TW201521860A - 導電性碳材料分散劑及導電性碳材料分散液 - Google Patents
導電性碳材料分散劑及導電性碳材料分散液 Download PDFInfo
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- TW201521860A TW201521860A TW103129538A TW103129538A TW201521860A TW 201521860 A TW201521860 A TW 201521860A TW 103129538 A TW103129538 A TW 103129538A TW 103129538 A TW103129538 A TW 103129538A TW 201521860 A TW201521860 A TW 201521860A
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Classifications
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F226/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen
- C08F226/06—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen by a heterocyclic ring containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/041—Carbon nanotubes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L101/02—Compositions of unspecified macromolecular compounds characterised by the presence of specified groups, e.g. terminal or pendant functional groups
- C08L101/025—Compositions of unspecified macromolecular compounds characterised by the presence of specified groups, e.g. terminal or pendant functional groups containing nitrogen atoms
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L101/02—Compositions of unspecified macromolecular compounds characterised by the presence of specified groups, e.g. terminal or pendant functional groups
- C08L101/06—Compositions of unspecified macromolecular compounds characterised by the presence of specified groups, e.g. terminal or pendant functional groups containing oxygen atoms
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L101/00—Compositions of unspecified macromolecular compounds
- C08L101/12—Compositions of unspecified macromolecular compounds characterised by physical features, e.g. anisotropy, viscosity or electrical conductivity
- C08L101/14—Compositions of unspecified macromolecular compounds characterised by physical features, e.g. anisotropy, viscosity or electrical conductivity the macromolecular compounds being water soluble or water swellable, e.g. aqueous gels
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D105/00—Coating compositions based on polysaccharides or on their derivatives, not provided for in groups C09D101/00 or C09D103/00
- C09D105/04—Alginic acid; Derivatives thereof
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
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Abstract
例如,使用如式(1)所示之含□唑啉基的單體而得,在側鏈具有□唑啉基的聚合物所成之導電性碳材料分散劑,係導電性碳材料的分散能力優異,同時與導電性碳材料一起薄膜化時,給予對集電基板的密接性優異之薄膜。
□(式中,X表示含聚合性碳-碳雙鍵之基,R1~R4互相獨立地表示氫原子、鹵素原子、碳數1~5之可具有分支構造的烷基、碳數6~20的芳基、或碳數7~20的芳烷基)。
Description
本發明關於導電性碳材料分散劑及導電性碳材料分散液,更詳述地,關於由在側鏈具有唑啉環的聚合物所成之導電性碳材料分散劑,及包含有此分散劑、導電性碳材料與溶劑,適合作為導電性薄膜用組成物之導電性碳材料分散液。
隨著智慧型手機或數位相機、攜帶式遊戲機等的攜帶式電子機器之小型輕量化或高機能化之要求,近年來,高性能電池的開發係積極地進展,藉由充電而可重複使用的蓄電池之需求係大幅成長。
其中,鋰離子蓄電池由於具有高能量密度、高電壓,且充放電時無記憶效應等,故為目前最傾注精力地進行開發之蓄電池。
又,由於近年的致力解決環境問題,電動汽車之開發亦活躍地進展,於作為其動力源的蓄電池中,要求更高的性能。
又,鋰離子蓄電池係具有將能吸藏、放出鋰之正極與
負極及介於此等之間存在的隔板收納於容器內,於其中裝滿電解液(於鋰離子聚合物蓄電池之情況,以凝膠狀或全固體型的電解質代替液狀電解液)之構造。
正極及負極一般係藉由將含有能吸藏、放出鋰之活性物質、主要由碳材料所構成的導電材、更且聚合物黏結劑之組成物,塗佈於銅箔或鋁箔等之集電體上而製造。該黏結劑係用於接著活性物質與導電材、更且此等與金屬箔之市售聚偏二氟乙烯(PVdF)等之可溶於N-甲基吡咯啶酮(NMP)中的氟系樹脂或、烯烴系聚合物之水分散體等。
如上述,亦期待鋰離子蓄電池作為電動汽車等的動力源之應用,要求迄今為止以上的長壽命或安全性。
然而,上述黏結劑對於集電體的接著力不能說是充分,於電極板的裁切步驟或捲繞步驟等之製造步驟時,成為活性物質或導電材的一部分自集電體剝離、脫落,發生微小短路或電池容量的偏差之原因。
再者,由於長期間之使用,電解液造成黏結劑的膨潤,或隨著活性物質的鋰吸藏、放出所造成的體積變化,而電極合材之體積變化,電極合材與集電體間之接觸電阻係增大,或活性物質或導電材之一部分係自集電體剝離、脫落,而發生電池容量的劣化之問題,更且在安全性之點亦有問題。
特別地,近年來正極系為固溶體系,負極系為矽等之合金系,充放電容量比既存者大,因此而充放電所致的體積變化亦大的活性物質之開發係進展,上述的電極合材自
集電體的剝離,係應盡快解決的問題。
嘗試解決上述問題,開發出在集電體與電極合材之間插入導電性的黏合層之手法。
例如,專利文獻1中揭示將以碳作為導電性填料的導電層當作黏合層,配設於集電體與電極合材之間的技術,藉由使用具備導電性黏合層的複合集電體(以下,亦稱為複合集電體),可減低集電體與電極合材之間的接觸電阻,且亦可抑制高速放電時的容量減少,更且也可抑制電池之劣化。又,專利文獻2或專利文獻3中亦揭示同樣的技術。
於此等之例中,使用碳粒子作為導電性填料,但由於碳粒子對於集電體不具有黏合作用,由於使用成為基質的聚合物來製作黏合層,當然其黏合力係隨著聚合物的含量增大而升高。另一方面,聚合物之含量若增大,則碳粒子間之接觸減少,故黏合層之電阻係急劇地增加,結果有電池全體的電阻增加之問題。
為了解決如此的問題,有報告使用如碳奈米管(以下亦簡稱CNT)之導電性碳奈米材料作為導電性填料之例。
例如,專利文獻4中報告藉由使用多層碳奈米管(以下亦稱為MWCNT),作為導電性碳奈米材料,在鋁箔上形成導電性黏合層,而能提高鋰離子蓄電池之循環壽命。然而,於專利文獻4中,在形成含有MWCNT的導電性黏合層之際,所使用的分散劑之碳奈米管分散能力低,為了得到充分膜厚的層,必須進行複數次的噴塗。
為了藉由塗佈程序將CNT予以成膜,一般地必須使CNT均勻分散在溶劑中,作為其分散手法,有藉由化學程序將CNT予以表面改質之手法(專利文獻5),或併用聚合物等的分散劑之手法(專利文獻6、7)等。其中,併用分散劑之手法,由於不使CNT之優異電氣特性惡化,於作為導電性填料使用時,可說是較佳的方法。
然而,使CNT高濃度分散而得之分散劑,係有對於蓄電池所用之集電體的密接性低之問題,為了得到優異的導電性黏合層,必須添加對於集電體具有密接性的聚合物等。於如此的情況下,由於導電性黏合層中的CNT之濃度降低,結果有導電性降低之問題。
基於如此的觀點,希望開發出不僅以碳奈米管為代表之導電性碳材料的分散能力優異,而且薄膜化時對於集電體的密接性亦優異之導電性碳材料分散劑。
[專利文獻1]特開平9-097625號公報
[專利文獻2]特開2000-011991號公報
[專利文獻3]特開平11-149916號公報
[專利文獻4]特開2009-170410號公報
[專利文獻5]特開2000-44216號公報
[專利文獻6]特開2005-162877號公報
[專利文獻7]國際公開第2008/139839號
本發明係鑑於如此的情事而完成者,目的在於提供以碳奈米管為代表的導電性碳材料之分散能力優異,同時與導電性碳材料一起薄膜化時,能給予對集電基板的密接性優異之薄膜的導電性碳材料分散劑、及含有此分散劑與導電性碳材料和溶劑之導電性碳材料分散液。
本發明者們為了達成上述目的,重複專心致力的檢討,結果發現在側鏈具有唑啉基的聚合物係以碳奈米管為代表的導電性碳材料之分散能力優異,同時由以該聚合物作為分散劑調製之導電性碳材料分散液所得之薄膜,係對於能量儲存裝置的電極之集電基板具有優異的密接性,適合作為導電性黏合層,而完成本發明。
即,本發明提供:1.一種導電性碳材料分散劑,其係由在側鏈具有唑啉基的聚合物所構成;2.如1之導電性碳材料分散劑,其中前述聚合物係水溶性;3.如2之導電性碳材料分散劑,其中前述聚合物係使在第2位具有含聚合性碳-碳雙鍵之基的唑啉單體、與具有親水性官能基的(甲基)丙烯酸系單體之至少2種單體進行自由基聚合而得;
4.一種導電性碳材料分散液,其包含如1~3中任一項之導電性碳材料分散劑、導電性碳材料、與溶劑,且前述導電性碳材料分散於前述溶劑;5.如4之導電性碳材料分散液,其中前述溶劑係水;6.如4或5之導電性碳材料分散液,其包含交聯劑;7.如4~6中任一項之導電性碳材料分散液,其包含成為基質的聚合物;8.一種導電性薄膜用組成物,其係由如4~7中任一項之導電性碳材料分散液所構成;9.一種導電性薄膜,其係由如8之導電性薄膜用組成物所得;10.如9之導電性薄膜,其係介於構成能量儲存裝置的電極之集電基板與活性物質層之間存在,使兩者黏合之導電性黏合層用;11.一種能量儲存裝置的電極用複合集電體,其具備集電基板、與形成於此基板上之由9之導電性薄膜所成的導電性黏合層;12.一種能量儲存裝置用電極,其具備如11之能量儲存裝置的電極用複合集電體;13.如12之能量儲存裝置用電極,其具備如11之能量儲存裝置的電極用複合集電體、與形成於此複合集電體之前述導電性黏合層上的活性物質層;14.一種能量儲存裝置,其具備如12或13之能量儲存裝置用電極;
15.一種薄膜,其係由如4~7中任一項之導電性碳材料分散液所得;16.一種導電性碳材料分散法,其係使用導電性碳材料分散劑,使導電性碳材料分散於溶劑中之導電性碳材料分散法,其特徵為:前述導電性碳材料分散劑係在側鏈具有唑啉基的聚合物;17.一種導電性碳材料分散液之製造方法,其係使用導電性碳材料分散劑,使導電性碳材料分散於溶劑中的導電性碳材料分散液之製造方法,其特徵為:混合由在側鏈具有唑啉基的聚合物所成之導電性碳材料分散劑、導電性碳材料與溶劑,對所得之混合物施予分散處理。
本發明之導電性碳材料分散劑,係不僅碳奈米管、碳黑或石墨烯等的導電性碳材料之分散能力優異,而且對於鋰離子蓄電池、電雙層電容器等之能量儲存裝置的電極所使用的金屬製之集電基板亦具有高密接性。
使用本發明之導電性碳材料分散劑所調製的導電性碳材料分散液,係適合作為導電性薄膜用組成物,其用於形成將構成能量儲存裝置的電極之集電基板與活性物質等予以接合的導電性黏合層。
即,若使用本發明之導電性碳材料分散劑,則即使不用其他的接著性聚合物,也可形成對於集電基板的接著性優異之導電性薄膜,故可以高濃度含有碳奈米管,形成對
於集電基板的接著性優異之導電性薄膜。此係意味可降低導電性黏合層之電氣電阻,尤其在電動汽車用途等需要瞬間大電流之用途中,可製作不引起電壓下降而可取出電流,同時循環壽命長之能量儲存裝置。
本發明之導電性碳材料分散液,係可藉由僅塗佈在基材上而容易地形成薄膜,而由於所得之薄膜顯示高導電性,故適合於導電性薄膜之製造,且如上述不僅給予對於基材的密接性優異之薄膜,而且可藉由濕式法以高再現性有效率地形成大面積之薄膜,故不僅於能量儲存裝置用途,而且可適用於各種半導體材料、電導體材料等之廣泛用途。
圖1係顯示實施例5-1、5-2及比較例5-1所製作的電雙層電容器之電阻測定結果之圖。
以下,更詳細說明本發明。
本發明之導電性碳材料分散劑係由在側鏈具有唑啉基的聚合物所構成者。
本發明中,所謂在側鏈具有唑啉基的聚合物(以下亦稱為唑啉聚合物),只要是在構成主鏈的重複單位中直接或經由伸烷基等的間隔基而鍵結有唑啉基之聚合
物,則沒有特別的限定,但具體地較佳為將如式(1)所示之在第2位具有含聚合性碳-碳雙鍵之基的唑啉單體予以自由基聚合而得,具有在唑啉環的第2位鍵結於聚合物主鏈或間隔基之重複單位的聚合物。
式中,X表示含聚合性碳-碳雙鍵之基,R1~R4互相獨立地表示氫原子、鹵素原子、碳數1~5之可具有分支構造的烷基、碳數6~20的芳基、或碳數7~20的芳烷基。
作為唑啉單體所具有的含聚合性碳-碳雙鍵之基,只要是含有聚合性碳-碳雙鍵,則沒有特別的限定,但較佳為含有聚合性碳-碳雙鍵的鏈狀烴基,例如較佳為乙烯基、烯丙基、異丙烯基等之碳數2~8的烯基等。
作為鹵素原子,可舉出氟原子、氯原子、溴原子、碘原子等。
作為碳數1~5之可具有分支構造的烷基之具體例,可舉出甲基、乙基、正丙基、異丙基、正丁基、第二丁基、第三丁基、正戊基等。
作為碳數6~20的芳基之具體例,可舉出苯基、二甲苯基、甲苯基、聯苯基、萘基等。
作為碳數7~20的芳烷基之具體例,可舉出苄基、苯基乙基、苯基環己基等。
作為式(1)所示之在第2位具有含聚合性碳-碳雙鍵之基的唑啉單體之具體例,可舉出2-乙烯基-2-唑啉、2-乙烯基-4-甲基-2-唑啉、2-乙烯基-4-乙基-2-唑啉、2-乙烯基-4-丙基-2-唑啉、2-乙烯基-4-丁基-2-唑啉、2-乙烯基-5-甲基-2-唑啉、2-乙烯基-5-乙基-2-唑啉、2-乙烯基-5-丙基-2-唑啉、2-乙烯基-5-丁基-2-唑啉、2-異丙烯基-2-唑啉、2-異丙烯基-4-甲基-2-唑啉、2-異丙烯基-4-乙基-2-唑啉、2-異丙烯基-4-丙基-2-唑啉、2-異丙烯基-4-丁基-2-唑啉、2-異丙烯基-5-甲基-2-唑啉、2-異丙烯基-5-乙基-2-唑啉、2-異丙烯基-5-丙基-2-唑啉、2-異丙烯基-5-丁基-2-唑啉等,但從取得容易性等之點來看,較佳為2-異丙烯基-2-唑啉。
又,若考慮使用水系溶劑來調製導電性碳材料分散液,則唑啉聚合物較佳為水溶性。
如此的水溶性唑啉聚合物,亦可為上述式(1)所示的唑啉單體的均聚物,但為了進一步提高在水中的溶解性,較佳為使上述唑啉單體與具有親水性官能基的(甲基)丙烯酸酯系單體之至少2種單體進行自由基聚合而得者。
作為具有親水性官能基的(甲基)丙烯酸系單體之具體例,可舉出(甲基)丙烯酸、丙烯酸2-羥基乙酯、丙烯酸甲氧基聚乙二醇、丙烯酸與聚乙二醇之單酯化物、丙烯
酸2-胺基乙酯及其鹽、甲基丙烯酸2-羥基乙酯、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、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,此等係可單獨使用,也可組合2種以上使用。於此等之中,宜為(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,於本發明中,在對所得之唑啉聚合物的導電性碳材料分散能力不造成不良影響之範圍內,可併用上述唑啉單體及具有親水性官能基的(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,可舉出(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)丙烯酸十八酯、(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;氯乙烯、偏二氯乙烯、氟乙烯等之鹵烯烴系單體;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基醚系單體等,此等係可各自單獨使用,也可組合2種以上使用。
於本發明所用的唑啉聚合物製造時所使用之單體成
分中,唑啉單體之含有率,從進一步提高所得之唑啉聚合物的導電性碳材料分散能力之點來看,較佳為10質量%以上,更佳為20質量%以上,尤更佳為30質量%以上。再者,單體成分中的唑啉單體之含有率的上限值為100質量%,此時得到唑啉單體的均聚物。
另一方面,從進一步提高所得之唑啉聚合物的水溶性之點來看,單體成分中之具有親水性官能基的(甲基)丙烯酸系單體之含有率較佳為10質量%以上,更佳為20質量%以上,尤更佳為30質量%以上。
又,單體成分中的其他單體之含有率係如上述,在對所得之唑啉聚合物的導電性碳材料分散能力不造成影響之範圍,而且由於取決於其種類而不能一概地決定,但可在5~95質量%以下、較佳10~90質量%以下之範圍內適宜設定。
唑啉聚合物之平均分子量係沒有特別的限定,但重量平均分子量較佳為1,000~2,000,000。該聚合物的重量平均分子量若未達1,000,則導電性碳材料之分散能力顯著地降低,或有無法發揮分散能力之虞。另一方面,重量平均分子量若超過2,000,000,則分散處理的操作有變極困難之虞。重量平均分子量為2,000~1,000,000之唑啉聚合物係更佳。
再者,本發明中的重量平均分子量係凝膠滲透層析術之測定值(聚苯乙烯換算)。
本發明所用之唑啉聚合物,係可藉由例如特開平6-
32844號公報或特開2013-72002號公報等中記載之眾所周知的自由基聚合法,使上述各種單體聚合而製造。
又,本發明所可使用的唑啉聚合物,亦可作為市售品取得,作為如此的市售品,例如可舉出Epocros WS-300((股)日本觸媒製,固體成分濃度10質量%,水溶液)、Epocros WS-700((股)日本觸媒製,固體成分濃度25質量%,水溶液)、Epocros WS-500((股)日本觸媒製,固體成分濃度39質量%,水/1-甲氧基-2-丙醇溶液)、聚(2-乙基-2-唑啉)(Aldrich)、聚(2-乙基-2-唑啉)(Alfa Aesar)、聚(2-乙基-2-唑啉)(VWR International,LLC)等。
再者,作為溶液市售時,可直接使用作為導電性碳材料分散液,也可溶劑置換而成為目的之溶劑系的導電性碳材料分散液。
與以上說明的唑啉聚合物一起使用的導電性碳材料,並沒有特別的限定,但用於形成蓄電池的黏合層時,較佳為纖維狀導電性碳材料、層狀導電性碳材料、粒狀導電性碳材料。再者,此等之導電性碳材料係可各自單獨或混合2種以上使用。
作為纖維狀導電性碳材料之具體例,可舉出碳奈米管(CNT)、碳奈米纖維(CNF)等,從導電性、分散性、取得性等之觀點來看,較佳為CNT。
CNT一般係藉由電弧放電法、化學氣相成長法(CVD法)、雷射燒蝕法等來製作,但使用於本發明的CNT係
可藉由任一方法獲得。又,於CNT中,有1片的碳膜(石墨烯‧薄片)捲繞成圓筒狀之單層CNT(以下亦簡稱SWCNT)、2枚的石墨烯‧薄片捲繞成同心圓狀之2層CNT(以下亦簡稱DWCNT)、與複數的石墨烯‧薄片捲繞成同心圓狀之多層CNT(MWCNT),但於本發明中,可將SWCNT、DWCNT、MWCNT各自以單質或組合複數而使用。
再者,以上述之方法製作SWCNT、DWCNT或MWCNT時,由於鎳、鐵、鈷、釔等之觸媒金屬亦會殘存,為了去除此雜質而有必須精製的情況。於雜質之去除中,藉由硝酸、硫酸等的酸處理,同時超音波處理係有效。然而,於藉由硝酸、硫酸等的酸處理中,由於構成CNT的π共軛系係被破壞,有損害CNT本來的特性之可能性,故宜在適當的條件下精製而使用。
作為層狀導電性碳材料之具體例,可舉出石墨、石墨烯等。石墨係沒有特別的限制,可使用市售的各種石墨。
石墨烯係1原子之厚度的sp2鍵結碳原子之薄片,採取由碳原子與該鍵結所形成之如蜂巢的六角形格子構造,其厚度可說是0.38nm左右。又,除了市售的氧化石墨烯,還可使用藉由Hummers法處理石墨而得之氧化石墨烯。
作為粒狀導電性碳材料之具體例,可舉出爐黑、槽黑、乙炔黑、熱黑等之碳黑等。碳黑係無特別的限制,可使用市售的各種碳黑,其粒徑較佳為5nm~500nm。
本發明之導電性碳材料分散液包含上述的唑啉聚合物(導電性碳材料分散劑)、導電性碳材料與溶劑,導電性碳材料係分散在溶劑中。
作為溶劑,例如可舉出水;四氫呋喃(THF)、二乙基醚、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;甲醇、乙醇、異丙醇、正丙醇等之醇類;正庚烷、正己烷、環己烷等之脂肪族烴類;苯、甲苯、二甲苯、乙苯等之芳香族烴類;乙二醇單乙基醚、乙二醇單丁基醚、丙二醇單甲基醚等之二醇醚類;乙二醇、丙二醇等之二醇類等的有機溶劑,此等之溶劑係可各自單獨或混合2種以上使用。
特別地,從能提高導電性碳材料的孤立分散之比例之點來看,較佳為水、NMP、DMF、THF、甲醇、異丙醇,此等之溶劑係可各自單獨或混合2種以上使用。再者,關於所用之溶劑,從能提高組成物的成膜性之點來看,宜含有少量的乙二醇單乙基醚、乙二醇單丁基醚、丙二醇單甲基醚等之二醇醚類;丙酮、甲基乙基酮、環己酮等之酮類、丙二醇等之二醇類等。
再者,使用上述唑啉聚合物時,即使於使用醇類、二醇醚類、二醇類等的親水性溶劑之情況,分散性及成膜性也良好,再者即使為上述親水性溶劑與水之混合溶劑、
或水單獨溶劑之情況,分散性、成膜性也不降低。
近年來,基於脫有機溶劑化之潮流,要求使用水作為溶劑之材料,故於本發明之導電性碳材料分散液中,較佳為亦使用親水性溶劑與水之混合溶劑或水單獨溶劑,最佳為水單獨溶劑。
本發明之導電性碳材料分散液的調製方法係任意,只要以任意之順序混合唑啉聚合物(分散劑)、導電性碳材料及溶劑而調製分散液即可。
此時,較佳為將由唑啉聚合物、導電性碳材料及溶劑所成之混合物予以分散處理,藉由此處理,可進一步提高導電性碳材料的分散比例。作為分散處理,可舉出機械處理之使用球磨機、珠磨機、噴射磨機等的濕式處理、或使用匯流排型或探針型的超音波振盪器之超音波處理。
分散處理之時間為任意,但較佳為1分鐘至10小時左右,更佳為5分鐘至5小時左右。
再者,本發明所用之唑啉聚合物,由於導電性碳材料之分散能力優異,即使在分散處理前等不施予加熱處理,也可得到導電性碳材料以高濃度分散之組成物,但視需要亦可施予加熱處理。
於本發明之導電性碳材料分散液中,唑啉聚合物與導電性碳材料之混合比率以質量比計可為1,000:1~1:100左右。
又,分散液中的唑啉聚合物之濃度,只要是可使導電性碳材料分散於溶劑中之濃度,則沒有特別的限定,但
在分散液中較佳為0.001~30質量%左右,更佳為0.002~20質量%左右。
再者,此分散液中的導電性碳材料之濃度,係隨著薄膜所要求的機械、電氣、熱特性等而變化,而且只要至少導電性碳材料的一部分孤立分散,則為任意,但在分散液中較佳為0.0001~30質量%左右,更佳為0.001~20質量%左右,尤更佳為0.001~10質量%左右。
於如以上所調製的導電性碳材料分散液中,推測分散劑係物理地吸附於導電性碳材料之表面,而形成複合體。
上述導電性碳材料分散液亦可含有可溶於上述溶劑中的交聯劑。
作為交聯劑,可為與唑啉聚合物的唑啉基發生交聯反應之化合物、自我交聯的化合物之任一者,但從進一步提高所得之薄膜的耐溶劑性之點來看,較佳為與唑啉基發生交聯反應的化合物。
作為與唑啉基發生交聯反應的化合物,例如只要是具有2個以上的羧基、羥基、硫醇基、胺基、亞碸酸基、環氧基等之與唑啉基有反應性的官能基之化合物,則沒有特別的限定,但較佳為具有2個以上的羧基之化合物。再者,於薄膜形成時的加熱或酸觸媒之存在下產生上述官能基而引起交聯反應的官能基,例如具有羧酸的鈉鹽、鉀鹽、鋰鹽、銨鹽等之化合物,亦可作為交聯劑使用。
作為與唑啉基發生交聯反應的化合物之具體例,可舉出在酸觸媒之存在下發揮交聯反應性的聚丙烯酸或其共
聚物等之合成高分子及羧甲基纖維素或海藻酸等天然高分子之金屬鹽,藉由加熱發揮交聯反應性的上述合成高分子及天然高分子之銨鹽等,但特別地較佳為酸觸媒之存在下或加熱條件下發揮交聯反應性的聚丙烯酸鈉、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。
如此與唑啉基發生交聯反應的化合物,亦可作為市售品取得,作為如此的市售品,例如可舉出聚丙烯酸鈉(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),海藻酸鈉(關東化學(股)製,鹿1級)、Aron 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)、海藻酸銨((股)KIMICA製)等。
作為自我交聯的化合物,例如可舉出對於羥基的醛基、環氧基、乙烯基、異氰酸酯基、烷氧基、對於羧基的醛基、胺基、異氰酸酯基、環氧基、對於胺基的異氰酸酯基、醛基等之在同一分子內具有互相反應的交聯性官能基之化合物,或具有以相同交聯性官能基彼此反應的羥基(脫水縮合)、巰基(二硫鍵結)、酯基(克萊森縮合)、矽烷醇基(脫水縮合)、乙烯基、丙烯酸基等之化合物等。
作為自我交聯的化合物之具體例,可舉出在酸觸媒的存在下發揮交聯反應性之多官能丙烯酸酯、四烷氧基矽
烷、具有封端異氰酸酯基的單體及具有羥基、羧酸、胺基之至少1個的單體之嵌段共聚物等。
如此之自我交聯的化合物,亦可作為市售品取得,作為如此的市售品,例如於多官能丙烯酸酯中,可舉出A-9300(乙氧基化異三聚氰酸三丙烯酸酯,新中村化學工業(股)製)、A-GLY-9E(乙氧基化甘油三丙烯酸酯(EO9mol),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),於四烷氧基矽烷中,可舉出四甲氧基矽烷(東京化成工業(股)製),四乙氧基矽烷(東橫化學(股)製),於具有封端異氰酸酯基的聚合物中,可舉出Elastron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。
此等之交聯劑係可各自單獨使用,也可組合2種類以上使用。
交聯劑之含量係隨著所使用的溶劑、所使用的基材、所要求的黏度或膜形狀等而變動,但通常相對於唑啉聚合物,為0.001~80質量%,較佳為0.01~50質量%,更佳為0.05~40質量%。
再者,本發明之導電性碳材料分散液亦可含有作為促進交聯反應用的觸媒之對甲苯磺酸、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、苯偶姻甲苯磺酸酯、2-硝基苄基甲苯磺酸
酯、有機磺酸烷酯等之熱酸產生劑。
相對於導電性碳材料分散劑(唑啉聚合物),觸媒之含量通常為0.0001~20質量%,較佳為0.0005~10質量%,更佳為0.001~3質量%。
再者,本發明之導電性碳材料分散液亦可含有成為基質的高分子。其含量係沒有特別的限定,但於分散液中較佳為0.0001~99質量%左右,更佳為0.001~90質量%左右。
作為成為基質的高分子,例如可舉出聚偏二氟乙烯(PVdF)、聚四氟乙烯、四氟乙烯-六氟丙烯共聚物、偏二氟乙烯-六氟丙烯共聚物[P(VDF-HFP)]、偏二氟乙烯-氯三氟乙烯共聚物[P(VDF-CTFE)]等之氟系樹脂、聚乙烯吡咯啶酮、乙烯-丙烯-二烯三元共聚物、PE(聚乙烯)、PP(聚丙烯)、EVA(乙烯-乙酸乙烯酯共聚物)、EEA(乙烯-丙烯酸乙酯共聚物)等之聚烯烴系樹脂;PS(聚苯乙烯)、HIPS(高衝擊聚苯乙烯)、AS(丙烯腈-苯乙烯共聚物)、ABS(丙烯腈-丁二烯-苯乙烯共聚物)、MS(甲基丙烯酸甲酯-苯乙烯共聚物)、苯乙烯-丁二烯橡膠等之聚苯乙烯系樹脂;聚碳酸酯樹脂;氯乙烯樹脂;聚醯胺樹脂;聚醯亞胺樹脂;聚丙烯酸鈉、PMMA(聚甲基丙烯酸甲酯)等之(甲基)丙烯酸樹脂;PET(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、聚萘二甲酸丁二酯、PLA(聚乳酸)、聚-3-羥基丁酸、聚己內酯、聚丁二酸丁二酯、聚丁二酸
乙二酯/己二酸酯等之聚酯樹脂;聚伸苯基醚樹脂;改性聚伸苯基醚樹脂;聚縮醛樹脂;聚碸樹脂;聚苯硫樹脂;聚乙烯醇樹脂;聚葡糖酸;改性澱粉;乙酸纖維素、羧甲基纖維素、三乙酸纖維素;幾丁質、甲殼素;木質素等之熱塑性樹脂,或聚苯胺及其半氧化物之翠綠亞胺鹼;聚噻吩;聚吡咯;聚伸苯基乙烯;聚伸苯基;聚乙炔等之導電性高分子,更且環氧樹脂;胺基甲酸酯丙烯酸酯;酚樹脂;三聚氰胺樹脂;尿素樹脂;醇酸樹脂等之熱硬化性樹脂或光硬化性樹脂等,但於本發明之導電性碳材料分散液中,從宜使用水作為溶劑來看,基質高分子亦是水溶性者,例如可舉出聚丙烯酸鈉、羧甲基纖維素鈉、水溶性纖維素醚、海藻酸鈉、聚乙烯醇、聚苯乙烯磺酸、聚乙二醇等,特佳為聚丙烯酸鈉、羧甲基纖維素鈉等。
如此成為基質的高分子亦可作為市售品取得,作為如此的市售品,例如可舉出聚丙烯酸鈉(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)、海藻酸鈉(關東化學(股)製,鹿1級)、Metolose SH系列(羥基丙基甲基纖維素,信越化學工業(股)製)、Metolose SE系列(羥基乙基甲基纖維素、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。
於本發明之導電性分散液含有交聯劑及/或成為基質的高分子時,作為分散液之調製方法,可對至少混合有導電性碳材料、導電性碳材料分散劑、溶劑、交聯劑及/或成為基質的高分子者,進行機械處理之使用球磨機、珠磨機、噴射磨機等的濕式處理、或使用匯流排型或探針型的超音波振盪器之超音波處理而調製,特宜為使用噴射磨機的濕式處理或超音波處理。再者,交聯劑或成為基質的高分子亦可藉由前述方法調製分散液後添加。
本發明之導電性碳材料分散液可與一般的導電性碳材料分散液同樣地,適用作為導電性薄膜用組成物。
如前述,本發明之導電性碳材料分散液中所含有的唑啉聚合物(分散劑),不僅導電性碳材料的分散能力優異,而且對於能量儲存裝置之電極所使用的集電基板亦具有高密接性。
因此,由本發明之導電性碳材料分散液(導電性薄膜用組成物)所得之導電性薄膜,係介於構成能量儲存裝置的電極之集電基板與活性物質層之間存在,特別適合於使兩者黏合的導電性黏合層。
再者,作為能量儲存裝置,可舉出電雙層電容器、鋰蓄電池、鋰離子蓄電池、質子聚合物電池、鎳氫電池、鋁固體電容器、電解電容器、鉛蓄電池等之各種能量儲存裝置,但由本發明之導電性薄膜用組成物所得之導電性薄膜,係可特別適用於電雙層電容器、鋰離子蓄電池之電
極。
使用本發明的導電性薄膜用組成物之電極製作時,較佳為首先製作由集電基板與導電性黏合層所成之複合集電體。
此複合集電體係可將上述導電性碳材料分散液(導電性薄膜用組成物)塗佈於集電基板上,將其自然或加熱乾燥,形成導電性黏合層而製作。
作為集電基板,可自以往作為能量儲存裝置用電極的集電基板使用者中適宜選擇,例如可使用銅、鋁、鎳、金、銀及彼等之合金或碳材料、金屬氧化物、導電性高分子等之薄膜。
其厚度係沒有特別的限定,但於本發明中較佳為1~100μm。
又,導電性黏合層之厚度亦沒有特別的限定,但若考慮減低內部電阻,則較佳為0.05~10μm。
作為塗佈方法,例如可舉出旋塗法、浸塗法、流動塗佈法、噴墨法、噴塗法、棒塗法、凹版塗佈法、縫塗法、輥塗法、膠版印刷法、轉印印刷法、刷毛塗佈、刮板塗佈法、氣刀塗佈法等,但從作業效率等之點來看,宜為噴墨法、澆鑄法、浸塗法、棒塗法、刮板塗佈法、輥塗法、凹版塗佈法、膠版印刷法、噴塗法。
加熱乾燥時的溫度亦任意,但較佳為50~200℃左右,更佳為80~150℃左右。
再者,能量儲存裝置用電極係可在上述複合集電體之
導電性黏合層上,形成活性物質層而製作。
此處,作為活性物質,可使用以往能量儲存裝置用電極所用之各種活性物質。
例如,於鋰蓄電池或鋰離子蓄電池之情況,作為正極活性物質,可使用能吸附‧離脫鋰離子的硫屬化合物或含鋰離子的硫屬化合物、聚陰離子系化合物、硫單質及其化合物等。
作為如此之能吸附‧離脫鋰離子的硫屬化合物,例如可舉出FeS2、TiS2、MoS2、V2O6、V6O13、MnO2等。
作為含鋰離子的硫屬化合物,例如可舉出LiCoO2、LiMnO2、LiMn2O4、LiMo2O4、LiV3O8、LiNiO2、LixNiyM1-yO2(惟,M表示由Co、Mn、Ti、Cr、V、Al、Sn、Pb及Zn中選出的至少1種以上之金屬元素,0.05≦x≦1.10,0.5≦y≦1.0)等。
作為聚陰離子系化合物,例如可舉出LiFePO4等。
作為硫化合物,例如可舉出Li2S、紅胺酸等。
另一方面,作為構成上述負極的負極活性物質,可使用鹼金屬、鹼合金、吸藏‧放出鋰離子的由週期表第4~15族的元素所選出的至少1種之單質、氧化物、硫化物、氮化物、或能可逆地吸藏‧放出鋰離子之碳材料。
作為鹼金屬,可舉出Li、Na、K等,作為鹼金屬合金,例如可舉出金屬Li、Li-Al、Li-Mg、Li-Al-Ni、Na、Na-Hg、Na-Zn等。
作為吸藏放出鋰離子的由週期表第4~15族的元素所
選出的至少1種之元素的單質,例如可舉出矽或錫、鋁、鋅、砷等。
同樣作為氧化物,例如可舉出錫矽氧化物(SnSiO3)、鋰氧化鉍(Li3BiO4)、鋰氧化鋅(Li2ZnO2)、鋰氧化鈦(Li4Ti5O12)等。
同樣作為硫化物,可舉出鋰硫化鐵(LixFeS2(0≦x≦3))、鋰硫化銅(LixCuS(0≦x≦3))等。
同樣作為氮化物,可舉出含鋰的過渡金屬氮化物,具體地可舉出LixMyN(M=Co、Ni、Cu,0≦x≦3、0≦y≦0.5)、鋰鐵氮化物(Li3FeN4)等。
作為能可逆地吸藏‧放出鋰離子之碳材料,可舉出石墨、碳黑、焦炭、玻璃狀碳、碳纖維、碳奈米管、或此等之燒結體等。
又,於電雙層電容器之情況,可使用碳質材料作為活性物質。
作為此碳質材料,可舉出活性碳等,例如將酚樹脂碳化後,進行活化處理而得之活性碳。
活性物質層係可將含有以上說明的活性物質、黏結劑聚合物及視需要的溶劑之電極漿體,塗佈在導電性黏合層上,進行自然或加熱乾燥而形成。
作為黏結劑聚合物,可自眾所周知的材料中適宜選擇而使用,例如可舉出聚偏二氟乙烯(PVdF)、聚乙烯吡咯啶酮、聚四氟乙烯、四氟乙烯-六氟丙烯共聚物、偏二氟乙烯-六氟丙烯共聚物[P(VDF-HFP)]、偏二氟乙烯-氯
三氟乙烯共聚物[P(VDF-CTFE)]、聚乙烯醇、聚醯亞胺、乙烯-丙烯-二烯三元共聚物、苯乙烯-丁二烯橡膠、羧甲基纖維素(CMC)、聚丙烯酸(PAA)、聚苯胺等之導電性高分子等。
再者,相對於活性物質100質量份,黏結劑聚合物之添加量較佳為0.1~20質量份,特佳為1~10質量份。
作為溶劑,可舉出在上述唑啉聚合物所例示之溶劑,可自彼等之中按照黏結劑之種類來適宜選擇,但於PVdF等的非水溶性黏結劑之情況,宜為NMP,於PAA等的水溶性黏結劑之情況,宜為水。
再者,上述電極漿體亦可含有導電助劑。作為導電助劑,例如可舉出碳黑、廚黑、乙炔黑、碳晶鬚、碳纖維、天然石墨、人造石墨、氧化鈦、氧化釕、鋁、鎳等。
作為電極漿體之塗佈方法,可舉出與上述導電性黏合層形成用組成物同樣之手法。
又,加熱乾燥時的溫度亦任意,但較佳為50~400℃左右,更佳為80~150℃左右。
又,電極視需要亦可進行加壓。加壓法係可使用一般採用的方法,但特佳為模具加壓法或輥加壓法。輥加壓法的加壓係沒有特別的限定,但較佳為0.2~3ton/cm。
本發明之能量儲存裝置係具備上述電極者,更具體地,具備至少一對的正負極、介於此等各極間存在的隔板、與電解質而構成,正負極的至少一者係由上述能量儲存裝置用電極所構成。
此能量儲存裝置由於具有特徵為在電極使用上述能量儲存裝置用電極,其他的裝置構成構件之隔板或電解質等係可自眾所周知的材料中適宜選擇。
作為隔板,例如可舉出纖維素系隔板、聚烯烴系隔板等。
作為電解質,可為液體、固體之任一者,而且亦可為水系、非水系之任一者,但本發明之能量儲存裝置用電極,即使採用於使用非水系電解質的裝置時,也能發揮實用上充分的性能。
作為非水系電解質,可舉出在非水系有機溶劑中溶解電解質鹽而成之非水系電解液。
作為電解質鹽,可舉出四氟硼酸鋰、六氟磷酸鋰、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四級銨鹽、鋰雙(三氟甲烷磺醯基)醯亞胺、鋰雙(氟磺醯基)醯亞胺等。
作為非水系有機溶劑,可舉出碳酸伸丙酯、碳酸伸乙酯、碳酸伸丁酯等之碳酸伸烷酯;碳酸二甲酯、碳酸甲基乙酯、碳酸二乙酯等之碳酸二烷酯;乙腈等之腈類、二甲基甲醯胺等醯胺類等。
以下,舉出實施例及比較例,更具體地說明本發明,
惟本發明不受下述的實施例所限定。再者,所用的裝置係如以下。
(1)探針型超音波照射裝置(分散處理)
Hielscher Ultrasonics公司製UIP1000
(2)線棒塗佈機(薄膜製作)
(股)SMT製PM-9050MC
(3)Select-Roller
松尾產業(股)製OSP-30
(4)充放電測定裝置(蓄電池評價)
北斗電工(股)製HJ1001SM8A
(5)測微計(黏結劑、活性物質層之膜厚測定)
(股)MITUTOYO製IR54
(6)T.K.機器人混合機(附均質分散器2.5型(Φ32))(PRIMIX(股)製)
(7)薄膜旋轉型高速混合機
Filmix 40型(PRIMIX(股)製)
(8)自轉‧公轉混合機
脫泡練太郎ARE-310((股)THINKY製)
(9)輥加壓裝置
超小型桌上熱輥壓機HSR-60150H(寶泉(股)製)
(10)電阻測定
PARSTAT 2273(Princeton Applied Research公司製)
[1]導電性碳材料分散液之調製
[實施例1-1]
將含有唑啉聚合物的水溶液之Epocros WS-300((股)日本觸媒製,固體成分濃度10質量%,重量平均分子量1.2×105,唑啉基量7.7mmol/g)4.9g與蒸餾水44.6g混合,更於其中混入多層CNT(Nanocyl公司製「NC7000」)0.5g。對於所得之混合物,使用探針型超音波照射裝置,在室溫進行30分鐘超音波處理,而調製導電性碳材料分散液A。
[實施例1-2]
將含有唑啉聚合物的水溶液之Epocros WS-700((股)日本觸媒製,固體成分濃度25質量%,重量平均分子量4×104,唑啉基量4.5mmol/g)2.0g與蒸餾水47.5g混合,更於其中混入多層CNT(Nanocyl公司製「NC7000」)0.5g。對於所得之混合物,使用探針型超音波照射裝置,在室溫進行30分鐘超音波處理,而調製導電性碳材料分散液B。
[實施例1-3]
使聚丙烯酸鈉(PAA-Na)(和光純藥工業(股)製,聚合度2,700~7,500)0.36g溶解於蒸餾水49.64g中。將所得之溶液與實施例1-1所調製之導電性碳材料分散液A 50g混合,而調製導電性碳材料分散液C。
[實施例1-4]
將含有聚丙烯酸銨(PAA-NH4)的水溶液之Aron A-30(東亞合成(股),固體成分濃度31.6質量%)1.09g與蒸餾水48.91g混合。將所得之溶液與實施例1-1之導電性碳材料分散液A 50g混合,而調製導電性碳材料分散液D。
[實施例1-5]
將聚丙烯酸鈉(PAA-Na)(和光純藥工業(股)製,聚合度2,700~7,500)0.33g、含有聚丙烯酸(PAA)的水溶液之Aron A-10H(東亞合成(股),固體成分濃度25.8質量%)0.11g與蒸餾水49.56g混合。將所得之溶液與實施例1-1之導電性碳材料分散液A 50g混合,而調製導電性碳材料分散液E。
[實施例1-6]
將聚丙烯酸鈉(PAA-Na)(和光純藥工業(股)製,聚合度2,700~7,500)0.33g、含有聚丙烯酸銨(PAA-NH4)的水溶液之Aron A-30(東亞合成(股),固體成分濃度31.6質量%)0.11g與蒸餾水49.56g混合。將所得之溶液與實施例1-1之導電性碳材料分散液A 50g混合,而調製導電性碳材料分散液F。
[實施例1-7]
將含有唑啉聚合物的水溶液之Epocros WS-300((股)日本觸媒製,固體成分濃度10質量%,重量平均分子量1.2×105,唑啉基量7.7mmol/g)4.9g與蒸餾水44.6g混合,於其中混入多層CNT(宇部興產(股)製「AMC」)0.5g。對於所得之混合物,使用探針型超音波照射裝置,在室溫進行30分鐘超音波處理,更於其中混入已使聚丙烯酸鈉(PAA-Na)(和光純藥工業(股)製,聚合度2,700~7,500)0.33g與含有聚丙烯酸(PAA)的水溶液之Aron A-10H(東亞合成(股),固體成分濃度25.8質量%)0.11g溶解在蒸餾水49.56g中者,而調製導電性碳材料分散液G。
[實施例1-8~11]
除了代替多層CNT(宇部興產(股)製「AMC」),分別使用多層CNT(昭和電工(股)製「VGCF-X」)、乙炔黑(電氣化學工業(股)製「Denka Black」)、石墨烯(Bridgestone KBG(股)製「WGNP」)、多層CNT(Bayer公司製「Baytubes」)以外,以與實施例1-7同樣之方法調製導電性碳材料分散液H~K。
[實施例1-12]
將含有聚丙烯酸銨(PAA-NH4)的水溶液之Aron A-
30(東亞合成(股),固體成分濃度31.6質量%)0.275g、海藻酸銨(海藻酸NH4)((股)KIMICA)的1%水溶液8g與蒸餾水11.73g混合。將所得之溶液與實施例1-1之導電性碳材料分散液A20g混合,而調製導電性碳材料分散液L。
[實施例1-13]
將含有聚丙烯酸銨(PAA-NH4)的水溶液之Aron A-30(東亞合成(股),固體成分濃度31.6質量%)0.7g、海藻酸鈉(海藻酸Na)(關東化學(股),鹿1級)0.2g與蒸餾水49.1g混合。將所得之溶液與實施例1-2之導電性碳材料分散液B 50g混合,而調製導電性碳材料分散液M。
[實施例1-14]
將含有聚丙烯酸銨(PAA-NH4)的水溶液之Aron A-30(東亞合成(股),固體成分濃度31.6質量%)0.7g、海藻酸鈉(海藻酸Na)(關東化學(股),鹿1級)0.2g與蒸餾水49.1g混合。將所得之溶液與實施例1-9之導電性碳材料分散液I 50g混合,而調製導電性碳材料分散液N。
[比較例1-1]
將聚乙烯吡咯啶酮(東京化成工業(股)製,分子量
630,000)0.5g與蒸餾水49.0g混合,更於其中混入多層CNT(Nanocyl公司製「NC7000」)0.5g。對於所得之混合物,使用探針型超音波照射裝置,在室溫進行30分鐘超音波處理,而調製導電性碳材料分散液。
[比較例1-2]
將聚乙烯吡咯啶酮(東京化成工業(股)製,分子量40,000)0.5g與蒸餾水49.0g混合,更於其中混入多層CNT(Nanocyl公司製「NC7000」)0.5g。對於所得之混合物,使用探針型超音波照射裝置,在室溫進行30分鐘超音波處理,而調製導電性碳材料分散液。
[比較例1-3]
將聚乙烯醇(東亞合成(股)製,JF-17)0.5g與蒸餾水49.0g混合,更於其中混入多層CNT(Nanocyl公司製「NC7000」)0.5g。對於所得之混合物,使用探針型超音波照射裝置,在室溫進行30分鐘超音波處理,嘗試導電性碳材料分散液之調製,但即使處理後也凝聚物存在於混合物中,無法得到均勻的分散液。
[比較例1-4]
將聚丙烯醯胺水溶液(Aldrich製,重量平均分子量10,000,固體成分濃度50質量%)1.0g與蒸餾水48.5g混合,更於其中混入多層CNT(Nanocyl公司製
「NC7000」)0.5g。對於所得之混合物,使用探針型超音波照射裝置,在室溫進行30分鐘超音波處理,嘗試導電性碳材料分散液之調製,但即使處理後也凝聚物存在於混合物中,無法得到均勻的分散液。
[比較例1-5]
將含有聚丙烯酸鈉(PAA-Na)的水溶液之Aron A-7195(東亞合成(股)製,固體成分濃度19質量%)2.63g與蒸餾水46.87g混合,更於其中混入多層CNT(Nanocyl公司製「NC7000」)0.5g。對於所得之混合物,使用探針型超音波照射裝置,在室溫進行30分鐘超音波處理,嘗試導電性碳材料分散液之調製,但即使處理後也凝聚物存在於混合物中,無法得到均勻的分散液。
[比較例1-6]
將含有聚丙烯酸銨(PAA-NH4)的水溶液之Aron A-30(東亞合成(股),固體成分濃度31.6質量%)1.58g與蒸餾水47.92g混合,更於其中混入多層CNT(Nanocyl公司製「NC7000」)0.5g。對於所得之混合物,使用探針型超音波照射裝置,在室溫進行30分鐘超音波處理,嘗試導電性碳材料分散液之調製,但即使處理後也凝聚物存在於混合物中,無法得到均勻的分散液。
如由以上之結果可知,於實施例之導電性碳材料分散液中,不發生凝聚物,此等之分散液為均勻,相對於其,
使用聚乙烯吡咯啶酮作為分散劑時,雖然可得到不含凝聚物的導電性碳材料分散液,但是使用聚乙烯醇、聚丙烯醯胺、聚丙烯酸鈉或聚丙烯酸銨時,發生凝聚物,無法得到均勻的導電性碳材料分散液。
根據以上,可知唑啉聚合物係作為使導電性碳材料分散到水中用的分散劑,有效地作用。
[2]導電性薄膜之製造
分別使用均勻的導電性碳材料分散液之實施例1-1~1-11及比較例1-1~1-2所調製的分散液,嘗試導電性薄膜之製造。
[實施例2-1]
以線棒塗佈機(Select-Roller:OSP-30,濕膜厚30μm),將實施例1-1之導電性碳材料分散液均勻地展開在鋁箔(厚度20μm)上後,將其在120℃乾燥20分鐘而製造導電性薄膜。
[實施例2-2~2-11]
除了代替實施例1-1之導電性碳材料分散液,分別使用實施例1-2~1-11所調製之各導電性碳材料分散液以外,以與實施例2-1同樣之方法調製導電性薄膜。
[實施例2-12]
以線棒塗佈機(Select-Roller:OSP-30,濕膜厚30μm),將實施例1-12之導電性碳材料分散液L均勻地展開在銅箔(厚度20μm)上後,將其在120℃乾燥20分鐘,更且在150℃於真空下乾燥20分鐘而製造導電性薄膜。
[實施例2-13~2-14]
除了代替實施例1-1之導電性碳材料分散液,使用實施例1-13~1-14所調製之各導電性碳材料分散液,不在120℃乾燥20分鐘,而在150℃乾燥20分鐘以外,分別以與實施例2-1同樣之方法製造導電性薄膜。
再者,使以上所得之鋁箔或銅箔與導電性薄膜之積層體,成為以鋁箔作為集電基板,以導電性薄膜作為黏合層之複合集電體(實施例2-1~2-9、2-13~2-14之複合集電體),或成為以銅箔作為集電基板,以導電性薄膜作為黏合層之複合集電體(實施例2-12之複合集電體),使用於後述之實施例中。
[比較例2-1、2-2]
以線棒塗佈機(Select-Roller:OSP-30,濕膜厚30μm),將比較例1-1、1-2所調製之各導電性碳材料分散液各自均勻地展開在鋁箔(厚度20μm)上,將彼等乾燥而嘗試導電性薄膜之製造,但任一的分散液皆被鋁所排斥而不能均勻地展開,無法製造導電性薄膜。
如由以上之結果可知,實施例之分散液係可在鋁、銅等之金屬上均勻地展開,可在鋁上製造導電性薄膜,相對於其,比較例之分散液係被鋁所排斥而無法薄膜化。
由以上可知,含有唑啉聚合物作為分散劑之導電性碳材料分散液,係具有對鋁等的金屬上之優異的成膜性。
將含CNT的導電性薄膜形成在金屬上而使用者係多,而且基於近來之脫有機溶劑化之潮流,要求使用水作為溶劑之材料,本發明之含有唑啉聚合物的水系導電性碳材料分散液可說是能應付此等要求之合適材料。
[3]密接性及耐溶劑性評價
對於實施例2-1~2-14所製作之導電性薄膜,藉由下述所示之手法,評價與集電基板的鋁或銅之密接性及耐溶劑性。表1中顯示結果。
<密接性試驗>
以縱橫各自1mm間隔,交叉切割導電性薄膜,形成100個1mm四方的方格。其次,於此交叉切割部分上貼附黏著膠帶(NICHIBAN(股)製,CT-12S2P),剝離該膠帶,進行密接性試驗。當時,將完全未剝下的情況評價為「○」,將一部分或全部剝下的情況評價為「×」。
<耐溶劑性試驗>
使浸有下述各溶劑之棉棒來回地接觸導電性黏合層,
進行耐溶劑性試驗。當時,將導電性黏合層未剝落之情況評價為「○」,將部分地剝落之情況評價「△」,將全部剝落之情況評價為「×」。
1.蒸餾水
2.碳酸二乙酯(DEC)
3.碳酸伸乙酯(EC)及碳酸二乙酯(DEC)之混合溶劑(EC/DEC=1/1(v/v))
4.碳酸伸丙酯(PC)
5.二甲亞碸(DMSO)(關東化學(股)製)
6.四氫呋喃(THF)(關東化學(股)製)
7.N-甲基吡咯啶酮(NMP)(純正化學(股)製)
可知由不含添加劑(基質聚合物及交聯劑)的實施例1-1、1-2所調製之分散液來製作的導電性黏合層,雖然對於鋁的密接性良好,但耐溶劑性差(實施例2-1、2-2)。
相對於其,由添加有PAA-Na的實施例1-3所調製之分散液來製作的導電性黏合層,係改善耐溶劑性(實施例2-3)。推測由於唑啉基不與PAA-Na發生交聯反應,PAA-Na係具有作為基質聚合物之機能,因此改善耐溶劑性。
又,由添加有PAA-NH4的實施例1-4、添加有PAA-Na及PAA的實施例1-5、1-7~1-11、添加有PAA-Na與
PAA-NH4的實施例1-6、添加有PAA-NH4與海藻酸NH4的實施例1-12、添加有PPA-NH4與海藻酸Na的實施例1-13~1-14所調製之分散液來分別製作的導電性黏合層,係進一步改善耐溶劑性(實施例2-4~2-11、2-13~14)。
推測PAA-NH4或海藻酸NH4係因加熱而氨脫離,變成與唑啉有高反應性的PAA或海藻酸,而且由於PAA-Na或海藻酸Na係在酸觸媒(PAA)之存在下可與唑啉反應,藉由此等化合物與唑啉基所參與的交聯,而進一步改善耐溶劑性
如以上,於剝離試驗中,使用唑啉聚合物所製作的導電性黏合層,係顯示與集電基板的鋁箔及銅箔之高密接性,完全未剝離。因此可知,藉由使用本發明之導電性碳材料分散劑,形成於集電基板上之薄膜係不易脫落,可製造耐久性優異之電極。
另一方面,於耐溶劑性試驗中,藉由在使用唑啉聚合物所製作的導電性黏合層中,添加適當的基質聚合物或交聯劑,可提高對於電極漿體之分散介質或電解液之耐久性。因此,可抑制導電性黏合層在電極漿體或電解液中溶出、膨潤、脫落等之劣化,結果可製作能不引起電池的電壓下降而取出電流,同時循環壽命長、安全性高之蓄電池,而且可製作安全性高的電雙層電容器。
[4]電極之製作
[實施例3-1]
將作為活性物質的磷酸鐵鋰(LFP,TATUNG FINE CHEMICALS製,17.3g)、作為黏結劑的PVdF之NMP溶液(12質量%,12.8g)、作為導電助劑的乙炔黑(AB,電氣化學工業(股)製,Denka Black,0.384g)及NMP(9.54g)混合,使用T.K.機器人混合機(附均質分散器2.5型(Φ32))(PRIMIX(股)製),以3,500rpm進行1分鐘處理。其次,使用薄膜旋轉型高速混合機Filmix 40型(PRIMIX(股)製),以周速:20m/秒進行30秒的混合處理,再使用自轉‧公轉混合機,以1000rpm進行2分鐘脫泡而製作電極漿體(固體成分濃度48質量%,LFP:PVdF:AB=8:90:2(質量比))。
於實施例2-1之集電體的黏合層之上,藉由刮板法,將先前調製的電極漿體均勻(濕膜厚200μm)地展開後,在80℃乾燥30分鐘,接著在120℃乾燥30分鐘,而在導電性黏合層上形成活性物質層,以輥壓機壓合此而製作電極(膜厚55μm)。
[實施例3-2~3-9]
除了代替實施例2-1之複合集電體,分別使用實施例2-2~2-9之複合集電體以外,以與實施例3-1同樣之方法製作電極。
[比較例3-1]
除了代替實施例2-1之複合集電體,僅使用集電基板
的鋁箔(厚度20μm)以外,以與實施例3-1之方法同樣的方法製作電極。
[實施例3-10]
將作為活性物質的矽(Si,(股)高純度化學研究所製、SIE23PB,8.89g)、作為黏結劑的聚醯胺酸(PI,4,4’-二胺基二苯基醚與3,3’,4,4’-聯苯基四羧酸二酐之反應物)之NMP溶液(15質量%,12.5g)、作為導電助劑的乙炔黑(AB,電氣化學工業(股)製,Denka Black,0.936g)及NMP(7.69g)混合,使用T.K.機器人混合機(附均質分散器2.5型(Φ32))(PRIMIX(股)製),以8,000rpm進行1分鐘處理。其次,使用薄膜旋轉型高速混合機,以周速:20m/秒進行60秒的混合處理,再使用自轉‧公轉混合機,以1000rpm進行2分鐘脫泡而製作電極漿體(固體成分濃度39質量%,Si:PI:AB=76:16:8(質量比))。
於實施例2-12之複合集電體的黏合層之上,藉由刮板法,將先前調製的電極漿體均勻(濕膜厚50μm)地展開後,在80℃乾燥30分鐘,接著在120℃乾燥30分鐘,而在導電性黏合層上形成活性物質層,以輥壓機壓合此,再者於真空下以350℃燒成40分鐘,而製作電極。
[比較例3-2]
除了代替實施例2-12之複合集電體,僅使用集電基
板的銅箔(厚度20μm)以外,以與實施例3-10同樣之方法製作電極。
[實施例3-11]
將作為電極材的活性碳(KURARAY化學(股)製,YP-50F)11.83g、作為黏結劑的羧甲基纖維素之銨鹽(CMC-NH4,DAICEL化學工業(股)製,Daicel CMC DN800H)的水溶液(1質量%)27.5g、作為導電助劑的乙炔黑(AB,電氣化學工業(股)製,Denka Black)0.69g、蒸餾水13.02g及含苯乙烯-丁二烯共聚物(SBR)的水系乳化溶液(JSR(股)製,固體成分48.5質量%,TRD2001)1.96g混合,使用T.K.機器人混合機(附均質分散器2.5型(Φ32))(PRIMIX(股)製),以5,000rpm進行3分鐘處理。其次,使用薄膜旋轉型高速混合機Filmix 40型(PRIMIX(股)製),以周速:20m/秒進行60秒的混合處理,再使用自轉‧公轉混合機,以1000rpm進行2分鐘脫泡而製作電極漿體(固體成分濃度25質量%,活性碳:CMC-NH4:AB:SBR=86:2:5:7(質量比))。
於實施例2-13之複合集電體的黏合層之上,藉由刮板法,將先前調製的電極漿體均勻(濕膜厚300μm)地展開後,在80℃乾燥30分鐘,接著在120℃乾燥30分鐘,而在導電性黏合層上形成活性物質層,以輥壓機壓合此而製作電極(膜厚120μm)。
[實施例3-12]
除了代替實施例2-13之複合集電體,使用實施例2-14之複合集電體以外,以與實施例3-11同樣之方法製作電極。
[比較例3-3]
除了代替實施例2-13之複合集電體,僅使用集電基板的鋁箔(厚度20μm)以外,以與實施例3-11同樣之方法製作電極。
[5]鋰離子蓄電池之製作及特性評價
[5-1]作為正極使用之電池
[實施例4-1]
將實施例3-1所製作之電極衝壓成直徑10mm之圓盤狀,測定質量後,在100℃真空乾燥15小時,移到經氬氣所充滿的手套箱內。於熔接有墊圈(washer)與間隔物的2032型硬幣式電池(寶泉(股)製)之帽(cap)上裝載墊片(gasket),設置重疊有6片之經衝壓成直徑14mm的鋰箔(本莊化學(股)製,厚度0.17mm)者,於其上,重疊一片之已浸入經電解液(KISHIDA化學(股)製,碳酸伸乙酯:碳酸二乙酯=1:1(體積比),含有1mol/L的電解質的六氟磷酸鋰)中24小時以上且經衝壓成直徑16mm的隔板(CELGARD(股)製,
2400)。再自上方,以塗佈有活性物質的面成為下,重疊先前經衝壓成圓盤狀的電極。滴下1滴的電解液後,裝上外殼,用硬幣式電池鉚接機進行密封。然後靜置24小時,而製作蓄電池。
[實施例4-2~4-9]
除了代替實施例3-1所製作之電極,分別使用實施例3-2~3-9所製作之電極以外,以與實施例4-1同樣之方法製作蓄電池。
[比較例4-1]
除了代替實施例3-1所製作之電極,使用比較例3-1所製作之電極以外,以與實施例4-1同樣之方法製作蓄電池。
評價實施例4-1~4-9及比較例4-1所製作之蓄電池的特性。以評價導電性黏合層對於正極中的導電性黏合層之安定性及電池電阻之影響為目的,於以下之條件下進行充放電試驗。表2中顯示第13循環的放電速率5C時之平均電壓(V)及放電容量(mAh/g)。
‧電流:0.5C恆定電流充電,依0.5C、3C、5C、10C、0.5C之順序各5循環的恆定電流放電(LFP之容量為170mAh/g)後,以5C恆定電流放電直到50循環為止
‧截止電壓:4.50V-2.00V
‧溫度:室溫
如表2所示,與比較例4-1所製作的電池比較下,實施例4-1~4-9所製作之電池顯示放電時較高的電壓與較大的放電容量。推測此係因為在實施例之電池中,存在於活性物質層與集電體之間的導電性黏合層係使彼等的密接性升高,結果活性物質層及集電體間之界面電阻變低。
又,於實施例4-1~4-9所製作之電池中,即使在50循環後,也沒有在放電容量看到大幅減少。因此,可知多層CNT層係對於鋰即使在4.5V附近的高電壓下也不引起氧化分解。可知本發明之具有導電性黏合層的電極,係可適用於鋰離子蓄電池之正極。此意味尤其在電動汽車用途等需要瞬間大電流的用途中,可製造能不引起電壓下降而取出電流,同時循環壽命長的能量儲存裝置。
根據以上,藉由本發明之導電性碳材料分散液,可藉由僅塗佈在基材上而容易地將導電性薄膜予以成膜,而且所得之導電性薄膜係適合作為蓄電池的導電性黏合層,再者,藉由將具有本發明之如此的導電性薄膜作為黏合層之
蓄電池用電極,使用當作蓄電池的電極,尤其當作鋰離子蓄電池的正極,而可得到具有良好特性的蓄電池。
[5-2]作為負極使用之電池
[實施例4-10]
將實施例3-10所製作之電極衝壓成直徑10mm之圓盤狀,測定質量後,在100℃真空乾燥15小時,移到經氬氣所充滿的手套箱內。於熔接有墊圈與間隔物的2032型硬幣式電池(寶泉(股)製)之帽上裝載墊片,設置重疊有6片之經衝壓成直徑14mm的鋰箔(本莊化學(股)製,厚度0.17mm)者,於其上,重疊一片之已浸入電解液(KISHIDA化學(股)製,碳酸伸乙酯:碳酸二乙酯=1:1(體積比),含有1mol/L的電解質之六氟磷酸鋰)中24小時以上且經衝壓成直徑16mm的隔板(CELGARD(股)製,2400)。再自上方,以塗佈有活性物質的面成為下,重疊先前經衝壓成圓盤狀的電極。滴下1滴的電解液後,裝上外殼,用硬幣式電池鉚接機進行密封。然後靜置24小時,而製作試驗用的蓄電池。
[比較例4-2]
除了代替實施例3-10所製作之電極,使用比較例3-2所製作之電極以外,以與實施例4-10同樣之方法製作蓄電池。
評價實施例4-10及比較例4-2所製作之蓄電池的特
性。以評價導電性黏合層對於陰極中的導電性黏合層之安定性及電池電阻之影響為目的,於以下之條件下進行充放電試驗。表3中顯示第30循環的放電容量。
‧電流:0.1C恆定電流充放電(僅第1循環以0.01V的恆定電流定電壓充電,Si之容量為4200mAh/g)
‧截止電壓:1.50V-0.01V
‧充電容量:以活性物質的重量作為基準,至2000mAh/g為止
‧溫度:室溫
於30循環時,與放電容量為731mAh/g的比較例4-2所製作之電池比較下,實施例4-10所製作之電池係維持1950mAh/g的高放電容量。
由以上可知,於鋰離子蓄電池之負極,尤其於具備矽作為活性物質的負極,採用本發明之導電性黏合層,可製造具有良好特性的蓄電池。
[6]電雙層電容器之製作及特性評價
[實施例5-1]
將實施例3-11所製作之電極衝壓2片成直徑10mm之圓盤狀,測定質量後,在130℃真空乾燥8小時,移到
經氬氣所充滿的手套箱內。將電極2片與經衝壓成直徑16mm的隔板(NIPPON高度紙工業(股)製,TF-40-50)1片,浸入電解液(KISHIDA化學(股)製,碳酸伸丙酯,含有1mol/L的電解質之四乙基銨四氟硼酸鹽)中,在0.05MPa進行20分鐘的減壓脫泡處理。於熔接有墊圈與間隔物的2032型硬幣式電池(寶泉(股)製)之外殼上,以塗佈有活性碳之面成為上,重疊先前經減壓脫泡處理的電極1片,於其上重疊隔板。再自上方,以塗佈有活性碳之面成為下,重疊先前經減壓脫泡處理的電極1片。滴下3滴的電解液後,載置墊片,於此上載置熔接有墊圈與間隔物的帽,用硬幣式電池鉚接機進行密封。然後靜置24小時,而製作電雙層電容器。
[實施例5-2]
除了代替實施例3-11所製作之電極,使用實施例3-12所製作之電極以外,以與實施例5-1同樣之方法製作電雙層電容器。
[比較例5-1]
除了代替實施例3-11所製作之電極,使用比較例3-3所製作之電極以外,以與實施例5-1同樣之方法製作電雙層電容器。
評價實施例5-1~5-2及比較例5-1所製作之電雙層電容器的特性。以評價導電性黏合層對於電池電阻之影響為
目的,於以下之條件下進行充放電試驗。表4中顯示自第31循環之電壓上升所算出的電池電阻(Ω)。
‧電流:以0.1mA/cm2進行8循環,依0.2mA/cm2、0.5mA/cm2、1.0mA/cm2、2.0mA/cm2、4.0mA/cm2、8.0mA/cm2之順序各5循環的恆定電流充放電後,以0.1mA/cm2進行恆定電流充電,最後恆定電流定電壓放電
‧截止電壓:僅最初的3循環在2.0V-0V,以後為2.5V-0V
‧溫度:室溫
又,以評價導電性黏合層對於集電體-活性物質之界面的影響為目的,於以下條件下進行電阻測定。圖1中顯示電阻測定之結果。
‧AC Amplitude:10mVrms
‧頻率:200kHz~100mHz
如表4、圖1中所示,與比較例5-1所製作之電雙層電容器比較下,實施例5-1~5-2所製作之電雙層電容器係顯示較低的電池電阻與較低的界面電阻。推測此係因為在實施例之電雙層電容器中,存在於活性物質層與集電體之間的導電性黏合層係使彼等的密接性升高,結果活性物質層及集電體間之界面電阻變低。
根據以上,藉由使用本發明之導電性碳材料分散液,係可藉由僅塗佈在基材上而容易地將導電性薄膜予以成膜,而且所得之導電性薄膜係適合作為電雙層電容器之導電性黏合層,藉由使用具有如此的導電性薄膜作為黏合層之電雙層電容器用電極,可得到具有良好特性的電雙層電容器。
Claims (17)
- 一種導電性碳材料分散劑,其係由在側鏈具有唑啉基的聚合物所構成。
- 如請求項1之導電性碳材料分散劑,其中前述聚合物係水溶性。
- 如請求項2之導電性碳材料分散劑,其中前述聚合物係使在第2位具有含聚合性碳-碳雙鍵之基的唑啉單體、與具有親水性官能基的(甲基)丙烯酸系單體之至少2種單體進行自由基聚合而得。
- 一種導電性碳材料分散液,其特徵為包含如請求項1~3中任一項之導電性碳材料分散劑、導電性碳材料、與溶劑,前述導電性碳材料係分散在前述溶劑中。
- 如請求項4之導電性碳材料分散液,其中前述溶劑係水。
- 如請求項4或5之導電性碳材料分散液,其包含交聯劑。
- 如請求項4~6中任一項之導電性碳材料分散液,其包含成為基質的聚合物。
- 一種導電性薄膜用組成物,其係由如請求項4~7中任一項之導電性碳材料分散液所構成。
- 一種導電性薄膜,其係由如請求項8之導電性薄膜用組成物所得。
- 如請求項9之導電性薄膜,其係介於構成能量儲 存裝置的電極之集電基板與活性物質層之間存在,使兩者黏合之導電性黏合層用。
- 一種能量儲存裝置的電極用複合集電體,其具備集電基板、與形成於此基板上之由請求項9之導電性薄膜所成的導電性黏合層。
- 一種能量儲存裝置用電極,其具備如請求項11之能量儲存裝置的電極用複合集電體。
- 如請求項12之能量儲存裝置用電極,其具備如請求項11之能量儲存裝置的電極用複合集電體、與形成於此複合集電體之前述導電性黏合層上的活性物質層。
- 一種能量儲存裝置,其具備如請求項12或13之能量儲存裝置用電極。
- 一種薄膜,其係由如請求項4~7中任一項之導電性碳材料分散液所得。
- 一種導電性碳材料分散法,其係使用導電性碳材料分散劑,使導電性碳材料分散於溶劑中之導電性碳材料分散法,其特徵為:前述導電性碳材料分散劑係在側鏈具有唑啉基的聚合物。
- 一種導電性碳材料分散液之製造方法,其係使用導電性碳材料分散劑,使導電性碳材料分散於溶劑中的導電性碳材料分散液之製造方法,其特徵為:混合由在側鏈具有唑啉基的聚合物所成之導電性碳材料分散劑、導電性碳材料與溶劑,對所得之混合物施予 分散處理。
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- 2014-08-25 EP EP14840163.1A patent/EP3040115B1/en active Active
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- 2014-08-25 WO PCT/JP2014/072165 patent/WO2015029949A1/ja active Application Filing
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- 2014-08-25 US US14/915,087 patent/US20160200850A1/en not_active Abandoned
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2015
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
TWI753133B (zh) * | 2017-03-15 | 2022-01-21 | 日商Kj化成品股份有限公司 | 碳材料用㗁唑啉系分散劑等及利用此等之碳複合材料 |
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US11326010B2 (en) | 2022-05-10 |
JP5773097B1 (ja) | 2015-09-02 |
US20190218326A1 (en) | 2019-07-18 |
US20160200850A1 (en) | 2016-07-14 |
JP2016006770A (ja) | 2016-01-14 |
CN106947280A (zh) | 2017-07-14 |
WO2015029949A1 (ja) | 2015-03-05 |
TW201827125A (zh) | 2018-08-01 |
KR101771506B1 (ko) | 2017-08-25 |
CN105473216B (zh) | 2018-04-20 |
EP3040115B1 (en) | 2021-02-24 |
EP3695899A1 (en) | 2020-08-19 |
KR20160149324A (ko) | 2016-12-27 |
CN106947280B (zh) | 2020-03-03 |
TWI649121B (zh) | 2019-02-01 |
TWI650172B (zh) | 2019-02-11 |
EP3040115A4 (en) | 2017-03-29 |
JP6044677B2 (ja) | 2016-12-14 |
JPWO2015029949A1 (ja) | 2017-03-02 |
KR20160045792A (ko) | 2016-04-27 |
KR101939154B1 (ko) | 2019-01-16 |
EP3040115A1 (en) | 2016-07-06 |
CN105473216A (zh) | 2016-04-06 |
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