TW201801377A - 能量貯藏裝置用電極 - Google Patents
能量貯藏裝置用電極 Download PDFInfo
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- TW201801377A TW201801377A TW105143933A TW105143933A TW201801377A TW 201801377 A TW201801377 A TW 201801377A TW 105143933 A TW105143933 A TW 105143933A TW 105143933 A TW105143933 A TW 105143933A TW 201801377 A TW201801377 A TW 201801377A
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- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical class [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229920000553 poly(phenylenevinylene) Polymers 0.000 description 1
- 229920001197 polyacetylene Polymers 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920000447 polyanionic polymer Polymers 0.000 description 1
- 229920002857 polybutadiene Polymers 0.000 description 1
- 229920002961 polybutylene succinate Polymers 0.000 description 1
- 239000004631 polybutylene succinate Substances 0.000 description 1
- 229920001610 polycaprolactone Polymers 0.000 description 1
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- MNCGMVDMOKPCSQ-UHFFFAOYSA-M sodium;2-phenylethenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C=CC1=CC=CC=C1 MNCGMVDMOKPCSQ-UHFFFAOYSA-M 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 229920001059 synthetic polymer Polymers 0.000 description 1
- WGHUNMFFLAMBJD-UHFFFAOYSA-M tetraethylazanium;perchlorate Chemical class [O-]Cl(=O)(=O)=O.CC[N+](CC)(CC)CC WGHUNMFFLAMBJD-UHFFFAOYSA-M 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- 238000010023 transfer printing Methods 0.000 description 1
- ITMCEJHCFYSIIV-UHFFFAOYSA-N triflic acid Chemical compound OS(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-N 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 229920001567 vinyl ester resin Polymers 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 125000005023 xylyl group Chemical group 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000004711 α-olefin Substances 0.000 description 1
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Abstract
本發明提供一種能量貯藏裝置用電極,其係具備集電基板、形成於該集電基板之至少一側的面上之含碳奈米管之底塗層、及形成於該底塗層表面上之含有包含含鈦氧化物的活性物質之活性物質層。
Description
本發明有關能量貯藏裝置用電極。
伴隨智慧型手機、數位相機、攜帶遊戲機等之攜帶電子機器之小型輕量化或高機能化之要求,近幾年來,已積極進行高性能電池之開發,藉由充電而可重複使用之二次電池之需求大為擴大。其中,鋰離子二次電池具有高能量密度、高電壓,且充放電時無記憶效果等,故係目前最致力進行開發之二次電池。又,基於近幾年專心致力於於環境問題,對於電動汽車之開發亦活躍進行,作為其動力源之二次電池被要求更高之性能。
鋰離子二次電池具有將可吸附、放出鋰之正極與負極、與介隔於其間之隔離片收容於容器內,並於其中充滿電解液(鋰離子聚合物二次電池時,則代替液狀電解液而使用凝膠狀或全固體型之電解質)之構造。
正極及負極一般係將包含可吸附、放出鋰之活性物質與主要由碳材料所成之導電材進而含聚合物黏合劑之組成物層狀形成於銅箔或鋁箔等之集電體上而製作。
作為負極活性物質已廣泛使用碳材料,但近幾年來由於要求電池之安全性更提高,故盛行電位高的負極活性物質之研究開發。例如已報導氧化鈦或鈦酸鋰等之含鈦氧化物作為此種負極活性物質為有用(專利文獻1、2)。
然而,含鈦氧化物與使用石墨等之碳材料之負極活性物質比較,由於導電性較低,故具備含鈦氧化物之活性物質層之二次電池,負極活性物質間彼此之接觸電阻或負極活性物質與集電體之界面之接觸電阻高,結果有二次電池之內部電阻或阻抗上升,而無法對於大電流急速充放電之問題。因此,使用含鈦氧化物作為負極活性物質時,作為提高負極活性物質層之導電性之對策,係進行於負極活性物質層中添加大量導電助材,於負極活性物質表面塗佈導電材料。然而,該情況下,會有負極活性物質層中添加無助於電容之材料之量,使負極活性物質層之體積基準或質量基準之容量降低之問題。
專利文獻3中,揭示藉由於負極活性物質層與集電基板之間配置底塗層而降低活性物質層與集電基板之間之接觸界面電阻,即使負極活性物質使用含鈦氧化物之情況,亦不於負極活性物質中添加大量導電助材,而製作二次電之內部電阻或阻抗小、能以大電流急速充放電之二次電池之技術。然而,專利文獻3中,使用乙炔黑作為底塗層之導電材,而無法使底塗層之單位面積質量充分減小,將底塗層認為電極之一部分時,結果有電極容量減少
的問題。
[專利文獻1]日本特開2001-143702號公報
[專利文獻2]國際公開第2008-114667號
[專利文獻3]日本特開2013-033685號公報
本發明係鑑於前述情況而完成者,其目的在於提供不會大為減少電極容量,且即使於活性物質中使用含鈦氧化物時,亦能以大電流急速充放電之能量貯藏裝置用電極。
本發明人等,基於不會大為減少電極容量,且使於活性物質中使用含鈦氧化物之電極低電阻化之觀點,積極重複檢討之結果,發現藉由將於集電基板之至少一側的面上形成之底塗層中所含之碳材料設為碳奈米管(CNT),即使底塗層之單位面積質量小之情況,亦可使於活性物質中使用含鈦氧化物之電極低電阻化,因而完成本發明。
因此,本發明提供下述能量貯藏裝置用電極。
1.一種能量貯藏裝置用電極,其係具備集電基板、形成於該集電基板之至少一側的面上之含碳奈米管(CNT)之底塗層、及形成於該底塗層表面上之含有包含含鈦氧化物之活性物質之活性物質層。
2.如1之能量貯藏裝置用電極,其中前述底塗層含有由側鏈含有噁唑啉基之聚合物所成之CNT分散劑。
(式中,X表示含有聚合性碳-碳雙鍵之基,R1~R4互相獨立表示氫原子、鹵原子、碳數1~5之直鏈狀、分支狀或環狀之烷基、碳數6~20之芳基、或碳數7~20之芳烷基)。
4.如1~3中任一項之能量貯藏裝置用電極,其中前述含鈦氧化物係氧化鈦。
5.如4之能量貯藏裝置用電極,其中前述氧化鈦係具有青銅型的結晶構造之氧化鈦。
6.如1~5中任一項之能量貯藏裝置用電極,其中前
述活性物質層含有苯乙烯-丁二烯橡膠作為黏合劑,且含有羧甲基纖維素之鹽作為增黏劑。
7.如1~6中任一項之能量貯藏裝置用電極,其中前述底塗層之前述集電基板之每一面之單位面積質量為0.1g/m2以下。
8.一種能量貯藏裝置,其係具備如1~7中任一項之能量貯藏裝置用電極。
9.如8之能量貯藏裝置,其中前述能量貯藏裝置用電極為負極。
10.如8或9之能量貯藏裝置,其係鋰離子二次電池。
11.一種如1之能量貯藏裝置用電極之製造方法,其係將含鈦氧化物、黏合劑與因應需要之增黏劑以水作為分散介質予以混合而製作之電極漿料,塗佈在形成於集電基板之至少一側的面上之含CNT之底塗層表面上並使其乾燥。
依據本發明,可提供不會大為減少電極容量,且即使於活性物質中使用含鈦氧化物時,亦能以大電流急速充放電之能量貯藏裝置用電極。
圖1係實施例1及比較例1、3之於0.5C之充放電曲線。
圖2係實施例2及比較例2、3之於0.5C之充放電曲線。
本發明之能量貯藏裝置用電極係具備集電基板、形成於該集電基板之至少一側的面上之含CNT之底塗層、及形成於該底塗層表面上之含有包含含鈦氧化物之活性物質之活性物質層者。
作為本發明之能量貯藏裝置用電極舉例為例如鋰二次電池、鋰離子二次電池、質子聚合物電池、鎳氫電池、電性雙層電容器(capacitor)、鋁固體電容器(condenser)、電解電容器、鉛蓄電池等之各種能量貯藏裝置。本發明之電極尤其可較好地使用於鋰離子二次電池或電性雙層電容器。
作為上述集電基板,只要自以往作為能量貯藏裝置電極之集電基板使用者適當選擇即可,可使用例如鋁、銅、鎳、金、銀及該等之合金、或碳材料、金屬氧化物、導電性聚合物等之薄膜。該等中,基於導電性、質量、成本等
之觀點,較好使用由鋁、鋁合金等所成之金屬箔。前述集電基板之厚度並未特別限制,但於本發明中較好為1~100μm。
前述底塗層含有CNT,進而因應需要含有CNT分散劑及/或基質聚合物。前述底塗層較好使用含有CNT及溶劑及因應需要之CNT分散劑及/或基質聚合物之含CNT組成物(分散液)製作。
CNT一般藉由電弧放電法、化學氣相成長法(CVD法)、雷射.燒蝕法等製作,但本發明中使用之CNT可為藉任何方法獲得者。且,CNT有將1片碳膜(石墨烯.薄片)捲成圓筒狀而成之單層CNT(SWCNT)、將兩片石墨烯.薄片捲成捲成同心圓狀而成之2層CNT(DWCNT)、及將複數片石墨烯.薄片捲成捲成同心圓狀而成之多層CNT(MWCNT)。本發明中可使用任一者,該等可單獨使用1種,或組合2種以上使用。
又,以前述方法製作SWCNT、DWCNT或MWCNT時,由於亦有殘存鎳、鐵、鈷、釔等之觸媒金屬之情況,故用以去除該雜質之純化變得必要。雜質去除時,與利用硝酸、硫酸等之酸處理同時進行超音波處理為有效。然而,利用硝酸、硫酸之酸處理有破壞構成CNT之π共軛系,並損及CNT本來之特性之可能性,故期望
以適當條件純化後使用。
CNT之平均纖維徑並未特別限定,但較好為1~100nm,更好為1~50nm。
作為本發明中可使用之CNT具體例,舉例為超光澤法CNT[國際研究開發法人新能源產業技術綜合開發機構製]、eDIPS-CNT[國際研究開發法人新能源產業技術綜合開發機構製]、SWNT系列[名城奈米碳(股)製:商品名]、VGCF系列[昭和電工(股)製:商品名]、FloTube系列[CNano技術公司製:商品名]、AMC[宇部興產(股)製:商品名]、NANOCYL NC7000系列[Nanocyl S.A.公司製:商品名]、Baytubes[拜耳公司製:商品名]、GRAPHISTRENGTH[ARKEMA公司製:商品名]、MWNT7[保土谷化學工業(股)製:商品名]、HYPEPRION CNT[Hypeprion國際觸媒公司製:商品名]等。
作為前述溶劑,若為以往含CNT之組成物之調製所用者則未特別限制。舉例為例如水;甲醇、乙醇、1-丙醇、2-丙醇等之醇類;四氫呋喃(THF)、二乙醚、1,2-二甲氧基乙烷(DME)等之醚類;二氯甲烷、氯仿、1,2-二氯乙烷等之鹵化烴類;N,N-二甲基甲醯胺(DMF)、N,N-二甲基乙醯胺(DMAc)、N-甲基-2-吡咯啶酮(NMP)等之醯胺類;丙酮、甲基乙基酮、甲基異丁基酮、環己酮等之酮類;正庚烷、正己烷、環己烷等之脂肪族烴類;苯、甲苯、二甲苯、乙基苯等之芳香族烴類;
乙二醇單乙醚、乙二醇單丁醚、丙二醇單甲醚等之二醇醚類;乙二醇、丙二醇等之二醇類等之有機溶劑。該等中,基於可提高CNT之孤立分散比例之觀點,較好為水、NMP、DMF、THF、甲醇、異丙醇。該等溶劑可單獨使用1種,亦可混合2種以上使用。
前述CNT分散劑較好為由側鏈含有噁唑啉基之聚合物所成者。作為前述聚合物,並未特別限制,較好為使於2位具有含有聚合性碳-碳雙鍵之基的噁唑啉單體進行自由基聚合而得者。作為此等噁唑啉單體舉例為以下述式(1)表示者。
式中,X表示含有聚合性碳-碳雙鍵之基,R1~R4互相獨立表示氫原子、鹵原子、碳數1~5之直鏈狀、分支狀或環狀之烷基、碳數6~20之芳基、或碳數7~20之芳烷基。
前述含有聚合性碳-碳雙鍵之基若為含有聚合性碳-碳雙鍵者則未特別限制,較好為含有聚合性碳-碳雙鍵之鏈狀烴基,較好例如為乙烯基、烯丙基、異丙烯基等之碳數2~8之烯基等。
作為前述鹵原子,舉例為氟原子、氯原子、
溴原子、碘原子等。作為前述烷基,舉例為甲基、乙基、正丙基、異丙基、正丁基、第二丁基、第三丁基、正戊基等。作為前述芳基,舉例為苯基、二甲苯基、甲苯基、聯苯基、萘基等。作為前述芳烷基舉例為苄基、苯乙基、苯基環己基等。
作為式(1)表示之噁唑啉單體,舉例為2-乙烯基-2-噁唑啉、2-乙烯基-4-甲基-2-噁唑啉、2-乙烯基-4-乙基-2-噁唑啉、2-乙烯基-4-丙基-2-噁唑啉、2-乙烯基-4-丁基-2-噁唑啉、2-乙烯基-5-甲基-2-噁唑啉、2-乙烯基-5-乙基-2-噁唑啉、2-乙烯基-5-丙基-2-噁唑啉、2-乙烯基-5-丁基-2-噁唑啉、2-異丙烯基-2-噁唑啉、2-異丙烯基-4-甲基-2-噁唑啉、2-異丙烯基-4-乙基-2-噁唑啉、2-異丙烯基-4-丙基-2-噁唑啉、2-異丙烯基-4-丁基-2-噁唑啉、2-異丙烯基-5-甲基-2-噁唑啉、2-異丙烯基-5-乙基-2-噁唑啉、2-異丙烯基-5-丙基-2-噁唑啉、2-異丙烯基-5-丁基-2-噁唑啉等。該等中,基於獲得容易性等之觀點,較好為2-異丙烯基-2-噁唑啉等。
前述底塗層較好使用含水系溶劑之含CNT組成物形成。因此,噁唑啉聚合物較好為水溶性。此等水溶性之噁唑啉聚合物可為式(1)表示之噁唑啉單體之均聚物,為了更提高對水之溶解性,亦可使前述噁唑啉單體與含親水性官能基之(甲基)丙烯酸酯系單體之至少2種單體經自由基聚合而得者。
含親水性官能基之(甲基)丙烯酸系單體之
具體例,舉例為(甲基)丙烯酸、(甲基)丙烯酸2-羥基乙酯、(甲基)丙烯酸甲氧基聚乙二醇酯、(甲基)丙烯酸與聚乙二醇之單酯化物、(甲基)丙烯酸2-胺基乙酯及其鹽、(甲基)丙烯酸鈉、(甲基)丙烯酸銨、(甲基)丙烯腈、(甲基)丙烯醯胺、N-羥甲基(甲基)丙烯醯胺、N-(2-羥基乙基)(甲基)丙烯醯胺、苯乙烯磺酸鈉等。該等可單獨使用1種,亦可組合2種以上使用。該等中,較好為(甲基)丙烯酸甲氧基聚乙二醇、(甲基)丙烯酸與聚乙二醇之單酯化物。
又,在不對噁唑啉聚合物之CNT分散能帶來不良影響之範圍內,可併用前述噁唑啉聚合物及含親水性官能基之(甲基)丙烯酸系單體以外之其他單體。作為其他單體之具體例,舉例為(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸丁酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸硬脂酯、(甲基)丙烯酸全氟乙酯、(甲基)丙烯酸苯酯等之(甲基)丙烯酸酯單體;乙烯、丙烯、丁烯、戊烯等之α-烯烴系單體;氯化乙烯、偏氯化乙烯、氟化乙烯等之鹵醯烴系單體;苯乙烯、α-甲基苯乙烯等之苯乙烯系單體;乙酸乙烯酯、丙酸乙烯酯等之羧酸乙烯酯系單體;甲基乙烯基醚、乙基乙烯基醚等之乙烯醚系單體等。該等可單獨使用1種,亦可組合2種以上使用。
本發明所用之噁唑啉聚合物之製造所用之單體成分中,噁唑啉單體之含量,基於更提高所得噁唑啉聚
合物之CNT分散能之觀點,較好為10質量%以上,更好為20質量%以上,又更好為30質量%以上。又,單體成分中之噁唑啉單體之含量之上限值為100質量%,該情況係獲得噁唑啉單體之均聚物。
另一方面,基於更提高所得噁唑啉聚合物之水溶性之觀點,單體成分中之含親水性官能基之(甲基)丙烯酸系單體含量,較好為10質量%以上,更好為20質量%以上,又更好為30質量%以上,較好為90質量%以下,更好為80質量%以下,又更好為70質量%以下。
且,單體成分中之其他單體含有率,係如前述,係不對所得噁唑啉聚合物之CNT分散能造成影響之範圍,且根據其種類而異,故無法一概官定,但只要在較好為5~95質量%,更好為10~90質量%之範圍適當設定即可。
噁唑啉聚合物之重量平均分子量(Mw)並未特別限定,較好為1,000~2,000,000,更好為2,000~1,000,000。又,本發明中之Mw係藉由凝膠滲透層析法之聚苯乙烯換算測定值。
本發明中可使用之噁唑啉聚合物,可使前述單體進行以往習知之自由基聚合而合成,亦可作為市售品獲得。作為此等市售品舉例為例如EPOCLOTH(註冊商標)WS-300(日本觸媒(股)製,固體成分濃度10質量%,水溶液)、EPOCLOTH WS-700(日本觸媒(股)製,固體成分濃度25質量%,水溶液)、EPOCLOTH
WS-500(日本觸媒(股)製,固體成分濃度39質量%,水/1-甲氧基-2-丙醇溶液)、聚(2-乙基-2-噁唑啉)(Aldrich公司製)、聚(2-乙基-2-噁唑啉)(AlfaAesar公司製)、聚(2-乙基-2-噁唑啉)(VWR International公司製)等。又,作為溶液而市售時,可直接使用,亦可置換為成為目的之溶劑後使用。
本發明所用之含CNT組成物中之CNT與分散劑之混合比例,以質量比計,可為1,000:1~1:100左右。又,含CNT組成物中之分散劑濃度若為可於溶劑中分散CNT之濃度,則未特別限定,但組成物中,較好為0.001~30質量%左右,更好為0.002~20質量%左右。再者,含CNT組成物中之CNT濃度,只要可針對成為目的之底塗層之單位面積質量或所要求之機械特性、電性、熱特性等而變化者,且可製作至少CNT之一部分孤立分散之底塗層,則可為任意,但組成物中,較好為0.0001~30質量%左右,更好為0.001~20質量%左右,又更好為0.001~10質量%左右。
作為前述基質聚合物,舉例為例如聚偏氟化乙烯(PVDF)、聚四氟乙烯(PTFE)、四氟乙烯-六氟丙烯共聚物(P(TFE-HFP))、偏氟化乙烯-六氟丙烯共聚物(P(VDF-HFP))、偏氟化乙烯-氯化三氟化乙烯共聚物(P(VDF-CTFE))等之氟系樹脂,聚乙烯吡咯啶酮(PVP)、乙烯-丙烯-二烯三元共聚物(EPDM)、聚乙烯(PE)、聚丙烯(PP)、乙烯-乙酸乙烯酯共聚物
(EVA)、乙烯-丙烯酸乙酯共聚物(EEA)等之聚烯烴系樹脂;聚苯乙烯(PS)、高衝擊聚苯乙烯(HIPS)、丙烯腈-苯乙烯共聚物(AS)、丙烯腈-丁二烯-苯乙烯共聚物(ABS)、甲基丙烯酸甲酯-苯乙烯共聚物(MS)、乙烯-丁二烯橡膠(SBR)等之聚苯乙烯系樹脂;聚碳酸酯樹脂;氯化乙烯樹脂;聚醯胺樹脂;聚醯亞胺樹脂;聚丙烯酸鈉、聚甲基丙烯酸甲酯(PMMA)等之(甲基)丙烯酸樹脂;聚對苯二甲酸乙二酯(PET)、聚對苯二甲酸丁二酯、對萘二甲酸乙二酯、聚萘二甲酸丁二酯、聚乳酸(PLA)、聚-3-羥基丁酸、聚己內酯、聚琥珀酸丁二酯、聚琥珀酸/己二酸乙二酯等之聚酯樹脂;聚苯醚樹脂;改性聚苯醚樹脂;聚縮醛樹脂;聚碸樹脂;聚苯硫醚樹脂;聚乙烯醇(PVA)樹脂;聚乙醇酸;改性澱粉;乙酸纖維素、羧甲基纖維素(CMC)、三乙酸纖維素;甲殼素、殼聚糖;木糖塑等之熱塑性樹脂,或聚苯胺或其半氧化物的鹼式聚苯胺(emeraldine base);聚噻吩;聚吡咯;聚伸苯基伸乙烯;聚伸苯基;聚乙炔等之導電性聚合物,進而舉例環氧樹脂;胺基甲酸酯丙烯酸酯;酚樹脂;三聚氰胺樹脂;脲樹脂;醇酸樹脂等之熱硬化性樹脂或光硬化性樹脂等。本發明之含CNT組成物由於較好使用水作為溶劑,故作為基質聚合物較好為水溶性者,例如聚丙烯酸鈉、羧甲基纖維素鈉、水溶性纖維素醚、褐藻酸鈉、聚乙烯醇、聚苯乙烯磺酸、聚乙二醇等,尤其較好為聚丙烯酸鈉、羧甲基纖維素鈉等。
基質聚合物亦可作為市售品獲得,作為此等市售品舉例為例如聚丙烯酸鈉(和光純藥工業(股)製,聚合度2,700~7,500)、羧甲基纖維素鈉(和光純藥工業(股)製)、褐藻酸鈉(關東化學(股)製,鹿1級)、METOLOSE(註冊商標)SH系列(羥丙基甲基纖維素,信越化學工業(股)製)、METOLOSE SE系列(羥乙基甲基纖維素,信越化學工業(股)製)、JC-25(完全皂化型聚乙烯醇,日本VAM & POVAL(股)製)、JM-17(中間皂化型聚乙烯醇,日本VAM & POVAL(股)製)、JP-03(部分皂化型聚乙烯醇,日本VAM & POVAL(股)製)、聚苯乙烯磺酸(Aldrich公司製,固體成分濃度18質量%,水溶液)等。
基質聚合物含量並未特別限定,但組成物中,較好為0.0001~99質量%左右,更好為0.001~90質量%左右。
又,本發明所用之含CNT組成物亦可含有與所用分散劑引起交聯反應之交聯劑或自我交聯之交聯劑。該等交聯劑較好溶解於使用之溶劑中。作為噁唑啉聚合物之交聯劑若為例如含有2個以上之羧基、羥基、硫醇基、胺基、亞磺酸基、環氧基等之具有與噁唑啉基之反應性之官能基的化合物,則未特別限定,但較好含有2個以上羧基之化合物。又,亦可使用含有於薄膜形成時之加熱或酸觸媒存在下產生前述官能基而引起交聯反應之官能基例如羧酸之鈉鹽、鉀鹽、鋰鹽、銨鹽等之化合物作為交聯劑。
作為與噁唑啉基引起交聯反應之化合物具體例,舉例為在酸觸媒存在下發揮交聯反應性之聚丙烯酸或其寡聚物等之合成聚合物及CMC或褐藻酸等之天然聚合物之金屬鹽、藉由加熱而發揮交聯反應性之前聚合成聚合物及天然聚合物之銨鹽等,但尤其較好為在酸觸媒存在下或加熱條件下發揮交聯反應性之聚丙烯酸鈉、聚丙烯酸鋰、聚丙烯酸銨、羧甲基纖維素鈉、羧甲基纖維素鋰、羧甲基纖維素銨等。
與此等噁唑啉基引起交聯反應之化合物可以市售品獲得,作為此種市售品舉例為例如聚丙烯酸鈉(和光純藥工業(股)製,聚合度2,700~7,500)、羧甲基纖維素鈉(和光純藥工業(股)製)、褐藻酸鈉(關東化學(股)製,鹿1級)、ARON(註冊商標)A-30(聚丙烯酸銨,東亞合成(股)製,固體成分濃度32質量%,水溶液)、DN-800H(羧甲基纖維素銨,DAICEL精密化學(股)製)、褐藻酸銨(KIMICA(股)製)等。
做為自我交聯之交聯劑舉例為例如於同一分子內含有對於羥基為醛基、環氧基、乙烯基、異氰酸酯基、烷氧基,對於羧基為醛基、胺基、異氰酸酯基、環氧基,對於胺基為異氰酸酯基、醛基等之可相互反應之交聯性官能基之化合物,或含有藉相同交聯性官能基彼此反應之羥基(脫水縮合)、巰基(二硫醚鍵)、酯基(克勞森(Claisen)縮合)、矽烷醇基(脫水縮合)、乙烯基、丙烯酸基等之化合物等。
作為自我交聯之交聯劑之具體例舉例為在酸觸媒存在下發揮交聯反應之多官能丙烯酸酯、四烷氧基矽烷、含封端異氰酸酯基之單體及含羥基、羧酸、胺基之至少一者之單體的嵌段寡聚物等。
此種自我交聯之交聯劑亦可作為市售品獲得。例如作為多官能丙烯酸酯舉例為A-9300(乙氧化異氰尿酸三丙烯酸酯,新中村化學工業(股)製)、A-GLY-9E(乙氧化甘油三丙烯酸酯(EO9莫耳),新中村化學工業(股)製)、A-TMMT(季戊四醇四丙烯酸酯,新中村化學工業(股)製)等,作為四烷氧基矽烷舉例為四甲氧基矽烷(東京化成工業(股)製)、四乙氧基矽烷(東橫化學(股)製),作為含封端異氰酸酯基之聚合物舉例為ERASTRON(註冊商標)系列E-37、H-3、H38、BAP、NEW BAP-15、C-52、F-29、W-11P、MF-9、MF-25K(第一工業製藥(股)製)等。
該等交聯劑之添加量,係根據使用之溶劑、使用之基材、要求之黏度、要求之膜形狀等而變動,但對於分散劑可為0.001~80質量%,較好為0.01~50質量%,更好為0.05~40質量%。該等交聯劑亦有藉由自我縮合引起交聯反應者,但為與交聯劑引起交聯反應者,於分散劑中存在交聯性取代基時,藉由該等交聯性取代基而促進交聯反應。
前述含CNT組成物中,作為用以促進交聯反應之觸媒,可添加對-甲苯磺酸、三氟甲烷磺酸、吡啶鎓
對-甲苯磺酸、水楊酸、磺基水楊酸、檸檬酸、苯甲酸、羥基苯甲酸、萘羧酸等之酸性化合物,及/或2,4,4,6-四溴環己二烯酮、苯偶因甲苯磺酸酯、2-硝基苄基甲苯磺酸酯、有機磺酸烷酯等之熱酸產生劑。觸媒之添加量對於CNT分散劑較好為0.0001~20質量%,更好為0.0005~10質量%,又更好為0.001~3質量%。
前述含CNT組成物之調製法並未特別限制,只要以任意順序混合CNT及溶劑、及因應需要使用之分散劑、基質聚合物及交聯劑而調製分散液即可。此時,較好對混合物進行分散處理,藉由該處理,可更提高CNT之分散比例。作為分散處理,舉例為機械處理的球磨機、珠磨機、噴射研磨機等之濕式處理,或使用匯流型或探頭型之音波器之超音波處理等,尤其較好為使用噴射研磨機之濕式處理或超音波處理。分散處理時間為任意,較好為1分鐘至10小時左右,更好5分鐘至5小時左右。此時,亦可因應需要施以加熱處理。又,使用交聯劑及/或基質聚合物時,該等亦可於調製由分散劑、CNT及溶劑所成之混合物之後添加。
將前述含CNT組成物塗佈於集電基板之至少一側的面上,藉由使其自然或加熱乾燥,可形成底塗層。底塗層可形成於集電體板面之一部分亦可形成於全面。
本發明中,集電基板之每一面之底塗層單位面積質量通常可設為1.5g/m2以下,但單位面積質量較小時亦可達成本發明效果。因此,單位面積質量較好可設為
0.1g/m2以下,更好為0.09g/m2以下,又更好為未達0.05g/m2。另一方面,為了擔保底塗層之機能且可再現性良好地獲得優異特性之電池,集電基板之每一面之底塗層單位面積質量較好為0.001g/m2以上,更好為0.005g/m2以上,又更好為0.01g/m2以上。
底塗層厚度只要滿足前述單位面積質量,則未特別限制,但考慮抑制所得裝置之應用於底塗層所致之容量降低時,較好為0.01~10μm。
本發明之底塗層單位面積質量係底塗層質量(g)相對於底塗層面積(m2)之比例,底塗層形成為圖型狀時,該面積係僅底塗層之面積,不包含形成為圖型狀之底塗層間露出之集電板面積。
底塗層之質量可例如自底塗層箔切出適當大小之試驗片,測定其質量W0,隨後,自底塗層箔剝離底塗層,測定底塗層剝離後之質量W1,由其差(W0-W1)算出,或者預先測定集電基板之質量W2,隨後,測定形成有底塗層之底塗層箔之質量W3,由其差(W3-W2)算出。剝離底塗層之方法舉例為例如將底塗層浸漬於可溶解或膨潤底塗層之溶劑中,藉由布等擦取底塗層等之方法。
單位面積質量可藉由習知方法調整。例如,藉由塗佈形成底塗層時,可藉由改變用以形成底塗層之塗佈液(含CNT組成物)之固體成分濃度、塗佈次數、塗佈機之塗佈液投入口之間隙等而調整。欲增多單位面積質量時,則提高固體成分濃度,增加塗佈次數,增大間隙。
欲減少單位面積質量時,則降低固體成分濃度,減少塗佈次數,減小間隙。
作為含CNT組成物之塗佈方法舉例為例如旋轉塗佈法、浸漬塗佈法、流動塗佈法、噴墨法、噴霧塗佈法、棒塗佈法、凹版塗佈法、狹縫塗佈法、輥塗佈法、軟版印刷法、轉印印刷法、刷毛塗佈法、刮刀塗佈法、空氣刀塗佈法等,但基於作業效率等之觀點,較好為噴墨法、澆鑄法、浸漬塗佈法、棒塗佈法、刮板塗佈法、輥塗佈法、凹版塗佈法、軟版印刷法、噴霧塗佈法。
加熱乾燥時之溫度為任意,但較好為50~200℃左右,更好為80~180℃左右。
本發明之能量貯藏裝置用電極於前述底塗層表面上具備活性物質層。前述活性物質層可將含有活性物質與黏合劑聚合物、與因應需要之增黏劑或溶劑的電極漿料塗佈於底塗層上,自然或加熱乾燥而形成。活性物質層之形成部位只要根據所用之裝置之電池(cell)形態等適當設定即可,可設於底塗層表面全部或其一部分,但基於使用於層合電池等之目的,而作為藉由超音波熔接等將金屬片與電極接合而成之電極構造體使用時,為了留下熔接部較好於底塗層表面之一部分塗佈電極漿料形成活性物質層。尤其較好於層合電池用途中,留下底塗層之周緣,於其以外之部分塗佈電極漿料形成活性物質層。
前述活性物質包含含鈦氧化物。作為前述含鈦氧化物,舉例為氧化鈦、鈦酸鋰等。該等中,基於容量或壽命、電壓等之觀點,較好為氧化鈦,特佳為具有青銅型之結晶構造之氧化鈦(TiO2(B))。
作為前述黏合劑聚合物,可自習知材料適當選擇使用,舉例為例如PVDF、PVP、PTFE、P(TFE-HFP)、P(VDF-HFP)、P(VDF-CTFE)、PVA、聚醯亞胺、EPDM、SBR、CMC、聚丙烯酸(PAA)、聚苯胺等之導電性聚合物等。黏合劑聚合物之添加量,相對於活性物質100質量份,較好為0.1~20質量份,更好為1~10質量份。
電極漿料之黏度低,塗佈困難時,可因應需要使用增黏劑。作為增黏劑,可自習知材料適當選擇使用,舉例為例如CMC之鈉鹽、銨鹽等。該等可作為市售品獲得,作為其具體例,舉例為於前述與噁唑啉基引起交聯反應之化合物中所例示者相同者。增黏劑之添加量只要適當選擇成為適於塗佈之電極漿料之量即可,但對於活性物質100質量份,較好為0.1~20質量份,更好為0.5~10質量份。
作為溶劑舉例為於前述含CNT組成物中例示之溶劑,只要自該等中因應黏合劑種類適當選擇即可,為PVDF等之非水溶性之黏合劑時較好為NMP,為SBR等之水溶性或水分散性之黏合劑時較好為水。
又,前述電極漿料亦可含有導電助劑,亦可
不含。作為導電助劑舉例為例如碳黑、科琴黑、乙炔黑、碳晶鬚、碳纖維、CNT、天然石墨、人造石墨、氧化釕、鋁、鎳等。導電助劑之添加量較好為10質量份以下,更好為5質量份以下。
作為電極漿料之塗佈方法,舉例為與前述含CNT組成物之塗佈方法同樣之方法。且加熱乾燥時之溫度為任意,但較好為50~400℃左右,更好為80~150℃左右。
前述活性物質層厚度,考慮電池容量與電阻之平衡時,較好為10~500μm,更好為10~300μm,又更好為20~100μm。
本發明之能量貯藏裝置用電極可因應需要壓製。壓製法可使用一般採用之方法,但特佳為模具壓製法或輥壓製法。滾壓製法之壓製壓力並未特別限制,但較好為0.2~3ton/cm。
本發明之能量貯藏裝置係具備前述能量貯藏裝置用電極者,具體而言,構成為具備至少一對正極及負極、介隔於該等各極間之隔離片、及電解質。於該等正極及負極之一者,使用本發明之能量貯藏裝置用電極。前述能量貯藏裝置用電極以外之裝置構成構件的電極、隔離片、電解質等可自習知材料適當選擇使用。
本發明之能量貯藏裝置用電極可作為能量貯
藏裝置之負極使用亦可作為正極使用,但基於所得能量貯藏裝置之電壓、能量密度之觀點,較好作為負極使用。
本發明之能量貯藏裝置用電極作為負極使用時,正極為一般能量貯藏裝置中使用者即可,可為例如具備集電基板與形成於其上之正極活性物質層者。作為集電基板舉例為與前述者同樣者。
正極活性物質層可將含有正極活性物質與黏合劑聚合物、及因應需要之溶劑或導電助劑之電極漿料塗佈於集電基板上,自然或加熱乾燥而形成。此處,作為黏合劑聚合物、溶劑及導電助劑舉例為與前述者同樣者。
作為正極用電極所用之正極活性物質舉例為可吸附、脫離鋰離子之硫屬化合物或含鋰離子之硫屬化合物、聚陰離子系化合物、硫單體及其化合物等。作為此等硫屬化合物舉例為例如FeS2、TiS2、MoS2、V2O6、V6O13、MnO2等。作為含鋰離子硫屬化合物舉例為例如LiCoO2、LiMnO2、LiMn2O4、LiMo2O4、LiV3O8、LiNiO2、LixNiyM1-yO2(惟M表示自Co、Mn、Ti、Cr、V、Al、Sn、Pb及Zn選擇之至少1種以上之金屬元素,0.05≦x≦1.10,0.05≦y≦1.0)等。作為聚陰離子系化合物舉例為例如LiFePO4等。作為硫化合物舉例為例如Li2S、紅胺酸(rubeanic acid)等。
本發明之能量貯藏裝置用電極作為正極使用時,負極為一般能量貯藏裝置中使用者即可,可為例如具備集電基板與形成於其上之負極活性物質層者。作為集電
基板舉例為與前述者同樣者。作為負極活性物質舉例為自金屬鋰、鋰合金、可吸附.放出鋰離子之周期表4~15族之元素選擇之至少1種之單體、氧化物、硫化物、氮化物、或可逆地吸附.放出鋰離子之碳材料等。又,作為負極活性物質使用金屬鋰或鋰合金時,該等可兼作為集電基板。
作為隔離片,舉例為例如纖維素系隔離片、聚烯烴系隔離片等。
作為電解質可為液體、固體之任一者,且可為水系、非水系之任一者,於本發明之能量貯藏裝置用電極應用於使用非水系電解質之裝置時均可發揮實用上充分之性能。
作為非水系電解質,舉例為將電解質鹽溶於非水系有機溶劑而成之非水系電解液。作為前述電解質鹽,舉例為四氟化硼酸鋰、六氟化磷酸鋰、過氯酸鋰、三氟甲烷磺酸鋰等之鋰鹽;四甲基銨六氟磷酸鹽、四乙基銨六氟磷酸鹽、四丙基銨六氟磷酸鹽、甲基三乙基銨六氟磷酸鹽、四乙基銨四氟硼酸鹽、四乙基銨過氯酸鹽等之4級銨鹽;雙(三氟甲烷磺醯基)醯亞胺鋰、雙(氟磺醯基)醯亞胺鋰等之醯亞胺鋰等。作為非水系有機溶劑舉例為碳酸伸丙酯、碳酸伸乙酯、碳酸伸丁酯等之碳酸伸烷酯;碳酸二甲酯、碳酸甲酯乙酯、碳酸二乙酯等之碳酸二烷酯;乙腈等之腈類;二甲基甲醯胺等之醯胺類等。
能量貯藏裝置之形態並未特別限制,可採用
圓筒型、扁平捲繞方型、層合方型、硬幣型、扁平捲繞層壓型、層合層壓型等之以往習知之各種形態之電池。
應用於硬幣型時,只要將本發明之能量貯藏裝置電極衝打成特定圓盤狀即可。例如鋰離子二次電池係於將硬幣電池之墊圈(washer)與間隔片熔接而成之蓋體上設置衝打成特定形狀之另一電極,於其上重疊含浸有電解液之同型狀之隔離片,進而於其上,以活性物質層朝下重疊本發明之能量貯藏裝置電極,載置外殼及墊圈,以硬幣電池鉚接機密封而製作。
應用於層合層壓型時,只要使用於在底塗層表面之一部分或全面形成有活性物質層之電極中之未形成活性物質層之部分(熔接部)與金屬片熔接而合之電極構造體即可。該情況下,構成電極構造體之電極可為一片亦可為複數片,但一般正負極均使用複數片。又,於形成有底塗層且未形成活性物質層之部分熔接時,集電基板之每一面之底塗層之單位面積質量較好為0.1g/m2以下,更好為0.09g/m2以下,又更好為未達0.05g/m2。
較好用以形成電極之複數片電極與用以形成負極之複數片負極板逐片相互重疊,此時,較好於正極與負極之間介隔前述隔離片。
金屬片可於複數片之電極最外側之電極熔接部熔接,亦可將金屬片夾持於複數片電極中之任意鄰接之2片電極之熔接部之間而熔接。金屬片材質若為一般能量貯藏裝置中使用者則未特別限制,舉例為例如鎳、鋁、
鈦、銅等金屬;不鏽鋼、鎳合金、鋁合金、鈦合金、銅合金等之合金等,但考慮熔接效率時,較好含有自鋁、銅及鎳選擇之至少1種金屬而構成。金屬片之形狀較好為箔狀,其厚度較好為0.05~1mm左右。
熔接方法可使用金屬彼此熔接所用之習知方法,其具體例舉例為TIG熔接、點熔接、雷射熔接、超音波熔接等,但於形成底塗層且未形成活性物質層之部分熔接時,本發明之底塗層由於亦具有特別適於超音波熔接之單位面積質量,故較好以超音波熔接接合電極與金屬片。
作為超音波熔接方法,舉例為例如將複數片電極配置於砧與尖頭之間,於熔接部配置金屬片施加超音波而一次熔接之方法,或先使電極彼此熔接,隨後熔接金屬片之方法等。本發明以任一方法,均不僅可於前述熔接部熔接金屬片與電極,亦可使複數片電極彼此相互進行超音波熔接。熔接時之壓力、頻率、輸出、處理時間等並未特別限制,只要考慮所用之材料或熔接部之底塗層之有無、單位面積質量適當設定即可。
將如上述製作之電極構造體收納於層壓封裝後,注入前述電解液後,藉由熱密封而獲得層壓電池。
以下舉例調製例、實施例及比較例更具體說明本發明,但本發明不限定於下述實施例。又下述例中,試料之調製及物性分析所用之裝置及條件如以下。
裝置:Hielscher Ultrasonics公司製,UIP1000
裝置:SMT(股)製,PM-9050MC
裝置:東洋系統(股)製,TOSCAT 3100
裝置:PRIMIX(股)製,T.K.ROBOMIX(附均質分散機2.5型(Φ32))
裝置:PRIMIX(股)製,FILMIX40型
裝置:THINKY(股)製,AWATORY練太郎ARE-310
裝置:寶泉(股)製,超小型桌上熱輥壓製機HSR-60150H
裝置:寶泉(股)製,手動硬幣電池鉚接機CR2032
將含作為分散劑之噁唑啉聚合物之水溶液的EPOCLOTH WS-700(日本觸媒(股)製,固體成分濃度25質量%,Mw=4×104,噁唑啉基量4.5mmol/g)2.0g與蒸餾水47.5g混合,進而於其中混合MWCNT(Nanocyl公司製NC7000,外徑10nm)0.5g。對所得混合物使用探頭型超音波照射裝置於室溫進行30分鐘超音波處理,獲得無沉降物且均一分散MWCNT之黑色含MWCNT之分散液。
於所得之含MWCNT之分散液50g中,添加含聚丙烯酸銨之水溶液的ARON A-30(東亞合成(股)製,固體成分濃度31.6質量%)0.7g、褐藻酸鈉(關東化學(股)製,鹿1級)0.2g及蒸餾水49.1g並攪拌,獲得底塗液A1。
將所得底塗液A1以線棒塗佈器(OSP30,濕膜厚30μm)於集電基板的鋁箔(厚15μm)上均一展開後,於150℃乾燥20分鐘,形成底塗層,製作底塗箔B1。準備20片將底塗箔切成5×10cm者,測定質量後,以浸染0.5mol/L鹽酸之紙擦掉底塗層後測定金屬箔質量,由擦掉
前後之質量差算出底塗層之單位面積質量之結果,為0.302g/m2。
除使用線棒塗佈器(OSP4,濕膜厚4μm)以外,與調製例1同樣,製作底塗箔B2。算出底塗箔B2之單位面積質量後,為0.044g/m2。
除代替MWCNT而使用乙炔黑(AB)(電氣化學工業(股)製,DENKA BLACK)以外,與調製例1同樣,製作底塗箔B3。算出底塗箔B3之單位面積質量後,為0.329g/m2。
除代替MWCNT而使用AB以外,與調製例2同樣,製作底塗箔B4。算出底塗箔B4之單位面積質量後,為0.052g/m2。
將作為活性物質之依據J.Electrochem.Soc.,159(1),A49-A54(2012)中記載之方法合成之TiO2(B)9.53g、作為黏合劑之苯乙烯-丁二烯橡膠(SBR)之水分
散液(48.5質量%,JSR(股)製TRD2001)0.378g、作為增黏劑之羧甲基纖維素銨鹽(NH4CMC,DAICEL(股)製,DN-800H)0.183g及純水19.9g,以均質分散機以6,000rpm混合5分鐘。其次,使用薄膜旋轉型高速混合機以周速25m/秒混合處理60秒,進而以自轉.公轉混合機以2,200rpm脫泡30秒,製作電極漿料(固體成分濃度33質量%,TiO2(B):SBR:NH4CMC=104:2:2(質量比))。
所得電極漿料於調製例1所製作之底塗箔B1上均一(濕膜厚200μm)上展開後,於80℃乾燥30分鐘,其次於120℃乾燥30分鐘,而於底塗層上形成活性物質層,進而藉輥壓製機壓著,製作活性物質層厚45μm之電極C1。
將所得電極C1衝打為直徑10mm之圓盤狀,測定質量後,於100℃真空乾燥15小時,移至充滿氬之手套箱中。
將熔接有2032型之硬幣電池(寶泉(股)製)之墊圈與間隔片之蓋體上,設置6片重疊之衝打為直徑14mm之鋰箔(本莊化學(股)製,厚0.17mm)者,於其上滲入電解液(KISHIDA化學(股)製,碳酸伸乙酯:碳酸二乙酯=1:1(體積比),含1mol/L之電解質的六氟磷酸鋰)24小時以上,重疊一片衝打成直徑16mm之隔離片(CELGUADR(股)製,2400),進而於其上,以塗佈活性物質之面朝下而重疊電極C1。滴加1滴電解液後,載
置外殼及墊片,以硬幣電池鉚接機密封。隨後靜置24小時,作成試驗用之二次電池。
除了代替底塗箔B1而使用調製例2製作之底塗箔B2以外,與實施例1同樣製作電極C2,製作試驗用之二次電池。
除了代替底塗箔B1而使用調製例3製作之底塗箔B3以外,與實施例1同樣製作電極C3,製作試驗用之二次電池。
除了代替底塗箔B1而使用調製例4製作之底塗箔B4以外,與實施例1同樣製作電極C4,製作試驗用之二次電池。
除了代替底塗箔B1而使用無垢之鋁箔以外,與實施例1同樣製作電極C5,製作試驗用之二次電池。
針對前述實施例1~2及比較例1~3製作之鋰離子二次電池,使用充放電測定裝置以下述條件評價電極物性。實施例1及比較例1、3中之於0.5C之充放電曲線
示於圖1,實施例2及比較例2、3中之於0.5C之充放電曲線示於圖2,各放電速率下之對於0.1C放電時之放電容量之容量維持率示於表1。
.電流:0.5C定電流充電,0.5C、1C、3C、5C、10C、20C定電流放電(TiO2(B)之容量設為336mAh/g,最初以0.1C進行5次循環之充放電後,充電速率設為0.5C,每5循環之放電速率上升後,最後使放電速率回到0.5C)。
.截斷電壓:3.00V-1.00V
.溫度:室溫
如圖1及2所示,於0.5C之充放電下,比較例3中製作之使用無垢鋁箔之二次電池僅充放電至40mAh/g左右之容量,相對地,實施例1及2製作之使用MWCNT之底塗箔之二次電池,即使於低單位面積質量,
亦可以65mAh/g左右之容量充放電。另一方面,比較例1及2製作之使用AB之底塗箔之二次電池,於單位面積質量為0.329g/m2時,無法僅能以55mAh/g左右之容量充放電,尤其單位面積質量為0.052g/m2而較小時,僅能獲得與無垢鋁箔同等程度之容量。又,如表1所示,於20C之前之各放電速度中,使用利用MWCNT之底塗箔之二次電池中,與無垢鋁箔相比維持高的放電容量。由此可知,使用TiO2(B)之二次電池中,使用MWCNT之底塗箔尤其於低單位面積質量中,可維持高速率下之容量。
Claims (11)
- 一種能量貯藏裝置用電極,其係具備集電基板、形成於該集電基板之至少一側的面上之含碳奈米管之底塗層、及形成於該底塗層表面上之含有包含含鈦氧化物之活性物質之活性物質層。
- 如請求項1之能量貯藏裝置用電極,其中前述底塗層含有由側鏈含有噁唑啉基之聚合物所成之碳奈米管分散劑。
- 如請求項1~3中任一項之能量貯藏裝置用電極,其中前述含鈦氧化物係氧化鈦。
- 如請求項4之能量貯藏裝置用電極,其中前述氧化鈦係具有青銅型的結晶構造之氧化鈦。
- 如請求項1~5中任一項之能量貯藏裝置用電極, 其中前述活性物質層含有苯乙烯-丁二烯橡膠作為黏合劑,且含有羧甲基纖維素之鹽作為增黏劑。
- 如請求項1~6中任一項之能量貯藏裝置用電極,其中前述底塗層之前述集電基板之每一面之單位面積質量為0.1g/m2以下。
- 一種能量貯藏裝置,其係具備如請求項1~7中任一項之能量貯藏裝置用電極。
- 如請求項8之能量貯藏裝置,其中前述能量貯藏裝置用電極為負極。
- 如請求項8或9之能量貯藏裝置,其係鋰離子二次電池。
- 一種如請求項1之能量貯藏裝置用電極之製造方法,其係將含鈦氧化物、黏合劑與因應需要之增黏劑以水作為分散介質予以混合而製作之電極漿料,塗佈在形成於集電基板之至少一側的面上之含碳奈米管之底塗層表面上並使其乾燥。
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JP3286516B2 (ja) * | 1995-12-06 | 2002-05-27 | 三洋電機株式会社 | 非水電解液二次電池 |
JP4623786B2 (ja) | 1999-11-10 | 2011-02-02 | 住友電気工業株式会社 | 非水二次電池 |
JP5400607B2 (ja) | 2007-03-16 | 2014-01-29 | 石原産業株式会社 | 電極活物質及びそれを用いてなるリチウム電池 |
KR101494435B1 (ko) * | 2008-01-15 | 2015-02-23 | 삼성전자주식회사 | 전극, 리튬 전지, 전극 제조 방법 및 전극 코팅용 조성물 |
US9218917B2 (en) | 2011-06-07 | 2015-12-22 | FastCAP Sysems Corporation | Energy storage media for ultracapacitors |
JP5871302B2 (ja) * | 2011-08-03 | 2016-03-01 | 昭和電工株式会社 | 二次電池用負極および二次電池 |
JP2013045984A (ja) | 2011-08-26 | 2013-03-04 | Nippon Zeon Co Ltd | 蓄電デバイス用電極、蓄電デバイスおよび蓄電デバイス用電極の製造方法 |
JP5468714B1 (ja) | 2012-08-29 | 2014-04-09 | 昭和電工株式会社 | 蓄電デバイスおよびその製造方法 |
WO2015029949A1 (ja) * | 2013-08-27 | 2015-03-05 | 日産化学工業株式会社 | 導電性炭素材料分散剤および導電性炭素材料分散液 |
US20150086860A1 (en) * | 2013-09-26 | 2015-03-26 | Semiconductor Energy Laboratory Co., Ltd. | Power storage device |
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2016
- 2016-12-21 CN CN201680078103.7A patent/CN108475771A/zh active Pending
- 2016-12-21 JP JP2017560093A patent/JP6962199B2/ja active Active
- 2016-12-21 EP EP16883786.2A patent/EP3401982B1/en active Active
- 2016-12-21 KR KR1020187022654A patent/KR20180100205A/ko not_active Application Discontinuation
- 2016-12-21 WO PCT/JP2016/088013 patent/WO2017119287A1/ja active Application Filing
- 2016-12-21 US US16/068,544 patent/US10749183B2/en active Active
- 2016-12-29 TW TW105143933A patent/TWI720103B/zh active
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JPWO2017119287A1 (ja) | 2018-10-25 |
WO2017119287A1 (ja) | 2017-07-13 |
JP6962199B2 (ja) | 2021-11-05 |
EP3401982A1 (en) | 2018-11-14 |
EP3401982A4 (en) | 2019-01-02 |
TWI720103B (zh) | 2021-03-01 |
US10749183B2 (en) | 2020-08-18 |
EP3401982B1 (en) | 2021-09-22 |
KR20180100205A (ko) | 2018-09-07 |
CN108475771A (zh) | 2018-08-31 |
US20190020038A1 (en) | 2019-01-17 |
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