US20100065434A1 - Method of manufacturing a solid electrolytic capacitor with a sufficiently low impedance in a high frequency range - Google Patents

Method of manufacturing a solid electrolytic capacitor with a sufficiently low impedance in a high frequency range Download PDF

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Publication number
US20100065434A1
US20100065434A1 US12/557,612 US55761209A US2010065434A1 US 20100065434 A1 US20100065434 A1 US 20100065434A1 US 55761209 A US55761209 A US 55761209A US 2010065434 A1 US2010065434 A1 US 2010065434A1
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Prior art keywords
oxidant
conductive polymer
solid electrolytic
electrolytic capacitor
oxide film
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US12/557,612
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English (en)
Inventor
Yasuhisa Sugawara
Kazuyuki Katoh
Masako Ohya
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Tokin Corp
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NEC Tokin Corp
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Assigned to NEC TOKIN CORPORATION reassignment NEC TOKIN CORPORATION ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: KATOH, KAZUYUKI, OHYA, MASAKO, SUGAWARA, YASUHISA
Publication of US20100065434A1 publication Critical patent/US20100065434A1/en
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    • 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
    • H01G9/008—Terminals
    • H01G9/012—Terminals specially adapted for solid capacitors
    • 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
    • H01G9/0036—Formation of the solid electrolyte 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
    • H01G9/022—Electrolytes; Absorbents
    • H01G9/025—Solid electrolytes
    • H01G9/028—Organic semiconducting electrolytes, e.g. TCNQ
    • 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
    • H01G9/15—Solid electrolytic capacitors

Definitions

  • This invention relates to a method of manufacturing a solid electrolytic capacitor using a conductive polymer as an electrolyte layer.
  • capacitors for use in a high frequency range of 100 kHz to several tens of MHz there are a mica capacitor and a multilayer ceramic capacitor. It is difficult to increase the capacitances of these capacitors because the sizes thereof become large.
  • electrolytic capacitors such as an aluminum electrolytic capacitor and a tantalum solid electrolytic capacitor.
  • an electrolyte layer of the aluminum electrolytic capacitor is in the form of an electrolyte solution
  • an electrolyte layer of the tantalum solid electrolytic capacitor is made of manganese dioxide. Since the conductivities of these electrolyte layers are low, it is difficult to design the capacitors to have sufficiently low impedances in a high frequency range.
  • Patent Document 1 JP-B-H4-56445 discloses a solid electrolytic capacitor using a conductive polymer compound with high conductivity as an electrolyte layer. Since the conductivity of the electrolyte layer is high, it is possible to reduce the impedance of this solid electrolytic capacitor in a high frequency range.
  • Patent Document 2 JP-A-H9-320900 discloses a solid electrolytic capacitor using polyethylenedioxythiophene with high conductivity as an electrolyte layer. Since the conductivity of the electrolyte layer is high, it is also possible to reduce the impedance of this solid electrolytic capacitor in a high frequency range.
  • a method of manufacturing a solid electrolytic capacitor which comprises a valve metal, a dielectric oxide film layer formed by anodizing a surface of the valve metal, and an electrolyte layer containing a conductive polymer, the electrolyte layer being formed on the dielectric oxide film layer by chemical oxidative polymerization, wherein a solution containing ammonium peroxodisulfate and adjusted to pH 6 to 8 is used as an oxidant for causing the chemical oxidative polymerization.
  • a method of manufacturing a solid electrolytic capacitor comprising preparing a valve metal, forming a dielectric oxide film layer by anodizing a surface of the valve metal, and forming an electrolyte layer containing a conductive polymer on the dielectric oxide film layer by chemical oxidative polymerization using an oxidant, wherein a solution containing ammonium peroxodisulfate and adjusted to pH 6 to 8 is used as the oxidant.
  • FIG. 1 is an exemplary sectional view for explaining a solid electrolytic capacitor manufacturing method according to an exemplary embodiment of this invention.
  • FIG. 2 is a partial enlarged view showing only a portion a of FIG. 1 in an enlarged manner.
  • This manufacturing method is basically nearly the same as a conventional solid electrolytic capacitor manufacturing method except an oxidant for use in forming a conductive polymer layer of a solid electrolyte. That is, materials of other than the oxidant, shapes, and so on can be known ones and are not particularly limited.
  • a solid electrolytic capacitor shown in FIGS. 1 and 2 can be manufactured by a manufacturing method which will be described hereinbelow.
  • a valve metal 1 is prepared and a dielectric oxide film layer 2 is formed by anodizing surfaces of the valve metal 1 .
  • an electrolyte layer containing a conductive polymer (hereinafter referred to as a “conductive polymer layer”) 3 is formed by chemical oxidative polymerization of a monomer such as pyrrole using as an oxidant an ammonium peroxodisulfate solution adjusted to pH 6 to 8.
  • a cathode layer 4 made of a conductive paste is formed on the conductive polymer layer 3 Further, predetermined packaging is carried out, thereby obtaining a solid electrolytic capacitor.
  • the reaction rate is suppressed as compared with a case of using, as an oxidant, iron ions or an ammonium peroxodisulfate solution with a pH of less than 6, Therefore, the conductive polymer layer 3 is densely formed on the dielectric oxide film layer 2 .
  • a low-impedance solid electrolytic capacitor excellent in tan ⁇ and ESR characteristics.
  • a dopant contained in the oxidant is preferably one or more selected from p-toluenesulfonic acid, phenolsulfonic acid, naphthalenesulfonic acid, and aromatic derivatives each having sulfonic groups.
  • the dopant is preferably a derivative of naphthalene having sulfonic groups.
  • a conductive polymer excellent in conductivity is obtained by selectively using p-toluenesulfonic acid, phenolsulfonic acid, and naphthalenesulfonic acid as the dopant.
  • this conductive polymer as the conductive polymer layer 3 , it is possible to obtain a low-impedance solid electrolytic capacitor excellent in tan ⁇ and ESR characteristics.
  • a conductive polymer more excellent in conductivity is obtained.
  • this conductive polymer as the conductive polymer layer 3 , it is possible to obtain a low-impedance solid electrolytic capacitor excellent in tans and ESR characteristics.
  • the concentration of ammonium peroxodisulfate in the ammonium peroxodisulfate solution used as the oxidant is preferably 1 to 50 mass %. If the concentration of ammonium peroxodisulfate is greater than 50 mass %, the ammonium peroxodisulfate becomes saturated in the aqueous solution at room temperature and thus crystals thereof remain in the solution. Therefore, there is a problem that when filling the oxidant into fine pores of the valve metal, the fine pores are plugged so that the coverage of a conductive polymer layer decreases.
  • the concentration of ammonium peroxodisulfate is smaller than 1 mass %, since the amount of a conductive polymer formed at a time is small, the number of times of polymerization for forming the conductive polymer layer 3 becomes very large.
  • the oxidant ammonium peroxodisulfate solution be adjusted to pH 6 to 8. If the pH is smaller than 6 the polymerization rate becomes high and therefore there is a problem that it is difficult to densely form a conductive polymer on the dielectric oxide film layer 2 and thus a capacitor with excellent tan ⁇ and ESR is not obtained.
  • the amount of cations used for pH adjustment increases in the oxidant so that the cations are entrapped as a dopant of a conductive polymer, and therefore, the conductivity decreases as compared with a conductive polymer using, as a dopant, one or more selected from p-toluenesulfonic acid, phenolsulfonic acid, naphthalenesulfonic acid, and aromatic derivatives each having sulfonic groups.
  • p-toluenesulfonic acid phenolsulfonic acid, naphthalenesulfonic acid, and aromatic derivatives each having sulfonic groups.
  • a solid electrolytic capacitor manufactured by the manufacturing method of Example 1 has the same structure as that of the solid electrolytic capacitor described in the embodiment and, therefore, a description will be given with reference to FIGS. 1 and 2 again.
  • a solid electrolytic capacitor shown in FIGS. 1 and 2 comprises a valve metal 1 as an anode-side electrode, a dielectric oxide film layer 2 formed by anodizing surfaces of the valve metal 1 , a conductive polymer layer 3 as a solid electrolyte, a cathode layer 4 made of a conductive paste, external electrodes 61 and 62 , and a packaging resin 8 .
  • valve metal 1 in the form of a sintered body of tantalum powder having a size of 3.5 mm (length) ⁇ 3.0 mm (width) ⁇ 1.5 mm (thickness) was first produced. A voltage of 30V was applied to the valve metal 1 in a phosphoric acid aqueous solution to anodize it, thereby obtaining a pellet covered with the dielectric oxide film layer 2 over its entire tantalum powder surfaces.
  • an aqueous solution as an oxidant, containing 20 mass % ammonium peroxodisulfate and 20 mass % 1,3,6-naphthalenetrisulfonic acid and adjusted to pH 7 using imidazole.
  • the pellet covered with the dielectric oxide film layer 2 was immersed for 10 minutes to fill the oxidant therein.
  • the pellet was immersed in pyrrole for 10 minutes and then maintained at room temperature for 30 minutes, thereby polymerizing the pyrrole.
  • the sequence of operations (polymerization operations) of filling the oxidant and filling the pyrrole was repeated five times to form the conductive polymer layer 3 in the form of a conductive polypyrrole layer.
  • the pellet formed with the conductive polymer layer 3 was washed with ethanol and, after drying, a silver paste was coated on surfaces of the conductive polypyrrole layer and then heated to be cured, thereby forming the cathode layer 4 with a thickness of 10 to 50 ⁇ m to obtain a capacitor element.
  • the cathode layer 4 of the capacitor element was connected to the external electrode 61 .
  • a valve metal wire 7 drawn out of the tantalum sintered body in advance was welded to the external electrode 62 .
  • the capacitor element was covered from the outside with an epoxy resin to form the packaging resin 8 , thereby completing the solid electrolytic capacitor having the structure shown in FIG. 1 .
  • Example 1 polypyrrole was used for forming the conductive polymer layer 3 .
  • an equivalent operation can be obtained using polythiophene, polyaniline, a derivative of such a conductive polymer, or the like
  • Example 2 In the manufacturing method of Example 2, the pH of an oxidant aqueous solution containing a dopant was adjusted to 6. The others were the same as in Example 1.
  • a valve metal 1 being the same as in Example 1 was prepared and a dielectric oxide film layer 2 was formed thereon by the same method as in Example 1, thereby obtaining a pellet.
  • an aqueous solution as an oxidant, containing 20 mass % ammonium peroxodisulfate and 20 mass % 1,3,6-naphthalenetrisulfonic acid and adjusted to pH 6 using imidazole.
  • the pellet covered with the dielectric oxide film layer 2 was immersed for 10 minutes to fill the oxidant therein.
  • the pellet was immersed in pyrrole for 10 minutes and then maintained at room temperature for 30 minutes, thereby polymerizing the pyrrole.
  • the sequence of polymerization operations of filling the oxidant and filling the pyrrole was repeated five times to form a conductive polymer layer 3 in the form of a conductive polypyrrole layer.
  • Example 2 polypyrrole was used for forming the conductive polymer layer 3 .
  • an equivalent operation can be obtained using polythiophene, polyaniline, a derivative of such a conductive polymer, or the like.
  • Example 3 In the manufacturing method of Example 3, the pH of an oxidant aqueous solution containing a dopant was adjusted to 8. The others were the same as in Example 1.
  • a valve metal 1 being the same as in Example 1 was prepared and a dielectric oxide film layer 2 was formed thereon by the same method as in Example 1, thereby obtaining a pellet.
  • an aqueous solution as an oxidant, containing 20 mass % ammonium peroxodisulfate and 20 mass % 1,3,6-naphthalenetrisulfonic acid and adjusted to pH 8 using imidazole.
  • the pellet covered with the dielectric oxide film layer 2 was immersed for 10 minutes to fill the oxidant therein.
  • the pellet was immersed in pyrrole for 10 minutes and then maintained at room temperature for 30 minutes, thereby polymerizing the pyrrole.
  • the sequence of polymerization operations of filling the oxidant and filling the pyrrole was repeated five times to form a conductive polymer layer 3 in the form of a conductive polypyrrole layer.
  • Example 3 polypyrrole was used for forming the conductive polymer layer 3 .
  • an equivalent operation can be obtained using polythiophene, polyaniline, a derivative of such a conductive polymer, or the like.
  • Example 4 In the manufacturing method of Example 4, use was made of an oxidant containing p-toluenesulfonic acid as a dopant The others were the same as in Example 1.
  • a valve metal 1 being the same as in Example 1 was prepared and a dielectric oxide film layer 2 was formed thereon by the same method as in Example 1, thereby obtaining a pellet.
  • an aqueous solution as an oxidant, containing 20 mass % ammonium peroxodisulfate and 20 mass % p-toluenesulfonic acid and adjusted to pH 7 using imidazole.
  • the pellet covered with the dielectric oxide film layer 2 was immersed for 10 minutes to fill the oxidant therein.
  • the pellet was immersed in pyrrole for 10 minutes and then maintained at room temperature for 30 minutes, thereby polymerizing the pyrrole.
  • the sequence of polymerization operations of filling the oxidant and filling the pyrrole was repeated five times to form a conductive polymer layer 3 in the form of a conductive polypyrrole layer.
  • Example 4 polypyrrole was used for forming the conductive polymer layer 3 .
  • an equivalent operation can be obtained using polythiophene, polyaniline, a derivative of such a conductive polymer, or the like.
  • Example 5 the concentration of ammonium peroxodisulfate in an oxidant aqueous solution containing a dopant was set to 1 mass %. The others were the same as in Example 1.
  • a valve metal 1 being the same as in Example 1 was prepared and a dielectric oxide film layer 2 was formed thereon by the same method as in Example 1, thereby obtaining a pellet.
  • an aqueous solution as an oxidant containing 1 mass % ammonium peroxodisulfate and 20 mass % 1,3,6-naphthalenetrisulfonic acid and adjusted to pH 7 using imidazole,
  • the pellet covered with the dielectric oxide film layer 2 was immersed for 10 minutes to fill the oxidant therein.
  • the pellet was immersed in pyrrole for 10 minutes and then maintained at room temperature for 30 minutes, thereby polymerizing the pyrrole.
  • the sequence of polymerization operations of filling the oxidant and filling the pyrrole was repeated five times to form a conductive polymer layer 3 in the form of a conductive polypyrrole layer.
  • Example 5 polypyrrole was used for forming the conductive polymer layer 3 .
  • an equivalent operation can be obtained using polythiophene, polyaniline, a derivative of such a conductive polymer, or the like.
  • Example 6 the concentration of ammonium peroxodisulfate in an oxidant aqueous solution containing a dopant was set to 50 mass %. The others were the same as in Example 1.
  • a valve metal 1 being the same as in Example 1 was prepared and a dielectric oxide film layer 2 was formed thereon by the same method as in Example 1, thereby obtaining a pellet.
  • an aqueous solution as an oxidant, containing 50 mass % ammonium peroxodisulfate and 20 mass % 1,3,6-naphthalenetrisulfonic acid and adjusted to pH 7 using imidazole,
  • the pellet covered with the dielectric oxide film layer 2 was immersed for 10 minutes to fill the oxidant therein.
  • the pellet was immersed in pyrrole for 10 minutes and then maintained at room temperature for 30 minutes, thereby polymerizing the pyrrole.
  • the sequence of polymerization operations of filling the oxidant and filling the pyrrole was repeated five times to form a conductive polymer layer 3 in the form of a conductive polypyrrole layer.
  • Example 6 polypyrrole was used for forming the conductive polymer layer 3 .
  • an equivalent operation can be obtained using polythiophene, polyaniline, a derivative of such a conductive polyme, or the like.
  • a valve metal 1 being the same as in Example 1 was prepared and a dielectric oxide film layer 2 was formed thereon by the same method as in Example 1 thereby obtaining a pellet.
  • This pellet was immersed in a ferric methanol p-toluenesulfonate solution being an oxidant for 10 minutes to fill the oxidant therein. Then, after drying the pellet at room temperature for 30 minutes, the pellet was immersed in pyrrole for 10 minutes and then maintained at room temperature for 30 minutes, thereby polymerizing the pyrrole.
  • the sequence of polymerization operations of filling the oxidant and filling the pyrrole was repeated five times to form a conductive polymer layer 3 in the form of a conductive polypyrrole layer.
  • a valve metal 1 being the same as in Example 1 was prepared and a dielectric oxide film layer 2 was formed thereon by the same method as in Example 1, thereby obtaining a pellet.
  • an aqueous solution as an oxidant, containing 20 mass % ammonium peroxodisulfate and 20 mass % 1,3,6-naphthalenetrisulfonic acid and having a pH of 1
  • the pellet covered with the dielectric oxide film layer 2 was immersed for 10 minutes to fill the oxidant therein.
  • the pellet was immersed in pyrrole for 10 minutes and then maintained at room temperature for 30 minutes, thereby polymerizing the pyrrole.
  • the sequence of polymerization operations of filling the oxidant and filling the pyrrole was repeated five times to form a conductive polymer layer 3 in the form of a conductive polypyrrole layer.
  • Table 1 shows capacitance, tan ⁇ , and ESR characteristics of the solid electrolytic capacitors obtained by the manufacturing methods of Examples 1 to 6 and the manufacturing methods of Comparative Examples 1 and 2.
  • the number of samples was 20 per Example or Comparative Example and a value shown for each of the characteristics is an average of 20 samples.
  • a solid electrolytic capacitor using a conductive polymer as an electrolyte if the state of formation of the conductive polymer formed on a dielectric oxide film layer is bad, the coverage of particularly the inner conductive polymer is lowered and thus the capacitor with excellent tan ⁇ and ESR cannot be obtained.
  • the conductive polymer is densely formed on the dielectric oxide film layer so that the solid electrolytic capacitor with a low impedance in a high frequency range is obtained.
  • the low-impedance solid electrolytic capacitor excellent in tan ⁇ and ESR characteristics is obtained.
  • the polymerization rate of the conductive polymer becomes moderate so that the film of the conductive polymer is more densely formed on the dielectric oxide film layer, and thus the low-impedance solid electrolytic capacitor excellent in tan ⁇ and ESR characteristics is obtained.

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Manufacturing & Machinery (AREA)
  • Polyoxymethylene Polymers And Polymers With Carbon-To-Carbon Bonds (AREA)
US12/557,612 2008-09-12 2009-09-11 Method of manufacturing a solid electrolytic capacitor with a sufficiently low impedance in a high frequency range Abandoned US20100065434A1 (en)

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JP2008-234354 2008-09-12
JP2008234354A JP2010067875A (ja) 2008-09-12 2008-09-12 固体電解コンデンサの製造方法

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TW (1) TW201017699A (ja)

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6229689B1 (en) * 1996-07-16 2001-05-08 Nec Corporation Solid electrolyte capacitor and method for manufacturing the same
US6552896B1 (en) * 1999-10-28 2003-04-22 Matsushita Electric Industrial Co., Ltd. Solid electrolytic capacitor and method for manufacturing the same
US20030224110A1 (en) * 2002-06-03 2003-12-04 Kemet Electronics Corporation Process for producing a conductive polymer cathode coating on aluminum capacitor anode bodies with minimal anodic oxide dielectric degradation
US6813141B2 (en) * 2002-03-04 2004-11-02 Showa Denko Kabushiki Kaisha Solid electrolytic capacitor and method for producing the same
US20060047030A1 (en) * 2004-08-30 2006-03-02 Shin-Etsu Polymer Co., Ltd Conductive composition and conductive cross-linked product, capacitor and production method thereof, and antistatic coating material, antistatic coating, antistatic film, optical filter, and optical information recording medium
WO2007097364A1 (ja) * 2006-02-21 2007-08-30 Shin-Etsu Polymer Co., Ltd. コンデンサ及びコンデンサの製造方法
US7651637B2 (en) * 2005-02-08 2010-01-26 Tayca Corporation Dopant solution for an electroconductive polymer, an oxidant and dopant solution for an electroconductive polymer, an electroconductive composition and a solid electrolytic capacitor

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005203662A (ja) * 2004-01-19 2005-07-28 Japan Carlit Co Ltd:The 固体電解コンデンサの製造方法

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6229689B1 (en) * 1996-07-16 2001-05-08 Nec Corporation Solid electrolyte capacitor and method for manufacturing the same
US6552896B1 (en) * 1999-10-28 2003-04-22 Matsushita Electric Industrial Co., Ltd. Solid electrolytic capacitor and method for manufacturing the same
US6813141B2 (en) * 2002-03-04 2004-11-02 Showa Denko Kabushiki Kaisha Solid electrolytic capacitor and method for producing the same
US20030224110A1 (en) * 2002-06-03 2003-12-04 Kemet Electronics Corporation Process for producing a conductive polymer cathode coating on aluminum capacitor anode bodies with minimal anodic oxide dielectric degradation
US20060047030A1 (en) * 2004-08-30 2006-03-02 Shin-Etsu Polymer Co., Ltd Conductive composition and conductive cross-linked product, capacitor and production method thereof, and antistatic coating material, antistatic coating, antistatic film, optical filter, and optical information recording medium
US7651637B2 (en) * 2005-02-08 2010-01-26 Tayca Corporation Dopant solution for an electroconductive polymer, an oxidant and dopant solution for an electroconductive polymer, an electroconductive composition and a solid electrolytic capacitor
WO2007097364A1 (ja) * 2006-02-21 2007-08-30 Shin-Etsu Polymer Co., Ltd. コンデンサ及びコンデンサの製造方法
US20100165546A1 (en) * 2006-02-21 2010-07-01 Shin-Etsu Polymer Co., Ltd. Capacitor and method for producing thereof

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CN101673623A (zh) 2010-03-17
TW201017699A (en) 2010-05-01
KR20100031459A (ko) 2010-03-22

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