and circulation stirring 6h are proportionally added into；
4) after mixing liquid is filtered by 0.1 μm of filter, obtain the ITO and do over again etching solution.
Comparative example 3：
ITO in this comparative example does over again etching solution, and its component includes by weight percentage:22% ferric trichloride,
18% sulfuric acid, 0.05% surfactant sodium dodecyl base benzene sulfonic acid ammonium salt and surplus pure water.ITO in this comparative example does over again
The preparation method of etching solution comprises the following steps：
1) ferric trichloride is dissolved in high purity water in proportion, and is added in mixing kettle；
2) under conditions of being stirred continuously, electronic-grade sulfuric acid, and circulation stirring 30min are proportionally added into；
3) under conditions of being stirred continuously, additive, surfactant, and circulation stirring 6h are proportionally added into；
4) after mixing liquid is filtered by 0.1 μm of filter, obtain the ITO and do over again etching solution.
Comparative example 4：
ITO in this comparative example does over again etching solution, and its component includes by weight percentage:22% ferric trichloride,
18% sulfuric acid, 0.1% additive dimethyl sulfourea and surplus pure water.
ITO in this comparative example does over again the preparation method of etching solution, comprises the following steps：
1) ferric trichloride is dissolved in high purity water in proportion, and is added in mixing kettle；
2) under conditions of being stirred continuously, electronic-grade sulfuric acid, and circulation stirring 30min are proportionally added into；
3) under conditions of being stirred continuously, additive, surfactant, and circulation stirring 6h are proportionally added into；
4) after mixing liquid is filtered by 0.1 μm of filter, obtain the ITO and do over again etching solution.
Embodiment described above is a kind of preferably scheme of the invention, not makees any formal to the present invention
Limitation, also has other variants and remodeling on the premise of without departing from the technical scheme described in claim.
Claims (6)
1. a kind of ITO does over again etching solution, it is characterised in that：The etching solution is by ferric trichloride, sulfuric acid, additive, surface-active
Agent and pure water are constituted, and the additive is thiourea process or imidazolidine derivatives, and surfactant is linear alkylbenzene (LAB)
Sulfonate sodium anion surfactant, ammonium salt anion surfactant or ethanolamine salt anion surfactant.
2. a kind of ITO according to right 1 does over again etching solution, it is characterised in that：The weight percent of the etching solution each component
It is as follows than content：10~25% ferric trichloride, 5~20% sulfuric acid, 0.01~1% additive, 0.01~0.1% table
Face activating agent, balance of pure water.
3. a kind of ITO according to right 1 does over again etching solution, it is characterised in that：The ferric trichloride, sulfuric acid raw material are respectively
The ferric chloride (FeCl36H2O) of mass fraction 99.5% and 50% electronic-grade sulfuric acid.
4. ITO according to claim 1 does over again etching solution, it is characterised in that：The additive is thiourea process
With any several combination in imidazolidine derivatives.
5. ITO according to claim 1 does over again etching solution, it is characterised in that：The LABS ammonium salt it is cloudy from
Sub- surfactant is the one kind in pelopon A, ammonium salt and ethanolamine salt.
6. the ITO described in a kind of claim 1-5 any one does over again the preparation method of etching solution, it is characterised in that：The system
Preparation Method comprises the following steps：
1) ferric trichloride is dissolved in high purity water in proportion, and is added in mixing kettle；
2) under conditions of being stirred continuously, electronic-grade sulfuric acid, and circulation stirring 30min are proportionally added into；
3) under conditions of being stirred continuously, additive, surfactant, and circulation stirring 6h are proportionally added into；
4) after mixing liquid is filtered by 0.1 μm of filter, obtain the ITO and do over again etching solution.
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| CN115505389A (en) * | 2022-08-22 | 2022-12-23 | 福建天甫电子材料有限公司 | ITO etching solution and use method thereof |
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| CN115011348A (en) * | 2022-06-30 | 2022-09-06 | 湖北兴福电子材料有限公司 | Aluminum nitride etching solution and application thereof |
| CN115011348B (en) * | 2022-06-30 | 2023-12-29 | 湖北兴福电子材料股份有限公司 | Aluminum nitride etching solution and application thereof |
| CN115261861A (en) * | 2022-08-15 | 2022-11-01 | 易安爱富(武汉)科技有限公司 | Thinning liquid and preparation method and application thereof |
| CN115261861B (en) * | 2022-08-15 | 2023-10-24 | 易安爱富(武汉)科技有限公司 | Thinning liquid and preparation method and application thereof |
| CN115505389A (en) * | 2022-08-22 | 2022-12-23 | 福建天甫电子材料有限公司 | ITO etching solution and use method thereof |
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