KR101537207B1 - Etching composition for silver or magnesium - Google Patents
Etching composition for silver or magnesium Download PDFInfo
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- KR101537207B1 KR101537207B1 KR1020130119796A KR20130119796A KR101537207B1 KR 101537207 B1 KR101537207 B1 KR 101537207B1 KR 1020130119796 A KR1020130119796 A KR 1020130119796A KR 20130119796 A KR20130119796 A KR 20130119796A KR 101537207 B1 KR101537207 B1 KR 101537207B1
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- silver
- magnesium
- etching
- thin film
- alloy
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- 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
- C23F1/44—Compositions for etching metallic material from a metallic material substrate of different composition
-
- 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
- C23F1/22—Acidic compositions for etching magnesium or alloys thereof
-
- 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
Abstract
The etching composition according to the present invention containing at least one compound selected from the group consisting of potassium nitrate, aluminum nitrate or a hydrate thereof, an optional pH controlling agent and any hydrogen peroxide may be a thin film containing silver or magnesium or an alloy thereof A thin film containing silver or magnesium or alloys thereof can be selectively etched in the multilayer film containing the undesired silver or magnesium or alloys thereof in the process chamber. The etching composition according to the present invention is easy to clean due to the absence of silver residue after etching, facilitates process control such as etching rate and / or etching time, can reduce manufacturing apparatus cost and manufacturing cost, There is an advantage to be able to.
Description
The present invention relates to an etching solution composition for silver (Ag) or magnesium (Mg), and more particularly to an etching solution composition for selectively etching a silver or magnesium-containing thin film.
The process of forming a metal wiring on a substrate in a semiconductor and a display device is usually performed by forming a metal film by sputtering and vapor deposition, forming a pattern on a metal film, and then etching.
Particularly, in a liquid crystal display device, for example, an active matrix liquid crystal display (LCD), which is one of the flat panel display devices, data lines, gate lines, and signal lines connecting them are formed on a lower substrate. These wirings are usually made of chrome, molybdenum, aluminum, neodymium or alloys thereof, which are metals with low electrical resistivity.
As a liquid crystal display device becomes larger in size and realized with high resolution tendency, a wiring material having a lower electrical resistance is required. As an ideal material for this purpose, attention is paid to a low resistance material such as silver (Ag) or magnesium (Mg).
Recently, techniques for IZO / Ag / IZO wiring, ITO / Ag / ITO wiring, Mo / Ag / ITO wiring and the like have been disclosed and multilayer films including silver or magnesium or alloys thereof are used as electrodes of color filters, And its application to reflectors has been proposed.
However, silver (Ag) is extremely poor in adhesion to an insulating substrate such as glass or a lower substrate such as a semiconductor substrate made of intrinsic amorphous silicon or doped amorphous silicon or the like, it is known that lifting or peeling is easily caused.
In this situation, when a conventional acid-based etchant is used to pattern a thin film made of silver (Ag) or a silver alloy, silver (Ag) is excessively etched or inhomogeneously etched to cause lifting or peeling of the wiring , The side profile of the wiring becomes poor.
The silver etching solution disclosed in Korean Patent No. 0579421 uses a small carbon surfactant together with an auxiliary oxide dissolving agent as an additive to phosphoric acid, nitric acid and acetic acid. However, the SO 4 2- compound used as a secondary oxide dissolving agent has a disadvantage that it reacts with silver (Ag) and remains as a residue in the form of silver sulfide (Ag 2 S). ClO 4 - There is a difficulty in specifying and using. Also, in the case of the Hambil small carbon surfactant, when the lower film of silver is an organic insulating film, the organic insulating film at the edge of the substrate is easily damaged by the etching solution, causing peeling.
Korean Patent Application No. 10-2010-7013662 discloses an etchant composition comprising an aqueous solution containing an alkali and comprising a laminate film comprising at least one metal film selected from the group consisting of Al, Al alloy, Cu, Cu alloy, Ag and Ag alloy, It is disclosed that the metal film is selectively etched, but an embodiment of Ag and Ag alloys is not described.
Korean Patent Application No. 10-2002-0018282 discloses a process for the preparation of a pharmaceutical composition containing hydrogen peroxide, a pH adjusting agent (eg NH 4 salt, Na salt, K salt), a chelating agent (eg acetic acid, glycolic acid, citric acid, oxalic acid or malonic acid) Discloses etching an Ag (Ag) thin film without an IZO attack as an etching composition.
Korean Patent Application No. 10-2002-0018283 discloses a method for etching a silver (Ag) thin film without an IZO attack using an etching composition containing a Fe 3+ salt compound, nitric acid, acetic acid, a corrosion inhibitor (e.g., amines, azoles) .
Korea Patent Application No. 10-2007-0058795 discloses a phosphoric acid, nitric acid, acetic acid, a single layer made of one sodium phosphate (NaH 2 PO 4) and by the etching composition containing water, silver (Ag) or silver alloy, and the single film And an indium oxide film are etched at the same time.
Since the etching solution composition for silver or magnesium mostly exhibits acidity or uses a strongly acidic substance, it is difficult to control the content or the pH of the etching solution composition so that the substrate or support (base material) There has been a problem that it can be corroded.
Therefore, there has been a great need for a highly selective etching solution composition capable of selectively etching a silver or magnesium thin film in a multilayer film containing silver or a magnesium thin film.
It is an object of the present invention to develop a highly selective etching composition capable of selectively etching only a silver or magnesium thin film in a multilayer film containing silver or a magnesium thin film.
The inventors of the present invention can selectively etch a silver thin film or a magnesium thin film in a multilayer film including a silver thin film or a magnesium thin film by using an aqueous solution containing a nitrate compound, an arbitrary pH adjusting agent and an optional hydrogen peroxide, The present invention has been accomplished based on the discovery that it is applicable to cleaning of a support or a base material made of an iron alloy or a nickel alloy, which is difficult to apply in the past.
Using the etching composition according to the present invention, only the silver thin film or the magnesium thin film can be selectively etched in the multi-layered film including the silver foil or the magnesium thin film, and since the silver or magnesium residue is not used, the cleaning can be simplified and the processing time can be shortened , Thereby reducing manufacturing costs and preventing environmental pollution.
Fig. 1 is a photograph showing the surface state of the material before and after etching and cleaning of the Ag thin film of Example 1, wherein a, b, and c are photographs of elapsed time before cleaning,
FIG. 2 is a photograph showing the surface state of the material before and after the etching and cleaning of the Ag thin film of Comparative Example 8, wherein a, b, and c are photographs of elapse of 10 hours,
FIG. 3 is a photograph showing the surface state of the material before and after the etching and cleaning of the Mg thin film of Example 8. FIG.
A first object of the present invention is to provide a highly selective etching composition of a silver-containing or magnesium-containing thin film containing a nitrate compound, an optional pH controlling agent and any hydrogen peroxide.
According to a preferred embodiment of the present invention, the etching composition consists of a nitrate compound, hydrogen peroxide and water.
According to another preferred embodiment of the present invention, the etching composition comprises a nitrate compound and water.
Hereinafter, the present invention will be described in more detail with reference to the drawings.
In the present invention, the thin film containing silver, magnesium or an alloy thereof is exemplified by a silver thin film, a magnesium thin film, a silver alloy thin film, a magnesium alloy thin film, a silver-magnesium alloy thin film, or a thin film of an alloy containing silver- can do.
In the present invention, the nitrate compounds include nitrates of typical metals, specifically nitrates of Group Ia, IIa and Group IIIb metals, more specifically nitrates of alkali metals such as Na and K, nitrates of alkaline earth metals such as Mg and Ca And aluminum nitrate.
According to the present invention, the nitrate compound is used in an amount of 0.1 to 60% by weight, preferably 0.2 to 50% by weight, more preferably 0.4 to 40% by weight, particularly 0.5 to 30% by weight, based on the total weight of the etching composition May be contained in an amount of 1 to 20% by weight. If the amount of the nitrate compound is less than 0.1% by weight, the etching rate will be too slow. If the amount of the nitrate compound exceeds 50% by weight, the etching rate will become excessively high and the overall etching may become uneven.
According to one preferred embodiment of the present invention, the nitrate compound may be aluminum nitrate or a hydrate thereof. The hydrate of aluminum nitrate is commercially available in the form of aluminum nitrate nonahydrate, but is not limited thereto. On the other hand, an aqueous solution of aluminum nitrate or its hydrate usually exhibits acidity.
The immersion or cleaning time is not particularly limited and can be easily determined by the skilled artisan according to the content of aluminum nitrate. Usually, the immersion or cleaning time can be determined so that the immersion or cleaning can be completed within 0.1 to 3 hours, particularly within 0.2 to 2 hours.
According to one variant of the present invention, the etching composition of the present invention may further contain hydrogen peroxide known to act as an initiator. The hydrogen peroxide may be contained in an amount of 0.05 to 10% by weight, preferably 0.1 to 8% by weight, more preferably 0.2 to 6% by weight, particularly 0.3 to 4% by weight, based on the total weight of the etching composition. If the amount of hydrogen peroxide is 0.05 wt% or less, the etching rate is excessively slow. If the amount of hydrogen peroxide is more than 50 wt%, the etching rate becomes too fast, and the overall etching may become uneven.
According to one variant, the etching composition of the present invention may further comprise a pH adjusting agent selected from the group consisting of nitric acid, inorganic acids such as phosphoric acid, and organic acids such as acetic acid. The pH adjusting agent may be contained in an amount of 0.01 to 5% by weight, preferably 0.02 to 4% by weight, more preferably 0.03 to 3% by weight, particularly 0.04 to 3% by weight, based on the total weight of the etching composition .
According to an additional advantage of the present invention, when silver, magnesium or a thin film thereof is formed by sputtering, not only a desired position on the substrate but also an undesired position, for example, on the periphery of a substrate, a process chamber such as a process chamber, A thin film can be formed. The thin films thus formed are removed through a cleaning process using the same or similar etching solution, but the surface of the base material to which the thin film is adhered may be corroded to damage expensive process equipment. Thus, in the process of forming a thin film by sputtering, a cleaning composition is additionally and / or separately required to remove unwanted contaminating thin films in process equipment such as a process chamber.
According to one embodiment, the etching composition for a thin film comprising silver, magnesium or an alloy thereof according to the present invention can be used as a cleaning composition of the process equipment used in forming the above-mentioned thin film. Since the composition of the present invention has a mild physical property, expensive nickel alloys such as nickel-containing stainless steel or nickel which are widely used as a base material for processing equipment, such as Cu, Cr, Fe, Mo. The subsequent cleaning process of the etching composition can be easily performed because the cleaning process can be performed without completely or substantially corroding the nickel alloy base material containing Ti, Co or a mixture thereof, as well as little or no residue left behind . Accordingly, in the present invention, the cleaning of the thin film may be used to include etching of the thin film or removal of the thin film.
The time required for etching or cleaning the thin film containing silver, magnesium or alloys thereof using the etching composition or cleaning composition according to the present invention can be controlled by varying the concentration of the composition. The process time may be completed within 24 hours, particularly within 12 hours, preferably within 5 hours, more preferably within 2 hours, considering the process efficiency, but it goes without saying that the process time is not particularly limited.
According to the present invention, an etching solution containing a nitrate compound and an optional hydrogen peroxide has mild properties such as acidity, is easy to store and transport, is easy to control the process, does not damage the base material of the process equipment, It is easy to remove or clean the etching solution since there is no residue or almost no residue after the etching and only the thin film made of silver or magnesium or an alloy thereof is selectively etched and the glass, There is an advantage that the base material made of the alloy or the lower substrate is not damaged. In addition, since the etching rate and / or the etching time can be easily controlled by adjusting the content of potassium nitrate, aluminum nitrate or hydrate thereof, the process control is easy and productivity is easily controlled.
Hereinafter, the present invention will be described in more detail based on examples, but the present invention is not limited by the following examples.
Example 1 :
An etching composition consisting of 5% by weight of aluminum nitrate nonahydrate, 1.5% by weight of hydrogen peroxide and 93.5% by weight of water is prepared. Using the obtained etching composition, the Ag alloy / Ni alloy double layer was immersed for about 1 hour to etch and clean the Ag alloy layer. A Ni-Fe alloy film and a Ni-Cr alloy film were used as nickel alloy films, respectively.
Fig. 1 shows photographs of Ag alloy / Ni alloy double films before and after the above etching and cleaning. Etching and cleaning were completed within 1 hour, but it showed no damage to the base metal (Ni alloy) after 10 hours.
Comparative Example 1 :
The procedure of Example 1 was followed except that a solution containing 20 wt% of nitric acid was used instead of aluminum nitrate to etch and clean the Ag alloy / Ni alloy double layer. In the condition of Comparative Example 1, since the rate at which corrosion of the base material occurred was greater than the cleaning rate of the Ag and Ag alloy thin films, cleaning could not proceed.
Fig. 2 shows a surface photograph before and after the cleaning treatment in Comparative Example 1. Fig.
Examples 2 to 6 :
Except that aluminum nitrate and hydrogen peroxide were used in the proportions shown in Table 1, respectively, to etch and clean the Ag alloy / Ni alloy double layer.
Example 7 :
The procedure of Example 1 was followed except that only aluminum nitrate was used to etch and clean the Ag alloy / Ni alloy double layer.
(weight%)
Etching time
Base material damage
Base material damage
Example 8 :
The Mg alloy / Ni alloy double layer was etched and cleaned in the same manner as in Example 1, except that magnesium (Mg) and magnesium alloy thin films were used.
Fig. 3 shows a surface photograph of the magnesium (Mg) and magnesium alloy thin films before and after cleaning.
Examples 9 to 14
As shown in Table 2 below, etching compositions of nitrate compounds, hydrogen peroxide and water were prepared.
An Ag alloy film was deposited on a base material selected from an Fe alloy, a Ni alloy, or a glass / ceramic and immersed in the etching composition to test the cleaning effect of the Ag-Mg alloy film and the damage of the base material. The results are shown in Table 2 below.
(weight%)
Cleaning effect
Base material damage
Base material damage
In Table 2, the Ag-Mg alloy cleaning effect and the evaluation results of the base material damage have the following meanings:
[Cleaning effect]
◎: Completely rinsed within 24 hours,
△: Completion of cleaning within 48 hours,
X: Not cleaned
[Base material damage]
◎: Within 24 hours No damage to base material,
○: Within 12 hours, there is no damage to the base material, but some base material is damaged within 24 hours,
△: slight base material damage occurred within 12 hours,
×: Less than 6 hours of material damage.
FIG. 4A is a photograph showing the result of cleaning the Ag-Mg alloy deposited on the surface of a base material made of a nickel alloy rod (a nickel alloy rod) and an iron alloy rod) with the etching solution of Example 10. FIG. 4a), it can be seen that the cleaning of the iron alloy and the nickel alloy base materials is completed without any damage.
The present invention can be used not only to selectively etch thin films containing silver, magnesium, or alloys thereof in semiconductors and display devices, but also to remove unwanted silver or magnesium thin films or debris from the substrate and process equipment after thin film formation Can also be used for.
Claims (7)
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| KR20120114131 | 2012-10-15 | ||
| KR1020120114131 | 2012-10-15 |
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| KR1020140156431A Division KR101695608B1 (en) | 2012-10-15 | 2014-11-11 | Cleaning composition for etching and removing a thin layer of silver or magnesium |
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| KR1020140156431A KR101695608B1 (en) | 2012-10-15 | 2014-11-11 | Cleaning composition for etching and removing a thin layer of silver or magnesium |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10611962B2 (en) | 2018-04-23 | 2020-04-07 | Samsung Display Co., Ltd. | Etchant composition and manufacturing method of metal pattern using the same |
| US10636666B1 (en) | 2018-10-11 | 2020-04-28 | Samsung Display Co., Ltd. | Etchant and method for manufacturing display device using the same |
| US11091694B2 (en) | 2018-11-14 | 2021-08-17 | Samsung Display Co., Ltd. | Etching composition, method for forming pattern and method for manufacturing a display device using the same |
| US11639470B2 (en) | 2020-12-28 | 2023-05-02 | Samsung Display Co., Ltd. | Etching composition for thin film containing silver, method for forming pattern and method for manufacturing a display device using the same |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015160006A1 (en) * | 2014-04-16 | 2015-10-22 | 피에스테크놀러지(주) | Etching composition for silver or magnesium |
| KR102546803B1 (en) * | 2016-05-23 | 2023-06-22 | 동우 화인켐 주식회사 | Etching solution composition for silver-containing layer and an display substrate using the same |
| KR20190058758A (en) | 2017-11-21 | 2019-05-30 | 삼성디스플레이 주식회사 | Etchant and manufacturing method of display device using the same |
| KR20210134177A (en) | 2020-04-29 | 2021-11-09 | 삼성디스플레이 주식회사 | Etchant and manufacturing method of display device using the same |
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| KR20080009866A (en) * | 2006-07-25 | 2008-01-30 | 동우 화인켐 주식회사 | Silver & silver alloy etchant for metal electrode & reflection layer |
| KR20090081566A (en) * | 2008-01-24 | 2009-07-29 | 동우 화인켐 주식회사 | Etchant composition for Ag thin layer and method for fabricating metal pattern using the same |
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| KR20020018282A (en) | 2000-09-01 | 2002-03-08 | 하덕린 | Adapter for charging mobile phone battery |
| KR100338671B1 (en) | 2000-09-01 | 2002-05-30 | 윤종용 | Fixing device for memory card in portable radiotelephone |
| KR20070058795A (en) | 2005-12-05 | 2007-06-11 | 삼성전자주식회사 | Semiconductor manufacturing device |
| KR20080009868A (en) * | 2006-07-25 | 2008-01-30 | 주식회사 만도 | Oil pressure control valve of steering apparatus for vehicle |
| KR20080016290A (en) * | 2006-08-18 | 2008-02-21 | 동우 화인켐 주식회사 | A composition of etching solution for metal film using in manufacturing process of thin film transistor liquid crystal display and etching method using the same |
| JP5642967B2 (en) | 2007-11-22 | 2014-12-17 | 関東化学株式会社 | Etching solution composition |
| KR101302827B1 (en) * | 2013-03-20 | 2013-09-02 | 동우 화인켐 주식회사 | Silver ＆ silver alloy etchant for metal electrode ＆ reflection layer |
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2013
- 2013-10-08 KR KR1020130119796A patent/KR101537207B1/en active IP Right Grant
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- 2014-11-11 KR KR1020140156431A patent/KR101695608B1/en active IP Right Grant
Patent Citations (2)
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| KR20080009866A (en) * | 2006-07-25 | 2008-01-30 | 동우 화인켐 주식회사 | Silver & silver alloy etchant for metal electrode & reflection layer |
| KR20090081566A (en) * | 2008-01-24 | 2009-07-29 | 동우 화인켐 주식회사 | Etchant composition for Ag thin layer and method for fabricating metal pattern using the same |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10611962B2 (en) | 2018-04-23 | 2020-04-07 | Samsung Display Co., Ltd. | Etchant composition and manufacturing method of metal pattern using the same |
| US10636666B1 (en) | 2018-10-11 | 2020-04-28 | Samsung Display Co., Ltd. | Etchant and method for manufacturing display device using the same |
| US11091694B2 (en) | 2018-11-14 | 2021-08-17 | Samsung Display Co., Ltd. | Etching composition, method for forming pattern and method for manufacturing a display device using the same |
| US11639470B2 (en) | 2020-12-28 | 2023-05-02 | Samsung Display Co., Ltd. | Etching composition for thin film containing silver, method for forming pattern and method for manufacturing a display device using the same |
Also Published As
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|---|---|
| KR20140048045A (en) | 2014-04-23 |
| KR20140138571A (en) | 2014-12-04 |
| KR101695608B1 (en) | 2017-01-13 |
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