CN106479505B - A kind of fine etching solution and preparation method thereof for ITO conductive films - Google Patents
A kind of fine etching solution and preparation method thereof for ITO conductive films Download PDFInfo
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- CN106479505B CN106479505B CN201610860973.1A CN201610860973A CN106479505B CN 106479505 B CN106479505 B CN 106479505B CN 201610860973 A CN201610860973 A CN 201610860973A CN 106479505 B CN106479505 B CN 106479505B
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- C09K13/06—Etching, surface-brightening or pickling compositions containing an inorganic acid with organic material
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Abstract
A kind of fine etching solution and preparation method thereof for ITO conductive films, weight percent composition are as follows：Nitric acid 2~8%, sulfuric acid 2~12%, additive 0.01~2%, excess water, the additive are the mixture of alkali metal salt and organic matter, and organic matter selects thiourea derivative, hexamethylenetetramine, imidazoles, benzotriazole and 2, any one in 4,6 trihydroxybenzoic acids.The etching solution of the present invention is using nitric acid and sulfuric acid as main component, and simple for process, acid concentration is moderate, has excellent etching performance to ITO conductive films, and etch-rate is moderate, etches the high noresidue of precision, disclosure satisfy that the etching requirement of different-thickness ITO.All there is excellent effect against corrosion to lower metal Al or Mo, can be good at meeting technical matters and process requirements as additive using a kind of alkali metal salt and a kind of organic matter simultaneously.In addition, the etching solution using inexpensive sulfuric acid as raw material, advantageously reduces the cost of etching solution on the basis of meeting technical matters and process requirements.
Description
Technical field
The present invention relates to wet electronic chemical product fields, more particularly to a kind of fine etching solution for ITO conductive films
And preparation method thereof.
Background technology
Transparent conductive oxide have more and more important commercial value, most widely used and Maximum Value field be
In FPD manufacturing industry.And application at present is mainly tin indium oxide (Indium-tin- as the transparent conductive oxide of electrode
Oxide, ITO).ITO etching solutions are widely used in the manufacturing process of the ito transparent electrode of TFT-LCD industries.The etching of ito film
It is last procedure of TFT patterns Array manufactures.After ito film sputtering, one layer photoresist of covering, light shield developing pattern, and
Ito film, then stripping photoresist are etched with etching solution, forms required pattern.In addition, with the development of display industry, producing line processing procedure
It constantly updates, etching precision is also had higher requirement, therefore, develops the ITO etching solutions of a fine, meet client's erosion
The requirement of carving technology and making technology just seems particularly necessary.
In the prior art, a kind of advanced lines tablet ITO etching solutions are disclosed in CN201510832036.0, with sulfuric acid/
Nitric acid/acetic acid is Main System, and the content of acid used is all higher, and etching reaction is violent, it is difficult to which control etching precision is not suitable for
The smaller ito film layer of thickness, and etching solution cost is higher, in addition, containing acetic acid in the liquid etching composition, is using process
In, acetic acid is readily volatilized, needs to be continuously replenished, increases technology difficulty.CN200910003907.2 discloses a kind of for losing
The etching agent composite of indium tin oxide layer and the method with its etching are carved, the etching agent composite is with sulfuric acid, nitric acid, etching control
Preparation is main component, and etching control agent is mainly sylvite, and the etching solution acid concentration is relatively low, and etch-rate is slower, and is easy
Lower layer Mo and Al are caused to corrode, it is difficult to meet technique and process requirements.
Invention content
It is an object of the invention to solve the deficiencies in the prior art, a kind of fine erosion for ITO conductive films is provided
Carve liquid and preparation method thereof.
The technical solution adopted by the present invention to solve the technical problems is：
For the fine etching solution of ITO conductive films, the weight percent composition of the high-precision etching solution is as follows：Nitre
Acid 2~8%, sulfuric acid 2~12%, additive 0.01~2%, excess water, the additive are the mixed of alkali metal salt and organic matter
Object is closed, organic matter selects thiourea derivative, hexamethylenetetramine, imidazoles, benzotriazole and 2, in 4,6- trihydroxybenzoic acids
Any one.
Preferably, alkali metal salt is selected from lithium nitrate, lithium acetate, sodium nitrate, sodium acetate, sodium phosphate, sodium dihydrogen phosphate, phosphoric acid
Any one in potassium, potassium acetate, potassium sulfate, potassium dihydrogen phosphate and potassium pyrophosphate.
Preferably, thiourea derivative is ethylene thiourea, N- methylthioureas, 4- methyl-thiosemicarbazide or benzoyl sulphur
Urea.
Preferably, the mass ratio of alkali metal salt and organic matter is：0.005-5:1
Additive in this patent is alkali metal salt and organic matter, and for the effect of additive, wherein alkali metal salt adds
Add agent presence can potential difference of the control targe metal (Al or Mo) between ionic state and free state, to reduce the corruption of metal
Erosion, and for organics additive, the group volume of organic matter is big and can be attached to metal surface, forms steric hindrance effect
It answers, to reduce corrosion of metal.In general, a kind of simple function and effect of additive are than relatively limited, and for metal
Type has certain selectivity, and for the lower metal of current etch target, it is various metals composite construction, therefore single
Single kind of additive can only often meet the requirement against corrosion of wherein a certain metal, and alkali metal salt and organic matter is used to make simultaneously
For additive when, the synergistic effects of two kinds of additives generates association so that the function and effect of two kinds of additives have prodigious reinforcement
Same effect, to substantially improve the metal etch resistant properties of etching solution.
A kind of preparation method of fine etching solution for ITO conductive films, the preparation method include the following steps：
(1) electronic-grade sulfuric acid is added in mixture kettle in proportion；
(2) under conditions of being stirred continuously, it is proportionally added into electronic grade nitric acid, and recycle 30min；
(3) under conditions of being stirred continuously, it is proportionally added into two kinds of additives and excess water, and recycle 5h；
(4) ITO etching solutions are obtained after being filtered mixing liquid using 0.1 μm of filter.
The present invention is used for the fine etching solution of ITO conductive films, and the thickness of etch target ITO layer isEtching period is 60~360s, and etch temperature is 35~45 DEG C.
Compared with prior art, the beneficial effects of the invention are as follows：The etching solution is using nitric acid and sulfuric acid as main component, technique
Simply, acid concentration is moderate, has excellent etching performance to ITO conductive films, and etch-rate is moderate, and etching precision height is without residual
It stays, disclosure satisfy that the etching requirement of different-thickness ITO.Simultaneously using a kind of alkali metal salt and a kind of organic matter as additive,
All there is excellent effect against corrosion to lower metal Al or Mo, can be good at meeting technical matters and process requirements.In addition,
The etching solution advantageously reduces etching solution using inexpensive sulfuric acid as raw material on the basis of meeting technical matters and process requirements
Cost.
Description of the drawings
Fig. 1 is the etch effect section SEM and plane SEM spectrum of embodiment 1；
Fig. 2 is the etch effect section SEM and plane SEM spectrum of embodiment 2；
Fig. 3 is the etch effect section SEM and plane SEM spectrum of embodiment 3；
Fig. 4 is the etch effect section SEM and plane SEM spectrum of embodiment 4；
Fig. 5 is the etch effect section SEM and plane SEM spectrum of embodiment 5；
Fig. 6 is the etch effect section SEM and plane SEM spectrum of embodiment 6；
Fig. 7 is the etch effect section SEM and plane SEM spectrum of embodiment 7；
Fig. 8 is the lower metal Mo corrosive effect SEM spectrums of embodiment 1；
Fig. 9 is the lower metal Al corrosive effect SEM spectrums of embodiment 1；
Figure 10 is the etch effect section SEM and plane SEM spectrum of comparative example 1；
Figure 11 is the lower metal Mo corrosive effect SEM spectrums of comparative example 2；
Figure 12 is the lower metal Al corrosive effect SEM spectrums of comparative example 3；
Specific implementation mode
With reference to embodiment, the specific embodiment of the present invention is further described.Following embodiment is only used for more
Add and clearly demonstrate technical scheme of the present invention, and not intended to limit the protection scope of the present invention.
Embodiment 1：
For the fine etching solution of ITO conductive films, which forms as follows by weight percentage：
The nitric acid of 5wt%, the sulfuric acid of 8wt%, the potassium pyrophosphate of 0.1wt%, the ethylene thiourea of 0.1wt%, surplus are water.
Preparation method includes the following steps：
(1) electronic-grade sulfuric acid is added in mixture kettle in proportion；
(2) under conditions of being stirred continuously, it is proportionally added into electronic grade nitric acid, and recycle 30min；
(3) under conditions of being stirred continuously, it is proportionally added into two kinds of additives and excess water, and recycle 5h；
(4) ITO etching solutions are obtained after being filtered mixing liquid using 0.1 μm of filter.
The thickness of the etching solution etch target ITO layer isEtching period is 300s, and etch temperature is 40 DEG C.
Embodiment 2：
For the fine etching solution of ITO conductive films, which forms as follows by weight percentage：
The nitric acid of 2wt%, the sulfuric acid of 12wt%, the potassium acetate of 0.1wt%, the N- methylthioureas of 0.1wt%, surplus is water.
Preparation method includes the following steps：
(1) electronic-grade sulfuric acid is added in mixture kettle in proportion；
(2) under conditions of being stirred continuously, it is proportionally added into electronic grade nitric acid, and recycle 30min；
(3) under conditions of being stirred continuously, it is proportionally added into two kinds of additives and excess water, and recycle 5h；
(4) ITO etching solutions are obtained after being filtered mixing liquid using 0.1 μm of filter.The etching solution etch target
The thickness of ITO layer isEtching period is 135s, and etch temperature is 45 DEG C.
Embodiment 3：
For the fine etching solution of ITO conductive films, which forms as follows by weight percentage：
The nitric acid of 4wt%, the sulfuric acid of 12wt%, the potassium dihydrogen phosphate of 0.01wt%, the imidazoles of 1.99wt%, surplus are water.
Preparation method includes the following steps：
(1) electronic-grade sulfuric acid is added in mixture kettle in proportion；
(2) under conditions of being stirred continuously, it is proportionally added into electronic grade nitric acid, and recycle 30min；
(3) under conditions of being stirred continuously, it is proportionally added into two kinds of additives and excess water, and recycle 5h；
(4) ITO etching solutions are obtained after being filtered mixing liquid using 0.1 μm of filter.The etching solution etch target
The thickness of ITO layer isEtching period is 360s, and etch temperature is 35 DEG C.
Embodiment 4：
For the fine etching solution of ITO conductive films, which forms as follows by weight percentage：
The nitric acid of 4wt%, the sulfuric acid of 8wt%, the sodium phosphate of 0.5wt%, the hexamethylenetetramine of 0.5wt%, surplus are water.
Preparation method includes the following steps：
(1) electronic-grade sulfuric acid is added in mixture kettle in proportion；
(2) under conditions of being stirred continuously, it is proportionally added into electronic grade nitric acid, and recycle 30min；
(3) under conditions of being stirred continuously, it is proportionally added into two kinds of additives and excess water, and recycle 5h；
(4) ITO etching solutions are obtained after being filtered mixing liquid using 0.1 μm of filter.
The thickness of the etching solution etch target ITO layer isEtching period is 150s, and etch temperature is 35 DEG C.
Embodiment 5：
For the fine etching solution of ITO conductive films, which forms as follows by weight percentage：
The nitric acid of 6wt%, the sulfuric acid of 6wt%, the sodium dihydrogen phosphate of 0.4wt%, the 2 of 1wt%, 4,6- trihydroxybenzoic acids, surplus is
Water.
Preparation method includes the following steps：
(1) electronic-grade sulfuric acid is added in mixture kettle in proportion；
(2) under conditions of being stirred continuously, it is proportionally added into electronic grade nitric acid, and recycle 30min；
(3) under conditions of being stirred continuously, it is proportionally added into two kinds of additives and excess water, and recycle 5h；
(4) ITO etching solutions are obtained after being filtered mixing liquid using 0.1 μm of filter.
The thickness of the etching solution etch target ITO layer isEtching period is 150s, and etch temperature is 40 DEG C.
Embodiment 6：
For the fine etching solution of ITO conductive films, which forms as follows by weight percentage：
The nitric acid of 8wt%, the sulfuric acid of 6wt%, the potassium sulfate of 0.5wt%, the benzoylthioureas of 0.5wt%, surplus are water.
Preparation method includes the following steps：
(1) electronic-grade sulfuric acid is added in mixture kettle in proportion；
(2) under conditions of being stirred continuously, it is proportionally added into electronic grade nitric acid, and recycle 30min；
(3) under conditions of being stirred continuously, it is proportionally added into two kinds of additives and excess water, and recycle 5h；
(4) ITO etching solutions are obtained after being filtered mixing liquid using 0.1 μm of filter.
The thickness of the etching solution etch target ITO layer isEtching period is 300s, and etch temperature is 40 DEG C.
Embodiment 7：
For the fine etching solution of ITO conductive films, which forms as follows by weight percentage：
The nitric acid of 3wt%, the sulfuric acid of 10wt%, the sodium acetate of 0.5wt%, the ethylene thiourea of 0.1wt%, surplus are water.
Preparation method includes the following steps：
(1) electronic-grade sulfuric acid is added in mixture kettle in proportion；
(2) under conditions of being stirred continuously, it is proportionally added into electronic grade nitric acid, and recycle 30min；
(3) under conditions of being stirred continuously, it is proportionally added into two kinds of additives and excess water, and recycle 5h；
(4) ITO etching solutions are obtained after being filtered mixing liquid using 0.1 μm of filter.The etching solution etch target
The thickness of ITO layer isEtching period is 60s, and etch temperature is 45 DEG C.
Embodiment 8：
For the fine etching solution of ITO conductive films, which forms as follows by weight percentage：
The nitric acid of 5wt%, the sulfuric acid of 8wt%, the lithium acetate of 0.1wt%, the benzotriazole of 0.1wt%, surplus are water.
Preparation method includes the following steps：
(1) electronic-grade sulfuric acid is added in mixture kettle in proportion；
(2) under conditions of being stirred continuously, it is proportionally added into electronic grade nitric acid, and recycle 30min；
(3) under conditions of being stirred continuously, it is proportionally added into two kinds of additives and excess water, and recycle 5h；
(4) ITO etching solutions are obtained after being filtered mixing liquid using 0.1 μm of filter.The etching solution etch target
The thickness of ITO layer isLower metal is Mo, and etching period 300s, etch temperature is 40 DEG C.
Embodiment 9：
For the fine etching solution of ITO conductive films, which forms as follows by weight percentage：
The nitric acid of 5wt%, the sulfuric acid of 8wt%, the lithium acetate of 0.1wt%, the benzotriazole of 0.1wt%, surplus are water.
Preparation method includes the following steps：
(1) electronic-grade sulfuric acid is added in mixture kettle in proportion；
(2) under conditions of being stirred continuously, it is proportionally added into electronic grade nitric acid, and recycle 30min；
(3) under conditions of being stirred continuously, it is proportionally added into two kinds of additives and excess water, and recycle 5h；
(4) ITO etching solutions are obtained after being filtered mixing liquid using 0.1 μm of filter.
The thickness of the etching solution etch target ITO layer isLower metal is Al, etching period 300s, etching
Temperature is 40 DEG C.
Comparative example 1：
Etching solution component forms as follows by weight percentage：The nitric acid of 1.5wt%, the sulfuric acid of 1.5wt%, 0.1wt%
Potassium pyrophosphate, the ethylene thiourea of 0.1wt%, surplus is water.
Preparation method includes the following steps：
(1) electronic-grade sulfuric acid is added in mixture kettle in proportion；
(2) under conditions of being stirred continuously, it is proportionally added into electronic grade nitric acid, and recycle 30min；
(3) under conditions of being stirred continuously, it is proportionally added into two kinds of additives and excess water, and recycle 5h；
(4) ITO etching solutions are obtained after being filtered mixing liquid using 0.1 μm of filter.The etching solution etch target
The thickness of ITO layer isEtching period is 300s, and etch temperature is 40 DEG C.
That difference lies in acid concentrations is different by comparative example 1 and embodiment 1-9, shows etching solution acid by the verification result of Figure 10
Etch residue is had when concentration is too low, cannot be satisfied requirement.
Comparative example 2：
Etching solution component forms as follows by weight percentage：The nitric acid of 5wt%, the sulfuric acid of 8wt%, the benzene of 0.1wt%
And triazole, surplus are water.
Preparation method includes the following steps：
(1) electronic-grade sulfuric acid is added in mixture kettle in proportion；
(2) under conditions of being stirred continuously, it is proportionally added into electronic grade nitric acid, and recycle 30min；
(3) under conditions of being stirred continuously, it is proportionally added into two kinds of additives and excess water, and recycle 5h；
(4) ITO etching solutions are obtained after being filtered mixing liquid using 0.1 μm of filter.
The thickness of the etching solution etch target ITO layer isLower metal is Mo, etching period 300s, etching
Temperature is 40 DEG C.
Comparative example 2 and embodiment 1-9 is shown only difference lies in organic matter is only added to by the verification result of Figure 11
Corrosion is will produce when being Mo to etch target lower metal when organics additive, two kinds of additives of side light must coexist
It can meet the requirements.
Comparative example 3：
Etching solution component forms as follows by weight percentage：The nitric acid of 5wt%, the sulfuric acid of 8wt%, the vinegar of 0.1wt%
Sour lithium, surplus are water.
Preparation method includes the following steps：
(1) electronic-grade sulfuric acid is added in mixture kettle in proportion；
(2) under conditions of being stirred continuously, it is proportionally added into electronic grade nitric acid, and recycle 30min；
(3) under conditions of being stirred continuously, it is proportionally added into two kinds of additives and excess water, and recycle 5h；
(4) ITO etching solutions are obtained after being filtered mixing liquid using 0.1 μm of filter.
The thickness of the etching solution etch target ITO layer isLower metal is Al, etching period 300s, etching
Temperature is 40 DEG C.
Comparative example 3 and embodiment 1-9 is shown only difference lies in alkali metal salt is only added to by the verification result of Figure 12
Having when alkali metal salt additive to etch target lower metal to will produce corrosion when Al, illustrating that two kinds of additives must coexist
It can meet the requirements.
By embodiment 1-9, compared with comparative example 1-3, the results showed that：The fine erosion of the ITO conductive films of the present invention
Liquid is carved, simple for process, acid concentration is moderate, has excellent etching performance to ITO conductive films, and etch-rate is moderate, etching essence
High noresidue is spent, disclosure satisfy that the etching requirement of different-thickness ITO.A kind of alkali metal salt and a kind of organic matter conduct are used simultaneously
Additive, synergistic effect between the two can ensure that etching solution all has excellent effect against corrosion to lower metal Al or Mo
Fruit can be good at meeting technical matters and process requirements.
Claims (2)
1. the fine etching solution for ITO conductive films, it is characterised in that：The weight percent of the fine etching solution
Composition is as follows：Nitric acid 2~8%, sulfuric acid 2~12%, additive 0.01~2%, excess water, the additive are alkali metal salt and have
The mixture of machine object, organic matter select thiourea derivative and 2, any one in 4,6- trihydroxybenzoic acids；
The mass ratio of alkali metal salt and organic matter is：0.005-5:1；
Any one of alkali metal salt in lithium nitrate, lithium acetate, sodium nitrate, sodium acetate, sodium phosphate and sodium dihydrogen phosphate;
The preparation method of the fine etching solution includes the following steps：
（1）Electronic-grade sulfuric acid is added in mixture kettle in proportion；
（2）Under conditions of being stirred continuously, it is proportionally added into electronic grade nitric acid, and recycle 30 min；
（3）Under conditions of being stirred continuously, it is proportionally added into two kinds of additives and excess water, and recycle 5h；
（4）ITO etching solutions are obtained after mixing liquid is filtered using 0.1 μm of filter.
2. the fine etching solution according to claim 1 for ITO conductive films, it is characterised in that：Thiourea derivative
For ethylene thiourea, N- methylthioureas, 4- methyl-thiosemicarbazide or benzoylthioureas.
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| CN113201345A (en) * | 2021-05-06 | 2021-08-03 | 合肥中聚合臣电子材料有限公司 | ITO etching solution for TFT-LCD display screen and preparation method thereof |
| CN114106835A (en) * | 2021-11-11 | 2022-03-01 | Tcl华星光电技术有限公司 | Etching solution composition and display panel |
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| CN102108512B (en) * | 2009-12-25 | 2013-09-18 | 比亚迪股份有限公司 | Chemical etching liquid for metals and etching method |
| CN103805203B (en) * | 2014-02-17 | 2015-11-04 | 昆山市板明电子科技有限公司 | Selective oxidation indium tin etching solution |
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