CN115679327A - Etching solution composition for silver-containing metal film - Google Patents
Etching solution composition for silver-containing metal film Download PDFInfo
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- CN115679327A CN115679327A CN202210852111.XA CN202210852111A CN115679327A CN 115679327 A CN115679327 A CN 115679327A CN 202210852111 A CN202210852111 A CN 202210852111A CN 115679327 A CN115679327 A CN 115679327A
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- Prior art keywords
- silver
- acid
- containing metal
- etching solution
- composition
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- 238000005530 etching Methods 0.000 title claims abstract description 109
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 102
- 239000002184 metal Substances 0.000 title claims abstract description 102
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 100
- 239000004332 silver Substances 0.000 title claims abstract description 100
- 239000000203 mixture Substances 0.000 title claims abstract description 87
- -1 salt compound Chemical class 0.000 claims abstract description 57
- 150000007524 organic acids Chemical class 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 25
- 239000002253 acid Substances 0.000 claims description 24
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 19
- 229910017604 nitric acid Inorganic materials 0.000 claims description 19
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 18
- 239000002356 single layer Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 15
- 229910001316 Ag alloy Inorganic materials 0.000 claims description 15
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 12
- 125000004432 carbon atom Chemical group C* 0.000 claims description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 12
- 239000010410 layer Substances 0.000 claims description 12
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 claims description 8
- 239000010955 niobium Substances 0.000 claims description 8
- 229910052797 bismuth Inorganic materials 0.000 claims description 7
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 7
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 claims description 7
- VSZWPYCFIRKVQL-UHFFFAOYSA-N selanylidenegallium;selenium Chemical compound [Se].[Se]=[Ga].[Se]=[Ga] VSZWPYCFIRKVQL-UHFFFAOYSA-N 0.000 claims description 7
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 claims description 6
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 6
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 6
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 229910052770 Uranium Inorganic materials 0.000 claims description 4
- 229910017052 cobalt Inorganic materials 0.000 claims description 4
- 239000010941 cobalt Substances 0.000 claims description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 4
- 229910052735 hafnium Inorganic materials 0.000 claims description 4
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims description 4
- 229940098779 methanesulfonic acid Drugs 0.000 claims description 4
- 229910052758 niobium Inorganic materials 0.000 claims description 4
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 4
- 229910052763 palladium Inorganic materials 0.000 claims description 4
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 claims description 4
- YVTHLONGBIQYBO-UHFFFAOYSA-N zinc indium(3+) oxygen(2-) Chemical compound [O--].[Zn++].[In+3] YVTHLONGBIQYBO-UHFFFAOYSA-N 0.000 claims description 4
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 3
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 3
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 3
- 229910052783 alkali metal Inorganic materials 0.000 claims description 3
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 3
- 150000003863 ammonium salts Chemical class 0.000 claims description 3
- CCIVGXIOQKPBKL-UHFFFAOYSA-M ethanesulfonate Chemical compound CCS([O-])(=O)=O CCIVGXIOQKPBKL-UHFFFAOYSA-M 0.000 claims description 3
- 229910052733 gallium Inorganic materials 0.000 claims description 3
- 239000004310 lactic acid Substances 0.000 claims description 3
- 235000014655 lactic acid Nutrition 0.000 claims description 3
- KCXFHTAICRTXLI-UHFFFAOYSA-N propane-1-sulfonic acid Chemical compound CCCS(O)(=O)=O KCXFHTAICRTXLI-UHFFFAOYSA-N 0.000 claims description 3
- 235000002906 tartaric acid Nutrition 0.000 claims description 3
- 239000011975 tartaric acid Substances 0.000 claims description 3
- 239000011787 zinc oxide Substances 0.000 claims description 3
- 238000011109 contamination Methods 0.000 abstract description 8
- 239000010408 film Substances 0.000 description 105
- 239000010409 thin film Substances 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 9
- 239000000758 substrate Substances 0.000 description 9
- 239000000356 contaminant Substances 0.000 description 7
- 238000001179 sorption measurement Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 230000003247 decreasing effect Effects 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 229910052750 molybdenum Inorganic materials 0.000 description 3
- 239000011733 molybdenum Substances 0.000 description 3
- 239000007800 oxidant agent Substances 0.000 description 3
- 229920002120 photoresistant polymer Polymers 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 2
- 239000002738 chelating agent Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 229910000449 hafnium oxide Inorganic materials 0.000 description 2
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910000166 zirconium phosphate Inorganic materials 0.000 description 2
- ZXAUZSQITFJWPS-UHFFFAOYSA-J zirconium(4+);disulfate Chemical compound [Zr+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZXAUZSQITFJWPS-UHFFFAOYSA-J 0.000 description 2
- LEHFSLREWWMLPU-UHFFFAOYSA-B zirconium(4+);tetraphosphate Chemical compound [Zr+4].[Zr+4].[Zr+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LEHFSLREWWMLPU-UHFFFAOYSA-B 0.000 description 2
- WWILHZQYNPQALT-UHFFFAOYSA-N 2-methyl-2-morpholin-4-ylpropanal Chemical compound O=CC(C)(C)N1CCOCC1 WWILHZQYNPQALT-UHFFFAOYSA-N 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229940011182 cobalt acetate Drugs 0.000 description 1
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 description 1
- 229910003437 indium oxide Inorganic materials 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 159000000014 iron salts Chemical class 0.000 description 1
- GQYHUHYESMUTHG-UHFFFAOYSA-N lithium niobate Chemical compound [Li+].[O-][Nb](=O)=O GQYHUHYESMUTHG-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- YJVFFLUZDVXJQI-UHFFFAOYSA-L palladium(ii) acetate Chemical compound [Pd+2].CC([O-])=O.CC([O-])=O YJVFFLUZDVXJQI-UHFFFAOYSA-L 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000000059 patterning Methods 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- CHKVPAROMQMJNQ-UHFFFAOYSA-M potassium bisulfate Chemical compound [K+].OS([O-])(=O)=O CHKVPAROMQMJNQ-UHFFFAOYSA-M 0.000 description 1
- 229910000343 potassium bisulfate Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 1
- WBHQBSYUUJJSRZ-UHFFFAOYSA-M sodium bisulfate Chemical compound [Na+].OS([O-])(=O)=O WBHQBSYUUJJSRZ-UHFFFAOYSA-M 0.000 description 1
- 229910000342 sodium bisulfate Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- KUKDDTFBSTXDTC-UHFFFAOYSA-N uranium;hexanitrate Chemical compound [U].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O KUKDDTFBSTXDTC-UHFFFAOYSA-N 0.000 description 1
- 229910002007 uranyl nitrate Inorganic materials 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
- C23F1/30—Acidic compositions for etching other metallic material
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Weting (AREA)
- ing And Chemical Polishing (AREA)
- Internal Circuitry In Semiconductor Integrated Circuit Devices (AREA)
Abstract
The present invention provides an etchant composition for silver (Ag) -containing metal films, which includes a specific metal salt compound. The etching solution composition according to the present invention can inhibit the occurrence of the mouse bite phenomenon and prevent the etching rate of the transparent conductive film from being lowered due to an external contamination source.
Description
Technical Field
The present invention relates to an etching solution composition for a silver (Ag) -containing metal film, and more particularly, to an etching solution composition for a silver (Ag) -containing metal film, which is capable of suppressing the occurrence of a mouse bite (mouse bite) phenomenon and preventing the etching rate of a transparent conductive film from being lowered due to an external contamination source.
Background
Since the OLED itself emits light and can be driven at a low voltage, it has been widely used for small displays such as portable devices and large-sized televisions.
In addition, conductive metals such as Indium Tin Oxide (ITO) and Indium Zinc Oxide (IZO) have relatively excellent light transmittance and conductivity, and thus are widely used as electrodes of color filters used in flat panel display devices.
Further, in the case of a reflection plate, an aluminum (Al) reflection plate has been mainly used in the past in products, but in order to achieve low power consumption by improving luminance, it is being sought to change the material to a metal having a higher reflectance.
Therefore, a method of using silver (Ag: specific resistance about 1.59. Mu. Omega. Cm) or a silver alloy having low resistivity and high brightness compared to a metal applied to a flat panel display device as an electrode of a color filter, a wiring of an LCD or OLED wiring, and a material of a reflective plate has been proposed, and it is required to develop an etching solution for applying silver or a silver alloy.
However, when the existing etching solution is used for silver (Ag) or silver alloy, there are the following problems: silver (Ag) is over-etched or is unevenly etched, thereby causing a wire lift-off or peeling phenomenon, and a side profile of the wire is poor. In addition, it is difficult to achieve Low Skew (Low Skew) to achieve high resolution.
In particular, silver (Ag) has a low oxidation/reduction potential, and therefore re-adsorption, residues, and the like are generated after etching, and in this case, short circuits and the like may occur between adjacent conductive patterns.
Further, when a multilayer film composed of a film made of silver (Ag) or a silver alloy and a transparent conductive film is etched at the same time using an existing etching solution, a phenomenon in which the etching rate of the transparent conductive film is lowered may occur due to an external contamination source (e.g., an organic chelating agent) generated in the etching process. When such a phenomenon that the etching rate of the transparent conductive film is lowered occurs, there is a problem in that: the desired wiring cannot be formed within the same process time and the probability of generating silver residue increases.
In addition, when a multi-layered film composed of a film made of silver (Ag) or a silver alloy and a transparent conductive film is simultaneously etched using an existing etching solution, a mouse bite phenomenon occurs due to a local over-etching phenomenon of a silver thin film, which may cause a defect of a subsequent process.
Korean patent laid-open No. 10-2013-0130515 relates to an etching solution for a silver-containing pattern, and discloses an etching solution which includes nitric acid, oxalic acid, acetic acid, a sulfate-based compound as an oxidizing agent, and an azole-based compound as a corrosion inhibitor, and is capable of simultaneously etching a single-layer film made of silver (Ag) or a silver alloy, and a multi-layer film composed of the single-layer film and a transparent conductive film.
However, the above etching solution does not completely solve the problems of the mouse bite phenomenon and the decrease in the etching rate of the transparent conductive film.
Disclosure of Invention
[ problems to be solved ]
An object of the present invention is to provide an etching solution composition for a silver (Ag) -containing metal film, which is capable of suppressing the occurrence of a mouse-bite phenomenon and preventing the etching rate of a transparent conductive film from being lowered due to an external contamination source.
Another object of the present invention is to provide a silver (Ag) -containing metal wiring formed using the above-described etchant composition for a silver (Ag) -containing metal film.
It is another object of the present invention to provide a method of manufacturing a silver (Ag) -containing metal wiring, the method including an etching process using the etchant composition for a silver (Ag) -containing metal film.
[ MEANS FOR SOLVING PROBLEMS ] A method for solving the problems
Further, the present invention provides an etching solution composition for a silver (Ag) -containing metal film, which includes nitric acid, an organic acid, and a metal salt compound, and the metal salt compound includes at least one metal selected from the group consisting of niobium (Nb), cobalt (Co), zirconium (Zr), hafnium (Hf), bismuth (Bi), palladium (Pd), and uranium (U).
In one embodiment of the present invention, the silver (Ag) -containing metal film may be a single-layer film made of silver (Ag) or a silver alloy, or a multi-layer film composed of the single-layer film and a transparent conductive film.
In one embodiment of the present invention, the transparent conductive film may be a film including at least one of Indium Tin Oxide (ITO), indium Zinc Oxide (IZO), indium tin oxide (ITZO), and gallium zinc oxide (IGZO). .
In one embodiment of the present invention, the organic acid may include an alkylsulfonic acid having 1 to 3 carbon atoms and an organic acid other than the alkylsulfonic acid.
In one embodiment of the present invention, the alkylsulfonic acid having 1 to 3 carbon atoms may include: at least one selected from the group consisting of methanesulfonic acid, ethanesulfonic acid, and propanesulfonic acid.
In one embodiment of the present invention, the organic acid other than the alkylsulfonic acid may include: at least one selected from the group consisting of acetic acid, citric acid, glycolic acid, malonic acid, lactic acid, and tartaric acid.
In one embodiment of the present invention, the metal salt compound may include: at least one metal selected from the group consisting of zirconium (Zr) and bismuth (Bi).
In one embodiment of the present invention, the metal salt compound may be contained in an amount of 0.01 to 0.5 wt% with respect to the total weight of the composition.
The etching solution composition for a silver (Ag) -containing metal film according to an embodiment of the present invention may further include a sulfate compound.
In one embodiment of the present invention, the sulfate compound may include: at least one selected from the group consisting of alkali metal salts of sulfuric acid, alkaline earth metal salts of sulfuric acid, and ammonium salts of sulfuric acid.
The etchant composition for a silver (Ag) -containing metal film according to an embodiment of the present invention may include nitric acid in an amount of 8 to 15 wt%, an organic acid in an amount of 30 to 63 wt%, and a metal salt compound in an amount of 0.01 to 0.5 wt% with respect to the total weight of the composition, and may include the remaining amount of water such that the total weight of the composition is 100 wt%.
An etchant composition for a silver (Ag) -containing metal film according to an embodiment of the present invention may include nitric acid in an amount of 8 to 15 wt%, an organic acid in an amount of 30 to 63 wt%, a sulfate compound in an amount of 7 to 25 wt%, and a metal salt compound in an amount of 0.01 to 0.5 wt%, relative to the total weight of the composition, and may include a remaining amount of water such that the total weight of the composition is 100 wt%.
In addition, the present invention provides a silver (Ag) -containing metal wiring formed using the etching solution composition for a silver (Ag) -containing metal film.
Further, the present invention provides a method of manufacturing a silver (Ag) -containing metal wiring including an etching process using the etching solution composition for a silver (Ag) -containing metal film.
[ Effect of the invention ]
The etching solution composition for a silver (Ag) -containing metal film according to the present invention can suppress the occurrence of a mouse-biting phenomenon and prevent the etching rate of a transparent conductive film from being lowered due to an external contamination source.
Detailed Description
Hereinafter, the present invention will be described in more detail.
One embodiment of the present invention relates to an etchant composition for a silver (Ag) -containing metal film, which includes nitric acid, an organic acid, and a metal salt compound, and the metal salt compound includes at least one metal selected from the group consisting of niobium (Nb), cobalt (Co), zirconium (Zr), hafnium (Hf), bismuth (Bi), palladium (Pd), and uranium (U).
In one embodiment of the present invention, the silver (Ag) -containing metal film may be a single-layer film made of silver (Ag) or a silver alloy, or a multi-layer film composed of the single-layer film and a transparent conductive film. That is, the etchant composition for a silver (Ag) -containing metal film of the present invention can etch not only a single layer film made of silver (Ag) or a silver alloy but also a multilayer film made of the single layer film and a transparent conductive film at the same time.
The silver alloy may be in the form of an alloy containing silver as a main component and other metals such as Nd, cu, pd, nb, ni, mo, ni, cr, mg, W, pa, ti, and the like; and various forms of silver such as nitride, silicide, carbide, and oxide forms.
In one embodiment of the present invention, the transparent conductive film may be a film including at least one of Indium Tin Oxide (ITO), indium Zinc Oxide (IZO), indium tin oxide (ITZO), and gallium zinc oxide (IGZO). .
The multilayer film may be formed of transparent conductive film/silver, transparent conductive film/silver alloy, transparent conductive film/silver/transparent conductive film, or transparent conductive film/silver alloy/transparent conductive film.
Hereinafter, components of the etching liquid composition according to an embodiment of the present invention will be described in more detail.
Nitric acid (A)
In one embodiment of the present invention, nitric acid (a) as an oxidizing agent may be used to oxidize a single-layer film made of silver (Ag) or a silver alloy, that is, a silver thin film and a transparent conductive film.
The nitric acid may be present in an amount of 8 to 15 wt.%, preferably 8 to 12 wt.%, relative to the total weight of the composition. When the nitric acid is contained within the above content range, it is easy to control the etching rate, so that the silver thin film and the transparent conductive film can be uniformly etched.
Organic acid (B)
In one embodiment of the present invention, the organic acid (B) may be used as an etchant for a silver thin film to etch the silver thin film oxidized by nitric acid.
The organic acid may include an alkylsulfonic acid (B-1) having 1 to 3 carbon atoms and an organic acid (B-2) other than the alkylsulfonic acid.
The organic acid may be present in an amount of 30 to 63 wt% with respect to the total weight of the composition. When the organic acid is contained within the above content range, since the etching rate of the silver thin film is easily controlled, defects due to silver residue and silver re-adsorption can be prevented.
Alkylsulfonic acid having 1 to 3 carbon atoms (B-1)
The alkylsulfonic acid (B-1) having 1 to 3 carbon atoms may be used together with a silver thin film oxidized by nitric acid for etching a transparent conductive film.
Examples of the alkylsulfonic acid having 1 to 3 carbon atoms include methanesulfonic acid, ethanesulfonic acid, propanesulfonic acid, and the like, and these may be used alone or in combination of two or more. Preferably, methanesulfonic acid may be used as the alkylsulfonic acid having 1 to 3 carbon atoms.
The content of the alkylsulfonic acid having 1 to 3 carbon atoms may be 3 to 8% by weight with respect to the total weight of the composition. When the alkyl sulfonic acid is contained within the above content range, the etching rate of the silver thin film and the etching rate of the transparent conductive film are easily controlled, and defects due to silver residue and silver re-adsorption can be prevented.
Organic acids other than alkylsulfonic acids (B-2)
The organic acid (B-2) other than the alkylsulfonic acid may be used as an etchant for the silver thin film to etch the silver thin film oxidized by nitric acid.
Examples of the organic acid other than the alkylsulfonic acid include acetic acid, citric acid, glycolic acid, malonic acid, lactic acid, tartaric acid, and the like, and these may be used alone or in combination of two or more. Preferably, acetic acid and citric acid may be used as the organic acid other than the alkylsulfonic acid.
The organic acid other than the alkylsulfonic acid may be present in an amount of 25 to 55 wt% relative to the total weight of the composition. When the organic acid is contained within the above content range, the etching rate of the silver thin film is easily controlled, and defects due to silver residue and silver re-adsorption can be prevented.
Metal salt Compound (C)
In one embodiment of the present invention, the metal salt compound (C) as an etching rate maintaining agent for the transparent conductive film may be used to prevent a reduction in the etching rate of the transparent conductive film due to an external contamination source (organic substance such as organic chelating agent) that may occur in an etching process. Specifically, the metal salt compound (C) prevents external contaminants generated in the etching process from being adsorbed to the transparent conductive film by adsorbing the external contaminants.
In fact, contaminants due to photoresist residues, organic materials within the substrate, or various impurities may be present in the etching apparatus used in the etching process, resulting in a phenomenon of disturbing the etching since such contaminants may be adsorbed onto the transparent conductive film.
As the metal salt compound, a metal salt compound capable of oxidizing a silver film (for example, a metal salt compound containing a metal such as iron, molybdenum, or the like) is not included.
In addition, since the etching solution composition for a silver (Ag) -containing metal film according to one embodiment of the present invention can oxidize a silver thin film, it is preferable not to include metal components such as iron, molybdenum, and the like.
The metal salt compound is at least one metal selected from the group consisting of niobium (Nb), cobalt (Co), zirconium (Zr), hafnium (Hf), bismuth (Bi), palladium (Pd), and uranium (U), and preferably includes at least one metal selected from zirconium (Zr) and bismuth (Bi).
For example, the metal salt compound may be zirconium phosphate, zirconium sulfate, bismuth nitrate, lithium niobate, cobalt acetate, hafnium oxide (HfO) 2 ) Palladium acetate, uranium nitrate, and the like, and they may be used alone or in a mixture of two or more. Preferably, as the metal salt compound, zirconium phosphate, zirconium sulfate and/or bismuth nitrate may be used.
The metal salt compound may be contained in an amount of 0.01 to 0.5 wt% with respect to the total weight of the composition. When the metal salt compound is included within the above content range, it is possible to prevent the etch rate of the transparent conductive film from being lowered due to an external contamination source, without causing a local over-etching phenomenon of some wirings, i.e., a mouse-bite phenomenon, due to the use of the metal salt compound.
Sulfate Compound (D)
The etching solution composition for a silver (Ag) -containing metal film according to an embodiment of the present invention may further include a sulfate compound (D).
In one embodiment of the present invention, the sulfate compound (D) can be used for etching a transparent conductive film as an etchant for the transparent conductive film. In addition, the sulfate compound (D) causes an etch stop phenomenon of the silver thin film, and thus can prevent an increase in side etch (side etch) even if an etch time during an etch process is increased. In other words, the sulfate compound (D) may control the occurrence of the etch stop (etch stop) phenomenon, thereby controlling the etch rate, and controlling the side etch.
The sulfate compound may include at least one selected from the group consisting of an alkali metal salt of sulfuric acid, an alkaline earth metal salt of sulfuric acid, and an ammonium salt of sulfuric acid.
For example, the sulfate compound may be, for example, potassium hydrogen sulfate, sodium hydrogen sulfate, ammonium hydrogen sulfate, or the like. These may be used alone or in combination of two or more.
The sulfate compound may be present in an amount of 7 to 25 wt% relative to the total weight of the composition. When the sulfate compound is within the content range, it is easy to control the etching rate (i.e., control the etching time in the etching process), and the etch stop phenomenon is regularly exhibited, so that the silver thin film and the transparent conductive film can be uniformly etched.
Water (E)
In addition, the etching solution composition according to one embodiment of the present invention may include a residual amount of water such that the total weight of the composition is 100 wt%. In the present invention, water is not particularly limited, but deionized water used for semiconductor processing is preferable, and deionized water having a specific resistance of 18M Ω · cm or more is more preferable to exhibit a degree of ion removal from water.
The "remaining amount" of the present invention means a remaining amount such that the weight of the total composition including the essential ingredients of the present invention and other additional ingredients becomes 100% by weight, and the composition of the present invention is not limited to the absence of additional ingredients due to the meaning of the "remaining amount".
An etchant composition for a silver (Ag) -containing metal film according to one embodiment of the present invention may include nitric acid in an amount of 8 to 15 wt%, an organic acid in an amount of 30 to 63 wt%, and a metal salt compound in an amount of 0.01 to 0.5 wt%, with respect to the total weight of the composition, and may include the remaining amount of water such that the total weight of the composition is 100 wt%.
An etchant composition for a silver (Ag) -containing metal film according to one embodiment of the present invention may include nitric acid in an amount of 8 to 15 wt%, an alkylsulfonic acid in an amount of 3 to 8 wt% having 1 to 3 carbon atoms, an organic acid other than the alkylsulfonic acid in an amount of 25 to 55 wt%, and a metal salt compound in an amount of 0.01 to 0.5 wt%, with respect to the total weight of the composition, and may include a remaining amount of water such that the total weight of the composition is 100 wt%.
An etchant composition for a silver (Ag) -containing metal film according to one embodiment of the present invention may include nitric acid in an amount of 8 to 15 wt%, an organic acid in an amount of 30 to 63 wt%, a sulfate compound in an amount of 7 to 25 wt%, and a metal salt compound in an amount of 0.01 to 0.5 wt%, with respect to the total weight of the composition, and may include the remaining amount of water such that the total weight of the composition is 100 wt%.
An etchant composition for a silver (Ag) -containing metal film according to one embodiment of the present invention may include nitric acid in an amount of 8 to 15 wt%, an alkylsulfonic acid in an amount of 3 to 8 wt% having 1 to 3 carbon atoms, an organic acid other than the alkylsulfonic acid in an amount of 25 to 55 wt%, a sulfate compound in an amount of 7 to 25 wt%, and a metal salt compound in an amount of 0.01 to 0.5 wt%, relative to the total weight of the composition, and may include a remaining amount of water such that the total weight of the composition is 100 wt%.
The components for the etchant composition according to one embodiment of the present invention may be prepared by a conventionally known method, and preferably have a purity for semiconductor processes.
The etching liquid composition according to one embodiment of the present invention can suppress the occurrence of mouse bite and can prevent the etching rate of the transparent conductive film from being lowered due to an external contamination source.
In addition, the etching solution composition according to an embodiment of the present invention may generate an etch stop phenomenon, thereby controlling an etch rate and controlling side etching. Therefore, in the etching solution composition according to one embodiment of the present invention, a fine pattern of the multilayer film can be realized.
Further, in the etching liquid composition according to one embodiment of the present invention, the etching performance can be maintained even if the number of the processing sheets is increased.
The etching solution composition for a silver (Ag) -containing metal film of the present invention may be used to form an OLED TFT array substrate for a reflective film, a trace or nanowire wiring for a touch screen panel, but is not limited thereto, and may be used for electronic element materials including single-layer films and multi-layer films.
Accordingly, one embodiment of the present invention relates to a silver (Ag) -containing metal wiring formed using the above-described etchant composition for a silver (Ag) -containing metal film.
The silver (Ag) -containing metal wiring according to an embodiment of the present invention may be manufactured by performing an etching process known in the art using the above-described etching solution composition.
One embodiment of the present invention relates to a method for manufacturing a silver (Ag) -containing metal wiring, which includes an etching process using the above-described etchant composition for a silver (Ag) -containing metal film.
Specifically, the method of manufacturing the silver (Ag) -containing metal wiring may include the steps of: i) Forming a single-layer film made of silver or a silver alloy, or a multilayer film composed of the single-layer film and a transparent conductive film on a substrate; ii) patterning after forming a photoresist film on the single-layer film or the multi-layer film; and iii) etching the single-layer film or the multilayer film using the above-mentioned etchant composition.
Hereinafter, the present invention will be described in more detail by examples, comparative examples and experimental examples. These examples, comparative examples and experimental examples are only for illustrating the present invention, and it is apparent to those skilled in the art that the scope of the present invention is not limited thereto.
Examples 1 to 5 and comparative examples 1 to 5:
as shown in table 1 below, the components were mixed, and an etchant composition was prepared by adding the remaining amount of deionized water so that the total amount was 100 weight% (unit: weight%).
[ TABLE 1 ]
Experimental example 1:
silver (Ag) re-adsorption, a decrease in the etching rate of the transparent conductive film, and a mouse-biting phenomenon with respect to the etching solution compositions of the examples and comparative examples prepared as above were evaluated in the following manner, and the results thereof are shown in table 2 below.
(1) Re-adsorption of silver (Ag)
After forming an ITO/silver/ITO triple layer film on a substrate, a photoresist is patterned on the triple layer film.
The etching liquid compositions of examples and comparative examples were put into a test apparatus (model: ETCHER (TFT), SEMES) of the spray etching method, and the temperature was raised to 40 ℃ and then the etching treatment of the sample was performed when the temperature reached 40. + -. 0.1 ℃. The total etch time was 85 seconds. The substrate (4X 4 cm) was placed and sprayed, taken out when the etching time of 85 seconds had ended, washed with deionized water and dried with a hot air dryer. After washing and drying, the substrate was cut to obtain an analysis sample (0.5X 0.5 cm), which was measured using a scanning electron microscope (SEM; model: SU-8010, manufactured by HITACHI corporation). Measured and evaluated according to the following evaluation criteria: the amount of silver particles adsorbed to the upper Ti of the Ti/Al/Ti triple-layer film exposed at the source/drain portion within the substrate due to the etching process.
< evaluation criteria >
Good: the amount of adsorbed silver is 10 or less
Poor: the quantity of silver adsorbed exceeds 10
(2) Etch rate reduction of transparent conductive film
After forming an ITO/silver/ITO triple layer film on a substrate, the etching solution compositions of examples and comparative examples were placed in a test apparatus (model: ETCHER (TFT), SEMES) of a spray etching method, respectively, and after raising the temperature by setting the temperature to 40 ℃, etching treatment of the sample was performed when the temperature reached 40. + -. 0.1 ℃. To simulate the effect of external contaminants, ethylene diamine and polyvinyl butyral were used as artificial organic contaminants at concentrations of 100ppm and 50ppm, respectively. Whether the etching rate was decreased was confirmed by comparing the etching time of the uppermost ITO film before/after the addition of the organic contaminants. When the etching completion time (EPD) of the initial upper ITO film was decreased by 5% or more, it was judged that the etching rate was decreased and marked with o, and when the decrease was less than 5%, it was judged that the experimental error was increased and marked with x.
(3) Mouse bite phenomenon (local over-etching of wiring)
The mouse bite phenomenon is a local over-etching phenomenon occurring in the etching process because the patterned wiring shape looks like being phagocytosed by a mouse.
This is because the etching liquid composition penetrates into pinholes present due to uneven formation of the upper indium oxide film and impurities such as dust, resulting in local over-etching, and is a phenomenon seen in etching solutions containing oxidizing agents for silver thin films such as some metals and some metal salts.
After forming an ITO/silver/ITO triple layer film on a substrate, the etching solution compositions of examples and comparative examples were placed in a test apparatus (model: ETCHER (TFT), SEMES) of a spray etching method, respectively, and after raising the temperature by setting the temperature to 40 ℃, etching treatment of the sample was performed when the temperature reached 40. + -. 0.1 ℃.
After the etching treatment, the occurrence of mouse bite was observed using an optical microscope (model: OLS5000, OLYMPUS Co.).
O: mouse bite phenomenon
X: no rat bite
[ TABLE 2 ]
As can be seen from table 2, the etching solution compositions of examples 1 to 5 containing the specific metal salt compound did not cause the mouse bite phenomenon, and the etching rate of the transparent conductive film was not lowered.
In contrast, in the etching solution compositions of comparative examples 1 to 3, which do not contain the specific metal salt compound or exceed the above content range, a phenomenon occurs in which the etching rate of the transparent conductive film is lowered, or precipitates occur in the etching solution due to the excessive use of the metal salt.
Further, it was found that the etching solution compositions of comparative examples 4 to 5 using molybdenum or iron salts cause the mouse bite phenomenon by oxidizing silver.
While certain embodiments of the present invention have been described in detail, it will be apparent to those skilled in the art that these specific techniques are only preferred embodiments of the invention, and that the scope of the invention is not limited thereto. Those skilled in the art to which the invention pertains will be able to make various applications and modifications within the scope of the present invention based on the above description.
Accordingly, the substantial scope of the present invention will be defined by the appended claims and equivalents thereof.
Claims (14)
1. An etching solution composition for a silver (Ag) -containing metal film, comprising nitric acid, an organic acid and a metal salt compound, and
the metal salt compound includes at least one metal selected from the group consisting of niobium (Nb), cobalt (Co), zirconium (Zr), hafnium (Hf), bismuth (Bi), palladium (Pd), and uranium (U).
2. The etching solution composition for silver (Ag) -containing metal films according to claim 1, wherein the silver (Ag) -containing metal film is a single-layer film made of silver (Ag) or a silver alloy, or a multi-layer film composed of the single-layer film and a transparent conductive film.
3. The etching solution composition for a silver (Ag) -containing metal film according to claim 2, wherein the transparent conductive film is a film comprising at least one of Indium Tin Oxide (ITO), indium Zinc Oxide (IZO), indium tin oxide (ITZO), and gallium zinc oxide (IGZO).
4. The etching solution composition for a silver (Ag) -containing metal film according to claim 1, wherein the organic acid includes an alkylsulfonic acid having 1 to 3 carbon atoms and an organic acid other than the alkylsulfonic acid.
5. The etching solution composition for a silver (Ag) -containing metal film according to claim 4, wherein the alkylsulfonic acid having 1 to 3 carbon atoms includes: at least one selected from the group consisting of methanesulfonic acid, ethanesulfonic acid, and propanesulfonic acid.
6. The etching solution composition for a silver (Ag) -containing metal film according to claim 4, wherein the organic acid other than the alkylsulfonic acid includes: at least one selected from the group consisting of acetic acid, citric acid, glycolic acid, malonic acid, lactic acid, and tartaric acid.
7. The etchant composition for silver (Ag) -containing metal film according to claim 1, wherein the metal salt compound comprises: at least one metal selected from the group consisting of zirconium (Zr) and bismuth (Bi).
8. The etching solution composition for a silver (Ag) -containing metal film according to claim 1, wherein the content of the metal salt compound is 0.01 to 0.5 wt% with respect to the total weight of the composition.
9. The etching solution composition for a silver (Ag) -containing metal film according to claim 1, further comprising a sulfate compound.
10. The etching solution composition for a silver (Ag) -containing metal film according to claim 9, wherein the sulfate compound comprises: at least one selected from the group consisting of an alkali metal salt of sulfuric acid, an alkaline earth metal salt of sulfuric acid, and an ammonium salt of sulfuric acid.
11. The etching solution composition for a silver (Ag) -containing metal film according to claim 1, comprising nitric acid in an amount of 8 to 15 wt%, an organic acid in an amount of 30 to 63 wt%, and a metal salt compound in an amount of 0.01 to 0.5 wt%, relative to the total weight of the composition, and comprising the remaining amount of water such that the total weight of the composition is 100 wt%.
12. The etching solution composition for a silver (Ag) -containing metal film according to claim 9, comprising nitric acid in an amount of 8 to 15 wt%, an organic acid in an amount of 30 to 63 wt%, a sulfate compound in an amount of 7 to 25 wt%, and a metal salt compound in an amount of 0.01 to 0.5 wt%, relative to the total weight of the composition, and comprising the remaining amount of water such that the total weight of the composition is 100 wt%.
13. A silver (Ag) -containing metal wiring formed using the etching solution composition for a silver (Ag) -containing metal film according to any one of claims 1 to 12.
14. A method of manufacturing a silver (Ag) -containing metal wiring, comprising an etching process using the etching solution composition for a silver (Ag) -containing metal layer according to any one of claims 1 to 12.
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| WO2002008491A1 (en) * | 2000-07-26 | 2002-01-31 | Mitsubishi Gas Chemical Company, Inc. | Palladium removing solution and method for removing palladium |
| JP2016025321A (en) * | 2014-07-24 | 2016-02-08 | 関東化學株式会社 | Etchant composition and etching method |
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| TW201900928A (en) * | 2017-05-10 | 2019-01-01 | 日商Ａｄｅｋａ股份有限公司 | Etching liquid composition and etching method |
| CN111172541A (en) * | 2018-11-12 | 2020-05-19 | 东友精细化工有限公司 | Silver thin film etching solution composition, etching method and metal pattern forming method |
| CN113026019A (en) * | 2017-05-22 | 2021-06-25 | 东友精细化工有限公司 | Silver thin film etching solution composition, etching method and metal pattern forming method |
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| KR101391603B1 (en) | 2012-05-22 | 2014-05-07 | 솔브레인 주식회사 | Echant for silver pattern |
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| WO2002008491A1 (en) * | 2000-07-26 | 2002-01-31 | Mitsubishi Gas Chemical Company, Inc. | Palladium removing solution and method for removing palladium |
| JP2016025321A (en) * | 2014-07-24 | 2016-02-08 | 関東化學株式会社 | Etchant composition and etching method |
| KR20180057957A (en) * | 2016-11-23 | 2018-05-31 | 창성나노텍 주식회사 | Ink composition for etching metallic thin film and Method for preparing the same |
| TW201900928A (en) * | 2017-05-10 | 2019-01-01 | 日商Ａｄｅｋａ股份有限公司 | Etching liquid composition and etching method |
| CN113026019A (en) * | 2017-05-22 | 2021-06-25 | 东友精细化工有限公司 | Silver thin film etching solution composition, etching method and metal pattern forming method |
| CN111172541A (en) * | 2018-11-12 | 2020-05-19 | 东友精细化工有限公司 | Silver thin film etching solution composition, etching method and metal pattern forming method |
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