KR20000004061A - Dielectric substance forming method on aluminum foil by sol-gel process - Google Patents
Dielectric substance forming method on aluminum foil by sol-gel process Download PDFInfo
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- KR20000004061A KR20000004061A KR1019980025444A KR19980025444A KR20000004061A KR 20000004061 A KR20000004061 A KR 20000004061A KR 1019980025444 A KR1019980025444 A KR 1019980025444A KR 19980025444 A KR19980025444 A KR 19980025444A KR 20000004061 A KR20000004061 A KR 20000004061A
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- aluminum foil
- sol solution
- sol
- dielectric
- dielectric substance
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 68
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 239000011888 foil Substances 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 40
- 238000003980 solgel method Methods 0.000 title claims abstract description 7
- 239000000126 substance Substances 0.000 title abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 15
- 239000003085 diluting agent Substances 0.000 claims abstract description 10
- 230000007062 hydrolysis Effects 0.000 claims abstract description 10
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims description 14
- 239000003381 stabilizer Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000005470 impregnation Methods 0.000 claims description 6
- 239000003989 dielectric material Substances 0.000 claims description 5
- NGCRLFIYVFOUMZ-UHFFFAOYSA-N 2,3-dichloroquinoxaline-6-carbonyl chloride Chemical compound N1=C(Cl)C(Cl)=NC2=CC(C(=O)Cl)=CC=C21 NGCRLFIYVFOUMZ-UHFFFAOYSA-N 0.000 claims description 3
- 150000004703 alkoxides Chemical class 0.000 claims description 3
- ZTILUDNICMILKJ-UHFFFAOYSA-N niobium(v) ethoxide Chemical compound CCO[Nb](OCC)(OCC)(OCC)OCC ZTILUDNICMILKJ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims 1
- 239000002184 metal Substances 0.000 claims 1
- 238000005530 etching Methods 0.000 abstract description 13
- 229940125725 tranquilizer Drugs 0.000 abstract 2
- 239000003204 tranquilizing agent Substances 0.000 abstract 2
- 230000002936 tranquilizing effect Effects 0.000 abstract 2
- 238000000151 deposition Methods 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 23
- 239000003990 capacitor Substances 0.000 description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 10
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- FGRBYDKOBBBPOI-UHFFFAOYSA-N 10,10-dioxo-2-[4-(N-phenylanilino)phenyl]thioxanthen-9-one Chemical compound O=C1c2ccccc2S(=O)(=O)c2ccc(cc12)-c1ccc(cc1)N(c1ccccc1)c1ccccc1 FGRBYDKOBBBPOI-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- -1 chlorine ions Chemical class 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hcl hcl Chemical compound Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/0029—Processes of manufacture
- H01G9/0032—Processes of manufacture formation of the dielectric layer
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/07—Dielectric layers
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
Abstract
Description
본 발명은 알루미늄 호일의 유전체 생성 공정에 관한 것으로, 특히 알루미늄 전해 콘덴서 제조시 사용하는 알루미늄 호일의 표면에 유전체층이 형성되도록 하여 에칭 공정을 생략할 수 있는 sol-gel 법에 의한 알루미늄 호일상의 유전체 생성방법에 관한 것이다.BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a dielectric generation process of aluminum foil. In particular, a dielectric layer is formed on an aluminum foil by a sol-gel method in which a dielectric layer is formed on the surface of an aluminum foil used in manufacturing an aluminum electrolytic capacitor, thereby eliminating an etching process. It is about a method.
알루미늄 전해 콘덴서는 99.9% 이상의 고순도 알루미늄호일을 전극으로 하여 제조된 콘덴서이다. 도 1은 알루미늄 전해 콘덴서의 제조 과정의 순서도로서, 각 공정을 설명하면 다음과 같다.An aluminum electrolytic capacitor is a capacitor manufactured using high purity aluminum foil of 99.9% or more as an electrode. 1 is a flowchart of a manufacturing process of an aluminum electrolytic capacitor, which will be described below.
압연된 알루미늄 호일의 평활면을 전기화학적으로 표면을 에칭하여 실효면적을 증가시키는 에칭과정(S1), 에칭된 알루미늄 호일을 전기분해하여 알루미늄 호일의 표면에 유전체가 되는 산화 알루미늄(Al2O3)피막을 생성하는 화성과정(S2), 화성 과정을 거쳐 화성된 전극박을 제품의 용량에 맞는 일정한 규격으로 절단하고 인출단자를 접속한 후 음극박과 전해지(separator)를 넣어 동심원으로 절단하는 절단 과정(S3), 권취한 소자에 전해액을 넣는 함침 공정(S4)을 거치게 된다.Etching process (S1) to increase the effective area by etching the surface of the rolled aluminum foil electrochemically, aluminum oxide (Al 2 O 3 ) which becomes a dielectric on the surface of the aluminum foil by electrolysis of the etched aluminum foil The process of forming the film (S2), the process of forming the electrode foil is cut to a certain standard according to the capacity of the product, the cutting terminal is connected to the lead terminal and the cathode foil and the separator (separator) to cut into concentric circles (S3), the impregnation process (S4) which inject | pours electrolyte solution into the wound element is passed.
상기와 같은 공정에 있어서, 도 2에 도시되어 있는 바와 같이, 알루미늄 전해 콘덴서의 공정중 에칭 공정은 염산 수용액(2)에 알루미늄 호일(1)이 지나가도록 하고, 외부에서 일정 전압을 가하여서 이루어지게 된다. 도 2에 도시되어 있는 에칭 공정을 수행하게 되면, 도 3에 도시되어 있는 것과 마찬가지로 알루미늄 호일의 단면이 형성되어 알루미늄 호일 표면의 실효 면적을 증가시키게 된다.In the above process, as shown in FIG. 2, the etching process of the aluminum electrolytic capacitor is performed by passing the aluminum foil 1 to the aqueous hydrochloric acid solution 2 and applying a constant voltage from the outside. do. When the etching process illustrated in FIG. 2 is performed, a cross section of the aluminum foil is formed, as shown in FIG. 3, thereby increasing the effective area of the aluminum foil surface.
위와 같이 알루미늄 호일에 에칭 공정을 거치게 되면 다음과 같은 문제점이 발생함을 알 수 있다.As described above, when the etching process is performed on the aluminum foil, the following problems may occur.
첫째, 알루미늄 호일의 단면이 도 3과 같이 되므로서 알루미늄 호일의 기계적 강도가 떨어지게 된다. 둘째, 에칭 공정시 염산(HCl)을 사용하기 때문에 염산 수용액의 염소 이온(Cl-)으로 인해 알루미늄 호일의 부식이 촉진되어 완성된 소자의 수명과 성능이 저하된다. 셋째, 유전체로 산화 알루미늄(Al2O3)만을 사용할 수 있기 때문에 용량 구현에 한계가 있다. 넷째, 완성된 알루미늄 전해 콘덴서의 용량을 증가시키기 위해서는 알루미늄 호일을 에칭하기 때문에 고가인 순도 99.99% 알루미늄 호일을 사용해야 한다.First, since the cross section of the aluminum foil is as shown in Figure 3, the mechanical strength of the aluminum foil is reduced. Second, since hydrochloric acid (HCl) is used in the etching process, chlorine ions (Cl − ) in an aqueous hydrochloric acid solution promote corrosion of the aluminum foil, thereby degrading the lifetime and performance of the finished device. Third, since only aluminum oxide (Al 2 O 3 ) can be used as the dielectric, there is a limit in implementing the capacity. Fourth, in order to increase the capacity of the finished aluminum electrolytic capacitor, since the aluminum foil is etched, an expensive 99.99% purity aluminum foil should be used.
본 발명은 위와같은 문제점을 해소하기 위해 안출된 것으로, 알루미늄 전해 콘덴서의 제조시 사용하는 알루미늄 호일의 표면에 유전체가 형성되도록 하여 에칭 공정이 없이도 알루미늄 전해 콘덴서의 용량 확대 한계를 극복할 수 있는 sol-gel 법에 의한 알루미늄 호일상의 유전체 생성방법을 제공하는 것을 목적으로 한다.The present invention has been made to solve the above problems, sol- so that the dielectric is formed on the surface of the aluminum foil used in the manufacture of the aluminum electrolytic capacitor can overcome the limit of the capacity expansion of the aluminum electrolytic capacitor without the etching process. An object of the present invention is to provide a method for producing a dielectric on an aluminum foil by gel method.
상기 목적을 달성하기 위한 본 발명 sol-gel 법에 의한 알루미늄 호일상의 유전체 생성방법은, 알루미늄 호일에 유전체를 형성시키는 위한 sol 용액을 제조하는 sol 용액 제조 공정, 상기 공정에서 만들어진 sol 용액에 희석제를 넣어 필요한 농도를 맞추는 희석제 첨가 공정, 반응 속도를 맞추기 위해 안정제를 첨가하는 안정제 첨가 공정, sol 용액에서 유전체 물질을 생성하기 위한 가수분해 공정, 상기 가수분해 공정을 거친 sol 용액에 알루미늄 호일을 함침시키는 알루미늄 호일 함침 공정, sol 용액이 묻은 알루미늄 호일을 상온에서 48시간 또는 200℃ 내지 350 ℃ 의 온도로 20 내지 40 분간 건조하는 건조 공정, 상기 건조 공정을 거친 알루미늄 호일을 550℃ 내지 650 ℃ 의 온도로 60 분간 열처리하는 열처리 공정으로 구성되는 것을 특징으로 한다.In order to achieve the above object, a method for producing a dielectric on an aluminum foil by the sol-gel method of the present invention includes a process for preparing a sol solution for forming a dielectric on an aluminum foil, and a diluent in a sol solution produced in the process. Diluent adding process to adjust the concentration required, stabilizer addition process to add stabilizer to adjust reaction rate, hydrolysis process to generate dielectric material in sol solution, aluminum impregnating aluminum foil in sol solution after the hydrolysis process Foil impregnation process, drying process for drying aluminum foil with sol solution at room temperature for 48 hours or for 20 to 40 minutes at a temperature of 200 ℃ to 350 ℃, aluminum foil subjected to the drying process at a temperature of 550 ℃ to 650 ℃ 60 It is characterized by consisting of a heat treatment step of heat treatment for a minute.
도 1은 일반적인 알루미늄 전해 콘덴서의 제조 공정을 나타내는 순서도.1 is a flowchart illustrating a manufacturing process of a general aluminum electrolytic capacitor.
도 2는 일반적인 알루미늄 전해 콘덴서의 에칭 공정을 나타내는 단면도.2 is a cross-sectional view showing an etching process of a general aluminum electrolytic capacitor.
도 3은 에칭 공정에 의해 생성된 알루미늄 호일의 단면도.3 is a cross-sectional view of an aluminum foil produced by an etching process.
도 4는 본 발명에 따른 sol-gel 법에 의한 유전체 생성 공정의 순서도.Figure 4 is a flow chart of the dielectric production process by the sol-gel method according to the present invention.
<도면의 주요부분에 대한 부호의 설명><Description of the symbols for the main parts of the drawings>
1 : 알루미늄 호일1: aluminum foil
2 : 염산 수용액2: aqueous hydrochloric acid solution
이하, 본 발명을 첨부된 도면들을 참조하여 상세히 설명한다.Hereinafter, the present invention will be described in detail with reference to the accompanying drawings.
본 발명 알루미늄 유전체 생성방법은, 알루미늄 호일에 유전체를 형성시키는 위한 sol 용액을 제조하는 sol 용액 제조 공정(S10), 상기 공정(S10)에서 만들어진 sol 용액에 희석제를 넣어 필요한 농도를 맞추는 희석제 첨가 공정(S20), 반응 속도를 맞추기 위해 안정제를 첨가하는 안정제 첨가 공정(S30), sol 용액에서 유전체 물질을 생성하기 위한 가수분해 공정(S40), 상기 가수분해 공정(S40)을 거친 sol 용액에 알루미늄 호일을 함침시키는 알루미늄 호일 함침 공정(S50), sol 용액이 묻은 알루미늄 호일을 상온에서 48시간 또는 200℃ 내지 350 ℃ 의 온도로 20 내지 40 분간 건조하는 건조 공정(S60), 상기 건조 공정(S60)을 거친 알루미늄 호일을 550℃ 내지 650 ℃ 의 온도로 60 분간 열처리하는 열처리 공정(S70)을 포함하여 구성되는 것을 특징으로 한다.The aluminum dielectric production method of the present invention is a sol solution manufacturing step (S10) of preparing a sol solution for forming a dielectric on an aluminum foil, a diluent addition step of adding a diluent to the sol solution made in the step (S10) to meet the required concentration ( S20), a stabilizer addition step of adding a stabilizer to adjust the reaction rate (S30), a hydrolysis step (S40) for generating a dielectric material in the sol solution, the aluminum foil is applied to the sol solution that has undergone the hydrolysis step (S40) Impregnated aluminum foil impregnation process (S50), drying step of drying the aluminum foil with the sol solution for 20 to 40 minutes at room temperature for 48 hours or from 200 ℃ to 350 ℃, the drying step (S60) It characterized in that it comprises a heat treatment step (S70) for heat-treating the aluminum foil for 60 minutes at a temperature of 550 ℃ to 650 ℃.
본 발명의 구성과 작용을 살펴보면 다음과 같다.Looking at the configuration and operation of the present invention.
금속알콕사이드(alkoxide)류인 탄탈 에톡사이드(Tantalum ethoxide) 또는 니오븀 에톡사이드(Niobum ethoxide) 등을 이용하여 SOL 상태의 용액을 만든다(S10). 만들어진 용액에 에탄올, 메탄올 또는 부탄올과 같은 희석제를 첨가하여, 필요로 하는 농도로 맞춘다(S20). 희석제의 첨가에 의해 필요로 하는 농도가 된 sol 원액을 아세틸아세톤, 염산, 황산과 같은 물질을 첨가하여 sol 용액과 다른 물질과의 반응 속도를 조절하도록 한다. 이때 아세틸아세톤, 염산, 황산은 안정제 및 촉매로서 작용하여 sol 용액과 물과의 급격한 반응이 일어나는 것을 방지하도록 한다(S30).Metallic alkoxides such as tantalum ethoxide or niobium ethoxide are used to make a SOL solution (S10). Diluents such as ethanol, methanol or butanol are added to the prepared solution and adjusted to the required concentration (S20). The concentration of the sol stock solution, which is required by the addition of the diluent, is added to acetylacetone, hydrochloric acid and sulfuric acid to control the reaction rate of the sol solution with other substances. At this time, acetylacetone, hydrochloric acid, sulfuric acid to act as a stabilizer and a catalyst to prevent the rapid reaction between the sol solution and water (S30).
안정제를 넣은 sol 용액에 증류수를 넣어 가수 분해 작용이 일어나도록 한다(S40). 가수분해에 의해 다음과 같은 유전체 물질이 생성됨을 알 수 있다.Distilled water is added to the sol solution containing the stabilizer so that hydrolysis occurs (S40). It can be seen that the following dielectric materials are produced by the hydrolysis.
알콕사이드(alkoxide) + H2O -> MO(금속산화물) + ROHAlkoxide + H 2 O-> MO (metal oxide) + ROH
탄탈 에톡사이드(Tantalum ethoxide) + H2O -> Ta2O5+ 10R(OH)Tantalum ethoxide + H 2 O-> Ta 2 O 5 + 10R (OH)
니오븀 에톡사이드(Niobum ethoxide) + H2O -> Nb2O5+ ROHNiobium ethoxide + H 2 O-> Nb 2 O 5 + ROH
[표 1]에서는 sol 원액에 따라 알루미늄 호일에 형성되는 유전체의 성분에 따른 유전율을 나타내고 있다.Table 1 shows the permittivity according to the components of the dielectric formed in the aluminum foil according to the sol stock solution.
[표 1]TABLE 1
가수 분해에 의해 유전체가 생성되어 있는 sol 용액에 알루미늄 호일을 함침시킨다. 알루미늄 호일에 sol 용액이 일정량 만큼 묻을 정도로 1 회이상 7회까지 반복하여 함침시키도록 한다(S50).The aluminum foil is impregnated into the sol solution in which the dielectric is produced by hydrolysis. In order to impregnate the aluminum foil by repeating at least one or seven times so that a sol solution is buried in a predetermined amount (S50).
함침 공정에 의해 필요한 양의 sol 용액이 묻어있는 알루미늄 호일을 다음과 같은 선택적 조건에 따라 건조 시키도록 한다(S60).The aluminum foil containing the required amount of sol solution by the impregnation process is to be dried according to the following optional conditions (S60).
상온에서 건조시는 48 시간을 건조시키고, 200 ~ 350 ℃ 온도 상태에서는 20 ~ 40분간 건조시키면다. 이때 2가지 건조 방법에 의해 얻어지는 결과는 같기 때문에 작업자가 필요에 따라 건조조건을 선택하면 된다.When drying at room temperature, 48 hours are dried, and 20 to 40 minutes is dried at a temperature of 200 ~ 350 ℃. At this time, since the results obtained by the two drying methods are the same, the operator may select the drying conditions as necessary.
알루미늄 호일상의 sol 상태의 용액은 위와 같은 건조 과정에 의해 gel 상태로 되고, 이를 550 ℃ 내지 650 ℃ 의 온도로 60 분간 열처리(S70)하게 되면, 알루미늄 호일의 표면에는 유전체층의 형성이 완성되어 알루미늄 전해 콘덴서의 제조에 사용할 수 있게 된다.The solution of the sol state on the aluminum foil becomes a gel state by the above drying process, and when it is heat-treated (S70) for 60 minutes at a temperature of 550 ° C. to 650 ° C., the formation of the dielectric layer is completed on the surface of the aluminum foil. It becomes possible to use for manufacture of an electrolytic capacitor.
이때 형성되는 유전체층은 이전에 알루미늄 호일의 표면에 형성되는 산화 알루미늄(Al2O3)보다 높은 유전율을 갖기 때문에 이전의 알루미늄 전해 콘덴서 제조공정에서 표면적을 증가시키기 위한 에칭 공정과 유전체를 코팅하는 화성 공정을 생략하고, 절단 공정과 함침 공정으로 바로 이행할 수 있게 된다.At this time, since the dielectric layer formed has a higher dielectric constant than aluminum oxide (Al 2 O 3 ) previously formed on the surface of the aluminum foil, an etching process for increasing the surface area of the previous aluminum electrolytic capacitor manufacturing process and a chemical conversion process for coating the dielectric material. Omitting, it is possible to immediately proceed to the cutting step and the impregnation step.
상기한 바와같이 본 발명은 알루미늄 전해 콘덴서를 제조하는 알루미늄 호일의 표면에 Ta2O5 ,Nb2O5또는ZrO2로 형성되는 유전체층을 형성하여 알루미늄 호일의 유전율을 증가시키게 되고, 알루미늄 호일 표면에 유전체층이 형성되므로써 알루미늄 호일의 에칭 공정과 화성 공정을 생략해도 되므로 공정수가 줄어들게 되는 효과가 있게 된다.As described above, the present invention forms a dielectric layer formed of Ta 2 O 5, Nb 2 O 5, or ZrO 2 on the surface of the aluminum foil to manufacture the aluminum electrolytic capacitor, thereby increasing the dielectric constant of the aluminum foil, Since the dielectric layer is formed, the etching process and the chemical conversion process of the aluminum foil may be omitted, thereby reducing the number of processes.
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KR1019980025444A KR20000004061A (en) | 1998-06-30 | 1998-06-30 | Dielectric substance forming method on aluminum foil by sol-gel process |
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KR1019980025444A KR20000004061A (en) | 1998-06-30 | 1998-06-30 | Dielectric substance forming method on aluminum foil by sol-gel process |
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1998
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