TW202301391A - 電解電容器、陰極體和電解電容器的製造方法 - Google Patents
電解電容器、陰極體和電解電容器的製造方法 Download PDFInfo
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- TW202301391A TW202301391A TW111123069A TW111123069A TW202301391A TW 202301391 A TW202301391 A TW 202301391A TW 111123069 A TW111123069 A TW 111123069A TW 111123069 A TW111123069 A TW 111123069A TW 202301391 A TW202301391 A TW 202301391A
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- Prior art keywords
- foil
- cathode
- electrolytic capacitor
- carbon layer
- acid
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
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Abstract
本發明提供一種抑制了電容的經時性減少的電解電容器、該電解電容器所包括的陰極體和電解電容器的製造方法。電解電容器包括陽極箔、陰極體以及電解液。陽極箔由閥金屬形成,且具有形成於箔表面的電介質氧化皮膜。陰極體具有閥金屬的陰極箔、以及積層於該陰極箔上的碳層。陰極箔與碳層的界面電阻為1.8 mΩ・cm
2以下。
Description
本發明是有關於一種電解電容器、該電解電容器所包括的陰極體、和電解電容器的製造方法。
電解電容器以使陽極箔與陰極箔相向的方式包括陽極箔與陰極箔,所述陽極箔於如鉭或鋁等般的閥金屬上形成有電介質氧化皮膜,所述陰極箔由與所述閥金屬為相同種類的閥金屬或其他閥金屬的箔形成。電解液介隔存在於陽極箔與陰極箔之間。電解液介隔存在於陽極箔與陰極箔之間並與陽極箔的凹凸面密接,作為真正的陰極發揮功能。
近年來,亦多使用代替電解液而使固體電解質介隔存在於陽極箔與陰極箔之間的電解電容器。包括該固體電解質的電解電容器為小型、大電容、低等效串聯電阻,對電子設備的小型化、高功能化而言不可缺少。作為固體電解質,已知有二氧化錳或7,7,8,8-四氰基醌二甲烷(7,7,8,8-tetracyanoquinodimethane,TCNQ)錯合物。另外,作為固體電解質,由具有π共軛雙鍵的單體衍生出的導電性高分子正急速普及。作為該導電性高分子,例如可列舉聚(3,4-伸乙基二氧基噻吩)(Poly(3,4-ethylenedioxythiophene),PEDOT)。關於導電性高分子,於化學氧化聚合或電解氧化聚合時,使用有機磺酸等聚陰離子作為摻雜劑而顯現出高的導電性,另外與電介質氧化皮膜的密接性優異。
其中,包括固體電解質的電解電容器與包括電解液的電解電容器相比,缺乏電介質氧化皮膜的缺陷部的修復作用。因此,使固體電解質介隔存在於陽極箔與陰極箔之間、並且含浸有電解液的所謂混合型電解電容器亦受到矚目。
此處,於電解電容器中,不僅於陽極箔上有目的地形成電介質氧化皮膜,而且因與空氣的反應或電解液的化成作用亦會於陰極箔的表面形成氧化皮膜。因此,電解電容器可看作是於陽極側與陰極側顯現出亦被稱為Cap(Capacitance,電容)的電容的串聯電容器。此種電解電容器重要的是使陰極側的電容理想地逐漸接近無限大以便效率良好地引出陽極側的電容。
因此,提出有使用如離子鍍法般的乾式鍍敷法於陰極箔的表面形成碳的電解電容器(例如,參照專利文獻1)。碳層阻擋電解液向陰極箔的表面的浸入、並阻止陰極箔的氧化皮膜的新的形成及成長,藉此使陰極側顯現的電容漸進為幾乎無限大,將電解電容器的電容僅設為陽極電容。
[現有技術文獻]
[專利文獻]
[專利文獻1]日本專利特開2006-190878號公報
[發明所欲解決之課題]
但是,於只是於陰極箔上形成碳層的情況下,電解電容器的電容的劣化會於長期間內進行,最終電解電容器的電容的減少率會低於極限,電解電容器的壽命會結束。
本發明是為了解決所述課題而提出者,其目的在於提供一種抑制了電容的經時性劣化的電解電容器、該電解電容器所包括的陰極體和電解電容器的製造方法。
[解決課題之手段]
本發明者等人進行了努力研究,結果獲得了如下般的見解。即,於在陰極箔上積層有碳層的情況下,若著眼於陰極箔與碳層的界面電阻,則於至少為1.8 mΩ・cm
2以下時,電解電容器的電容的減少率與初期相比較被抑制為30%以下。
基於該見解,為了解決所述課題,本發明的電解電容器包括陽極箔、陰極體以及電解液,所述電解電容器的特徵在於:所述陽極箔由閥金屬形成,且具有形成於箔表面的電介質氧化皮膜,所述陰極體具有閥金屬的陰極箔、以及積層於所述陰極箔上的碳層,所述陰極箔與所述碳層的界面電阻為1.8 mΩ・cm
2以下。
另外,本發明者等人進行了努力研究,結果進而獲得了如下般的見解。即,於在陰極箔上積層有碳層的情況下,若著眼於陰極箔與碳層的界面電阻,則以至少1.6 mΩ・cm
2為界,電容的由經時劣化導致的減少率大幅發生變化。實際上,與超過約1.63 mΩ・cm
2相比,於陰極箔與碳層的界面電阻為約1.63 mΩ・cm
2以下的情況下,良好地抑制了電解電容器的電容的經時劣化。
基於該進一步的見解,亦可設為:所述陰極箔與所述碳層的界面電阻為1.6 mΩ・cm
2以下。
亦可設為:所述陰極箔於表面具有擴面層,且於該擴面層上具有所述碳層。若於形成碳層的基礎上形成擴面層,則藉由碳進入擴面層的凹凸的凹陷而產生的錨定效果,陰極箔與碳層密接,陰極箔與碳層的界面電阻更容易下降。
亦可設為:所述碳層壓接於所述陰極箔。若於形成碳層的基礎上使碳層壓接於陰極箔,則更容易使陰極箔與碳層的界面電阻下降。再者,進而佳為碳層對於陰極箔的壓接、與向陰極箔的擴面層的形成併存。若將碳層壓接於形成有擴面層的陰極箔,則碳層的碳材料被壓入至擴面層的凹凸的細孔中,另外碳層沿著擴面層的凹凸面變形,碳層與陰極箔的密接性及固著性進一步提高。因此,陰極箔與碳層的界面電阻更容易下降。
另外,為了解決所述課題,電解電容器的陰極體亦為本發明的一態樣,該電解電容器的陰極體的特徵在於:包括陰極箔以及形成於該陰極箔的表面的碳層,所述陰極箔與所述碳層的界面電阻為1.8 mΩ・cm
2以下。
亦可設為:所述陰極箔與所述碳層的界面電阻為1.6 mΩ・cm
2以下。
另外,為了解決所述課題,電解電容器的製造方法亦為本發明的一態樣,該電解電容器的製造方法為包括陽極箔、陰極體以及電解液的電解電容器的製造方法,其特徵在於包括:陰極體製作步驟,於在閥金屬的陰極箔上形成碳層後,藉由壓製加工將所述碳層壓接於所述陰極箔上,直至界面電阻成為1.8 mΩ・cm
2以下,藉此製作所述陰極體;電容器元件製作步驟,使表面形成有電介質氧化皮膜的所述陽極箔與所述陰極體製作步驟中所製作的所述陰極體相向,製作電容器元件;以及含浸步驟,使電解液含浸於所述電容器元件中。
亦可設為:於所述陰極體製作步驟中,藉由壓製加工將所述碳層壓接於所述陰極箔上,直至界面電阻為1.6 mΩ・cm
2以下。
[發明的效果]
根據本發明,可抑制電解電容器的電容的經時劣化。
以下,對本發明的實施方式的電解電容器及製造方法進行說明。再者,本發明並不限定於以下所說明的實施形態。
(整體結構)
電解電容器為藉由電介質氧化皮膜的介電極化作用而獲得靜電電容並藉由靜電電容進行電荷的蓄電及放電的被動元件。該電解電容器包括:表面形成有電介質氧化皮膜的陽極箔、陰極體、電解液以及隔板。陽極箔與陰極體相向配置,隔板及電解液介隔存在於陽極箔與陰極體之間。陽極箔與陰極體以夾著隔板交替地積層的積層型來配置,或者以於夾著隔板的同時進行捲繞的捲繞型來配置。於陽極箔與陰極體之間,除了配置有電解液以外,亦配置有固體電解質層。
(電極箔)
陰極體包括陰極箔。陽極箔及陰極體的陰極箔是以閥金屬為材料的箔體。閥金屬為鋁、鉭、鈮、氧化鈮、鈦、鉿、鋯、鋅、鎢、鉍及銻等。關於純度,陽極箔理想的是99.9%以上,陰極箔理想的是99%左右以上,亦可包含矽、鐵、銅、鎂、鋅等雜質。
陽極箔及陰極箔於箔一面或箔兩面形成有具有擴面結構的擴面層。擴面層是藉由電解蝕刻、化學蝕刻或噴砂等形成,或者藉由在箔體上蒸鍍或燒結金屬粒子等形成。即,擴面層包含隧道狀的坑、海綿狀的坑、或密集的粉體間的空隙。作為電解蝕刻,可列舉於鹽酸等的存在鹵素離子的酸性水溶液中施加直流電或交流電的直流蝕刻或交流蝕刻。另外,於化學蝕刻中,使陽極箔及陰極箔浸漬於酸溶液或鹼溶液中。再者,隧道狀的坑可以貫通箔的長度形成,亦可以未達箔中心的長度形成。
陽極箔的電介質氧化皮膜典型的是形成於陽極箔的表層的氧化皮膜。關於該電介質氧化皮膜,例如若陽極箔為鋁箔,則為使擴面層的表層氧化而成的氧化鋁。電介質氧化皮膜是藉由在己二酸、硼酸或磷酸等水溶液等不存在鹵素離子的溶液中施加電壓的化成處理而有目的地形成。於陰極箔的表層,亦可藉由該化成處理有目的地形成氧化皮膜,或者自然地形成氧化皮膜。於陰極箔的表層自然地產生的自然氧化皮膜是藉由陰極箔與空氣中的氧進行反應而形成。
(陰極體)
陰極體除了包括陰極箔以外,亦包括碳層。碳層積層於陰極箔上。碳層為含有碳材料的層。碳材料為纖維狀碳、碳粉末、或該些的混合。纖維狀碳或碳粉末較佳為被實施有活化處理或形成孔的開口處理等多孔質化處理。
碳粉末例如為椰子殼等天然植物組織、酚等合成樹脂、以煤炭、焦炭或瀝青等源自化石燃料的物質為原料的活性碳、科琴黑、乙炔黑、槽黑或熱碳黑等碳黑、碳奈米角(carbon nanohorn)、無定形碳、天然石墨、人造石墨、石墨化科琴黑、介孔碳等。纖維狀碳例如為碳奈米管、碳奈米纖維等。碳奈米管可為石墨烯片為一層的單層碳奈米管,亦可為兩層以上的石墨烯片呈同軸狀蜷曲、且管壁呈多層的多層碳奈米管(多層壁碳奈米管(multi-wall carbon nanotube,MWCNT))。
該碳層較佳為以碳層與陰極箔的界面電阻至少成為1.6 mΩ・cm
2以下的方式形成。若該界面電阻為1.6 mΩ・cm
2以下,則電解電容器的電容的經時性減少率被抑制得低。另一方面,若該界面電阻超過1.6 mΩ・cm
2,則電解電容器的電容的減少率會急劇變大。
於1.6 mΩ・cm
2這一界面電阻前後電容的經時性減少率大幅變化的現象為推測,雖然並不限定於此,但可如以下般推測。即,碳層與陰極箔的界面電阻和碳層與陰極箔之間的細孔的直徑及容積具有相關性。而且,1.6 mΩ・cm
2以下這一界面電阻與電解液難以進入碳層與陰極箔之間而電解液無法與陰極箔的表面接觸的直徑及容積的間隙相對應。因此,若界面電阻為1.6 mΩ・cm
2以下,則陰極箔上的氧化皮膜的成長得到抑制,陰極側維持為大電容的狀態。若陰極側維持為大電容的狀態,則可效率良好地持續引出陽極側的電容,將電解電容器的電容的經時性減少率抑制得低。
不過,於碳層與陰極箔的界面電阻為超過1.63 mΩ・cm
2至1.8 mΩ・cm
2以下時,雖然電解電容器的電容的減少率急劇變大,但電解電容器的電容的減少率與初期相比較被抑制為30%以下。所謂初期,是指將電解電容器暴露於125℃的溫度環境下,施加2.4 V的直流電壓的高溫環境下的負荷試驗前。因此,將碳層與陰極箔的界面電阻設為至少1.8 mΩ・cm
2以下。
作為碳層與陰極箔的界面電阻的調整方法,適宜的是可列舉使碳層與陰極箔壓接的壓製加工。於壓製加工中,利用壓輥夾著碳層與陰極箔的積層體,施加壓製線壓。壓製線壓理想的是0.01 t/cm~100 t/cm左右。另外,壓製時的壓輥的溫度即壓製溫度理想的是0℃~200℃左右。
再者,作為壓製加工的前階段,藉由真空蒸鍍、濺鍍、離子鍍、化學氣相沈積(chemical vapor deposition,CVD)法、塗佈、電解鍍敷、無電解鍍敷等在陰極箔上預先形成碳層。於利用塗佈的情況,使碳材料分散於分散溶媒中製作漿料,利用漿料流延法、刮刀法或噴射噴霧法等在陰極箔上塗佈漿料並使其乾燥。於利用真空蒸鍍法的情況下,藉由在真空中對碳材料進行通電加熱而使其蒸發,或者在真空中對碳材料照射電子束而使其蒸發,從而於陰極箔上將碳材料成膜。另外,於利用濺鍍法的情況下,將包含碳材料的靶與陰極箔配置於真空容器中,向真空容器內導入惰性氣體並施加電壓,藉此使已電漿化的惰性氣體與靶碰撞,使自靶敲打出的碳材料的粒子堆積於陰極箔上。
另外,為了使碳層與陰極箔的界面電阻下降,較佳為藉由化成處理有目的地於陰極箔上形成0.5 V以上且3 V左右的氧化皮膜。形成於陰極箔上的氧化皮膜雖於使電解電容器的電容下降的方面產生影響,但亦有提高碳層與陰極箔的密接性的影響。於在具有0.5 V以上且3 V左右的氧化皮膜的陰極箔上形成有碳層的情況下,與該範圍外的氧化皮膜相比,密接性提高受到強烈影響,碳層與陰極箔的界面電阻容易下降到1.6 mΩ・cm
2以下。因此,若有目的地於陰極箔上形成0.5 V以上且3 V左右的氧化皮膜,則可淩駕於由氧化皮膜引起的電容減少的影響,抑制電解電容器的靜電電容的減少。
另外,作為調整碳層與陰極箔的界面電阻的方法,可列舉於陰極箔的表面形成擴面層。藉由亦於陰極箔的表面形成擴面層,碳層的碳材料進入擴面層的凹凸,可使碳層與陰極箔的界面電阻下降。若於在陰極箔上形成擴面層後,對碳層與陰極箔進行壓製加工,則可更簡便地使界面電阻下降。
另外,作為調整碳層與陰極箔的界面電阻的方法,可列舉碳層中所含有的碳材料的選擇。作為碳材料,較佳為作為球狀碳的碳黑。藉由使用一次粒徑平均為100 nm以下的球狀的碳黑,碳層變得緻密,另外碳層容易與擴面層密接,因此界面電阻容易下降。
另外,碳層中所含有的碳材料可為鱗片狀或鱗狀的石墨與作為球狀碳的碳黑。鱗片狀或鱗狀的石墨較佳為短徑與長徑的縱橫比為1:5~1:100的範圍。若將含有該組合的碳材料的碳層積層於陰極箔上,壓縮碳層,且使其壓接於擴面層,則碳黑容易藉由石墨而擦入擴面層。石墨容易沿著擴面層的凹凸面變形,容易堆積於凹凸面上。而且,石墨成為按壓蓋,將球狀碳限制於擴面層內部。因此,碳層與陰極箔的界面電阻容易下降。
再者,界面電阻可以如下方式來測定。即,於多個位置對形成有碳層的陰極體的碳層的表面的電位進行測定。換言之,電位被測定的碳層的表面為位於和與陰極箔密接的面相反的位置的面、或者陰極體的露出面。於電位的測定中,使施加用檢查針與碳層的表面接觸,同時亦使測定用檢查針與碳層的表面接觸,對檢查針間施加規定的直流電流,此時所算出的電阻為「陰極的界面電阻」。作為用於獲得陰極的界面電阻的適宜的裝置,例如可列舉日置電機股份有限公司製造的電極電阻測定系統RM2610。
(電解液)
電解液的溶媒為水、質子性有機極性溶媒或非質子性有機極性溶媒,可為單獨一種或組合兩種以上。溶質包含陰離子及陽離子的成分。溶質典型的是有機酸的鹽、無機酸的鹽、或有機酸與無機酸的複合化合物的鹽,可單獨使用或將兩種以上組合使用。亦可將成為陰離子的酸及成為陽離子的鹼作為溶質成分分別添加至電解液中。
作為質子性有機極性溶媒,可列舉:一元醇類、多元醇類及含氧醇化合物類等。作為一元醇類,可列舉:乙醇、丙醇、丁醇、戊醇、己醇、環丁醇、環戊醇、環己醇、苄醇等。作為多元醇類及含氧醇化合物類,可列舉:乙二醇、丙二醇、甘油、甲基溶纖劑、乙基溶纖劑、甲氧基丙二醇、二甲氧基丙醇等。
作為非質子性有機極性溶媒,可列舉碸系、醯胺系、內酯類、環狀醯胺系、腈系、亞碸系等作為代表。作為碸系,可列舉:二甲基碸、乙基甲基碸、二乙基碸、環丁碸、3-甲基環丁碸、2,4-二甲基環丁碸等。作為醯胺系,可列舉:N-甲基甲醯胺、N,N-二甲基甲醯胺、N-乙基甲醯胺、N,N-二乙基甲醯胺、N-甲基乙醯胺、N,N-二甲基乙醯胺、N-乙基乙醯胺、N,N-二乙基乙醯胺、六甲基磷醯胺等。作為內酯類、環狀醯胺系,可列舉:γ-丁內酯、γ-戊內酯、δ-戊內酯、N-甲基-2-吡咯啶酮、碳酸伸乙酯、碳酸伸丙酯、碳酸伸丁酯、碳酸伸異丁酯等。作為腈系,可列舉:乙腈、3-甲氧基丙腈、戊二腈等。作為亞碸系,可列舉:二甲基亞碸等。
作為有機酸,可列舉:草酸、琥珀酸、戊二酸、庚二酸、辛二酸、癸二酸、鄰苯二甲酸、間苯二甲酸、對苯二甲酸、馬來酸、己二酸、苯甲酸、甲苯甲酸、庚酸、丙二酸、1,6-癸烷二羧酸、1,7-辛烷二羧酸、壬二酸、十一烷二酸、十二烷二酸、十三烷二酸等羧酸、酚類、磺酸。另外,作為無機酸,可列舉:硼酸、磷酸、亞磷酸、次磷酸、碳酸、矽酸等。作為有機酸與無機酸的複合化合物,可列舉:硼合二水楊酸(borodisalicylic acid)、硼合二草酸(borodioxalic acid)、硼合二甘醇酸(borodiglycolic acid)等。
作為該些有機酸的鹽、無機酸的鹽、以及有機酸與無機酸的複合化合物的至少一種的鹽,可列舉:銨鹽、四級銨鹽、四級化脒鎓鹽、胺鹽、鈉鹽、鉀鹽等。作為四級銨鹽的四級銨離子,可列舉:四甲基銨、三乙基甲基銨、四乙基銨等。作為四級化脒鎓,可列舉:乙基二甲基咪唑啉鎓、四甲基咪唑啉鎓等。作為胺鹽的胺,可列舉:一級胺、二級胺、三級胺。作為一級胺,可列舉:甲基胺、乙基胺、丙基胺等,作為二級胺,可列舉:二甲基胺、二乙基胺、乙基甲基胺、二丁基胺等,作為三級胺,可列舉:三甲基胺、三乙基胺、三丙基胺、三丁基胺、乙基二甲基胺、乙基二異丙基胺等。於電解液中,添加具有該些有機酸、無機酸、有機酸與無機酸的複合化合物即成為陰離子的成分、以及該些鹼即成為陽離子的成分的離子解離性的鹽即可。
進而,亦可於電解液中添加其他添加劑。作為添加劑,可列舉:聚乙二醇、硼酸與多糖類(甘露糖醇、山梨糖醇等)的錯化合物、硼酸與多元醇的錯化合物、硼酸酯、硝基化合物、磷酸酯、膠體二氧化矽等。該些可單獨使用,亦可將兩種以上組合使用。硝基化合物抑制電解電容器內的氫氣的產生量。作為硝基化合物,可列舉:鄰硝基苯甲酸、間硝基苯甲酸、對硝基苯甲酸、鄰硝基苯酚、間硝基苯酚、對硝基苯酚等。
此種電解液是於製備後含浸於電容器元件中。電容器元件是使形成有電介質氧化皮膜的陽極箔、與於陰極箔上積層有碳層的陰極體介隔隔板相向而成。於向電容器元件含浸電解液時,為了促進含浸,亦可視需要進行減壓處理或加壓處理。含浸步驟亦可反覆進行多次。再者,於併用固體電解質層的情況下,使電解液含浸於形成有固體電解質層的電容器元件中。
固體電解質層包含導電性高分子。導電性高分子為共軛系高分子或經摻雜的共軛系高分子。共軛系高分子是藉由對具有π共軛雙鍵的單體或其衍生物進行化學氧化聚合或電解氧化聚合而獲得。藉由對共軛系高分子進行摻雜反應,導電性高分子顯現出高的導電性。
作為共軛系高分子,可並無特別限定地使用公知的物質。例如,可列舉:聚吡咯、聚噻吩、聚呋喃、聚苯胺、聚乙炔、聚伸苯、聚伸苯伸乙烯、聚並苯(polyacene)、聚噻吩伸乙烯等。作為導電性聚合物,可代表性地列舉摻雜有聚苯乙烯磺酸(Polystyrene sulfonic acid,PSS)的被稱為PEDOT的聚(3,4-伸乙基二氧基噻吩)。該些共軛系高分子可單獨使用,亦可組合兩種以上,亦可進而為兩種以上的單體的共聚物。
摻雜劑可並無特別限定地使用公知的物質。例如可列舉:硼酸、硝酸、磷酸等無機酸、乙酸、草酸、檸檬酸、抗壞血酸、酒石酸、方形酸、玫棕酸、克酮酸、水楊酸、對甲苯磺酸、1,2-二羥基-3,5-苯二磺酸、甲磺酸、三氟甲磺酸、硼合二水楊酸、雙草酸硼酸、磺醯基醯亞胺酸、十二烷基苯磺酸、丙基萘磺酸、丁基萘磺酸等有機酸。另外,作為摻雜劑,可使用聚陰離子,作為聚陰離子,可列舉:聚乙烯基磺酸、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-丙烯醯胺-2-甲基丙磺酸)、聚異戊二烯磺酸、聚丙烯酸、聚甲基丙烯酸、聚馬來酸等。摻雜劑可單獨使用,亦可將兩種以上組合使用。另外,亦可使用高分子或單量體。
固體電解質層是藉由使分散有導電性高分子的分散液含浸於電容器元件中而形成。作為分散液的溶媒,只要是分散導電性高分子的粒子或粉末的溶媒即可,主要使用水。視需要,亦可使用乙二醇作為分散液的溶媒。判明:若使用乙二醇作為分散液的溶媒,則可減低製品的電氣特性中的尤其是ESR特性。為了提高分散液的含浸性及電導度,亦可於分散液中使用各種添加劑,或者藉由添加陽離子進行中和。
作為導電性高分子的分散液的含浸方法,亦可於分散液中浸漬電容器元件,或者進行滴加塗佈或噴射塗佈等。另外,並不限於電極對整體,亦可於使分散液含浸於陽極箔或陰極體後,裝配電容器元件。為了意圖促進分散液向電極對的含浸,亦可視需要實施減壓處理或加壓處理。該附著步驟亦可反覆進行多次。
另外,固體電解質層亦可藉由公知的電解聚合法或化學聚合法來形成。於化學聚合中,固體電解質層是藉由如下方法而形成:使於溶媒中溶解單體與氧化劑而成的液體含浸於電容器元件中後進行乾燥的方法;或使於溶媒中溶解單體而成的液體、與於溶媒中溶解氧化劑而成的液體交替地含浸於電極對中後進行乾燥。例如,使用3,4-伸乙基二氧基噻吩作為聚合性單體、使用對甲苯磺酸鐵的醇溶液(乙醇等)作為氧化劑,將電容器元件浸漬於所述聚合性單體與氧化劑的混合液中,並藉由加熱產生導電性聚合物的聚合反應,藉此形成固體電解質。另外,亦可於該加熱處理前後進行藉由水洗將未反應單體或剩餘的單體去除的水洗處理。
於電解聚合中,固體電解質層是藉由如下方式而進行:於至少包含單體、支撐電解質以及溶媒的電解聚合溶液中導入電容器元件,並對陽極與陰極之間施加電壓。作為該電解聚合溶液,可使用藉由電解聚合而具有導電性的單體。作為單體,適宜的是噻吩單體或吡咯單體。於使用該些單體的情況下,對電容器元件於不鏽鋼容器中在含有單體及作為支撐電解質的1-萘磺酸鈉的電解聚合用水溶液中進行含浸,施加規定的電壓。藉此,可藉由電解聚合利用水溶性單體(例如,噻吩或吡咯等)均勻地形成固體電解質層。
(隔板)
隔板可列舉牛皮紙、馬尼拉麻(Manila hemp)、西班牙草(esparto)、麻(hemp)、嫘縈等纖維素及該些的混合紙、聚對苯二甲酸乙二酯、聚對苯二甲酸丁二酯、聚萘二甲酸乙二酯、該些的衍生物等聚酯系樹脂、聚四氟乙烯系樹脂、聚偏二氟乙烯系樹脂、維尼綸(vinylon)系樹脂、脂肪族聚醯胺、半芳香族聚醯胺、全芳香族聚醯胺等聚醯胺系樹脂、聚醯亞胺系樹脂、聚乙烯樹脂、聚丙烯樹脂、三甲基戊烯樹脂、聚苯硫醚樹脂、丙烯酸樹脂、聚乙烯基醇樹脂等,該些樹脂可單獨使用或者混合使用。
再者,該隔板負責保持固體電解質層及電解液以及阻止陽極箔與陰極體的短路。於即便沒有隔板固體電解質層亦可保持形狀、包含固體電解質層的電容器元件的各部分可保持電解液、另外固體電解質層具備可阻止陽極箔與陰極體的短路的厚度的情況下,亦可沒有隔板。
(製造方法)
此種電解電容器可經過如下步驟而製作:陽極箔製作步驟,製作陽極箔;陰極體製作步驟,製作陰極體;元件製作步驟,製作將陽極箔與陰極體相向配置的電容器元件;固體電解質層形成步驟,於電容器元件上形成固體電解質層;以及電解液含浸步驟,使電解液含浸於形成有固體電解質層的電容器元件中。
於陽極箔製作步驟中,使閥金屬延伸而形成陽極箔,在該陽極箔上形成擴面層後,在該擴面層的表面形成電介質氧化皮膜。於陰極體製作步驟中,使閥金屬延伸而形成陰極箔,在該陰極箔上形成擴面層。進而,於陰極體製作步驟中,在陰極箔上形成碳層,藉由壓製加工使碳層壓接於陰極箔,將碳層與陰極箔的界面電阻設為1.8 mΩ・cm
2以下、較佳為1.6 mΩ・cm
2以下。
於元件製作步驟中,將形成有電介質氧化皮膜的陽極箔與陰極體介隔隔板重合。於積層型的情況下,將陽極箔、陰極體以及隔板交替地積層多層。於捲繞型的情況下,對介隔隔板重合的陽極箔與陰極體進行捲繞。於固體電解質層形成步驟中,使分散有導電性高分子的分散液含浸於電容器元件中。於電解液含浸步驟中,使電解液含浸於藉由經過固體電解質層形成步驟而形成有固體電解質層的電容器元件中。
藉此,製作陰極箔與碳層的界面電阻為1.8 mΩ・cm
2以下或1.6 mΩ・cm
2以下的電解電容器。該電解電容器中,經時性的電容的減少得到抑制。
[實施例]
以下,基於實施例進一步詳細地說明本發明的電解電容器及製造方法。再者,本發明並不限定於下述實施例。
如以下般,製作電解電容器。首先,使用鋁箔作為陰極箔。對鋁箔實施交流蝕刻處理,於箔兩面形成包含海綿狀的蝕刻坑的擴面層。於交流蝕刻處理中,將陰極箔浸於液溫25℃及以約8重量%的鹽酸為主要電解質的酸性水溶液中,對基材施加約5分鐘的交流10 Hz及電流密度0.14 A/cm
2的電流,使鋁箔的兩面擴面化。
繼而,對鋁箔實施化成處理,於擴面層的表面形成氧化皮膜。於化成處理中,利用磷酸水溶液將交流蝕刻處理時所附著的氯去除後,在磷酸二氫銨的水溶液內施加電壓。
於陰極體的碳層中,選擇碳黑作為碳材料。將碳黑的粉末、作為黏合劑的苯乙烯丁二烯橡膠(styrene butadiene rubber,SBR)、以及作為含有分散劑的水溶液的羧甲基纖維素鈉(carboxymethyl cellulose sodium,CMC-Na)水溶液混合並進行混練,藉此製作漿料。
將該漿料均勻地塗佈於陰極箔上。然後,對漿料進行加熱乾燥而使溶媒揮發後,對陰極體實施壓製加工。於壓製加工中,利用壓輥夾入陰極體並施加壓製線壓,使碳層固著於陰極箔上。
另外,使用鋁箔作為陽極箔。於鋁箔的箔兩面形成包含海綿狀的蝕刻坑的擴面層。於交流蝕刻處理中,將陰極箔浸於液溫25℃及以約8重量%的鹽酸為主要電解質的酸性水溶液中,對基材施加約5分鐘的交流10 Hz及電流密度0.14 A/cm
2的電流。進而,對陽極箔實施化成處理,於陽極箔的擴面層的表面形成電介質氧化皮膜。於化成處理中,利用磷酸水溶液將交流蝕刻處理時所附著的氯去除後,在己二酸的水溶液內施加電壓。
於陽極箔與陰極體上,分別利用超音波連接鋁製的標籤形狀的引出端子。然後,準備折成九十九折的隔板,將陰極體與陽極箔交替地夾入各折痕中,藉此使陰極體與陽極箔介隔隔板相向,同時製作陰極體與陽極箔以及隔板的積層體。作為隔板,使用再生纖維素纖維。再者,積層體利用醯亞胺膠帶固定,以免打開。
使電解液含浸於積層體。電解液是將γ-丁內酯設為溶媒,並添加鄰苯二甲酸四甲基咪唑啉鎓作為溶質。含浸電解液後,將積層體密封於層壓材料中。藉此,製作層壓電池的電解電容器。作為層壓材料,使用厚度110 μm的鋁製材料。於製作層壓電池後,實施老化處理。於老化處理中,在105℃的溫度環境下施加60分鐘、3.35 V的電壓。
製作多個此種電解電容器。關於各電解電容器的陰極體,藉由使將碳層壓接於陰極箔的壓製條件不同而碳層與陰極箔的界面電阻不同。將各電解電容器的陰極體的壓製線壓、壓製溫度及界面電阻示於下表1中。
(表1)
壓製線壓 (kN/cm) | 壓製溫度 (℃) | 界面電阻 (mΩ・cm 2) | |
陰極體1 | 6 | 150 | 0.87 |
陰極體2 | 4 | 150 | 0.98 |
陰極體3 | 8 | 70 | 1.13 |
陰極體4 | 6 | 70 | 1.38 |
陰極體5 | 2 | 70 | 1.63 |
陰極體6 | 4 | 70 | 1.80 |
陰極體7 | 3 | 70 | 2.21 |
陰極體8 | 1 | 150 | 2.75 |
陰極體9 | 1 | 70 | 4.96 |
(電容試驗)
對具有表1所示的各種界面電阻的各電解電容器的經時劣化後的電容進行測定。為了測定該電容,將電解電容器暴露於125℃的溫度環境下,施加2.4 V的直流電壓。對在125℃的溫度環境下施加2.4 V的直流電壓前的初期電容、與經過750小時後的電容進行測定。電容是對電解電容器提供10 kHz的交流訊號來測定。然後,計算經過750小時後的電容相對於初期電容的變化率(ΔCap)。
將電容的計算結果示於以下表2中。另外,將表2的結果示於圖1的圖表中。圖1是表示界面電阻與電容的變化率(ΔCap)的關係的圖表。於圖1所示的圖表中,橫軸取界面電阻,縱軸取電容的變化率(ΔCap)。
(表2)
界面電阻 (mΩ・cm 2) | ΔCap(10 kHz) (%) | |
陰極體1 | 0.87 | -24.1 |
陰極體2 | 0.98 | -23.3 |
陰極體3 | 1.13 | -25.8 |
陰極體4 | 1.38 | -26.5 |
陰極體5 | 1.63 | -26.2 |
陰極體6 | 1.80 | -31.5 |
陰極體7 | 2.21 | -47.4 |
陰極體8 | 2.75 | -61.0 |
陰極體9 | 4.96 | -71.6 |
如表2及圖1所示,可確認到:於碳層與陰極箔的界面電阻為1.63 mΩ・cm
2以下的情況下,即便於高溫環境下施加750小時的負荷,電解電容器的電容與初期相比亦被抑制為約26%以下的減少。另一方面,可確認到:於碳層與陰極箔的界面電阻超過1.80 mΩ・cm
2的情況下,若界面電阻上升,則電解電容器的電容急劇減少。其中,可確認到:於碳層與陰極箔的界面電阻至多為1.80 mΩ・cm
2時,電解電容器的電容的減少率與初期相比被抑制為30%以下。
藉此,確認到:若電解電容器的陰極體具有閥金屬的陰極箔、以及積層於該陰極箔上的碳層,且陰極箔與碳層的界面電阻於考慮到誤差在內時亦為至少1.6 mΩ・cm
2以下,則電容的經時性減少得到抑制。尤其是,於藉由在陰極箔上形成0.5 V~3 V左右的氧化皮膜來提高陰極箔與碳層的密接性的情況下,儘管有因氧化皮膜而電容減少率變大的擔憂,但藉由如本發明般將界面電阻調整為1.6 mΩ・cm
2以下,即便於陰極箔的表面形成氧化皮膜亦可抑制靜電電容的減少。
另外,藉此,確認到:若電解電容器的陰極體具有閥金屬的陰極箔、以及積層於該陰極箔上的碳層,且陰極箔與碳層的界面電阻於考慮到誤差在內時亦為至少1.8 mΩ・cm
2以下,則電容的經時性減少與初期相比被抑制為30%以下。
圖1是表示界面電阻與電容的變化率(ΔCap)的關係的圖表。
Claims (8)
- 一種電解電容器,包括陽極箔、陰極體以及電解液,所述電解電容器的特徵在於: 所述陽極箔由閥金屬形成,且具有形成於箔表面的電介質氧化皮膜, 所述陰極體具有閥金屬的陰極箔、以及積層於所述陰極箔上的碳層, 所述陰極箔與所述碳層的界面電阻為1.8 mΩ・cm 2以下。
- 如請求項1所述的電解電容器,其中 所述陰極箔與所述碳層的界面電阻為1.6 mΩ・cm 2以下。
- 如請求項1或請求項2所述的電解電容器,其中 所述陰極箔於表面具有擴面層,且於所述擴面層上具有所述碳層。
- 如請求項1至請求項3中任一項所述的電解電容器,其中 所述碳層壓接於所述陰極箔。
- 一種陰極體,為電解電容器的陰極體,其特徵在於: 包括陰極箔以及形成於所述陰極箔的表面的碳層, 所述陰極箔與所述碳層的界面電阻為1.8 mΩ・cm 2以下。
- 如請求項5所述的陰極體,其中 所述陰極箔與所述碳層的界面電阻為1.6 mΩ・cm 2以下。
- 一種電解電容器的製造方法,為包括陽極箔、陰極體以及電解液的電解電容器的製造方法,其特徵在於包括: 陰極體製作步驟,於在閥金屬的陰極箔上形成碳層後,藉由壓製加工將所述碳層壓接於所述陰極箔上,直至界面電阻成為1.8 mΩ・cm 2以下,藉此製作所述陰極體; 電容器元件製作步驟,使表面形成有電介質氧化皮膜的所述陽極箔與所述陰極體製作步驟中所製作的所述陰極體相向,製作電容器元件;以及 含浸步驟,使電解液含浸於所述電容器元件中。
- 如請求項7所述的電解電容器的製造方法,其中 於所述陰極體製作步驟中,藉由壓製加工將所述碳層壓接於所述陰極箔上,直至界面電阻為1.6 mΩ・cm 2以下。
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