CN115298780A - 电解电容器 - Google Patents
电解电容器 Download PDFInfo
- Publication number
- CN115298780A CN115298780A CN202180022207.7A CN202180022207A CN115298780A CN 115298780 A CN115298780 A CN 115298780A CN 202180022207 A CN202180022207 A CN 202180022207A CN 115298780 A CN115298780 A CN 115298780A
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- CN
- China
- Prior art keywords
- acid
- epoxy resin
- electrolytic capacitor
- electrolyte
- examples
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- 239000003990 capacitor Substances 0.000 title claims abstract description 127
- 239000003822 epoxy resin Substances 0.000 claims abstract description 127
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 127
- 229920005989 resin Polymers 0.000 claims abstract description 67
- 239000011347 resin Substances 0.000 claims abstract description 67
- 239000011888 foil Substances 0.000 claims abstract description 38
- 238000007789 sealing Methods 0.000 claims abstract description 38
- 239000003792 electrolyte Substances 0.000 claims abstract description 37
- 239000000203 mixture Substances 0.000 claims abstract description 29
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 78
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 58
- 150000001412 amines Chemical class 0.000 claims description 37
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 claims description 24
- 239000003795 chemical substances by application Substances 0.000 claims description 24
- 150000001875 compounds Chemical class 0.000 claims description 23
- 239000000126 substance Substances 0.000 claims description 20
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 18
- 150000001768 cations Chemical class 0.000 claims description 15
- 239000007784 solid electrolyte Substances 0.000 claims description 15
- 239000004848 polyfunctional curative Substances 0.000 claims description 10
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 9
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 claims description 9
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 239000008151 electrolyte solution Substances 0.000 description 60
- 239000010410 layer Substances 0.000 description 49
- 239000002904 solvent Substances 0.000 description 33
- -1 glycidyl epoxy resins Chemical compound 0.000 description 29
- 239000002253 acid Substances 0.000 description 27
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 14
- 238000006243 chemical reaction Methods 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 14
- 229940021013 electrolyte solution Drugs 0.000 description 13
- 230000008646 thermal stress Effects 0.000 description 13
- 229920000547 conjugated polymer Polymers 0.000 description 12
- 150000008065 acid anhydrides Chemical class 0.000 description 11
- 235000013824 polyphenols Nutrition 0.000 description 11
- 229910052782 aluminium Inorganic materials 0.000 description 10
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- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 10
- 125000002091 cationic group Chemical group 0.000 description 9
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- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 7
- 229910021529 ammonia Inorganic materials 0.000 description 7
- 229910052796 boron Inorganic materials 0.000 description 7
- 230000008859 change Effects 0.000 description 7
- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 description 7
- 150000002989 phenols Chemical class 0.000 description 7
- GKWLILHTTGWKLQ-UHFFFAOYSA-N 2,3-dihydrothieno[3,4-b][1,4]dioxine Chemical compound O1CCOC2=CSC=C21 GKWLILHTTGWKLQ-UHFFFAOYSA-N 0.000 description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 6
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 6
- 238000005530 etching Methods 0.000 description 6
- 238000001704 evaporation Methods 0.000 description 6
- 239000000178 monomer Substances 0.000 description 6
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 description 6
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- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 description 5
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- 229930185605 Bisphenol Natural products 0.000 description 4
- 229920002943 EPDM rubber Polymers 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 4
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 4
- 125000000129 anionic group Chemical group 0.000 description 4
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 4
- 229920000172 poly(styrenesulfonic acid) Polymers 0.000 description 4
- 229920000768 polyamine Polymers 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 229940005642 polystyrene sulfonic acid Drugs 0.000 description 4
- YMMGRPLNZPTZBS-UHFFFAOYSA-N 2,3-dihydrothieno[2,3-b][1,4]dioxine Chemical class O1CCOC2=C1C=CS2 YMMGRPLNZPTZBS-UHFFFAOYSA-N 0.000 description 3
- FJKROLUGYXJWQN-UHFFFAOYSA-N 4-hydroxybenzoic acid Chemical compound OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 125000001931 aliphatic group Chemical group 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 229920005549 butyl rubber Polymers 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 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
- 230000007423 decrease Effects 0.000 description 3
- 125000003700 epoxy group Chemical group 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 238000007740 vapor deposition Methods 0.000 description 3
- WXTMDXOMEHJXQO-UHFFFAOYSA-N 2,5-dihydroxybenzoic acid Chemical compound OC(=O)C1=CC(O)=CC=C1O WXTMDXOMEHJXQO-UHFFFAOYSA-N 0.000 description 2
- OWCLRJQYKBAMOL-UHFFFAOYSA-N 2-butyloctanedioic acid Chemical compound CCCCC(C(O)=O)CCCCCC(O)=O OWCLRJQYKBAMOL-UHFFFAOYSA-N 0.000 description 2
- XWVFEDFALKHCLK-UHFFFAOYSA-N 2-methylnonanedioic acid Chemical compound OC(=O)C(C)CCCCCCC(O)=O XWVFEDFALKHCLK-UHFFFAOYSA-N 0.000 description 2
- VEORPZCZECFIRK-UHFFFAOYSA-N 3,3',5,5'-tetrabromobisphenol A Chemical compound C=1C(Br)=C(O)C(Br)=CC=1C(C)(C)C1=CC(Br)=C(O)C(Br)=C1 VEORPZCZECFIRK-UHFFFAOYSA-N 0.000 description 2
- YQUVCSBJEUQKSH-UHFFFAOYSA-N 3,4-dihydroxybenzoic acid Chemical compound OC(=O)C1=CC=C(O)C(O)=C1 YQUVCSBJEUQKSH-UHFFFAOYSA-N 0.000 description 2
- CWLKGDAVCFYWJK-UHFFFAOYSA-N 3-aminophenol Chemical compound NC1=CC=CC(O)=C1 CWLKGDAVCFYWJK-UHFFFAOYSA-N 0.000 description 2
- VPWNQTHUCYMVMZ-UHFFFAOYSA-N 4,4'-sulfonyldiphenol Chemical class C1=CC(O)=CC=C1S(=O)(=O)C1=CC=C(O)C=C1 VPWNQTHUCYMVMZ-UHFFFAOYSA-N 0.000 description 2
- OZJPLYNZGCXSJM-UHFFFAOYSA-N 5-valerolactone Chemical compound O=C1CCCCO1 OZJPLYNZGCXSJM-UHFFFAOYSA-N 0.000 description 2
- 229920003026 Acene Polymers 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- FFVAYYZTSSNEAY-UHFFFAOYSA-N C(C=1C(O)=CC=CC1)(=O)O.C(C=1C(O)=CC=CC1)(=O)O.[B] Chemical compound C(C=1C(O)=CC=CC1)(=O)O.C(C=1C(O)=CC=CC1)(=O)O.[B] FFVAYYZTSSNEAY-UHFFFAOYSA-N 0.000 description 2
- 244000025254 Cannabis sativa Species 0.000 description 2
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 description 2
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 2
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 description 2
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 2
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- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
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- 239000000654 additive Substances 0.000 description 2
- 239000001361 adipic acid Substances 0.000 description 2
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- 125000000217 alkyl group Chemical group 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- QMKYBPDZANOJGF-UHFFFAOYSA-N benzene-1,3,5-tricarboxylic acid Chemical compound OC(=O)C1=CC(C(O)=O)=CC(C(O)=O)=C1 QMKYBPDZANOJGF-UHFFFAOYSA-N 0.000 description 2
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- AKEUNCKRJATALU-UHFFFAOYSA-N 2,6-dihydroxybenzoic acid Chemical compound OC(=O)C1=C(O)C=CC=C1O AKEUNCKRJATALU-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明是涉及一种包括树脂层的电解电容器,且提供一种ESR经时性增大得到了抑制的电解电容器。电解电容器包括:电容器元件,具有阳极箔、阴极箔以及电解液;壳体,收容电容器元件;封口构件,对壳体进行封口;以及树脂层,配置在封口构件的附近。配置在封口构件的附近的树脂层包含不具有酯键的环氧树脂组合物。
Description
技术领域
本发明是涉及一种包括树脂层的电解电容器。
背景技术
利用钽或铝等阀作用金属的电解电容器通过将作为阳极侧相向电极的阀作用金属形成为烧结体或者蚀刻箔等形状来将电介质扩面化,而获得小型且大容量。此种电解电容器是为了使阳极的电介质氧化皮膜与相向电极密接,利用电解质填埋空隙而成。即,作为电解电容器,包括仅具有电解液的液体电解电容器、包括电解液与固体电解质的混合电解电容器、在电极双方形成有电介质皮膜的双极性电解电容器。
电解液含有乙二醇或γ-丁内酯作为溶媒、含有1,6-癸烷二羧酸、1,7-辛烷二羧酸、壬二酸等羧酸或其盐等作为溶质。所述电解液直接接触于电介质皮膜,并作为真正的阴极发挥作用,并且具有电介质皮膜的修复作用。然而,电解液会随着时间的经过发生向电解电容器的外部漏出的蒸发挥散。因此,电解电容器面临干涸,静电电容经时性下降,另外,损耗角的正切(tanδ)经时性上升,最终到达寿命终点。
因此,电容器元件被收容在有底的外装壳体中,利用封口构件密封外装壳体的开口,由此将含浸在电容器元件中的电解液密闭来抑制电解液的蒸发挥散,从而实现长寿命化。但是,封口构件使用丁基橡胶或乙烯丙烯二烯橡胶(三元乙丙橡胶(ethylenepropylene diene monomer,EPDM))等弹性体。因此,电解液并不完全封闭在壳体内,而是透过封口构件,逐渐挥散到电解电容器的外部。因此,如专利文献1那样,为了抑制因透过封口构件引起的电解液的挥散,提出了利用树脂层覆盖封口构件的方案。
树脂层一般而言具有优异的隔热作用。若电解电容器的隔热性变高,则壳体内产生的热难以发散,而容易蓄热。因此,如专利文献2那样,提出了使用乙二醇作为电解液的溶媒。原因在于,乙二醇与γ-丁内酯或环丁砜等相比,热传导率大2倍左右。在专利文献2中,暗示了乙二醇在溶媒中的含有比例越大,热传导性越得到提高,但为了含有其他种类的溶媒,乙二醇被设为优选为90质量%以下。
[现有技术文献]
[专利文献]
专利文献1:日本专利特开昭60-245106号公报
专利文献2:WO2018/123525
发明内容
[发明所要解决的问题]
树脂层中含有硬化性树脂组合物。作为硬化性树脂组合物,可列举包含环氧树脂与酸酐硬化剂的环氧树脂组合物。环氧树脂组合物是利用酸酐系的硬化剂硬化而成的环氧树脂的组合物。包含酸酐硬化剂的环氧树脂组合物的耐热性提高,且环氧树脂与酸酐硬化剂的反应温度为100℃以上,因此可将温度作为触发信号来促进硬化反应,由此认为包含环氧树脂与酸酐硬化剂的环氧树脂组合物适合于树脂层。
本发明者等人利用使用了酸酐硬化剂硬化而成的环氧树脂在电解电容器的一部分上形成树脂层。然后,将所述电解电容器暴露在150℃的温度环境下。若如此,确认到在所述温度环境下暴露400小时的电解电容器的等效串联电阻(equivalent seriesresistance,ESR)会大幅度增大。
本发明是为了解决所述课题而提出,其目的在于涉及一种包括树脂层的电解电容器,且提供一种ESR经时性增大得到了抑制的电解电容器。
[解决问题的技术手段]
本发明者等人进行了努力研究,结果获得如下见解:在包括包含环氧树脂与酸酐硬化剂的环氧树脂组合物(以下,称为酸酐硬化环氧树脂)且使用乙二醇作为电解液的溶媒时,电解电容器的ESR经时性增大显著。
而且,本发明者等人基于所述见解进行了努力研究,结果查明了酸酐硬化环氧树脂与水或乙二醇反应并进行分解,会溶出到电解液中,电解液中存在酸酐硬化环氧树脂是电解电容器的ESR增大的原因。
此处,酸酐硬化环氧树脂在化学结构中包含酯键。另一方面,即使在电解电容器中未特意添加水的情况下,在制造过程中也会在电解电容器中混入少量的水。乙二醇是具有羟基的化合物,具有羟基的化合物是水容易接近的结构。在此种状况下,当具有羟基的化合物透过封口构件时,水也一起透过,水与酸酐硬化环氧树脂的酯键反应,酸酐硬化环氧树脂被水解。另外,也会发生通过水解生成的羰基与具有羟基的化合物的酯化反应。如此,认为与水或具有羟基的化合物反应的酸酐硬化环氧树脂成分的一部分透过封口构件会溶出到电解液中。
本发明是基于所述见解而成者,本发明的电解电容器的特征在于,包括:电容器元件,具有阳极箔、阴极箔以及电解液;壳体,收容所述电容器元件;封口构件,对所述壳体进行封口;以及树脂层,配置在所述封口构件的附近,所述树脂层包含不具有酯键的环氧树脂组合物。
所述环氧树脂组合物可将酚系硬化剂或胺系硬化剂与环氧树脂作为原材料。所述环氧树脂组合物可具有包含酚系硬化剂或胺系硬化剂与环氧树脂的化学结构。
所述电解液可包含具有羟基的化合物、环丁砜及γ-丁内酯中的至少一种。
所述具有羟基的化合物可为乙二醇、二乙二醇及聚乙二醇中的至少一种。
所述电容器元件还可具有固体电解质。
所述电解液中的阳离子成分相对于所述电解液每100g可含有76mmol以下。或者,所述电解液中的阳离子成分相对于所述电解液每100g可含有25mmol以下。
[发明的效果]
根据本发明,可抑制包括树脂层的电解电容器的ESR经时性增大。
附图说明
图1是从比较例1、实施例1及实施例2的多个方向拍摄的透视图像。
具体实施方式
以下,对本发明的实施方式的电解电容器进行说明。再者,本发明并不限定于以下所说明的实施方式。
(整体结构)
电解电容器为通过静电电容进行电荷的蓄电及放电的被动元件。所述电解电容器包含仅具有电解液的液体电解电容器、并用了导电性聚合物或凝胶等固体电解质与电解液的混合电解电容器。另外,所述电解电容器包含仅在阳极侧特意地形成了电介质氧化皮膜的电解电容器、在电极双方形成了电介质氧化皮膜的双极性电解电容器。进而,所述电解电容器在外观上包含引出有引线端子的电解电容器、设置有底座且表面安装于基板的电解电容器、及与其他电子电路零件一起由树脂整体包覆的电解电容器。以下,将这些各种组合的电解电容器总称,并简称为电解电容器。
电解电容器具有电容器元件、壳体以及封口构件。壳体收容电容器元件。封口构件通过紧固加工而安装于壳体的开口处,并对壳体的开口进行密封。电容器元件包括阳极箔、阴极箔、隔板及电解液。阳极箔与阴极箔介隔隔板而相向。在阳极箔的表面形成有电介质氧化皮膜。阴极箔也视需要形成有电介质氧化皮膜。除了电解液以外,也可包含固体电解质。固体电解质介隔存在于阳极箔与阴极箔之间,与电介质氧化皮膜密接。电解液被填充在电容器元件的空隙部。另外,电解电容器也可视需要具有底座。
(封口构件)
封口构件通过紧固加工被安装在壳体。壳体为铝、含有铝或锰的铝合金、或不锈钢制,且是有底且其他端为开口的例如筒体,在紧固加工中,将壳体的开口向内侧弯曲而压扁,从而使壳体密接于封口构件。具备弹性力的封口构件为包含弹性体的板体、或相对于弹性体层叠合成树脂板或金属板而成的板体。弹性体通过弹性力与经紧固加工的壳体密接,并保持壳体内的气密性。但是,关于包含弹性体的封口构件,挥发的电解液的透过率不为零。作为所述弹性体,可列举:丁基橡胶、乙烯丙烯二烯橡胶(EPDM)、硅橡胶及丁基橡胶等。
(树脂层)
电解电容器还包括树脂层。树脂层抑制电解液的蒸发。即,只要为有电解液通过之虞的封口构件的附近部位,则可设置于电解电容器的任意部位。例如,树脂层包覆封口构件的表面的至少一部分区域。所述树脂层通过树脂成型包覆封口构件,而使电解液透过封口构件的透过性下降。即,所谓附近,可不隔开,也包含接触配置。另外,例如在电解电容器为包括底座的芯片类型的情况下,树脂层例如配备在为底座与壳体接触的部位或其周围且封口构件附近。透过封口体的电解液通过所述树脂层来抑制蒸发。换句话说,所述树脂层也有与通过封口体的电解液中的水或乙二醇反应并通过封口体而溶出到电解液中之虞。
所述树脂层不使用酸酐硬化环氧树脂,且包含酚系硬化环氧树脂或胺系硬化环氧树脂。所述树脂层中也可包含酚系硬化环氧树脂或胺系硬化环氧树脂以外的化合物。
酚系硬化环氧树脂是利用酚系硬化剂硬化而成的环氧树脂,将酚系硬化剂与环氧树脂作为原材料,是在化学结构中包含酚系硬化剂与环氧树脂的环氧树脂组合物。胺系硬化环氧树脂是利用胺系的硬化剂硬化而成的环氧树脂,将胺系硬化剂与环氧树脂作为原材料,是在化学结构中包含胺系硬化剂与环氧树脂的环氧树脂组合物。酸酐硬化环氧树脂在化学结构中具有酯键,相对于此,这些酚系硬化环氧树脂及胺系硬化环氧树脂的酸酐硬化环氧树脂在化学结构中不存在酯键。
具体而言,酚系硬化环氧树脂是通过酚系硬化剂的酚性羟基与环氧基反应并键结而生成。另外,胺系硬化环氧树脂是通过胺系硬化剂的氨基与环氧基反应并键结而生成。这些硬化剂与环氧树脂的键为醚键,不存在被水解之虞。
如根据所述反应体系得知,所谓在化学结构中包含酚系硬化剂与环氧树脂的环氧树脂组合物,并不是指在与反应前保持不变的状态下直接取入到化学结构中的环氧树脂组合物。所谓在化学结构中包含酚系硬化剂与环氧树脂,是指为了键结而产生各基的取代等,然后取入到化学结构中。另外,如根据所述反应体系得知,所谓在化学结构中包含胺系硬化剂与环氧树脂的环氧树脂组合物,并不是指在与反应前保持不变的状态下直接取入到化学结构中的环氧树脂组合物。所谓在化学结构中包含胺系硬化剂与环氧树脂,是指为了键结而产生各基的取代等,然后取入到化学结构中。
酚系硬化环氧树脂及胺系硬化环氧树脂中所含的环氧树脂是在末端具有两个以上的反应性的环氧基的环氧寡聚物。所述环氧树脂通过酸酐硬化剂的加成反应在环氧树脂成分相互间进行交联,从液状物变化为固体树脂。作为环氧树脂,典型而言可列举作为双酚A与表氯醇的缩合物的双酚A二缩水甘油醚。作为环氧树脂,可列举其他缩水甘油型环氧树脂、及3,4-环氧基环己基甲基-3',4'-环氧基环己烷羧酸酯等脂环族环氧化物。
作为缩水甘油型环氧树脂,可列举将双酚类缩水甘油化而成的双酚型。双酚类可列举:双酚A、双酚F、双酚AD、双酚S、四甲基双酚A、四甲基双酚F、四甲基双酚AD、四甲基双酚S、四溴双酚A、四氯双酚A、四氟双酚A等。
另外,作为缩水甘油型环氧树脂,可列举将二元酚类缩水甘油化而成的环氧树脂。二元酚类可列举联苯酚(biphenol)、二羟基萘、9,9-双(4-羟基苯基)芴等。
另外,作为缩水甘油型环氧树脂,可列举将三酚类缩水甘油化而成的环氧树脂。作为三酚类,可列举:1,1,1-三(4-羟基苯基)甲烷、4,4-(1-(4-(1-(4-羟基苯基)-1-甲基乙基)苯基)亚乙基)双酚等。
另外,作为缩水甘油型环氧树脂,可列举将四酚类缩水甘油化而成的环氧树脂。作为四酚类,可列举1,1,2,2-四(4-羟基苯基)乙烷等。
另外,作为缩水甘油型环氧树脂,可列举将酚醛清漆类缩水甘油化而成的酚醛清漆型环氧树脂。酚醛清漆类可列举:苯酚酚醛清漆、甲酚酚醛清漆、双酚A酚醛清漆、溴化苯酚酚醛清漆、溴化双酚A酚醛清漆等。
另外,作为缩水甘油型环氧树脂,可列举将多元酚类缩水甘油化而成的环氧树脂、将甘油或聚乙二醇等多元醇缩水甘油化而成的脂肪族醚型环氧树脂。
另外,作为缩水甘油型环氧树脂,可列举:将羟基羧酸缩水甘油化而成的醚酯型环氧树脂、将聚羧酸缩水甘油化而成的酯型环氧树脂、胺化合物的缩水甘油化物或胺型环氧树脂。作为羟基羧酸,可列举对羟基苯甲酸、β-羟基萘甲酸等。作为聚羧酸,可列举邻苯二甲酸、对苯二甲酸等。作为胺化合物,可列举4,4-二氨基二苯基甲烷、间氨基苯酚。作为胺型环氧树脂,可列举三缩水甘油基异氰脲酸酯等。
作为酚系硬化环氧树脂中所含的酚系硬化剂,可列举二官能酚类及多官能酚类等。作为二官能酚类,可列举对苯二酚、间苯二酚、双酚F、联苯酚、四溴双酚A及萘二醇等。作为多官能酚类,例如可列举苯酚酚醛清漆树脂。
作为胺系硬化环氧树脂中所含的胺系硬化剂,可列举脂肪族多胺、芳香族多胺及改性胺等。作为脂肪族多胺,可列举二亚乙基三胺及三亚乙基四胺等。作为芳香族多胺,可列举间苯二胺、二氨基二苯基甲烷、二氨基二苯基砜等。作为改性胺,可列举胺加合物及酮亚胺等。
(电容器元件)
(电解液)
含浸在电容器元件中的电解液例如为分解成阴离子成分与阳离子成分的离子分解性盐的溶液或不包含离子分解性盐的溶媒。作为溶媒,例如可列举具有羟基的化合物、环状内酯类、砜化合物。作为具有羟基的化合物,可列举质子性的有机极性溶媒。作为质子性的有机溶媒,可列举:一元醇类、多元醇类及含氧醇化合物类等。作为一元醇类,可列举:乙醇、丙醇、丁醇、戊醇、己醇、环丁醇、环戊醇、环己醇、苄醇等。作为多元醇类及含氧醇化合物类,可列举:乙二醇、二乙二醇、丙二醇、甘油、甲基溶纤剂、乙基溶纤剂、甲氧基丙二醇、二甲氧基丙醇、聚乙二醇或聚氧乙烯甘油等多元醇的环氧烷烃加成物等。作为环状内酯类,可列举γ-丁内酯、γ-戊内酯、δ-戊内酯等。作为砜化合物,可列举链状砜及环状砜。作为链状砜,例如可列举二甲基砜、二乙基砜、二丙基砜、二苯基砜。作为环状砜,例如可列举环丁砜、3-甲基环丁砜、2,4-二甲基环丁砜。
此处,封口构件所包括的树脂层是酚系硬化环氧树脂或胺系硬化环氧树脂。酚系硬化环氧树脂及胺系硬化环氧树脂中不存在酯键。因此,即使电解液的溶媒包含具有羟基的化合物,酚系硬化环氧树脂及胺系硬化环氧树脂也不会被具有羟基的化合物分解。因此,即使电解液的溶媒包含具有羟基的化合物,只要封口构件所包括的树脂层是酚系硬化环氧树脂或胺系硬化环氧树脂,则树脂成分也不会溶出到电解液中,电解电容器的ESR经时性的上升也得到抑制。
再者,在并用将乙二醇作为溶媒的电解液与固体电解质的情况下,通过导电性高分子的高阶结构的变化及聚合物链的结晶结构再取向来提高导电性高分子的导电度。环状内酯类改善低温下的ESR特性。砜化合物为高沸点,因此会抑制电解液的蒸发,高温特性变得良好。作为溶媒,特别优选为乙二醇。
就抑制电解液从电解电容器通过树脂层漏出的观点而言,电解液的溶媒优选为乙二醇,接着优选为环丁砜。也可将乙二醇与环丁砜的混合溶媒用于电解液中。
作为溶质的是阴离子成分的有机酸,可列举:草酸、琥珀酸、戊二酸、庚二酸、辛二酸、癸二酸、邻苯二甲酸、间苯二甲酸、对苯二甲酸、马来酸、己二酸、苯甲酸、甲苯酸(toluicacid)、庚酸、丙二酸、1,6-癸烷二羧酸、1,7-辛烷二羧酸、壬二酸、间苯二酚酸、均苯三酚酸、没食子酸、龙胆酸(gentisic acid)、原儿茶酸(protocatechuic acid)、焦儿茶酸(pyrocatechuic acid)、偏苯三甲酸、均苯四甲酸等羧酸、或酚类、磺酸。另外,作为无机酸,可列举:硼酸、磷酸、亚磷酸、次磷酸、碳酸、硅酸等。作为有机酸与无机酸的复合化合物,可列举:硼合二水杨酸、硼合二草酸、硼合二甘醇酸、硼合二丙二酸、硼合二琥珀酸、硼合二己二酸、硼合二壬二酸、硼合二苯甲酸、硼合二马来酸、硼合二乳酸、硼合二苹果酸、硼合二酒石酸、硼合二柠檬酸、硼合二邻苯二甲酸、硼合二(2-羟基)异丁酸、硼合二间苯二酚酸、硼合二甲基水杨酸、硼合二萘甲酸、硼合二苦杏仁酸及硼合二(3-羟基)丙酸等。
另外,作为有机酸、无机酸以及有机酸与无机酸的复合化合物的至少一种的盐,例如可列举铵盐、四级铵盐、四级化脒盐、胺盐、钠盐、钾盐等。作为四级铵盐的四级铵离子,可列举四甲基铵、三乙基甲基铵、四乙基铵等。作为四级化脒盐,可列举乙基二甲基咪唑鎓、四甲基咪唑鎓等。作为胺盐,可列举一级胺、二级胺、三级胺的盐。作为一级胺,可列举甲胺、乙胺、丙胺等,作为二级胺,可列举二甲胺、二乙胺、乙基甲胺、二丁胺等,作为三级胺,可列举三甲胺、三乙胺、三丁胺、乙基二甲胺、乙基二异丙胺等。
溶质中的阳离子成分优选为以相对于电解液每100g而为76mmol以下的量来添加,进而优选为以相对于电解液每100g而为51mmol以下的量来添加,更优选为以相对于电解液每100g而为34mmol以下的量来添加,特别优选为以相对于电解液每100g而为25mmol以下的量来添加,最优选为以相对于电解液每100g而为17mmol以下的量来添加。再者,溶质的阳离子成分与阴离子成分的比率可为等摩尔量,也可为阳离子成分过剩或阴离子成分过剩。
阳离子成分在安装电解电容器时的回流步骤等的高热环境下,容易促进固体电解质中的导电性高分子的脱掺杂反应。若通过阳离子成分促进脱掺杂反应,则固体电解质的导电度下降,电解电容器的ESR增大。另一方面,在封口构件的附近配置有树脂层的情况下,树脂层会阻碍阳离子成分通过封口构件蒸发,从而电解电容器内的阳离子成分减少得到抑制。因此,若在封口构件的附近配置有树脂层,则发生很多起因于阳离子成分的脱掺杂反应,电解电容器的ESR会增大。
然而,电解液中的溶质的阳离子成分只要是相对于电解液每100g而为76mmol以下的量,则与超过76mmol的情况相比,ESR增大得到抑制。进而,电解液中的溶质的阳离子成分只要是相对于电解液每100g而为51mmol以下的量,则例如与相对于电解液每100g而为76mmol的情况相比,ESR增大得到飞跃性的抑制。电解液中的溶质的阳离子成分只要是相对于电解液每100g而为25mmol以下的量,则例如与相对于电解液每100g而为51mmol的情况相比,ESR增大进一步得到飞跃性的抑制。
进而,在液体中也可添加其他添加剂。作为添加剂,可列举:硼酸与多糖类(甘露糖醇、山梨糖醇等)的络合化合物、硼酸与多元醇的络合化合物、硼酸酯、硝基化合物(邻硝基苯甲酸、间硝基苯甲酸、对硝基苯甲酸、邻硝基苯酚、间硝基苯酚、对硝基苯酚、对硝基苄醇等)、磷酸酯等。这些可单独使用,也可组合使用两种以上。
(电极箔)
阳极箔及阴极箔是将阀作用金属作为材料的长条的箔体。阀作用金属为铝、钽、铌、氧化铌、钛、铪、锆、锌、钨、铋及锑等。关于纯度,阳极箔理想为99.9%以上,阴极箔理想为99%左右以上,也可包含硅、铁、铜、镁、锌等杂质。
阳极箔作为将阀作用金属的粉体烧结而成的烧结体、或对经延伸的箔实施蚀刻处理而成的蚀刻箔,表面被扩面化。扩面结构包括隧道状的凹坑(pit)、海绵状的凹坑、或密集的粉体间的空隙。典型而言,扩面结构是通过在盐酸等存在卤素离子的酸性水溶液中施加直流或交流的直流蚀刻或交流蚀刻而形成,或者通过在芯部蒸镀或烧结金属粒子等而形成。关于阴极箔,也可通过蒸镀、烧结或蚀刻而具有扩面结构。
电介质氧化皮膜典型而言为在阳极箔的表层形成的氧化皮膜,只要是阳极箔为铝制,则是使多孔质结构区域氧化而成的氧化铝。所述电介质氧化皮膜是通过在己二酸、硼酸或磷酸等的水溶液中进行电压施加的化学转化处理而形成。另外,也可根据需要在阴极箔的表层通过化学转化处理而形成薄的电介质氧化皮膜(1V~10V左右)。进而,电介质氧化皮膜也可使用通过蒸镀法而形成包含金属氮化物、金属碳化物、金属碳氮化物的层者,或者表面含有碳者来制作。
(隔板)
隔板可列举:牛皮纸(kraft)、马尼拉麻(manila hemp)、茅草(esparto)、大麻(hemp)、人造丝(rayon)等纤维素及这些的混合纸;聚对苯二甲酸乙二酯、聚对苯二甲酸丁二酯、聚萘二甲酸乙二酯、这些的衍生物等聚酯系树脂;聚四氟乙烯系树脂;聚偏二氟乙烯系树脂;维尼纶(vinylon)系树脂;脂肪族聚酰胺、半芳香族聚酰胺、全芳香族聚酰胺等聚酰胺系树脂;聚酰亚胺系树脂;聚乙烯树脂;聚丙烯树脂;三甲基戊烯树脂;聚苯硫醚树脂;丙烯酸树脂;聚乙烯醇树脂等,可将这些树脂单独或混合使用。
(固体电解质)
在将固体电解质形成于电容器元件内的情况下,固体电解质中包含导电性高分子。导电性高分子为共轭系高分子或经掺杂的共轭系高分子。共轭系高分子通过对具有π共轭双键的单体或其衍生物进行化学氧化聚合或电解氧化聚合而获得。通过向共轭系高分子中添加少量容易接受电子的受体(acceptor)、或者容易给予电子的施体(donor),而表现出导电性。若在共轭系高分子中加入受体或施体,则在受体的情况下,自共轭系高分子中抽出π电子而产生负的荷电单体(空穴、hole);在施体的情况下,被供给电子而产生负的荷电载流子,表现出导电性。
作为共轭系高分子,可并无特别限定地使用公知的共轭系高分子。例如可列举:聚吡咯、聚噻吩、聚呋喃、聚苯胺、聚乙炔、聚亚苯、聚亚苯亚乙烯(polyphenylene vinylene)、多并苯(polyacene)、聚噻吩亚乙烯等。这些共轭系高分子可单独使用,也可组合两种以上,进而也可为两种以上单体的共聚物。
在所述共轭系高分子中,优选为噻吩或其衍生物聚合而成的共轭系高分子,优选为3,4-乙烯二氧噻吩(即2,3-二氢噻吩并[3,4-b][1,4]二恶英)、3-烷基噻吩、3-烷氧基噻吩、3-烷基-4-烷氧基噻吩、3,4-烷基噻吩、3,4-烷氧基噻吩或这些的衍生物聚合而成的共轭系高分子。作为噻吩衍生物,优选为选自在3位及4位具有取代基的噻吩中的化合物,噻吩环的3位及4位的取代基可与3位及4位的碳一同形成环。烷基或烷氧基的碳数适合为1~16,尤其是特别优选为被称为EDOT(3,4-ethylene dioxythiophene)的3,4-乙烯二氧噻吩的聚合物,即被称为PEDOT(Poly(3,4-polyethylene dioxythiophene))的聚(3,4-乙烯二氧噻吩)。另外,也可为在3,4-乙烯二氧噻吩上加成有烷基的烷基化乙烯二氧噻吩,例如可列举:甲基化乙烯二氧噻吩(即2-甲基-2,3-二氢-噻吩并〔3,4-b〕〔1,4〕二恶英)、乙基化乙烯二氧噻吩(即2-乙基-2,3-二氢-噻吩并〔3,4-b〕〔1,4〕二恶英)等。
掺杂剂可并无特别限定地使用公知的掺杂剂。例如可列举:硼酸、硝酸、磷酸等无机酸;乙酸、草酸、柠檬酸、抗坏血酸、酒石酸、方酸(squaric acid)、玫棕酸(rhodizonicacid)、克酮酸(croconic acid)、水杨酸、对甲苯磺酸、1,2-二羟基-3,5-苯二磺酸、甲磺酸、三氟甲磺酸、硼合二水杨酸、双草酸硼酸酯、磺酰基酰亚胺酸、十二烷基苯磺酸、丙基萘磺酸、丁基萘磺酸等有机酸。另外,作为聚阴离子,可列举:聚乙烯磺酸、聚苯乙烯磺酸、聚烯丙基磺酸、聚丙烯酸磺酸、聚甲基丙烯酸磺酸、聚(2-丙烯酰胺-2-甲基丙磺酸)、聚异戊二烯磺酸、聚丙烯酸、聚甲基丙烯酸、聚马来酸等。
这些掺杂剂可单独使用,也可将两种以上组合使用。另外,这些掺杂剂可为单独单体的聚合物,也可为两种以上的单体的共聚物。另外,掺杂剂也可使用高分子或单量体。
[实施例]
以下,基于实施例进一步对本发明的电解电容器进行详细说明。再者,本发明并不限定于下述实施例。利用包含环氧树脂组合物的树脂层包覆封口构件,来制作各种电解电容器。
(实施例1至实施例4)
比较例1以及实施例1至实施例4的电解电容器在具有并用了电解液与固体电解质的电解质这一点上共通。实施例1至实施例4相对于比较例1的不同点是树脂层的组成,环氧树脂组合物的种类不同。另外,实施例1至实施例4相对于比较例1的不同点在于,使用乙二醇或γ-丁内酯作为电解液的溶媒。乙二醇是具有羟基的化合物的例子。
对比较例1以及实施例1至实施例3的电解电容器的共通点进行详述。阳极箔为铝箔,通过蚀刻处理而扩面化,通过化学转化处理而形成电介质氧化皮膜。阴极箔设为平面箔,即未进行蚀刻处理的铝箔。将相同的阳极箔与阴极箔用于全电解电容器,并在各个上连接引线,介隔马尼拉系隔板而使阳极箔与阴极箔相向地卷绕。电容器元件通过在相同浓度的磷酸二氢铵水溶液中浸渍10分钟而进行修复化学转化。
接着,以相同浓度准备作为导电性高分子的掺杂有相同制品的聚苯乙烯磺酸的聚乙烯二氧噻吩(PEDOT/聚苯乙烯磺酸(polystyrene sulfonic acid,PSS)的分散液,浸渍电容器元件,并提起电容器元件,在150℃下干燥30分钟。反复进行相同次数的浸渍及干燥。由此,在电容器元件上形成固体电解质。接着,通过各电解电容器来制备不同的电解液,将形成有固体电解质的电容器元件浸渍于电解液中。将所述电容器元件插入至相同金属种类、相同尺寸及相同形状的有底筒状的外装壳体,在开口端部安装封口构件,利用相同加压力并通过紧固加工进行密封。各电解电容器使用包含丁二烯橡胶制的封口构件。
各电解电容器被收容在相同尺寸的铝容器中,以利用相同种类的环氧树脂完全埋设的方式形成了树脂层。但是,从电解电容器引出的引线预先从环氧树脂引出,以便可向电解电容器通电。由此,各电解电容器成为封口构件的外表面被环氧树脂组合物完全覆盖的状况。
在比较例1以及实施例1至实施例4的电解电容器中所制备的电解液及树脂层中使用的环氧树脂组合物如下表1所示。
(表1)
如上表1所示,比较例1的电解电容器使用酸酐硬化环氧树脂而形成树脂层。相对于此,实施例1及实施例2的电解电容器使用胺系硬化环氧树脂而形成树脂层。另外,实施例3及实施例4的电解电容器使用酚系硬化环氧树脂而形成树脂层。比较例1的酸酐硬化环氧树脂是利用酸酐系硬化剂硬化而成的环氧树脂。实施例1及实施例2的胺系硬化环氧树脂是利用胺系硬化剂硬化而成的环氧树脂。实施例3及实施例4的酚系硬化环氧树脂是利用酚系硬化剂硬化而成的环氧树脂。
上表1中,溶媒的组成比表示相对于溶媒总量的重量比例。如上表1所示,比较例1的电解电容器中,在将酸酐硬化环氧树脂用于树脂层中的同时,将电解液的溶媒总量设为乙二醇。实施例1的电解电容器中,电解液的溶媒总量为乙二醇,但树脂层中使用胺系硬化环氧树脂。实施例2的电解电容器中,电解液的溶媒总量为γ丁内酯,但树脂层中使用胺系硬化环氧树脂。实施例3的电解电容器中,电解液的溶媒总量为乙二醇,但树脂层中使用酚系硬化环氧树脂。实施例4的电解电容器中,电解液的溶媒总量为γ丁内酯,但树脂层中使用酚系硬化环氧树脂。
利用上表1所示的各环氧树脂组合物填埋各电解电容器,然后在对各电解电容器施加35V的恒定电压的同时,在150℃的温度环境下放置400小时。测定了所述热应力负荷前后的ESR。在100kHz下测定了ESR。另外,利用X射线拍摄装置对热应力负荷后的各电解电容器的内部进行拍摄,通过透视图像观察内部的状态。
各电解电容器的热应力负荷前后的ESR与利用透视图像所得的内部状态的结果如下表2所示。
(表2)
如表2所示,相对于比较例1而言的实施例1至实施例4中,ESR相差悬殊变小。相对于比较例1,实施例1至实施例4的群组最低也被抑制为56分之一的ESR,最大被抑制为约74分之一的ESR。其结果,确认到只要由胺系硬化环氧树脂或酚系硬化环氧树脂形成树脂层,则无论溶媒种类如何,负荷试验后的ESR均得到抑制。
另外,如表2所示,与使用γ-丁内酯作为溶媒的实施例2及实施例4相比,使用乙二醇作为溶媒的实施例1及实施例3的ESR的增加得到进一步抑制。若在并用固体电解质作为电解质的同时,在溶媒中存在乙二醇,则通过导电性高分子的高阶结构的变化及聚合物链的结晶结构再取向,导电性高分子的导电度提高,但γ-丁内酯无法获得此种效果,因此若将溶媒设为乙二醇,并将树脂层设为胺系硬化环氧树脂或酚系硬化环氧树脂,则确认到ESR进一步减少。
此处,如表2所示,根据利用X射线拍摄装置所得的透视图像,在填埋有比较例1的电解电容器的酸酐硬化环氧树脂的树脂层中产生了裂纹。相对于此,无法在填埋有实施例1至实施例4的电解电容器的胺系硬化环氧树脂或酚系硬化环氧树脂的树脂层中发现裂纹。将从比较例1、实施例1及实施例2的多个方向拍摄的透视图像示于图1。如图1所示,在比较例1中,在以虚线所包围的范围内可观察到裂纹。另一方面,在实施例1及实施例2的各透视图像中不存在裂纹。可观察到裂纹的范围是丁二烯橡胶制的封口构件与酸酐硬化环氧树脂的树脂层之间。
其结果可理解,若将具有酯键的酸酐硬化环氧树脂用于树脂层中,且将具有羟基的化合物即乙二醇用于溶媒中,则酸酐硬化环氧树脂通过水解而分解,分解生成物与具有羟基的化合物反应,这些反应生成物溶出到电解液中,电解液中的来自树脂层的成分会使ESR增大。而且,确认到通过将不存在酯键的胺系硬化环氧树脂或酚系硬化环氧树脂用于树脂层中,不会发生此种环氧树脂的水解反应,来自树脂层的成分不会溶出到电解液中,ESR的增大得到抑制。
(实施例5至实施例12)
接着,制作了实施例5至实施例12的电解电容器。实施例5至实施例12中,向电解液中添加作为溶质的阴离子成分的壬二酸,且向电解液中添加作为溶质的阳离子成分的氨。实施例5至实施例12的电解电容器中,电解液中的溶质中的阳离子成分的量不同。实施例5至实施例12的电解电容器被收容在与实施例1至实施例4相同尺寸的铝容器中,与实施例1同样地,利用胺系硬化环氧树脂来完全埋设。此外,实施例5至实施例12的电解电容器在与实施例1至实施例4的相同制法及相同条件下来制作。
利用胺系硬化环氧树脂来填埋所述实施例5至实施例12的电解电容器,然后在对各电解电容器施加35V的恒定电压的同时,在150℃的温度环境下放置800小时。对所述热应力负荷前后的ESR进行测定,并计算出热应力负荷后的ESR的变化率。在100kHz下测定了ESR。
实施例5至实施例12的电解液的组成及添加量、以及热应力负荷前的ESR(初始ESR)、热应力负荷后的ESR(试验后ESR)及热应力负荷后的ESR的变化率如下表3所示。再者,表3中的溶媒的量表示相对于溶媒整体的含量,表3中的溶质的量以相对于电解液每100g进行换算。实施例5至实施例12的电解电容器为直径6mm×全长6mm的卷绕型,额定电压为35V,额定电容为47μF。
(表3)
如表3所示,相对于作为阳离子成分的氨为86mmol的实施例12的电解电容器,氨为76mmol的实施例11的电解电容器的ESR的变化率被抑制为约55%。进而,相对于氨为76mmol的实施例11的电解电容器,氨为51mmol的实施例10的电解电容器的ESR的变化率被抑制为约24%。进而,相对于氨为51mmol的实施例10的电解电容器,氨为25mmol的实施例7的电解电容器的ESR的变化率被抑制为约18%。
如此,若电解电容器具有树脂层,则阳离子成分有促进脱掺杂反应而使ESR增大的倾向。但是,确认到通过将阳离子成分调整为相对于电解液每100g而为76mmol以下,可抑制ESR的增大,通过将阳离子成分调整为相对于电解液每100g而为51mmol以下,可进一步抑制ESR的增大,通过将阳离子成分调整为相对于电解液每100g而为25mmol以下,可大大地抑制热应力负荷后的ESR。
(实施例13至实施例16)
制作了实施例13至实施例16的电解电容器。实施例13至实施例16的电解液的溶媒为乙二醇、γ-丁内酯、环丁砜或这些中的两种的混合液,但组成比不同。在实施例13至实施例16的电解电容器中,就仅使电解液的溶媒的影响明确的观点而言,设为未添加溶质。此外,关于实施例13至实施例16的电解电容器,包括收容在相同尺寸的铝容器中并利用树脂来完全埋设在内,而利用与实施例1至实施例4的相同制法及相同条件来制作。再者,树脂层中使用胺系硬化环氧树脂。
在利用树脂填埋后,将各电解电容器在150℃的温度环境下放置3500小时。测定了所述热应力负荷后的电解液的漏出量。电解液的漏出量是从热应力负荷前的电解电容器的重量中减去热应力负荷后的电解电容器的重量而求出。实施例13至实施例16的电解液的组成及添加量、以及热应力负荷后的电解液的漏出量如下表4所示。再者,各实施例的电解电容器为直径10mm×全长10mm的卷绕型。
(表4)
如表4所示,相对于将γ-丁内酯作为电解液的溶媒的实施例13,在将环丁砜作为电解液的溶媒的实施例14中,电解液的漏出量被抑制为一半以下。进而,相对于将环丁砜作为电解液的溶媒的实施例14,在将乙二醇作为电解液的溶媒的实施例16中,电解液的漏出量被抑制为74%。
Claims (8)
1.一种电解电容器,其特征在于,包括:
电容器元件,具有阳极箔、阴极箔以及电解液;
壳体,收容所述电容器元件;
封口构件,对所述壳体进行封口;以及
树脂层,配置在所述封口构件的附近,
所述树脂层包含不具有酯键的环氧树脂组合物。
2.根据权利要求1所述的电解电容器,其特征在于,
所述环氧树脂组合物将酚系硬化剂或胺系硬化剂与环氧树脂作为原材料。
3.根据权利要求1所述的电解电容器,其特征在于,
所述环氧树脂组合物具有包含酚系硬化剂或胺系硬化剂与环氧树脂的化学结构。
4.根据权利要求1至3中任一项所述的电解电容器,其特征在于,
所述电解液包含具有羟基的化合物、环丁砜及γ-丁内酯中的至少一种。
5.根据权利要求4所述的电解电容器,其特征在于,
所述具有羟基的化合物为乙二醇、二乙二醇及聚乙二醇中的至少一种。
6.根据权利要求1至5中任一项所述的电解电容器,其特征在于,
所述电容器元件还具有固体电解质。
7.根据权利要求6所述的电解电容器,其特征在于,
所述电解液中的阳离子成分相对于所述电解液每100g而含有76mmol以下。
8.根据权利要求6所述的电解电容器,其特征在于,
所述电解液中的阳离子成分相对于所述电解液每100g而含有25mmol以下。
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