JP4241495B2 - 導電性高分子の製造方法と製造装置 - Google Patents
導電性高分子の製造方法と製造装置 Download PDFInfo
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- 229920001940 conductive polymer Polymers 0.000 title claims description 88
- 238000000034 method Methods 0.000 title claims description 22
- 238000006116 polymerization reaction Methods 0.000 claims description 90
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 50
- 239000012298 atmosphere Substances 0.000 claims description 32
- 239000000178 monomer Substances 0.000 claims description 24
- 230000001590 oxidative effect Effects 0.000 claims description 23
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- 239000007800 oxidant agent Substances 0.000 claims description 22
- 239000000126 substance Substances 0.000 claims description 20
- 239000000758 substrate Substances 0.000 claims description 17
- GKWLILHTTGWKLQ-UHFFFAOYSA-N 2,3-dihydrothieno[3,4-b][1,4]dioxine Chemical compound O1CCOC2=CSC=C21 GKWLILHTTGWKLQ-UHFFFAOYSA-N 0.000 claims description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 239000001301 oxygen Substances 0.000 claims description 11
- 229910052760 oxygen Inorganic materials 0.000 claims description 11
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 10
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 claims description 8
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 6
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical class [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 5
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 4
- 229930192474 thiophene Natural products 0.000 claims description 4
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 3
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical class [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims description 2
- 230000000379 polymerizing effect Effects 0.000 claims description 2
- 239000003021 water soluble solvent Substances 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims 1
- 239000010410 layer Substances 0.000 description 68
- 239000004020 conductor Substances 0.000 description 47
- 239000003990 capacitor Substances 0.000 description 43
- 239000007787 solid Substances 0.000 description 30
- 239000000243 solution Substances 0.000 description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 15
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 15
- 229910052799 carbon Inorganic materials 0.000 description 15
- 239000007784 solid electrolyte Substances 0.000 description 15
- 229910052709 silver Inorganic materials 0.000 description 14
- 239000004332 silver Substances 0.000 description 14
- 239000011521 glass Substances 0.000 description 11
- 229920000642 polymer Polymers 0.000 description 11
- 230000003647 oxidation Effects 0.000 description 10
- 238000007254 oxidation reaction Methods 0.000 description 10
- 229920005989 resin Polymers 0.000 description 10
- 239000011347 resin Substances 0.000 description 10
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 239000007788 liquid Substances 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000010419 fine particle Substances 0.000 description 6
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 230000009471 action Effects 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 4
- 239000003973 paint Substances 0.000 description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 239000003822 epoxy resin Substances 0.000 description 3
- 239000011888 foil Substances 0.000 description 3
- 238000000879 optical micrograph Methods 0.000 description 3
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- 239000011148 porous material Substances 0.000 description 3
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- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 2
- 239000007900 aqueous suspension Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
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- 238000001035 drying Methods 0.000 description 2
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- 239000007789 gas Substances 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- 239000010955 niobium Substances 0.000 description 2
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- 229920006254 polymer film Polymers 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 229910052715 tantalum Inorganic materials 0.000 description 2
- 229910001936 tantalum oxide Inorganic materials 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000004581 coalescence Methods 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- 229910000366 copper(II) sulfate Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 description 1
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 1
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000002120 nanofilm Substances 0.000 description 1
- 238000010525 oxidative degradation reaction Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 229920000123 polythiophene Polymers 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 229910001925 ruthenium oxide Inorganic materials 0.000 description 1
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- PCCVSPMFGIFTHU-UHFFFAOYSA-N tetracyanoquinodimethane Chemical compound N#CC(C#N)=C1C=CC(=C(C#N)C#N)C=C1 PCCVSPMFGIFTHU-UHFFFAOYSA-N 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- Other Resins Obtained By Reactions Not Involving Carbon-To-Carbon Unsaturated Bonds (AREA)
- Polyoxymethylene Polymers And Polymers With Carbon-To-Carbon Bonds (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
Description
ガラス基板上に化学酸化重合における水蒸気濃度の相違による導電性高分子膜の性状を確認した。そのときの断面模式図を図1に示す。
弁作用を有するタンタル金属の比表面積が100000μF・V/gである微粉末を、0.3mm×3.0mm×3.8mmに成形し、陽極引き出し用タンタルワイヤーリードを備えた形で真空焼結し、焼結体ペレットからなる陽極導体を作製した。次に、この陽極導体を90℃の5重量%リン酸水溶液中で印加電圧7.5Vの条件で化成することにより、陽極導体の表面に誘電体層として酸化タンタル膜を形成した。
弁作用を有するタンタル金属の比表面積が100000μF・V/gである微粉末を、0.3mm×3.0mm×3.8mmに成形し、陽極引き出し用タンタルワイヤーリードを備えた形で真空焼結し、焼結体ペレットからなる陽極導体を作製した。次に、この陽極導体を90℃の5重量%リン酸水溶液中で印加電圧7.5Vの条件で化成することにより、陽極導体の表面に誘電体層として酸化タンタル膜を形成した。
1.本文に記載するいずれかの方法により得られた導電性高分子膜であって、平坦な導電性高分子膜を用いたことを特徴とする電子部品。
2.前記導電性高分子膜の表裏密度がほぼ等しい前記第1項に記載の電子部品。
3.前記電子部品が、弁金属からなる陽極導体と、前記陽極導体の表面に形成された誘電体層と、前記誘電体層の表面に形成され少なくとも導電性高分子層を含む固体電解質とを含む固体電解コンデンサである前記第1項または第2項に記載の電子部品。
4.弁金属からなる陽極導体と、前記陽極導体の表面に形成された誘電体層と、前記誘電体層の表面に形成され少なくとも導電性高分子層を含む固体電解質とを含む固体電解コンデンサの製造方法において、前記陽極導体は、モノマーと酸化剤の反応を60℃以下で行う工程と85℃以上の過飽和水蒸気雰囲気の重合槽中で行われる工程により製造されることを特徴とする固体電解コンデンサの製造方法。
2 誘電体層
3 固体電解質
4 陰極導体
5 カーボン層
6 外装銀導電性樹脂層
7 重合用陽極(陽電極)
8 重合用陰極(陰電極)
9 重合溶液
10 導電性高分子膜
11 ガラス基板
Claims (11)
- 少なくともモノマーと酸化剤とを反応させ、導電性高分子を得る化学重合法において、前記モノマーと酸化剤の反応を少なくとも過飽和水蒸気雰囲気の重合槽中で行うことを特徴とする導電性高分子の製造方法。
- 前記過飽和水蒸気雰囲気の水蒸気濃度が、5体積%以上である請求項1に記載の導電性高分子の製造方法。
- 前記過飽和水蒸気雰囲気の温度が、85℃以上である請求項1に記載の導電性高分子の製造方法。
- モノマーと酸化剤の反応を過飽和水蒸気雰囲気の重合槽中で行う前に、予め85℃未満の温度で予備重合する請求項1に記載の導電性高分子の製造方法。
- 前記過飽和水蒸気雰囲気の酸素濃度が21体積%未満である請求項1に記載の導電性高分子の製造方法。
- 前記モノマーがピロール、チオフェン、3,4−エチレンジオキシチオフェン、アニリン及びそれらの誘導体から選ばれる少なくとも1つである請求項1に記載の導電性高分子の製造方法。
- 前記酸化剤が酸化マンガン、鉄(III)塩、銅(II)塩、過酸化水素及び過硫酸塩から選ばれる少なくとも1つである請求項1に記載の導電性高分子の製造方法。
- 前記モノマーと前記酸化剤が少なくとも水溶性の溶媒もしくは水に溶解している請求項1に記載の導電性高分子の製造方法。
- 前記導電性高分子層を側面から観察したとき、基体からの剥離距離dと、長さLとの比率d/Lが、0.02以下である請求項1に記載の導電性高分子の製造方法。
- 少なくともモノマーと酸化剤とを重合槽中で重合するための製造装置であって、
前記過飽和水蒸気雰囲気の重合槽には、少なくとも前記重合槽にドライエアーと熱交換器により発生された水蒸気とを前記重合槽に送気する装置を含み、
前記モノマーと酸化剤の反応を少なくとも過飽和水蒸気雰囲気の重合槽中で行うことを特徴とする導電性高分子の製造装置。 - 前記熱交換器により発生された水蒸気の温度が前記ドライエアーの温度より高い請求項10に記載の導電性高分子の製造装置。
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JP4241495B2 true JP4241495B2 (ja) | 2009-03-18 |
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JP2006351609A (ja) * | 2005-06-13 | 2006-12-28 | Rohm Co Ltd | 固体電解コンデンサ |
US8274777B2 (en) | 2008-04-08 | 2012-09-25 | Micron Technology, Inc. | High aspect ratio openings |
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