KR20000038843A - Method for manufacturing tantalum electrolysis capacitor using conductive polymer layer - Google Patents
Method for manufacturing tantalum electrolysis capacitor using conductive polymer layer Download PDFInfo
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- KR20000038843A KR20000038843A KR1019980053971A KR19980053971A KR20000038843A KR 20000038843 A KR20000038843 A KR 20000038843A KR 1019980053971 A KR1019980053971 A KR 1019980053971A KR 19980053971 A KR19980053971 A KR 19980053971A KR 20000038843 A KR20000038843 A KR 20000038843A
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- pellet
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- polypyrrole
- tantalum
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 229910052715 tantalum Inorganic materials 0.000 title claims abstract description 54
- 239000003990 capacitor Substances 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- 229920001940 conductive polymer Polymers 0.000 title claims abstract description 10
- 238000005868 electrolysis reaction Methods 0.000 title abstract 3
- 239000008188 pellet Substances 0.000 claims abstract description 49
- 239000003792 electrolyte Substances 0.000 claims abstract description 34
- 239000007800 oxidant agent Substances 0.000 claims abstract description 15
- 239000000243 solution Substances 0.000 claims description 47
- 229920000128 polypyrrole Polymers 0.000 claims description 46
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 38
- 239000000178 monomer Substances 0.000 claims description 18
- 238000006116 polymerization reaction Methods 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- 230000001590 oxidative effect Effects 0.000 claims description 7
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical group [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 6
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 230000000379 polymerizing effect Effects 0.000 claims description 4
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 2
- SOCTUWSJJQCPFX-UHFFFAOYSA-N dichromate(2-) Chemical compound [O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O SOCTUWSJJQCPFX-UHFFFAOYSA-N 0.000 claims description 2
- AXZAYXJCENRGIM-UHFFFAOYSA-J dipotassium;tetrabromoplatinum(2-) Chemical compound [K+].[K+].[Br-].[Br-].[Br-].[Br-].[Pt+2] AXZAYXJCENRGIM-UHFFFAOYSA-J 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- 239000011812 mixed powder Substances 0.000 claims description 2
- VKJKEPKFPUWCAS-UHFFFAOYSA-M potassium chlorate Chemical compound [K+].[O-]Cl(=O)=O VKJKEPKFPUWCAS-UHFFFAOYSA-M 0.000 claims description 2
- 229910001487 potassium perchlorate Inorganic materials 0.000 claims description 2
- 239000012286 potassium permanganate Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 239000011550 stock solution Substances 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims 2
- 239000012895 dilution Substances 0.000 claims 1
- 238000010790 dilution Methods 0.000 claims 1
- 238000005470 impregnation Methods 0.000 claims 1
- 239000010410 layer Substances 0.000 description 55
- 239000000126 substance Substances 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 6
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- WBIQQQGBSDOWNP-UHFFFAOYSA-N 2-dodecylbenzenesulfonic acid Chemical compound CCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O WBIQQQGBSDOWNP-UHFFFAOYSA-N 0.000 description 2
- QWHHBVWZZLQUIH-UHFFFAOYSA-N 2-octylbenzenesulfonic acid Chemical compound CCCCCCCCC1=CC=CC=C1S(O)(=O)=O QWHHBVWZZLQUIH-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000011162 core material Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000003085 diluting agent Substances 0.000 description 2
- 229940060296 dodecylbenzenesulfonic acid Drugs 0.000 description 2
- 239000002019 doping agent Substances 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- -1 butylbenzenesulfonic acid (butylbenzenesulfonic acid) Chemical compound 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- RLSSMJSEOOYNOY-UHFFFAOYSA-N m-cresol Chemical compound CC1=CC=CC(O)=C1 RLSSMJSEOOYNOY-UHFFFAOYSA-N 0.000 description 1
- 229940100630 metacresol Drugs 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002904 solvent Substances 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
- H01G9/004—Details
- H01G9/022—Electrolytes; Absorbents
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Polyoxymethylene Polymers And Polymers With Carbon-To-Carbon Bonds (AREA)
Abstract
Description
본 발명은 전도성 고분자를 이용한 탄탈전해캐패시터의 제조에 관한 것으로서, 보다 상세하게는 폴리피롤을 전해질로 이용한 탄탈캐패시터의 제조방법에 관한 것이다.The present invention relates to the production of tantalum electrolytic capacitors using conductive polymers, and more particularly, to a method of manufacturing tantalum capacitors using polypyrrole as an electrolyte.
일반적으로 탄탈캐패시터는 체적당 용량이 크고 우수한 주파수 특성 및 온도특성을 가질뿐만 아니라 낮은 누설전류, 낮은 손실 및 낮은 임피던스 값으로 인하여 점차 그 사용이 증가하고 있는 추세이다. 탄탈캐패시터는 칩형(chip type; 일명 `표면실장형'), 딥형(dip type;일명 `리드형') 및 금속케이스형으로 분류되며, 그 용도는 칩형인 경우 주로 캠코더, 휴대용 전화기, 노트북 PC 등과 같은 민생기기의 표면실장 부품(SMD) 세트에 장착, 사용되며, 딥형인 경우 오디오, TV 등의 민생기기에, 그리고 금속 케이스형의 경우 군용과 같이 고신뢰성이 요구되는 특수용도에 사용된다.In general, tantalum capacitors have a larger capacity per volume, have excellent frequency characteristics and temperature characteristics, and are increasingly used due to low leakage current, low loss, and low impedance values. Tantalum capacitors are classified into chip type (aka surface mount type), dip type (lead type) and metal case type, and their uses are mainly camcorders, mobile phones, notebook PCs, etc. It is mounted and used in the surface mount parts (SMD) set of the same civil equipment, and in the case of the deep type, it is used in the civil devices such as audio and TV, and in the case of the metal case type, which is required for high reliability such as military use.
보통 탄탈캐패시터는 도1에 도시된 바와같이, 내부에 핵심소자인 탄탈륨펠릿(10)이 위치하고, 상기 탄탈륨 펠릿(10)에는 도2와 같이, 양극단자(20)과 음극단자(30)가 형성된 구조를 갖는다. 상기 탄탈륨 펠릿(10)은 캐패시터의 용량을 결정하고, 기타 주요특성에 중요한 영향을 미치는 탄탈캐패시터의 핵심소재로서, 미세하고 복잡한 형태의 탄탈륨 분말을 사용하여 일정크기로 성형 및 소결되어 약 0.7-2μm의 미세기공이 50-60% 차지하고 있는 다공질체이다.In general, as shown in FIG. 1, a tantalum capacitor includes a tantalum pellet 10, which is a core element, and the tantalum pellet 10 includes a positive electrode terminal 20 and a negative electrode terminal 30 as shown in FIG. 2. Has a structure. The tantalum pellet 10 is a core material of the tantalum capacitor which determines the capacity of the capacitor and has a significant influence on other main characteristics. The tantalum pellet 10 is formed and sintered to a predetermined size using fine and complex forms of tantalum powder, and is about 0.7-2 μm. It is a porous body that accounts for 50-60% of micropores.
상기한 구조를 갖는 탄탈전해캐패시터의 제조는 크게 (탄탈륨 펠릿 제조)→(화성)→(소성)→(케이스조립)→(검사)의 순으로 행해진다. 상기 탄탈륨 펠릿(10)은 화성처리를 통해 유전체층(Ta2O5)을 형성하고, 이후 소성과정에서 캐패시터의 음극층(MnO2/C/Ag층)이 형성된다. 이러한 화성 및 소성단계에서 화성 및 소성처리액을 탄탈륨 펠릿의 미세한 공극을 따라 침투시키면, 소정시간 경과후 처리액이 열화학적 반응에 의해 고체화되고, 이 고체가 전해질을 대신하므로써, 캐패시터의 특성을 나타내게 된다. 따라서, 탄탈캐패시터의 특성은 여러 제조공정 단계중에서도 특히 화성 및 소성공정에 의해 큰영향을 받게 된다.The production of a tantalum electrolytic capacitor having the above structure is largely performed in the order of (tantalum pellet production)-(chemical conversion)-(calcination)-(case assembly)-(inspection). The tantalum pellet 10 is formed by forming a dielectric layer (Ta 2 O 5 ) through a chemical conversion treatment, and then a cathode layer (MnO 2 / C / Ag layer) of a capacitor is formed in the firing process. If the chemical and calcined liquids are permeated along the fine pores of the tantalum pellet in this chemical and calcining step, after a predetermined time, the treated liquid is solidified by a thermochemical reaction, and this solid replaces the electrolyte, thereby exhibiting the characteristics of the capacitor. do. Therefore, the properties of tantalum capacitors are greatly affected by the chemical conversion and firing processes, among other manufacturing process steps.
한편, 탄탈을 유전체로 사용하는 탄탈고체 전해캐패시터의 전해질로 사용되는 이산화망간(MnO2)의 문제점에 대한 해결방안으로 최근에는 비교적 전기적 특성과 신뢰성이 우수한 전도성 고분자를 전해질로 사용한 제품들이 생산되고 있다. 전도성 고분자중의 하나인 폴리피롤(polypyrrole)은 고주파 특성이 우수하고 비교적 내열특성이 양호하여 여러 종류의 전해캐패시터의 전해질로 사용되는 추세이다.On the other hand, as a solution to the problem of manganese dioxide (MnO 2 ) used as the electrolyte of tantalum solid electrolytic capacitors using tantalum as a dielectric, products using conductive polymers having relatively high electrical characteristics and reliability have been produced as electrolytes. Polypyrrole, one of the conductive polymers, has a tendency to be used as an electrolyte of various types of electrolytic capacitors because of its high frequency characteristics and relatively good heat resistance.
전도성 고분자인 폴리피롤을 이용한 탄탈전해캐패시터에 대한 종래의 제조방법은 유전체 피막이 형성된 탄탈륨 펠릿에 피롤을 직접 화학중합하여 폴리피롤층을 형성하거나 또는 화학중합후 전기중합을 하는 방법이 있다. 그러나, 화학중합에 의한 방법만으로는 탄탈전해캐패시터의 후막 형성이 어렵고 화학중합과 전기중합을 병행하여 폴리피롤 후막을 형성하려면 장치비가 많이 들고 공정이 복잡해질뿐만아니라 무엇보다도 적정한 두께의 후막을 얻기도 힘들다. 특히, 처음부터 폴리피롤용액에 함침하여 전해질층을 형성하려 하여도 건조후 용제의 기공이 존재하고, 폴리피롤의 분자크기가 크므로 유전체 피막에 형성된 피트의 내부까지 함침시키기 어렵다는 단점이 있다.Conventional manufacturing methods for tantalum electrolytic capacitors using polypyrrole, which is a conductive polymer, have a method of directly polymerizing pyrrole to tantalum pellets on which dielectric films are formed to form a polypyrrole layer, or electropolymerization after chemical polymerization. However, it is difficult to form a thick film of a tantalum electrolytic capacitor only by the method of chemical polymerization, and to form a polypyrrole thick film by a combination of chemical polymerization and electropolymerization, it is difficult to obtain a thick film having an appropriate thickness and, above all, a complicated process. In particular, even when the electrolyte layer is formed by impregnating the polypyrrole solution from the beginning, pores of the solvent exist after drying, and since the molecular size of the polypyrrole is large, it is difficult to impregnate the inside of the pit formed in the dielectric film.
따라서, 본 발명은 폴리피롤을 전해질로 이용하는 탄탈전해캐패시터의 제조시 전해질층을 유전체 피막에 형성된 피트의 내부까지 치밀하게 밀착시키고 후막을 형성시키므로써 전기적 특성을 개선하고 양극단자와 음극단자의 단락을 방지함은 물론 내전압을 향상시킬 수 있는 탄탈전해캐패시터의 제조방법을 제공함에 그 목적이 있다.Therefore, the present invention improves the electrical properties and prevents short circuit between the positive and negative terminals by closely contacting the electrolyte layer to the inside of the pit formed in the dielectric film and forming a thick film when manufacturing a tantalum electrolytic capacitor using polypyrrole as an electrolyte. In addition, the purpose of the present invention is to provide a method for manufacturing a tantalum electrolytic capacitor which can improve the breakdown voltage.
도1은 일반적인 탄탈전해캐패시터의 내부 구조도1 is an internal structure diagram of a typical tantalum electrolytic capacitor
도2는 도1의 탄탈전해캐패시터용 펠릿의 정면도Figure 2 is a front view of the pellet for tantalum electrolytic capacitor of Figure 1
도3은 본 발명의 탄탈전해캐패시터용 펠릿의 표면층 구조도Figure 3 is a structure diagram of the surface layer of the pellet for tantalum electrolytic capacitor of the present invention
* 도면의 주요부분에 대한 부호의 설명 *Explanation of symbols on the main parts of the drawings
10 ...... 탄탈륨 펠릿 12 ....... 유전체층10 ...... Tantalum Pellets 12 ....... Dielectric Layer
14 ...... 폴리피롤전해질층 15 ....... 전기전도성층14 ...... Polypyrrole Electrolyte Layer 15 ....... Conductive Layer
상기 목적 달성을 위한 본 발명은 탄탈륨 펠릿에 유전체층을 마련한 후, 유전체층이 마련된 펠릿에 전도성 고분자층을 형성함을 포함하여 구성되는 탄탈전해캐패시터의 제조방법에 있어서,In the present invention for achieving the above object, in the manufacturing method of the tantalum electrolytic capacitor comprising the formation of a conductive polymer layer on the pellet provided with a dielectric layer, the dielectric layer is provided in the pellet,
상기 유전체층이 마련된 펠릿을 피롤단량체 함유 용액과 산화제 용액을 이용하여 중합처리하는 단계;Polymerizing the pellet provided with the dielectric layer using a pyrrole monomer-containing solution and an oxidant solution;
상기 중합처리된 펠릿을 다시 폴리피롤 함유 용액에 함침하여 펠릿의 표면에 폴리피롤층을 형성하는 단계;Impregnating the polymerized pellet into a polypyrrole-containing solution to form a polypyrrole layer on the surface of the pellet;
폴리피롤 전해질층이 형성된 펠릿에 전기전도성층을 형성하는 단계; 를 포함하여 구성되는 전도성 고분자층을 이용한 탄탈전해캐패시터의 제조방법에 관한 것이다.Forming an electrically conductive layer on the pellet on which the polypyrrole electrolyte layer is formed; It relates to a method of manufacturing a tantalum electrolytic capacitor using a conductive polymer layer comprising a.
이하, 본 발명을 상세히 설명한다.Hereinafter, the present invention will be described in detail.
탄탈전해캐패시터의 전해질층을 구성하는 폴리피롤 용액은, 보통 5-고리 복소환 피롤단량체와 도판트가 용해된 용액에 산화제를 적하하여 중합된 폴리피롤을 클로로포름이나 메타크레졸에 녹인 전도성 용액을 이용한다. 탄탈전해캐패시터의 표층에 폴리피롤 전해질층을 형성하기 위해 직접 상기 폴리피롤용액에 함침하여 형성하거나 유전체에 화학중합을 하거나 또는 화학중합후 전기중합을 하는 경우 폴리피롤 분자의 크기가 크기 때문에 탄탈륨 펠릿에 형성되어 있는 유전체 피막에 형성된 피트 내부까지 폴리피롤의 침투가 어렵고, 내부기공이 생기거나 유전체층과 전해질층간의 밀착이 저하되고 후막 형성이 어렵다.In the polypyrrole solution constituting the electrolyte layer of the tantalum electrolytic capacitor, an oxidizing agent is added dropwise to a solution in which a 5-ring heterocyclic pyrrole monomer and a dopant are dissolved, and a conductive solution in which the polymerized polypyrrole is dissolved in chloroform or metacresol is used. In order to form the polypyrrole electrolyte layer on the surface of the tantalum electrolytic capacitor, the polypyrrole solution is formed by directly impregnating the polypyrrole solution, chemically polymerizing the dielectric, or electropolymerizing after the chemical polymerization. It is difficult to penetrate the polypyrrole to the inside of the pit formed in the dielectric film, to form internal pores or to decrease the adhesion between the dielectric layer and the electrolyte layer and to form a thick film.
이런 단점을 해결하고자 본 발명은 상기 폴리피롤 용액을 이용함에 있어 우선, 유전체층이 마련된 탄탈륨 펠릿을 피롤단량체가 함유된 용액에 함침하여 탄탈륨 펠릿 피막의 내부까지 완전히 폴리피롤 전해질층을 마련하여 내부기공이 없도록 하고 그 위에 폴리피롤 용액을 이용하여 후막을 형성함에 특징으로 한다.In order to solve this drawback, the present invention, in using the polypyrrole solution, first impregnates the tantalum pellet having the dielectric layer in the solution containing the pyrrole monomer to prepare the polypyrrole electrolyte layer completely up to the inside of the tantalum pellet coating so that there are no internal pores. It is characterized by forming a thick film using a polypyrrole solution thereon.
도3은 본 발명에 따라 제조된 탄탈륨 펠릿의 표층 구조를 보이고 있다. 본 발명의 펠릿(10)은, 도3과 같이 탄탈륨 펠릿의 표면에 화성처리를 통해 유전체층(Ta2O5)(12)이 형성되고, 그 위에 폴리피롤 전해질층(14)이 형성된다. 이때, 본 발명의 탄탄펠릿소자에 형성된 전해질층(14)은 유전층이 형성된 탄탈펠릿소자를 피롤단량체가 함유된 용액에 함침하고, 여기에 산화제를 이용하여 중합시키므로써 폴리피롤 전해질층(14a)을 마련한 다음, 폴리피롤 전해질층(14a)이 형성된 펠릿소자를 폴리피롤 용액에 침적하여 다시 폴리피롤 전해질층(14b)을 형성시킨다. 상기 폴리피롤 전해질층은 그 두께가 5~100㎛의 범위를 갖도록 함이 적당하다.Figure 3 shows the surface structure of tantalum pellets prepared according to the present invention. In the pellet 10 of the present invention, as shown in FIG. 3, a dielectric layer (Ta 2 O 5 ) 12 is formed on the surface of the tantalum pellet through chemical conversion, and a polypyrrole electrolyte layer 14 is formed thereon. At this time, the electrolyte layer 14 formed in the tantalum pellet element of the present invention is impregnated with a tantalum pellet element having a dielectric layer in a solution containing a pyrrole monomer, and polymerized by using an oxidizing agent to prepare a polypyrrole electrolyte layer 14a Next, a pellet element on which the polypyrrole electrolyte layer 14a is formed is deposited in a polypyrrole solution to form the polypyrrole electrolyte layer 14b again. The polypyrrole electrolyte layer is appropriate to have a thickness of 5 ~ 100㎛ range.
그리고, 상기 중합처리는 유전체층이 마련된 펠릿을 피롤단량체 함유 용액에 함침한 후 꺼내고, 다시 산화제 용액에 함침시켜도 중합처리가 가능하지만 꺼낸 펠릿의 표면에 산화제 용액을 분사하여도 가능하다. 또한, 그 반대 순서로도 유전체층이 마련된 펠릿을 산화제 용액에 함침한 후 꺼내고, 다시 피롤단량체 함유 용액에 함침시키거나 혹은 꺼낸 펠릿의 표면에 피롤단량체 함유 용액을 분사하여도 무방하다.In the polymerization treatment, the pellets provided with the dielectric layer are impregnated with a pyrrole monomer-containing solution, and then taken out, and then impregnated with the oxidant solution. In the reverse order, the pellet provided with the dielectric layer may be impregnated with the oxidant solution, and then taken out, and may be impregnated again with the pyrrole monomer-containing solution or sprayed with the pyrrole monomer-containing solution on the surface of the taken out pellet.
본 발명은 폴리피롤 전해질층(14)을 형성함에 있어, 피롤 단량체 용액에 탄탈소자를 함침하여 탄탈펠릿의 유전체 표층 사이에 조밀한 피트(pit)까지 폴리피롤 전해질층(14a)를 형성시키고 그 위에 폴리피롤 용액을 이용하여 전해질층(14a)을 형성하여 친화력과 접착력이 우수하고, 후막 형성이 가능하다.In forming the polypyrrole electrolyte layer 14, the pyrrole monomer solution is impregnated with a tantalum element to form a polypyrrole electrolyte layer 14a up to a dense pit between the dielectric surface layers of the tantalum pellet and the polypyrrole solution thereon. By forming the electrolyte layer (14a) using the excellent affinity and adhesion, it is possible to form a thick film.
상기 폴리피롤 용액은 기존의 도데실벤젠술폰산은 물론 부틸벤젠술폰산(butylbenzenesulfonic acid) 또는 옥틸벤젠술폰산(octylbenzenesulfonic acid)과 같이, n≥4이상인 알킬벤젠술폰산(alkylbenzenesulfonic acid; CnH2n+1C6H4SO3H)을 도판트로 하는 폴리피롤 용액을 사용할 수 있다. 피롤 단량체 함유 용액은 원액 또는 그 희석액을 사용할 수 있으며, 희석액을 사용하는 경우 그 농도를 적어도 20%이상으로 희석함이 보다 바람직하다.The polypyrrole solution is not only conventional dodecylbenzenesulfonic acid but also butylbenzenesulfonic acid (butylbenzenesulfonic acid) or octylbenzenesulfonic acid (octylbenzenesulfonic acid), n≥4 or more alkylbenzenesulfonic acid (alkylbenzenesulfonic acid; C n H 2n + 1 C 6 H A polypyrrole solution having 4 SO 3 H) as a dopant can be used. The pyrrole monomer-containing solution may use a stock solution or a diluent thereof, and more preferably dilute the concentration to at least 20% when the diluent is used.
또한, 본 발명의 경우 폴리피롤 중합에 사용되는 산화제로는 암모늄퍼술페이트[ammonium persulfate;(NH4)2S2O8], 염화제이철(FeCl3), 과망간산칼륨(KMnO4), 디크롬산염(K2Cr2O7), 요오드산염칼륨(KIO3), 과염소산칼륨(KClO4) 또는 염소산칼륨(KClO3) 등 다양한 산화제가 적용될 수 있다.In the present invention, the oxidizing agent used in the polypyrrole polymerization may be ammonium persulfate (NH 4 ) 2 S 2 O 8 ], ferric chloride (FeCl 3 ), potassium permanganate (KMnO 4 ), dichromate ( K 2 Cr 2 O 7 ), potassium iodide (KIO 3 ), potassium perchlorate (KClO 4 ) or potassium chlorate (KClO 3 ) can be applied.
이후, 상기 폴리피롤 전해질층(14a)(14b)이 마련된 탄탈펠릿소자(10)에 도3과 같이, 전기전도성층(15)을 형성한다. 상기 전기전도성층은 탄소 또는 금속분말이나 혼합분말로 구성되어진 페이스트를 사용하여 형성될 수 있으며, 바람직하게는, 탄소함유용액에 함침시키므로써 탄소층을 마련한 다음, 이 탄소층이 형성된 펠릿을 은함유 용액에 함침시켜 최종적으로 Ag층을 형성하는 것이다.Thereafter, an electrically conductive layer 15 is formed on the tantalum pellet element 10 provided with the polypyrrole electrolyte layers 14a and 14b, as shown in FIG. The electrically conductive layer may be formed using a paste composed of carbon or metal powder or mixed powder. Preferably, the carbon layer is prepared by impregnating the carbon-containing solution, and then containing the silver pellet containing the carbon layer. The solution is impregnated to finally form an Ag layer.
이하, 본 발명을 실시예를 통하여 구체적으로 설명한다.Hereinafter, the present invention will be described in detail through examples.
[실시예]EXAMPLE
종래예1Conventional Example 1
화성처리하여 Ta2O5유전층을 형성한 탄탈펠릿소자에 폴리피롤 전해질층을 화학중합하여 형성한 다음, 탄소층과 Ag층을 형성시켰다.The polypyrrole electrolyte layer was chemically polymerized and formed on a tantalum pellet device having a Ta 2 O 5 dielectric layer formed by chemical conversion, and then a carbon layer and an Ag layer were formed.
종래예2Conventional Example 2
화성처리하여 Ta2O5유전층을 형성한 탄탈펠릿소자를 폴리피롤 용액에 침적하여 폴리피롤 전해질층을 형성한 후, 탄소층과 Ag층을 형성시켰다.A tantalum pellet element having a Ta 2 O 5 dielectric layer formed by chemical treatment was deposited on a polypyrrole solution to form a polypyrrole electrolyte layer, and then a carbon layer and an Ag layer were formed.
발명예Inventive Example
동일한 탄탈펠릿소자를 먼저 피롤 단량체에 함침하고, 여기에 산화제로서 20%FeCl3용액으로 중합하였다. 이어서, 상기 탄탈소자를 폴리피롤 용액에 침적하여 약 50㎛ 두께의 폴리피롤 전해질층을 형성한 다음, 탄소층과 Ag층을 마련하였다. 이때, 사용된 폴리피롤 용액은 피롤단량체:도데실벤젠술폰산:암모늄퍼설페이트를 1:0.5:0.13의 몰비로 혼합하여 중합한 후 클로로포름 용액을 이용하여 용액화시켰다.The same tantalum pellet element was first impregnated into the pyrrole monomer, and then polymerized with a 20% FeCl 3 solution as an oxidizing agent. Subsequently, the tantalum element was deposited in a polypyrrole solution to form a polypyrrole electrolyte layer having a thickness of about 50 μm, and then a carbon layer and an Ag layer were prepared. In this case, the polypyrrole solution used was polymerized by mixing a pyrrole monomer: dodecylbenzenesulfonic acid: ammonium persulfate in a molar ratio of 1: 0.5: 0.13 and then liquefied using a chloroform solution.
이와같이, 제조된 탄탈캐퍼시터에 대해 두 종류의 주파수에서 전기적 특성을 측정하고, 그 결과를 표1에 나타내었다.As such, the electrical properties of the manufactured tantalum capacitors were measured at two kinds of frequencies, and the results are shown in Table 1.
표1에서와 같이, 동일한 용량의 탄탈전해캐패시터를 제조하는 경우 본 발명에 따라 제조된 것이 기존보다 전기용량, 임피던스, 및 내전압 등에서 우수함을 알 수 있었다.As shown in Table 1, when the tantalum electrolytic capacitor of the same capacity is manufactured, it was found that the one manufactured according to the present invention is superior in capacitance, impedance, and withstand voltage than the conventional one.
상술한 바와 같이, 본 발명은 탄탈소자의 유전체 피막에 형성된 피트의 내부까지 치밀하게 폴리피롤 전해질층을 밀착 형성시키고, 그 위에 폴리피롤 용액을 이용하여 전해질층을 형성함으로써 친화력, 접착력이 우수한 후막을 형성하여 전기적 특성이 보다 향상된 탄탈전해캐패시터를 제공할 수 있는 매우 유용한 효과가 있다.As described above, the present invention closely forms a polypyrrole electrolyte layer to the inside of the pit formed in the dielectric film of the tantalum element, and forms an electrolyte layer using a polypyrrole solution thereon to form a thick film having excellent affinity and adhesion. It is very useful to provide a tantalum electrolytic capacitor with improved electrical characteristics.
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US7623284B2 (en) | 2003-04-15 | 2009-11-24 | Lg Chem, Ltd. | Electropolymerization method for preparing nano-tube type conducting polymer using porous template, method for preparing electrochromic device, and electrochromic device prepared therefrom |
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US7204895B2 (en) | 2002-04-15 | 2007-04-17 | Lg Chem, Ltd. | Electropolymerization method for preparing nano-tube type conducting polymer using porous template, method for preparing electrochromic device, and electrochromic device prepared therefrom |
US7623284B2 (en) | 2003-04-15 | 2009-11-24 | Lg Chem, Ltd. | Electropolymerization method for preparing nano-tube type conducting polymer using porous template, method for preparing electrochromic device, and electrochromic device prepared therefrom |
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