CN104498951B - Oxydol etching solution for copper-molybdenum alloy films - Google Patents
Oxydol etching solution for copper-molybdenum alloy films Download PDFInfo
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Abstract
The invention discloses an oxydol etching solution for copper-molybdenum alloy films. The etching solution is free of fluorides, and comprises the following main components in percentage by weight: 1-35% of hydrogen peroxide, 0.05-5% of inorganic acid, 0.1-5% of hydrogen peroxide stabilizer, 0.1-5% of metal chelator, 0.1-5% of etching additive, 0.1-5% of surfactant, 0.1-5% of defoaming agent and the balance of deionized water. The etching solution has the advantages of no environment pollution, mild and controllable reaction, proper cone angle after etching, small CD loss, favorable defoaming property and higher overall performance, and lays foundation for high-precision processing.
Description
Technical field
The application is related to etching solution field, more particularly to a kind of dioxygen water system copper-molybdenum alloy film etching solution.
Background technology
Etching is the technology for removing materials'use chemical reaction or physical shock effect；Etching technique is divided into wet etching
And dry ecthing.Wherein, wet etching is to adopt chemical reagent, and via chemical reaction the purpose of etching is reached.
In recent years, the quality and picture precision while people are continuously increased to the demand of liquid crystal display, to product
Higher requirement is it is also proposed, and the effect for etching can directly result in the quality of circuit board manufacturing process, affect high density carefully to lead
The precision and quality of line image.Aluminum or aluminum alloy used in the metal wiring of conventional liquid crystal indicator, but with liquid
The maximization of crystal display and high resolution, the gate line being connected with thin film transistor (TFT) and data wire can be elongated, and these are matched somebody with somebody
The resistance of line also can increase, therefore the problems such as generation signal delay.So, research steering in the lower material of resistance be copper or with
Copper is the wiring combination of main constituent.Molybdenum have it is high with the adaptation of the substrate such as glass, be difficult to produce diffusion to silicon semiconductor film,
And have block concurrently；Therefore, by comprising copper, copper molybdenum alloy with copper as main constituent stacked film by film-forming process such as sputtering methods
The film forming on the substrates such as glass, then becomes electrode figure through the etching work procedure for being etched resist etc. as mask
Case.
Existing dioxygen water system copper molybdenum alloy etching solution, in order to improve the speed of etching molybdenum alloy, usually adds fluorination
Thing.Addition fluoride etching solution be disadvantageous in that, first, fluoride is extremely unfriendly to environment；Second, corrosive power
By force, in reagent etching process, it tends to be difficult to control etching angle and etching period；3rd, due to its severe corrosive, to operation
The danger of personnel and client device is also higher.At present, it is right as increasing Producer begins to use copper-molybdenum alloy film
The demand of the etching solution of machining accuracy is greatly increased, therefore, it is high to need a kind of environmental friendliness, production safety, machining accuracy badly, and easily
In the etching solution of control.
The content of the invention
The purpose of the application is to provide a kind of improved dioxygen water system copper-molybdenum alloy film etching solution.
To achieve these goals, the application employs technical scheme below：
This application discloses a kind of dioxygen water system copper-molybdenum alloy film etching solution, without fluorination in the etching solution of the application
Thing, also, the main component of etching solution include accounting for the hydrogen peroxide of etching solution gross weight 1-35%, the mineral acid of 0.05-5%,
The stabilizer of hydrogen peroxide of 0.1-5%, the metal-chelator of 0.1-5%, the etching additive of 0.1-5%, the surface of 0.1-5%
The defoamer of activating agent and 0.1-5%, balance of deionized water.
It should be noted that the etching solution of the application substitutes fluoride using appropriate mineral acid, and with surfactant,
Defoamer etc. coordinates, and has both avoided pollution of the fluoride to environment, and etching performance is improve again；Also, the etching solution after replacing
Reaction it is relatively mild, entirely etch it is easily controllable, it is also safer to operator and client device.Wherein, mineral acid is main
It is to promote by the dissolving of the copper of hydrogen peroxide oxidation；In the preferred version of the application, mineral acid is selected from nitric acid, sulphuric acid, phosphoric acid, boron
At least one in acid.
Preferably, the consumption of hydrogen peroxide is the 5-35% of etching solution gross weight；It is furthermore preferred that the consumption of hydrogen peroxide is
The 10-30% of etching solution gross weight.
It should be noted that primary oxidizers of the hydrogen peroxide for copper molybdenum alloy, the content of hydrogen peroxide is the application's
In the range of when, both can ensure that etching is effectively carried out, while etching speed is maintained in suitable scope when also can control, so as to lose
The quarter control of amount also becomes easy.
Preferably, the consumption of mineral acid is the 0.05-3% of etching solution gross weight；The consumption of metal-chelator is etching solution
The 0.1-3% of gross weight；The consumption of defoamer is the 0.1-3% of etching solution gross weight.
In the application, the effect of stabilizer of hydrogen peroxide is stable peroxide hydrogen, therefore, as long as usually as peroxidating
The material that stabilized hydrogen agent is used；In the preferred version of the application, it is contemplated that the overall performance of etching solution, hydrogen peroxide stabilizers
Agent is selected from one or two of diethyl triamine pentaacetic acid, N-hydroxyethyl-ethylenediamine triacetic acid and poly amic acid.
In the application, the Main Function of metal-chelator is to form chelating with the metal ion produced in etching process,
Make its deactivation, so as to suppress etching solution in hydrogen peroxide decomposition reaction；Preferably, metal-chelator is selected from ethylenediamine tetraacetic
Acetic acid, aminotriacetic acid, diethylene-triamine pentaacetic acid, diethylene triamine pentacetic acid (DTPA), hydroxyethylethylene diamine tri-acetic acid, glucose
At least one of acid, sodium tartrate, citric acid and hydroxyacetic acid.
In the application, the Main Function for etching additive is in order to adjust etch-rate, while extending the use of etching solution
In the life-span, additive is etched in the preferred scheme of the application at least two of organic acid, nitrogen-containing heterocycle compound and salt apoplexy due to endogenous wind；Its
In, organic acid is in acetic acid, phenol, ortho-methyl phenol, m-methyl phenol, p-methyl phenol, butanoic acid, valeric acid and glycine
It is at least one；Nitrogen-containing heterocycle compound is selected from quinoline, 8-hydroxyquinoline, benzotriazole, methylol benzotriazole, imidazoles and benzo
At least one in imidazoles；At least one of the salt in tartrate, heptose hydrochlorate, sodium gluconate and sodium alginate.
In the application, the Main Function of surfactant is the wettability and infiltration that can effectively improve etching solution to substrate
Property, while being not likely to produce residue, it is preferred to use sulfonic acid type material；In the preferred version of the application, it is contemplated that the entirety of etching solution
Performance, it is preferred that surfactant is selected from least in alkyl sulfonic acid, alkyl benzene sulphonate and dioctyl succinate disulfonate acid
Kind.
In the application, because the addition of surfactant strengthens the foaming characteristic of etching solution, so as to hinder substrate with erosion
The contact of liquid is carved, causes etching low precision, the defect such as etching face is coarse, therefore, defoamer is with the addition of in the etching solution of the application,
It is preferred that adopting polyethers defoamer；In the preferred version of the application, it is contemplated that the overall performance of etching solution, it is preferred that defoamer
Selected from the ether of Nonyl pheno 5, the ether of Nonyl pheno 10, Brij 35, octyl phenol Polyethylene oxide 5
At least one in ether, the ether of octyl phenol Polyethylene oxide 5, polyoxyethylated alkyl phenol and polyoxyethylene aliphatic alcohol ether.
Due to being using the beneficial effect of above technical scheme, the application：
The etching solution of the application, without fluoride, to environment friendly and pollution-free；Also, reaction is gently easily controlled, after etching
Etching cone angle is suitable, the CD little, antifoam performances of loss are good, improves the overall performance of etching solution, is that base has been established in high accuracy processing
Plinth.
Specific embodiment
With widely using for copper-molybdenum alloy film, a kind of demand of the etching solution that can improve machining accuracy is increased
Plus；And existing etching solution, it is as previously described, not only unfriendly to environment, and etching be difficult to control to, it is impossible to meet high accuracy
The demand of processing；Therefore, the application develops a kind of preferably not fluorine-containing dioxygen water system copper-molybdenum alloy film etching solution, not only
Good etching performance is can ensure that, while corrosion will not be produced to glass substrate, silicon layer etc., and not fluoride, to ring
Border is pollution-free.It should be noted that fluoride is mainly and Mo reactions, and the thickness of Mo is relatively in the middle of the system of copper-molybdenum
It is little, although so not fluoride, the impact very little to etching speed in the etching solution of the application；Also, due to adopting
Mineral acid, stabilizer of hydrogen peroxide, metal-chelator, etching additive, defoamer of surfactant sum etc. coordinate, and are protecting
While barrier etching performance, its etching speed is also very nearly the same with the etching speed of addition fluoride.
The application is described in further detail below by specific embodiment.Following examples only are entered to advance to the application
The explanation of one step, should not be construed as the restriction to the application.
Embodiment
The etching solution of this example is by hydrogen peroxide, mineral acid, stabilizer of hydrogen peroxide, metal-chelator, etching additive, table
Face activating agent, defoamer and deionized water composition.In this example, inorganic acid-specific adopts sulphuric acid；Stabilizer of hydrogen peroxide is using poly-
Acrylic amine；Metal-chelator adopts hydroxyacetic acid；Etching additive is made up of nitrogen-containing heterocycle compound and salt, specifically,
Nitrogen-containing heterocycle compound adopts imidazoles, salt to adopt sodium alginate；The OT surfactants that surfactant is bought using market；
The NP-5 that defoamer is bought using market, the i.e. ether of Nonyl pheno 5.This example is tried the consumption of above component respectively
Test, and be provided with four contrast tests, refer to table 1, each percentage ratio is weight percentage in table 1, i.e., the component accounts for etching solution
The percentage ratio of gross weight, balance of deionized water.
The consumption and contrast test of each component of table 1
Consumption according to table 1 prepares etching solution, and the defoaming to etching solution is tested, specifically, by the erosion of 30mL ketone
Carve liquid to be contained in 100mL test tubes, vertical concussion is multiple, and after stopping 1 minute foam height is measured.Test result is as shown in table 2,
It can be seen that, the test group and contrast groups foam height for adding defoamer NP-5 is controlled in below 0.5cm, and is not added with the contrast groups of NP-5
2, its foam height illustrates that NP-5 can effectively play the effect of froth breaking in more than 1.0cm；So as to reduce the bubble of etching solution
Impact to etching precision and etching quality.
The consumption for pressing table 1 is prepared into etching solution, the copper-containing metal film and film containing molybdenum to electrodes such as TFT-LCD display
It is etched.Specifically, the barrier film that formed by molybdenum system material is stacked gradually using sputtering method on the glass substrate and by copper or
On copper/molybdenum system plural layers that material with copper as main constituent is formed, development, exposure form expected etch-resistant coating pattern；Glass
Glass substrate is respectively adopted the etching solution of each group test or contrast test in this example table 1 at 32 DEG C and is etched, etching period about 3
Minute, after etching terminates, cleaned in a conventional manner and dried up.And according to conventional measuring method, cone is etched to it
Angle, residual, CD loss uniformities etc. are tested.Meanwhile, the service life of etching solution is conventionally measured, using the longevity
The highest Cu content that the test of life is dissolved when still keeping preferable performance with etching solution is represented.All test results are as shown in table 2.
The etching solution of table 2 and etch effect measurement result
As shown in the result of table 2, (1) is visible by the comparison of test group 2 and contrast groups 4, the etching solution of this example, addition or not
Addition fluoride, its etching speed almost has no impact；But, etch cone angle after addition fluoride and greatly improve, it is seen then that this
The etching solution without fluoride of application, etching process is more easily controlled, and more conducively high accuracy is processed.(2) test group 4 due to
The consumption of hydrogen peroxide is bigger than normal so that its etching taper and CD losses are bigger than normal；Therefore, through substantial amounts of this example through substantial amounts of
Test is final to be determined, the consumption of hydrogen peroxide is the 1-35% of total etching solution weight, preferably 5-35%, and in order to ensure erosion
Carve effect, more preferably 10-30%.(3) according to contrast groups 1 and the data display of contrast groups 3, etching additive is to etching solution
Service life and etch-rate have a significant impact, and must nitrogen-containing heterocycle compound and salt use cooperatively；Further, since
The consumption of imidazoles is low in test group 1 so that service life is affected；Additionally, this example additionally uses organic acid tested,
As a result show, etch additive simultaneously using at least two of organic acid, nitrogen-containing heterocycle compound and salt apoplexy due to endogenous wind, its effect is most
It is good.(4) for residue problem, test group 2 and the effect of test group 4 are reasonable, but, the hydrogen peroxide use of test group 4
Larger, other have impact on the overall performance of etching solution；Test group 1 is because the consumption of imidazoles is low, and the consumption of the imidazoles of test group 3 is inclined
Greatly, all it is unfavorable for improving the overall performance of etching solution, so there is residual；And the consumption of hydrogen peroxide is relatively small in test group 5,
So also generate residual, therefore, the optimum consumption of hydrogen peroxide or 10-30%.
On the basis of test group 2, this example continues to test etching solution component and each component consumption.As a result show
Show, mineral acid can also be replaced in addition to can be using sulphuric acid using nitric acid, phosphoric acid, boric acid etc., and the consumption of mineral acid is in etching
The 0.05-5% of liquid gross weight, optimum 0.05-3% effects are best；Stabilizer of hydrogen peroxide may be used also in addition to poly amic acid
Etching solution gross weight is preferably with the consumption using diethylamine pentaacetic acid and N-hydroxyethyl-ethylenediamine triacetic acid, stabilizer of hydrogen peroxide
The 0.1-5% of amount；Metal-chelator can also using ethylenediaminetetraacetic acid, aminotriacetic acid, diethylene-triamine pentaacetic acid, two
Ethylene pentaacetic acid, hydroxyethylethylene diamine tri-acetic acid, gluconic acid, sodium tartrate, citric acid etc., the consumption of metal-chelator
For the 0.1-5% of etching solution gross weight, preferably 0.1-3%；For etching additive, wherein salt is removed and can use alginic acid
Outside sodium, can be replaced using tartrate, heptose hydrochlorate, sodium gluconate, nitrogen-containing heterocycle compound can adopt quinoline, 8- hydroxyls
Base quinoline, benzotriazole, methylol benzotriazole, benzimidazole etc. are replaced, and organic acid can be using acetic acid, phenol, adjacent first
Base phenol, m-methyl phenol, p-methyl phenol, butanoic acid, valeric acid and glycine etc., the total consumption for etching additive is etching solution weight
The consumption of the 0.1-5% of amount, wherein nitrogen-containing heterocycle compound is greater than 0.01%, and less than 3.5%, otherwise affects etching solution
Overall performance；Surfactant adopts sulfonic acid type material, and such as alkyl sulfonic acid, alkyl benzene sulphonate and dioctyl succinate disulfonate acid is equal
Can, its consumption is the 0.1-5% of etching solution weight；Defoamer can also use the ether of Nonyl pheno 10, dodecyl alcohol
Polyoxyethylene ether, the ether of octyl phenol Polyethylene oxide 5, the ether of octyl phenol Polyethylene oxide 5, polyoxyethylated alkyl phenol and Polyoxyethylene fatty
Alcohol ether etc., its consumption is also the 0.1-5% of etching solution weight, preferably 0.1-3%.
The etching solution for obtaining is prepared according to above consumption and component, etching cone angle is suitable, CD loses little, the performance of etching solution
Increase；Disclosure satisfy that the demand of high accuracy processing.
Above content is to combine the further description that specific embodiment is made to the application, it is impossible to assert this Shen
Being embodied as please is confined to these explanations.For the application person of an ordinary skill in the technical field, do not taking off
On the premise of conceiving from the application, some simple deduction or replace can also be made, should all be considered as belonging to the protection of the application
Scope.
Claims (9)
1. a kind of dioxygen water system copper-molybdenum alloy film etching solution, it is characterised in that：Not fluoride in the etching solution, also,
The main component of etching solution includes accounting for the hydrogen peroxide of etching solution gross weight 1-35%, the mineral acid of 0.05-5%, 0.1-5%
Stabilizer of hydrogen peroxide, the metal-chelator of 0.1-5%, 0.1-5% etching additive, the surfactant of 0.1-5% and
The defoamer of 0.1-5%, balance of deionized water；
At least one of the surfactant in alkyl sulfonic acid, alkyl benzene sulphonate and dioctyl succinate disulfonate acid.
2. etching solution according to claim 1, it is characterised in that：The consumption of the hydrogen peroxide is etching solution gross weight
5-35%.
3. etching solution according to claim 2, it is characterised in that：The consumption of the hydrogen peroxide is etching solution gross weight
10-30%.
4. etching solution according to claim 1, it is characterised in that：The consumption of the mineral acid is etching solution gross weight
0.05-3%；The consumption of the metal-chelator is the 0.1-3% of etching solution gross weight；The consumption of the defoamer is etching solution
The 0.1-3% of gross weight.
5. the etching solution according to any one of claim 1-4, it is characterised in that：The mineral acid is selected from nitric acid, sulphuric acid, phosphorus
At least one in acid, boric acid.
6. the etching solution according to any one of claim 1-4, it is characterised in that：The stabilizer of hydrogen peroxide is selected from diethyl
Triamine pentaacetic acid, N-hydroxyethyl-ethylenediamine triacetic acid and poly amic acid one or two.
7. the etching solution according to any one of claim 1-4, it is characterised in that：The metal-chelator is selected from ethylenediamine tetraacetic
Acetic acid, aminotriacetic acid, diethylene-triamine pentaacetic acid, diethylene triamine pentacetic acid (DTPA), hydroxyethylethylene diamine tri-acetic acid, glucose
At least one of acid, sodium tartrate, citric acid and hydroxyacetic acid.
8. the etching solution according to any one of claim 1-4, it is characterised in that：It is described etching additive selected from organic acid,
At least two of nitrogen-containing heterocycle compound and salt；
The organic acid is selected from acetic acid, phenol, ortho-methyl phenol, m-methyl phenol, p-methyl phenol, butanoic acid, valeric acid and sweet ammonia
At least one in acid；
The nitrogen-containing heterocycle compound is selected from quinoline, 8-hydroxyquinoline, benzotriazole, methylol benzotriazole, imidazoles and benzo
At least one in imidazoles；
At least one of the salt in tartrate, heptose hydrochlorate, sodium gluconate and sodium alginate.
9. the etching solution according to any one of claim 1-4, it is characterised in that：The defoamer is selected from polyoxyethylene nonyl phenyl second
The ether of alkene 5, the ether of Nonyl pheno 10, Brij 35, the ether of octyl phenol Polyethylene oxide 5, octyl phenol polyoxy second
At least one in the ether of alkene 5, polyoxyethylated alkyl phenol and polyoxyethylene aliphatic alcohol ether.
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| CN201410764798.7A CN104498951B (en) | 2014-12-11 | 2014-12-11 | Oxydol etching solution for copper-molybdenum alloy films |
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| CN201410764798.7A CN104498951B (en) | 2014-12-11 | 2014-12-11 | Oxydol etching solution for copper-molybdenum alloy films |
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| KR101271414B1 (en) * | 2010-02-15 | 2013-06-05 | 미쯔비시 가스 케미칼 컴파니, 인코포레이티드 | Etching solution for multilayer thin film having copper layer and molybdenum layer contained therein |
| US9365770B2 (en) * | 2011-07-26 | 2016-06-14 | Mitsubishi Gas Chemical Company, Inc. | Etching solution for copper/molybdenum-based multilayer thin film |
| KR101243847B1 (en) * | 2011-08-18 | 2013-03-20 | 주식회사 이엔에프테크놀로지 | Method for etching cu/mo alloy film with etching capacity of etching solution improved |
| CN103924242B (en) * | 2013-01-14 | 2016-05-11 | 易安爱富科技有限公司 | The etchant of copper/molybdenum film or copper/molybdenum alloy film |
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