CN108780747A - Etchant and engraving method - Google Patents

Etchant and engraving method Download PDF

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Publication number
CN108780747A
CN108780747A CN201780019215.XA CN201780019215A CN108780747A CN 108780747 A CN108780747 A CN 108780747A CN 201780019215 A CN201780019215 A CN 201780019215A CN 108780747 A CN108780747 A CN 108780747A
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etchant
mass
filament
etching
ingredient
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CN108780747B (en
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大宫大辅
青木珠美
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Adeka Corp
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Asahi Denka Kogyo KK
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Priority claimed from JP2016059470A external-priority patent/JP6662671B2/en
Priority claimed from JP2016089354A external-priority patent/JP2017199791A/en
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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
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/10—Etching compositions
    • C23F1/14—Aqueous compositions
    • C23F1/16—Acidic compositions
    • C23F1/18—Acidic compositions for etching copper or alloys thereof
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    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
    • H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
    • H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
    • H01L21/308—Chemical or electrical treatment, e.g. electrolytic etching using masks
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
    • H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
    • H—ELECTRICITY
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    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
    • H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
    • H01L21/321—After treatment
    • H01L21/3213—Physical or chemical etching of the layers, e.g. to produce a patterned layer from a pre-deposited extensive layer
    • H—ELECTRICITY
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    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
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    • H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
    • H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
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    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/52—Arrangements for conducting electric current within the device in operation from one component to another, i.e. interconnections, e.g. wires, lead frames
    • H01L23/522—Arrangements for conducting electric current within the device in operation from one component to another, i.e. interconnections, e.g. wires, lead frames including external interconnections consisting of a multilayer structure of conductive and insulating layers inseparably formed on the semiconductor body
    • H01L23/532—Arrangements for conducting electric current within the device in operation from one component to another, i.e. interconnections, e.g. wires, lead frames including external interconnections consisting of a multilayer structure of conductive and insulating layers inseparably formed on the semiconductor body characterised by the materials

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Abstract

A kind of etchant, even if not containing hydrogen chloride, the etching also for the indium oxide system layer that can form following filaments is useful, and the filament attenuates caused by etching, and width is few, linearity is good and there is desired width, the etchant to contain：(A) mass of hydrogen peroxidase 10 .01~15 %；(B) 1~40 mass % of sulfuric acid；(C) (C-1) the following general formula (1) (R1、R2And R3：The alkyl etc. of hydrogen, carbon atom number 1~8) shown in 0.01~20 mass % of 0.01~10 mass % of amide compound or (C-2) amino-acid compound；And water.

Description

Etchant and engraving method
Technical field
The present invention relates to etchant and use its engraving method.More specifically, it is directed to indium oxide It is that layer is etched and the etchant that uses and uses its engraving method.
Background technology
It is known with transparent conductive film etc. in the related various technologies of the wet etching of indium oxide system layer that uses.Wherein, by It is good in cheap and etching speed, thus use the aqueous solution comprising hydrochloric acid as etchant more.
For example, Patent Document 1 discloses indium-tin-oxide (being also denoted as below " ITO ") containing iron chloride and hydrochloric acid Use etchant.
In addition, disclosing the etching as copper or copper alloy as the etching solution without using hydrochloric acid, such as in patent document 2 Agent, aqueous solution containing copper ion, organic acid, halide ion, pyrroles and polyalkylene glycol.
Existing technical literature
Patent document
Patent document 1：Japanese Unexamined Patent Publication 2009-231427 bulletins
Patent document 2：Japanese Unexamined Patent Publication 2006-111953 bulletins
Invention content
Problems to be solved by the invention
However, using the etching solution containing hydrogen chloride as etchant disclosed in Patent Document 1, to ITO When layer or the laminated body being made of ITO layer and layers of copper are disposably etched, it may appear that following problem：Be easy to happen base material, The discoloration of surrounding member；Base material, surrounding member surface roughening；Metal component is dissolved out from base material, surrounding member surface；And The linearity for being formed by filament is bad etc..
In addition, using the etching solution for not containing hydrogen chloride as etchant disclosed in Patent Document 2, to ITO layer or When the laminated body being made of ITO layer and layers of copper is disposably etched, it may appear that following problem：It is meticulous to be formed by filament, It is difficult to form the filament of desired width, and the linearity of filament reduces or generates defect on filament top.In turn, filament it Between etching after when continuing etching process, further leading to the problem of significantly to attenuate on filament can also become.
Therefore, the present invention makes to solve the above-mentioned problems, and project is to provide a kind of etchant, Even if the etchant does not contain hydrogen chloride, the etching also for the indium oxide system layer that can form following filaments is useful, The filament attenuates caused by etching, and width is few, linearity is good and has desired width.
In addition, the purpose of the present invention is to provide a kind of etchant, even if the etchant does not contain Hydrogen chloride, can also be formed caused by etching the width that attenuates is few, can inhibit filament top generate defect, with the thin of desired width Line, etching even if between filament after, can inhibit attenuating for filament continuing etching process.In turn, of the invention Project be to provide a kind of engraving method having used above-mentioned etchant.
The solution to the problem
The inventors of the present invention have made intensive studies to solve the above-mentioned problems, as a result, it has been found that the etching containing special component Liquid composition can solve the above problems, so that complete the present invention.
That is, according to the present invention, a kind of etchant is provided, is used to be etched indium oxide system layer, the erosion Liquid composition is carved to contain：(A) mass of hydrogen peroxidase 10 .01~15 %；(B) 1~40 mass % of sulfuric acid；(C) (C-1) the following general formula (1) 0.01~20 mass % of 0.01~10 mass % of amide compound or (C-2) amino-acid compound shown in；And water.
(in aforementioned formula (1), R1、R2And R3Separately indicate hydrogen, the alkyl of carbon atom number 1~8, carbon atom number 2 ~8 alkenyl can be by the aryl of the alkyl-substituted carbon atom number 6~8 of carbon atom number 1 or 2)
Amino-acid compound is preferably selected to be made of glutamic acid, the following general formula (2) compound represented and their salt Group in it is at least one kind of.In addition, amino-acid compound is preferably selected from the group being made of glutamic acid, tyrosine and phenylalanine In it is at least one kind of.
(in aforementioned formula (2), R1Indicate hydrogen atom or the alkyl of carbon atom number 1~4, R2Indicate hydrogen atom, hydroxyl, halogen Atom or nitro, A indicate that the alkane diyl of carbon atom number 1~4, n indicate 1~5 number)
In the present invention, preferably also contain (D) halide ion supply source.
In addition, according to the present invention, a kind of engraving method is provided, with following process：Use above-mentioned etchant Indium oxide system layer is etched.
The effect of invention
According to the present invention it is possible to a kind of etchant be provided, even if hydrogen chloride is not contained, also for it can be formed under The etching for stating the indium oxide system layer of filament is useful, and the filament attenuates caused by etching, and width is few, linearity is good and has Desired width.
In addition, according to the present invention it is possible to provide a kind of etchant, the thin portion width caused by etching can be formed Less, can inhibit and generate defect, with the filament of desired width on filament top, though continue after etching between filament into Row etching process can also inhibit attenuating for filament.Even if the etchant of the present invention is to indium oxide system layer and metal system Layer also plays said effect in the case of being etched together.Therefore, etchant of the invention be suitable as pair The etching solution that the laminated body being made of indium oxide system layer and metal system layer is etched together.In turn, according to the present invention it is possible to carry For having used the engraving method of above-mentioned etchant.
Specific implementation mode
Embodiments of the present invention are specifically explained below." etching " in this specification refers to that chemistry is utilized The method of the moulding or surface processing of the corrosiveness of drug etc..The specific purposes of etchant as the present invention, Such as it can enumerate：Remover, rough surface agent, pattern formation chemical reagent, micro is attached to matrix at smooth surface agent On ingredient cleaning solution etc..The etchant of the present invention can be fitted since the removal speed of the layer containing indium oxide is fast Preferably it is used as remover.In addition, when being used to form the fine shape pattern with three-dimensional structure, rectangle etc. can be obtained and it is expected shape The pattern of shape, therefore pattern formation chemical reagent can also be suitable for use as.
" indium oxide system layer " in this specification as long as the layer of indium oxide as long as including be not particularly limited." indium oxide system Layer " is, for example, by the general name of the layer constituted selected from one or more of indium oxide, indium-tin-oxide and indium-zinc oxide.
" metal system layer " in this specification is not particularly limited as long as layer made of metal." metal system layer " example In this way by representated by the metal layers such as copper, nickel, titanium, chromium, silver, molybdenum, platinum, palladium, CuNi, CuNiTi, NiCr, Ag-Pd-Cu etc. The general name for the layer that one or more of metal alloy is constituted.
Using the etchant of the present invention, place is etched together to the laminated body of indium oxide system layer and metal system layer When reason, metal system layer is preferably the conductive layer containing 10 mass % of copper or more.As the conductive layer containing 10 mass % of copper or more, Such as it can enumerate：The conductive layer that is formed by metallic copper is formed by copper alloys such as CuNi, CuNiTi, NiCr, Ag-Pd-Cu Conductive layer etc..In turn, indium oxide system layer is the layer containing indium-tin-oxide and metal system layer is to contain 10 mass % of copper or more When layer, desired filament can be formed with higher precision and etching speed is also fast, so it is preferred that.
The etchant of the present invention contains (A) hydrogen peroxide (being also denoted as below " (A) ingredient ").Etchant In (A) ingredient a concentration of 0.01~15 mass % range.(A) when the concentration of ingredient is less than 0.01 mass %, etching speed Degree becomes too slow and productivity is made to significantly reduce.On the other hand, when the concentration of (A) ingredient is more than 15 mass %, etching speed becomes Obtain too fast and uncontrollable etching speed.(A) concentration of ingredient is preferably the range of 0.1~12 mass %, and more preferably 1~10 The range of quality %.
The etchant of the present invention contains (B) sulfuric acid (being also denoted as below " (B) ingredient ").In etchant (B) range of a concentration of 1~40 mass % of ingredient.(B) when the concentration of ingredient is less than 1 mass %, etching speed becomes too slow And productivity is made to reduce.On the other hand, when the concentration of (B) ingredient is more than 40 mass %, etching speed becomes too fast and difficult sometimes To control etching speed or make the deteriorations such as the component, the resist that are etched body periphery sometimes.(B) concentration of ingredient be preferably 5~ The range of 30 mass %, the more preferably range of 10~25 mass %.
The etchant of the present invention contains amide compound shown in (C) (C-1) the following general formula (1) (also to be remembered below For " (C-1) ingredient ") or (C-2) amino-acid compound (being also denoted as below " (C-2) ingredient ").It should be noted that by (C- 1) ingredient and (C-2) ingredient are referred to as " (C) ingredient ".
In general formula (1), R1、R2And R3Separately indicate hydrogen, the alkyl of carbon atom number 1~8, carbon atom number 2~8 Alkenyl can be by the aryl of the alkyl-substituted carbon atom number 6~8 of carbon atom number 1 or 2.Alkane as carbon atom number 1~8 Base, such as can enumerate：Methyl, ethyl, propyl, isopropyl, butyl, sec-butyl, tertiary butyl, isobutyl group, amyl, isoamyl Base, tertiary pentyl, hexyl, 2- hexyls, 3- hexyls, cyclohexyl, 1- methylcyclohexyls, heptyl, 2- heptyl, 3- heptyl, different heptyl, uncle Heptyl, n-octyl, iso-octyl, t-octyl, 2- ethylhexyls etc..
As the alkenyl of carbon atom number 2~8, such as can enumerate：Vinyl, 1- methyl ethylenes, 2- ethylene methacrylics Base, acrylic, cyclobutenyl, isobutenyl, pentenyl, hexenyl, heptenyl, octenyl etc..
As can be by the aryl of the alkyl-substituted carbon atom number 6~8 of carbon atom number 1 or 2, such as can enumerate： Phenyl, 2- aminomethyl phenyls, 3- aminomethyl phenyls, 4- aminomethyl phenyls, 2,3- 3,5-dimethylphenyls, 2,4- 3,5-dimethylphenyls, 2,5- diformazans Base phenyl, 2,6- 3,5-dimethylphenyls, 3,4- 3,5-dimethylphenyls, 3,5- 3,5-dimethylphenyls etc..
As the preferred specific example of amide compound shown in general formula (1), can enumerate：Formamide, acetamide, Propionamide, butyramide, N,N-dimethylformamide, N-METHYLFORMAMIDE, N, N- diethylformamides, Methacrylamide, third Acrylamide, N- phenyl formamides, benzamide, N- methylacetamides, DMAC N,N' dimethyl acetamide etc..Wherein, using formamide In the case of, the width of corrosion-resisting pattern and the difference (deviation) of the width of filament for being etched and being formed become smaller and are formed The linearity of filament further improve, so it is preferred that.
The range of a concentration of 0.01~10 mass % of (C-1) ingredient in etchant.(C-1) concentration of ingredient When less than 0.01 mass %, the linearity of filament for being etched and being formed reduces.On the other hand, the concentration of (C-1) ingredient is super When crossing 10 mass %, etching speed becomes too slow and productivity is made to significantly reduce.(C-1) concentration of ingredient is preferably 0.05~5 The range of quality %, the more preferably range of 0.1~1 mass %.
As long as amino-acid compound is respectively provided with the compound of 1 or more amino and carboxyl, can use known Common amino-acid compound.As the specific example of amino-acid compound, can enumerate：Glycine, alanine, figured silk fabrics ammonia Acid, leucine, serine, phenylalanine, tryptophan, glutamic acid, aspartic acid, lysine, arginine, histidine, tyrosine, Methionine, 4- chlorophenylalanines, 4- bromophenyl alanines, 4- nitrophenylalanines, 3- (3,4- dihydroxy phenyls) alanine, α-first The salt etc. of base phenylalanine and they.As above-mentioned salt, such as can enumerate：Alkali metal salt, ammonium salt etc..These amino are acidified Object is closed to can be used alone or two or more is applied in combination.
As amino-acid compound, it is preferable to use selected from by glutamic acid, the following general formula (2) compound represented and they It is at least one kind of in the group of salt composition.By making to contain these amino-acid compounds in etchant, and make to indium oxide system Layer is etched the width smaller that attenuates for being formed by filament, can efficiency form the filament of desired width well.Into And can more effectively inhibit to generate defect on filament top, and even if etching between filament after continue to etch In the case of processing, it also can more effectively inhibit the deterioration of filament, so it is preferred that.In particular, as amino-acid compound, it is excellent Choosing uses at least one kind of in the group being made of glutamic acid, tyrosine and phenylalanine.
In general formula (2), R1Indicate hydrogen atom or the alkyl of carbon atom number 1~4.As the alkyl of carbon atom number 1~4, example It can such as enumerate：Methyl, ethyl, propyl, butyl, sec-butyl, tertiary butyl etc..
In general formula (2), R2Indicate hydrogen atom, hydroxyl, halogen atom or nitro.As halogen atom, such as can enumerate Go out：Fluorine atom, chlorine atom, bromine atom etc..
In general formula (2), A indicates the alkane diyl of carbon atom number 1~4.As the alkane diyl of carbon atom number 1~4, such as can be with It enumerates：Methylene, ethylidene, butylidene etc..
In general formula (2), (i) R1For hydrogen atom or methyl；(ii)R2For hydrogen atom or hydroxyl；Or (iii) A is methylene When, make to be etched indium oxide system layer and the width smaller that attenuates of filament that is formed, can efficiency form the phase well Hope the filament of width.In turn, can more effectively inhibit that defect occurs on filament top, and even if the etching between filament terminates After continue in the case of being etched, also can more effectively inhibit the deterioration of filament, so it is preferred that.In addition, general formula (2) In, n is preferably 1 or 2.
The range of a concentration of 0.01~20 mass % of (C-2) ingredient in etchant.(C-2) concentration of ingredient When less than 0.01 mass %, the width increase that attenuates for being formed by filament is etched to indium oxide system layer.On the other hand, even if The concentration of (C-2) ingredient is set as more than 20 mass %, effect will not improve as obtained from compounding (C-2) ingredient.(C- 2) concentration of ingredient is preferably the range of 0.05~15 mass %, more preferably the range of 0.1~10 mass %.
The etchant of the present invention contain water as in addition to (A) ingredient, (B) ingredient and (C) ingredient must be at Point.In addition, within the scope of the effect of the invention, well known addition can be compounded in etchant of the invention Agent is as the ingredient in addition to (A) ingredient, (B) ingredient, (C) ingredient and water.As additive, can enumerate：Etching solution group The stabilization agent of object, the solubilizer of each ingredient, antifoaming agent, pH adjusting agent, proportion conditioning agent, viscosity modifier, wettability is closed to change Kind agent, chelating agent, oxidant, reducing agent, surfactant etc..The concentration of these additives is usually 0.001~50 mass % Range.
As chelating agent, such as can enumerate：Ethylenediamine tetra-acetic acid, diethylene-triamine pentaacetic acid, triethylene four Hexaacetic acid, TPHA tetraethylenepentaamine heptaacetic acid, eight acetic acid of penten, nitrilotriacetic acid and their alkali metal are (excellent It is selected as sodium) the amino carboxylic acids system chelating agent such as salt；1-hydroxy ethylidene-1,1-diphosphonic acid, nitrilo trimethylene phosphonic acids, phosphonobutane tricarboxylic acids With the phosphonic acids system chelating agent such as their alkali metal (preferably sodium) salt；Oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, heptan Diacid, maleic acid, fumaric acid, malic acid, tartaric acid, citric acid, their acid anhydrides and their alkali metal (preferably sodium) salt Monoester anhydride or dicarboxylic anhydride made of carboxylic acid compound dehydration Deng 2 yuan or more of carboxylic acid compounds or 2 yuan or more.These chelatings The concentration of agent is usually the range of 0.01~40 mass %.
When etching speed is fast, reducing agent is preferably used as additive.As the specific example of reducing agent, can enumerate： Copper chloride, frerrous chloride, copper powder, silver powder etc..The concentration of these reducing agents is usually the range of 0.01~10 mass %.
It preferably further (is also denoted as below containing (D) halide ion supply source in the etchant of the present invention " (D) ingredient ").For example, when forming filament by etching, by further containing (D) ingredient, so as to make corrosion-resisting pattern Width and be etched and difference (deviation) smaller of the width of filament for being formed.
As the halide ion of halide ion supply source supply, can enumerate：Chloride ion, bromide from Son, iodide ion etc..As halide ion supply source, the water soluble salt containing halide ion can be used for example.Make For the specific example of the water soluble salt containing halide ion, can enumerate：The halide salts such as sodium chloride, potassium chloride；Chlorination Ammonium etc..When wherein, using halide salts, it can be etched with more good speed, so it is preferred that, further preferred alkali metal Chloride salt, particularly preferred sodium chloride.
The concentration of (D) ingredient in etchant is preferably the range of 0.00001~0.1 mass %.(D) ingredient When concentration is less than 0.00001 mass %, it is unable to get the compound effects of (D) ingredient sometimes.On the other hand, even if by (D) ingredient Concentration be set as more than 0.1 mass %, the compound effects of (D) ingredient will not further increase.(D) concentration of ingredient is excellent in turn It is selected as the range of 0.0001~0.01 mass %.
The engraving method of the present invention has following process：Using the etchant of the above-mentioned present invention to indium oxide system Layer is etched.As long as using the etchant of the present invention, it can be to by indium oxide system layer and the layer that constitutes of metal system layer Stack is etched together.The indium oxide system layer of composition laminated body can be 1 layer and can also be 2 layers or more.In addition, constituting stacking The metal system layer of body can also be 1 layer and can also be 2 layers or more.For laminated body, metal system layer can be only fitted to indium oxide system The upper layer of layer, can be only fitted to lower layer, can also configure in the upper and lower.In turn, indium oxide system can also be alternately laminated Layer and metal system layer.
The method being etched together to the laminated body of indium oxide system layer, indium oxide system layer and metal system layer does not limit especially It is fixed, using common engraving method.Such as it can enumerate：Etching based on the progress such as impregnated, atomizing, spin-coating Method.For example, when the engraving method using impregnated has Cu/ITO layers of base material to be etched to forming a film on pet substrate, Lift after the base material is immersed in etchant under suitable etching condition, so as to the Cu/ on pet substrate ITO layer is etched together.
Etching condition in the engraving method of impregnated is not particularly limited, according to the shape of base material (being etched body), film The progress such as thickness are arbitrarily set.For example, etch temperature is preferably 10~60 DEG C, further preferably 20~40 DEG C.Etching The temperature of liquid composition rises because of reaction heat sometimes.Therefore, as needed, well known means can also be utilized into trip temperature control System, the temperature of etchant is maintained within the above range.In addition, etching period is set as being enough to make when etching completes Between, it is not particularly limited.For example, when manufacturing the wiring of electronic circuit board, if film thickness is 5~500nm or so, upper State the etching of progress 10~600 seconds or so in temperature range.
When thering is Cu/ITO layers of base material to be etched to forming a film on pet substrate using aerosol engraving method, pass through Etchant is sprayed on base material under the suitable conditions, so as to be lost to the Cu/ITO layers on pet substrate It carves.
Etching condition in aerosol engraving method is not particularly limited, according to shape, film thickness for being etched body etc. into Row is arbitrarily set.For example, spray condition can be selected from the range of 0.01~1.0MPa, preferably 0.02~0.5MPa's The range of range and then preferably 0.05~0.2MPa.In addition, etch temperature is preferably 10~60 DEG C, is more preferably 20 ~40 DEG C.The temperature of etchant rises because of reaction heat sometimes.Therefore, as needed, well known hand can also be utilized Section is controlled into trip temperature, and the temperature of etchant is maintained within the above range.In addition, etching period is set as being enough to make The time completed is etched, is not particularly limited.For example, manufacture electronic circuit board wiring when, if film thickness be 5~ 500nm or so then carries out etching in 5~600 seconds or so within the said temperature range.
For the engraving method of the present invention, in order to make due to repeating to etch and the performance of the etchant of deterioration Restored, preferably further there is the process that bulking liquor is added in etchant.For example, automatic control as described above In the case of the engraving method of standard, as long as pre-setting bulking liquor in Etaching device, so that it may in etchant Add bulking liquor.The aqueous solution containing (A) ingredient, (B) ingredient, (C) ingredient and water can be used for example in bulking liquor；Or contain (C) aqueous solution etc. of ingredient and water.Each constituent concentration in these aqueous solutions (bulking liquor) is for example set as in etchant 3~20 times or so of each constituent concentration.In addition, the etching in the present invention can also be added in bulking liquor as needed The aforesaid components contained as essential component or as optional member in liquid composition.
The present invention etchant and used the engraving method of the etchant can be suitably main To the electrode of liquid crystal display, plasma scope, touch screen, organic EL, solar cell, luminaire etc., connect up into It is used when row processing.
Embodiment
The present invention is described in detail following with embodiment and comparative example, but the present invention is not limited to these.
<Etchant (1)>
(embodiment I-1~12)
Using amide compound shown in table 1, each ingredient is mixed in a manner of as being formulated shown in table 2 for each ingredient And obtain etchant (embodiment I-1~12).It should be noted that by ingredient add up to 100 mass % in a manner of It is compounded with water.
Table 1
Amide compound A Formamide
Amide compound B Acetamide
Amide compound C Propionamide
Amide compound D N-METHYLFORMAMIDE
Table 2
(Comparative Example I -1~5)
Each ingredient is mixed in a manner of as being formulated shown in table 3 for each ingredient and obtains etchant and (compares Example I-1~5).It should be noted that by ingredient add up to 100 mass % in a manner of be compounded with water.
Table 3
<Engraving method (1)>
(embodiment I-13~24)
For stacking gradually matrix made of ITO layer (15nm) and Cu layers (400nm) on glass matrix, eurymeric liquid is used State resist form 30 μm of width, 30 μm of opening portion corrosion-resisting pattern.The matrix cut growth of corrosion-resisting pattern will be formd 20mm × wide 20mm and obtain test film.For obtained test film, using the etchant of embodiment I-1~12, 35 DEG C, 1 minute, stirring under carry out foring filament based on the etching process of impregnated.
(Comparative Example I -6~10)
For stacking gradually matrix made of ITO layer (15nm) and Cu layers (400nm) on glass matrix, eurymeric liquid is used State resist form 30 μm of width, 30 μm of opening portion corrosion-resisting pattern.The matrix cut growth of corrosion-resisting pattern will be formd 20mm × wide 20mm and obtain test film.For obtained test film, using the etchant of Comparative Example I -1~5,35 DEG C, 1 minute, stirring under carry out foring filament based on the etching process of impregnated.
<It evaluates (1)>
The deviation of the linearity of filament and the width of the width of corrosion-resisting pattern and filament is carried out using laser microscope Evaluation.It for the linearity of filament, will confirm that filament is evaluated as "-" in winding situation, will not can confirm that filament is in Winding situation is evaluated as "+".In addition, the deviation of the width of width and filament for corrosion-resisting pattern, is based on following formula (A) absolute value of the difference " L of the width of the corrosion-resisting pattern before etching process and the width on the filament top of formation is calculated1" add With evaluation."L1" value when being " 0 ", the filament of corrosion-resisting pattern width and formation before etching process is of same size, it is meant that shape At the filament of desired width.On the other hand, " L1" the more big then etching process of value before corrosion-resisting pattern width and formation it is thin The difference of line width is bigger, illustrates the filament for not forming desired width.Evaluation result is shown in table 4.
L1=│ (width of the corrosion-resisting pattern before etching process)-(width on the filament top of formation) │ ... (A)
Table 4
Composition Linearity L1/μm
Comparative Example I -6 Comparative Example I -1 + 12
Comparative Example I -7 Comparative Example I -2 ※1 ※1
Comparative Example I -8 Comparative Example I -3 ※1 ※1
Comparative Example I -9 Comparative Example I -4 - 21
Comparative Example I -10 Comparative Example I -5 - 18
Embodiment I-13 Embodiment I-1 + 3
Embodiment I-14 Embodiment I-2 + 2
Embodiment I-15 Embodiment I-3 + 5
Embodiment I-16 Embodiment I-4 + 1
Embodiment I-17 Embodiment I-5 + 4
Embodiment I-18 Embodiment I-6 + 6
Embodiment I-19 Embodiment I-7 + 6
Embodiment I-20 Embodiment I-8 + 1
Embodiment I-21 Embodiment I-9 + 0
Embodiment I-22 Embodiment I-10 + 2
Embodiment I-23 Embodiment I-11 + 3
Embodiment I-24 Embodiment I-12 + 3
※1：It is almost totally insoluble to be etched body.
Result as shown in Table 4 has been respectively formed the good filament of linearity it is found that in embodiment I-13~24.In addition, real It applies in I-13~24, " the L compared with Comparative Example I -1~51" value it is small, the filament of desired width can be formed.Embodiment I-13 In~19, " L in embodiment I-13, I-14 and I-161" value it is especially small.In addition, it is appreciated that containing (D) for having used Embodiment I-20~24 of the etchant of embodiment I-8~12 of ingredient, and have used the implementation without containing (D) ingredient Embodiment I-13~19 of the etchant of example I-1~7 are compared, " L1" value reduce 50% or so.
<Etchant (2)>
(embodiment II-1~9)
Using amino-acid compound shown in table 5, each ingredient is mixed in a manner of as being formulated shown in table 6 and is lost Carve liquid composition (embodiment II-1~9).It should be noted that by ingredient add up to 100 mass % in a manner of be compounded with water.
Table 5
Amino acid A Glutamic acid
Amino acid B Tyrosine
Amino acid C Phenylalanine
Amino acid D Methionine
Amino acid E Glycine
Amino acid F Aspartic acid
Table 6
(Comparative Example I I-1~5)
Each ingredient is mixed in a manner of as being formulated shown in table 7 and obtains etchant (Comparative Example I I-1~5). It should be noted that by ingredient add up to 100 mass % in a manner of be compounded with water.
Table 7
<Engraving method (2)>
(embodiment II-10~18)
For stacking gradually matrix made of ITO layer (15nm) and Cu layers (400nm) on glass matrix, eurymeric liquid is used State resist form 10 μm of width, 10 μm of opening portion corrosion-resisting pattern.The matrix cut growth of corrosion-resisting pattern will be formd 20mm × wide 20mm and obtain test film.For obtained test film, using the etchant of embodiment II-1~9, 35 DEG C, the pattern etching (etching process) based on spray-on process has been carried out under conditions of atomisation pressure 0.05MPa.It is etched Until residue between it can confirm wiring by visual observation disappears.It should be noted that in this specification " when most suitable etching Between " refer to " etch processes time until the residue between wiring disappears ".
(Comparative Example I I-6~10)
The etchant of Comparative Example I I-1~5 is used, in addition to this in the same manner as above-described embodiment II-10~18 The pattern etching based on spray-on process is carried out.
<It evaluates (2)>
The deviation of the state of filament and the width of the width of corrosion-resisting pattern and filament is commented using laser microscope Valence.For the state of filament, evaluated by confirming whether there is or not the defects of 3 μm or more length in the corner of filament.It is specific and Speech, will be it is observed that the case where 3 μm or more length defects, be evaluated as "+", will be it is observed that the case where 3 μm or more length defects It is evaluated as "-".In addition, the deviation of the width of width and filament for corrosion-resisting pattern, calculates the resist pattern before etching process Absolute value of the difference " the L of the width of case and the width on the filament top of formation1" evaluated."L1" value " 0 " be when, etching The width of corrosion-resisting pattern before processing and the filament of formation it is of same size, it is meant that form the filament of desired width.It is another Aspect, " L1" the more big then etching process of value before corrosion-resisting pattern width and formation filament width difference it is bigger, meaning The filament for not forming desired width.In addition, by " L1" value be less than 3 μm the case where be evaluated as "+", by " L1" value be 3 μm with On situation be evaluated as "-".It will be evaluation result is shown in table 8.
Table 8
Composition The state of filament L1Evaluation
Comparative Example I I-6 Comparative Example I I-1 + -
Comparative Example I I-7 Comparative Example I I-2 ※1 ※1
Comparative Example I I-8 Comparative Example I I-3 ※1 ※1
Comparative Example I I-9 Comparative Example I I-4 - -
Comparative Example I I-10 Comparative Example I I-5 ※1 ※1
Embodiment II-10 Embodiment II-1 + +
Embodiment II-11 Embodiment II-2 + +
Embodiment II-12 Embodiment II-3 + +
Embodiment II-13 Embodiment II-4 + +
Embodiment II-14 Embodiment II-5 + +
Embodiment II-15 Embodiment II-6 + +
Embodiment II-16 Embodiment II-7 + +
Embodiment II-17 Embodiment II-8 + +
Embodiment II-18 Embodiment II-9 + +
※1：It is almost totally insoluble to be etched body.
Result as shown in Table 8 etches it is found that do not confirm the defect of 3 μm or more length in embodiment II-10~18 Treated, and detail mode is good.In addition, understanding " L in embodiment II-10~181" value be below 3 μm.According to the above knot Fruit, it is known that if using the etchant of the present invention, even if being etched together to indium oxide system layer and metal system layer In the case of processing, it can also inhibit that defect occurs on filament top, and the filament of desired width can be formed.
<Engraving method (3)>
(embodiment II-19~27)
Etch processes time is set as 2 times of most suitable etching period, it is same as previous embodiment II-10~18 in addition to this Ground has carried out the etching of the pattern based on spray-on process.
(Comparative Example I I-11~15)
The etchant of Comparative Example I I-1~5 is used, in addition to this in the same manner as above-described embodiment II-19~27 The pattern etching based on spray-on process is carried out.
<It evaluates (3)>
" L is calculated using laser microscope1", have rated the deviation of the width of corrosion-resisting pattern and the width of filament.By " L1” Value be less than 5 μm the case where be evaluated as " ++ ", by " L1" value be 5~10 μm the case where be evaluated as "+", by " L1" value be more than 10 μm of the case where, are evaluated as "-".It will be evaluation result is shown in table 9.
Table 9
Composition L1Evaluation
Comparative Example I I-11 Comparative Example I I-1 -
Comparative Example I I-12 Comparative Example I I-2 ※2
Comparative Example I I-13 Comparative Example I I-3 ※2
Comparative Example I I-14 Comparative Example I I-4 -
Comparative Example I I-15 Comparative Example I I-5 ※2
Embodiment II-19 Embodiment II-1 ++
Embodiment II-20 Embodiment II-2 ++
Embodiment II-21 Embodiment II-3 ++
Embodiment II-22 Embodiment II-4 ++
Embodiment II-23 Embodiment II-5 ++
Embodiment II-24 Embodiment II-6 ++
Embodiment II-25 Embodiment II-7 +
Embodiment II-26 Embodiment II-8 +
Embodiment II-27 Embodiment II-9 +
※2：It is almost totally insoluble to be etched body.
Result as shown in Table 9 is it is found that in embodiment II-19~27, although to be more than substantially the side of most suitable etching period Formula is etched, but can also form the filament of desired width, therefore process window is extensive.Wherein, it is known that, it is real Attenuating for filament can substantially be inhibited by applying in II-19~24, therefore the etchant of embodiment II-1~6 is especially excellent Different etching solution.

Claims (5)

1. a kind of etchant is used to be etched indium oxide system layer, the etchant contains：
(A) mass of hydrogen peroxidase 10 .01~15 %；
(B) 1~40 mass % of sulfuric acid；
(C) 0.01~10 mass % of amide compound or (C-2) amino-acid compound 0.01 shown in (C-1) the following general formula (1) ~20 mass %；And
Water,
In the general formula (1), R1、R2And R3Separately indicate hydrogen, the alkyl of carbon atom number 1~8, carbon atom number 2~8 Alkenyl can be by the aryl of the alkyl-substituted carbon atom number 6~8 of carbon atom number 1 or 2.
2. etchant according to claim 1, wherein the amino-acid compound be selected from by glutamic acid, under State general formula (2) compound represented and they salt form group in it is at least one kind of,
In the general formula (2), R1Indicate hydrogen atom or the alkyl of carbon atom number 1~4, R2Indicate hydrogen atom, hydroxyl, halogen atom, Or nitro, A indicate that the alkane diyl of carbon atom number 1~4, n indicate 1~5 number.
3. etchant according to claim 1 or 2, wherein the amino-acid compound be selected from by glutamic acid, It is at least one kind of in the group of tyrosine and phenylalanine composition.
4. etchant according to claim 1, wherein also contain (D) halide ion supply source.
5. a kind of engraving method, with following process：Use the etchant described in any one of Claims 1 to 44 Indium oxide system layer is etched.
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