TW201921785A - 電極用黏合劑樹脂、電極合劑糊劑、電極及電極之製造方法 - Google Patents
電極用黏合劑樹脂、電極合劑糊劑、電極及電極之製造方法Info
- Publication number
- TW201921785A TW201921785A TW107129043A TW107129043A TW201921785A TW 201921785 A TW201921785 A TW 201921785A TW 107129043 A TW107129043 A TW 107129043A TW 107129043 A TW107129043 A TW 107129043A TW 201921785 A TW201921785 A TW 201921785A
- Authority
- TW
- Taiwan
- Prior art keywords
- electrode
- binder resin
- group
- electrode mixture
- polyimide
- Prior art date
Links
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Abstract
本發明係關於一種由熔點為300℃以下之聚醯亞胺系樹脂構成之電極用黏合劑樹脂。又,本發明係關於一種電極合劑糊劑,該電極合劑糊劑包含該電極用黏合劑樹脂、電極活性物質、及溶劑;與一種電極及電極之製造方法,該電極具有含有該電極用黏合劑樹脂及電極活性物質之電極合劑層。
Description
本發明係關於鋰離子二次電池、電雙層電容器等之電化學元件之電極用之黏合劑樹脂。
鋰離子二次電池,具有高能量密度且為高容量,因此廣泛利用作為行動式資訊終端機之驅動電源等。近年來,向要求大容量之電動、混和動力車之搭載等產業用途上的使用亦逐漸擴展,為了更加高容量化、高性能化,研究正在進行。其中一項嘗試,例如使用每單位體積之鋰吸留量多之矽、錫,或含有該等之合金作為負極活性物質,使充放電容量增大者。
但,若使用矽、錫、或含有該等之合金這般充放電容量大之活性物質,活性物質隨著充放電會發生非常大的體積變化,因此在至今廣泛使用碳作為活性物質的電極中之將聚偏二氟乙烯、橡膠系之樹脂作為黏合劑樹脂使用的情形,活性物質層容易破壞,或於集電體與活性物質層之界面變得容易發生剝離,因此有電極內之集電構造被破壞、電極之電子傳導性下降而使電池之循環特性容易地下降之問題。
因此,期望開發即使活性物質發生非常大的體積變化,電極之破壞、剝離亦不易發生、電池環境下之靭性高的黏合劑樹脂。
如專利文獻1所記載,使用聚醯亞胺樹脂作為鋰離子二次電池之電極用之黏結劑係公知。
專利文獻2中,提議對於含有矽、矽合金之活性物質,使用具有特定的機械特性之聚醯亞胺作為黏合劑樹脂。藉此,呈現了即使活性物質隨著充放電發生大的體積變化,亦可抑制活性物質層之破壞、集電體與活性物質層之剝離。然而,此處雖揭示了聚醯亞胺之機械特性、玻璃轉移溫度、線膨脹係數、及熱分解開始溫度,但並未揭示其具體的化學結構。
專利文獻3中,提議具有3,3’,4,4’-聯苯四羧酸殘基之聚醯亞胺等作為靭性高之黏合劑樹脂。
專利文獻4中,作為具備固體電解質層的固體電池之負極的黏結劑,揭示了使用黏結於固體電解質且對該固體電解質為非活性之第1黏結劑,與對於負極集電體之黏結性相較第1黏結劑更優異的第2黏結劑,且作為第2黏結劑可列舉含有全芳香族聚醯亞胺之高彈性樹脂。 [先前技術文獻] [專利文獻]
[專利文獻1]日本特開平6-163031號公報 [專利文獻2]國際公開第2004/004031號 [專利文獻3]國際公開第2011/040308號 [專利文獻4]日本特開2014-116154號公報
[發明所欲解決之課題]
聚醯亞胺具有作為黏合劑樹脂之優異的特性,另一方面,對溶劑溶解性不高,因而有難以處理的問題。因此,多採用使用為聚醯亞胺前驅物之聚醯胺酸溶液製作電極合劑糊劑,並將它塗佈於集電體上形成電極合劑層後,藉由熱處理進行醯亞胺化使其成為聚醯亞胺之方法。但醯亞胺化反應需要於高溫加熱,又,因反應會生成水,有對電極合劑層含有的電極活性物質、固體電解質等給予不良影響的疑慮。又,亦有人採用使用可溶性聚醯亞胺,使其溶解於溶劑中,製作電極合劑糊劑,將其塗佈於集電體上,之後,藉由熱處理去除溶劑而形成電極合劑層的方法。但可溶解聚醯亞胺之溶劑,一般而言為N-甲基-2-吡咯烷酮(NMP)等之極性溶劑,不宜使用。
本發明之目的係提供一種由聚醯亞胺系樹脂構成之電極用黏合劑樹脂,可不使用極性溶劑而藉由相較低溫的熱處理形成集電體與電極合劑層之黏接性優異的電極,又,製作電極時不需進行會伴隨水之生成的醯亞胺化反應。 [解決課題之手段]
本案發明者們,經各種探討,結果發現藉由使用熔點相較特定的溫度低之聚醯亞胺系樹脂作為黏合劑樹脂,可不使用極性溶劑而藉由相較低溫的熱處理形成集電體與電極合劑層之黏接性優異的電極,而完成了本發明。
即,本發明係關於以下事項。 1.一種電極用黏合劑樹脂,係由熔點為300℃以下之聚醯亞胺系樹脂構成。 2.如前述第1項之電極用黏合劑樹脂,其中,該聚醯亞胺系樹脂含有聚醯亞胺,該聚醯亞胺係由四羧酸成分與二胺成分獲得且四羧酸成分或二胺成分之至少一方含有50莫耳%以上之脂肪族化合物。 3.如前述第2項之電極用黏合劑樹脂,其中,該聚醯亞胺係由下列化學式(1)表示之結構單元1種以上構成。 [化1](式中,R1
係具有1個或2個芳香環之4價基,R2
係碳數1~20之2價伸烷基。) 4.如前述第3項之電極用黏合劑樹脂,其中,該化學式(1)中的R1
係選自由下列化學式(2)~(5)之4價基構成的群組中之1種以上。 [化2]。
5.如前述第1項之電極用黏合劑樹脂,其中,該聚醯亞胺系樹脂含有加成反應性醯亞胺寡聚物,該加成反應性醯亞胺寡聚物於平均聚合度為50以下之醯亞胺寡聚物之至少一邊的末端具有加成反應基。 6.如前述第5項之電極用黏合劑樹脂,其中,前該加成反應基為苯乙炔基、或含有乙炔鍵之基。 7.如前述第6項之電極用黏合劑樹脂,其中,該加成反應性醯亞胺寡聚物係下列化學式(6)表示之加成反應性醯亞胺寡聚物。 [化3](式中,R3
係選自由具有1個或2個芳香環之4價基構成之群組中之1種以上,R4
係選自由碳數1~20之2價烴基構成之群組中之1種以上,R5
係含有乙炔鍵之1價基,n係1~15之整數;在此,各結構單元含有的R3
及R4
可為相同亦可為不同。)
8.一種電極用黏合劑樹脂組成物,包含如前述1至7項中任一項之電極用黏合劑樹脂。 9.一種電極合劑糊劑,包含如前述1至7項中任一項之電極用黏合劑樹脂、電極活性物質、及溶劑。 10.如第9項之電極合劑糊劑,其中,該溶劑為非極性溶劑。 11.如第9或10項之電極合劑糊劑,更包含固體電解質。
12.一種電極之製造方法,其特徵為包括下列步驟: 將如9至11項中任一項之電極合劑糊劑塗佈於由金屬箔構成之集電體的表面;及, 將已塗佈之電極合劑糊劑以該電極合劑糊劑含有之聚醯亞胺系樹脂之熔點以上、350℃以下的溫度進行熱處理。
13.一種電極,具有電極合劑層,該電極合劑層含有如1至7項中任一項之電極用黏合劑樹脂、及電極活性物質。 14.如第13項之電極,其中,該電極合劑層形成於由金屬箔構成之集電體的表面。 15.如第13或14項之電極,其中,該電極合劑層更含有固體電解質。 [發明之效果]
依據本發明,可提供一種由聚醯亞胺系樹脂構成之電極用黏合劑樹脂,該電極用黏合劑樹脂可不使用極性溶劑而藉由相較低溫的熱處理形成集電體與電極合劑層之黏接性優異的電極。又,本發明之電極用黏合劑樹脂,製作電極時不需進行醯亞胺化反應,因此可防止因醯亞胺化反應而生成的水所致之對電極合劑層含有的電極活性物質、固體電解質等給予不良影響之情形。並且,黏合劑樹脂即便不溶解於溶劑中而以分散的狀態使用於電極合劑層之形成,亦可得到充足的黏結力、集電體與電極合劑層之黏接性。又,可藉由相較低溫的熱處理形成電極,製作電極時不需使用極性溶劑,亦不需進行會生成水之醯亞胺化反應,因此亦可抑制對電極合劑層含有的電極活性物質、固體電解質等給予不良影響。結果依據本發明,可得到具有良好特性之電極。
使用本發明之電極用黏合劑樹脂而獲得之電極,可適宜地使用作為鋰離子二次電池之電極,尤其係充放電容量大的鋰離子二次電池用之電極。
本發明之電極用黏合劑樹脂使用的聚醯亞胺系樹脂,其特徵為醯亞胺化反應實質地完結且熔點為300℃以下。聚醯亞胺系樹脂的熔點更宜為250℃以下,又以200℃以下更佳。此處,「醯亞胺化反應實質地完結」,係指即使製作電極時進行加熱處理,醯亞胺化反應進行而生成之水不至於對電極合劑層含有的電極活性物質、固體電解質等產生不良影響,且只要在可得到本發明之效果的範圍內,本發明之電極用黏合劑樹脂使用的聚醯亞胺系樹脂,亦可含有醯亞胺化反應前之醯胺酸結構之重複單元。
本發明之電極用黏合劑樹脂,可由熔點為300℃以下,宜為250℃以下之聚醯亞胺系樹脂之1種構成,亦可為熔點為300℃以下,宜為250℃以下之聚醯亞胺系樹脂之2種以上的混合物。惟,本發明之電極用黏合劑樹脂,通常宜為呈現單一的熔點者。
本發明中之聚醯亞胺系樹脂,係指來自四羧酸成分及二胺成分之具有兩個環狀醯亞胺基之重複單元,即,意指具有1個以上下列化學式表示的重複單元之聚合物及寡聚物。又,四羧酸成分中,除了四羧酸,亦包括四羧酸二酐等四羧酸衍生物。 [化4](式中,A係自四羧酸成分去除了羧基之4價基,B係自二胺成分去除了胺基之2價基。)
作為前述聚醯亞胺系樹脂,可舉例以四羧酸成分及二胺成分構成且該等之至少一方,又宜為四羧酸成分或二胺成分之任一方,含有50莫耳%以上之脂肪族化合物,又以80莫耳%以上更佳。藉由使用脂肪族化合物,可容易得到熔點為300℃以下之聚醯亞胺。某一實施態様中,尤以由芳香族四羧酸成分及脂肪族二胺成分而獲得之聚醯亞胺,或由脂肪族四羧酸成分及芳香族二胺成分而獲得之聚醯亞胺為佳。
作為前述四羧酸成分,可舉例如3,3’,4,4’-聯苯四羧酸二酐、2,3,3’,4’-聯苯四羧酸二酐、2,2’,3,3’-聯苯四羧酸二酐、苯均四酸二酐、二苯酮四羧酸二酐、4,4’-氧基二鄰苯二甲酸二酐、二苯基碸四羧酸二酐、對聯三苯四羧酸二酐、間聯三苯四羧酸二酐等芳香族四羧酸二酐,及丁烷-1,2,3,4-四羧酸二酐等脂肪族四羧酸二酐。
作為前述二胺成分,可舉例如1,2-丙烷二胺、1,3-二胺基丙烷、2-甲基-1,3-丙烷二胺、1,4-二胺基丁烷、1,3-二胺基戊烷、1,5-二胺基戊烷、2-甲基-1,5-二胺基戊烷、1,6-二胺基己烷(己二胺)、1,7-二胺基庚烷、1,8-二胺基辛烷、1,9-二胺基壬烷、1,10-二胺基癸烷、1,11-二胺基十一烷、1,12-二胺基十二烷等脂肪族二胺。
又,作為前述二胺成分,可舉例如對苯二胺、間苯二胺、2,4-二胺基甲苯、間苯二甲胺、對苯二甲胺、4,4’-二胺基二苯醚、3,4’-二胺基二苯醚、4,4’-二胺基二苯甲烷、3,3’-二胺基二苯甲烷、3,4’-二胺基二苯甲烷、4,4’-二胺基二苯硫醚、4,4’-二胺基二苯碸、3,3’-二胺基二苯碸、1,5-二胺基萘、雙(4-胺基-3-羧基苯基)甲烷、1,3-雙(4-胺基苯氧基)苯、1,4-雙(4-胺基苯氧基)苯、2,2-雙[4-(4-胺基苯氧基)苯基]丙烷、雙[4-(4-胺基苯氧基)苯基]碸、4,4’-雙(4-胺基苯氧基)聯苯等芳香族二胺。
如前述,四羧酸成分或二胺成分之至少一方含有50莫耳%以上之脂肪族化合物之聚醯亞胺,宜為由芳香族四羧酸成分及脂肪族二胺成分獲得的聚醯亞胺,考量作為電極用黏合劑樹脂之性能的觀點,尤宜為由下列化學式(1)所示之結構單元1種以上構成之聚醯亞胺。 [化5]化學式(1)中,R1
係具有1個或2個芳香環之4價基,R2
係碳數1~20之2價伸烷基。
化學式(1)中,R1
宜為具有1個或2個苯環作為芳香環之4價基,更宜為下列化學式(2)~(5)之4價基。 [化6]。
化學式(1)中,R2
宜為碳數3~16之伸烷基,更宜為碳數3~14之伸烷基。又,R2
可為直鏈伸烷基,亦可為分支伸烷基。
前述聚醯亞胺,可藉由使二胺成分與四羧酸成分於溶劑中進行反應來製造。適宜的反應方法宜為將四羧酸成分一次、或分批添加入已將二胺成分溶解於溶劑之溶液,加熱並進行聚合(醯亞胺化反應)之方法。反應溫度通常宜為120℃~220℃,又以150℃~200℃更佳,160℃~190℃尤佳。反應溫度若低於120℃則醯亞胺化反應會變慢,因此不理想,若高於220℃則會高於溶劑的沸點,因此不理想。反應時間通常宜為0.5小時~72小時之範圍,又以1小時~60小時更佳,1.5小時~48小時尤佳。反應時間若低於0.5小時則會有醯亞胺化反應未完結之情況,另一方面,花費72小時以上的時間的話在考量生產性方面並不理想。
四羧酸成分與二胺成分之莫耳比[四羧酸成分/二胺成分]約為等莫耳,具體而言宜設為0.95~1.05,又宜為0.97~1.03。若在此莫耳比之範圍外,會有得到的聚醯亞胺之靭性降低之虞。
將藉由前述反應而得之含有聚醯亞胺之溶液,藉由與例如水、醇、己烷等不良溶劑混合,可將聚醯亞胺以粉末的形式析出。藉由將該粉末以過濾等手段與溶劑分離並乾燥,可得到聚醯亞胺。
前述聚醯亞胺之製備中使用的溶劑,可使用公知的有機溶劑。可舉例如N,N-二甲基甲醯胺、N,N-二甲基乙醯胺、N,N-二乙基乙醯胺、N-甲基-2-吡咯啶酮、N-乙基-2-吡咯啶酮、1,3-二甲基-2-咪唑啶酮、N-甲基己內醯胺、六甲基磷醯胺、1,2-二甲氧乙烷、雙(2-甲氧乙基)醚、1,2-雙(2-甲氧乙氧基)乙烷、四氫呋喃、雙[2-(2-甲氧乙氧基)乙基]醚、1,4-二烷、二甲基亞碸、二甲基碸、二苯醚、環丁碸、二苯碸、四甲基脲、苯甲醚、間甲酚、酚、γ-丁內酯。這些溶劑,可單獨使用,或將2種以上混合使用亦無妨。
又,作為使用於本發明之電極用黏合劑樹脂之聚醯亞胺系樹脂,亦可舉例在醯亞胺寡聚物之至少一邊的末端具有加成反應基之加成反應性醯亞胺寡聚物,該加成反應性醯亞胺寡聚物按四羧酸成分及二胺成分計,構成之平均聚合度為50以下,宜為40以下,又以30以下更佳。藉由設平均聚合度為50以下,可容易得到熔點為300℃以下之加成反應性醯亞胺寡聚物。又,醯亞胺寡聚物的聚合度為50係表示四羧酸成分及二胺成分各自反應了25個分子之狀態。
作為構成加成反應性醯亞胺寡聚物之四羧酸成分及二胺成分,可適宜地使用與前述例示作為構成聚醯亞胺之四羧酸成分及二胺成分者相同者。又,該情況下,芳香族四羧酸成分與芳香族二胺成分的組合(全芳香族醯亞胺寡聚物)亦為適宜。
加成反應性醯亞胺寡聚物的末端之加成反應基,只要係藉由加熱進行加成聚合反應(硬化反應)之基即可,並無特別限定,考量電極用黏合劑樹脂之性能的觀點,宜為選自由苯乙炔基等含有乙炔鍵之基、納迪克酸基(nadic acid group)、及馬來醯亞胺基構成之群組之中任一反應基,以含有苯乙炔基等含有乙炔鍵之基更佳,又以苯乙炔基更佳。
這些加成反應基,係藉由於分子內同時具有加成反應基及酸酐基或胺基之化合物和醯亞胺寡聚物之末端的胺基或酸酐基進行反應,而導入到醯亞胺寡聚物之末端。該反應,宜為形成醯亞胺環之反應。於分子內同時具有加成反應基及酸酐基或胺基之化合物,可舉例如4-(2-苯乙炔基)苯二甲酸酐、苯乙炔基偏苯三甲酸酐、4-(2-苯乙炔基)苯胺、4-乙炔基-苯二甲酸酐、4-乙炔基苯胺、納迪克酸酐、馬來酸酐。
使用於本發明之電極用黏合劑樹脂之加成反應性醯亞胺寡聚物,宜為下列化學式(6)所示的加成反應性醯亞胺寡聚物。 [化7]化學式(6)中,R3
係選自由具有1個或2個芳香環之4價基構成之群組中之1種以上,R4
係選自由碳數1~20之2價烴基構成之群組中之1種以上,R5
係含有乙炔鍵之1價基,宜為具有苯乙炔基之1價基,n係1~15之整數。惟,各結構單元含有的R3
及R4
可為相同亦可為不同。
化學式(6)中,R3
宜為具有1個或2個苯環作為芳香環之4價基,更宜為前述化學式(2)~(5)之4價基。R4
宜為具有1~3個苯環之2價基、或碳數1~20之伸烷基。
前述加成反應性醯亞胺寡聚物,可藉由使作為四羧酸成分之四羧酸二酐、二胺成分、及於分子內同時具有加成反應基及酸酐基或胺基之化合物,以藉由各酸酐基之合計與各胺基之合計約為等量,具體而言,藉由所用之化合物含有的酸酐基之合計量與胺基之合計量的比值[酸酐基之合計量/胺基之合計量]成為0.95~1.05,宜成為0.97~1.03之方式使用,且適宜於溶劑中反應而可輕易製造。反應的方法,適宜為與前述聚醯亞胺之製造相同的方法,溶劑亦可使用相同者。
本發明之電極用黏合劑樹脂組成物,如前述係含有本發明之電極用黏合劑樹脂者,本發明之電極合劑糊劑係含有本發明之電極用黏合劑樹脂、電極活性物質、與溶劑者。溶劑宜為非極性溶劑。藉由將本發明之電極用黏合劑樹脂、或電極用黏合劑樹脂組成物與電極活性物質及溶劑混合,可製備電極合劑糊劑。
此處,為了得到高容量,期望電極中之電極活性物質的量為多,因此,期望以較少量之黏合劑樹脂而得到充分的黏結力。電極的製作中,相較粉末之狀態的黏合劑樹脂,使用溶解於溶劑的狀態之黏合劑樹脂,即使少量,亦可使黏合劑樹脂無集中情形且輕易得到高黏結力,因此聚醯亞胺系之黏合劑樹脂的情況,自以往係使用為聚醯亞胺前軀體之聚醯胺酸之溶液、或可溶性聚醯亞胺之溶液來製作電極合劑糊劑。但,使用聚醯胺酸之溶液、及可溶性聚醯亞胺之溶液,有如前述的問題。聚醯亞胺一般而言無熔點存在,或係至400℃以上、更甚者至500℃以上之非常高的熔點,本發明中,藉由將熔點為300℃以下,宜為250℃以下之特殊的聚醯亞胺系樹脂作為電極用黏合劑樹脂,可不使用極性溶劑,即,黏合劑樹脂即便不溶解於溶劑中而以分散的狀態使用於電極合劑層之形成,亦可得到充足的黏結力、集電體與電極合劑層之黏接性。又,可藉由相較低溫的熱處理形成電極,製作電極時不需使用極性溶劑,亦不需進行會生成水之醯亞胺化反應,因此亦可抑制對電極合劑層含有的電極活性物質、固體電解質等給予不良影響。結果依據本發明,可得到具有良好特性之電極。
電極活性物質可適宜地使用公知者,宜為含鋰複合金屬氧化物、碳粉末、矽粉末、錫粉末、或含有矽或錫之合金粉末。電極合劑糊劑中之電極活性物質的量並無特別限定,通常相對於電極用黏合劑樹脂,按質量基準計為0.1~1000倍,宜為1~1000倍,以5~1000倍更佳,又以10~1000倍更佳。若活性物質量過多則活性物質不充分地黏結於集電體而容易脫落。另一方面,若活性物質量過少,形成於集電體之活性物質層(亦稱作電極合劑層)中非活性的部分變多,作為電極之機能會不夠充分。
使用於電極合劑糊劑之溶劑,可為不會溶解本發明之電極用黏合劑樹脂者,宜為非極性溶劑。作為電極合劑糊劑之溶劑,可舉例如二甲苯、甲苯、乙苯等芳香族烴、戊烷、己烷、庚烷等脂肪族烴類等非極性溶劑。
電極合劑糊劑除了本發明之電極用黏合劑樹脂外,亦可含有聚醯亞胺系樹脂以外之其他的黏合劑樹脂。聚醯亞胺系樹脂以外之黏合劑樹脂的含量,相對於黏合劑成分的總量,宜為未達50質量%,又以未達30質量%更佳。
作為前述黏合劑樹脂,可舉例如聚偏二氟乙烯、聚四氟乙烯、苯乙烯-丁二烯橡膠、丁二烯橡膠、腈橡膠、聚丙烯腈、乙烯-乙烯醇共聚合樹脂、乙烯丙烯橡膠、聚胺酯、聚丙烯酸、聚醯胺、聚丙烯酸酯、聚乙烯醚、氟橡膠、羧甲基纖維素、羧甲基纖維素鈉。
又,電極合劑糊劑亦可含有固體電解質。作為固體電解質,可舉例如鈣鈦礦型結晶之La0.51
Li0.34
TiO2.94
、石榴石型結晶之Li7
La3
Zr2
O12
、NASICON型結晶之Li1.3
Al0.3
Ti1.7
(PO4
)3
、非晶質之LIPON(Li2.9
PO3.3
N0.46
)等氧化物系固體電解質、Li2
S-SiS2
系、Li2
S-P2
S5
系等硫化物系固體電解質。
電極合劑糊劑中,更可因應需要加入界面活性劑、黏度調整劑、導電補助劑等之添加劑。
本發明之電極為具有電極合劑層者,該電極合劑層含有如前述本發明之電極用黏合劑樹脂、及電極活性物質。電極合劑層,例如形成於由金屬箔構成之集電體的表面。本發明之電極的電極合劑層,更可含有如前述之聚醯亞胺系樹脂以外之其他的黏合劑樹脂、固體電解質。又,本發明之電極用黏合劑樹脂,為如前述至少一邊的末端具有加成反應基之加成反應性醯亞胺寡聚物等具有反應性之官能基者的情況下,亦可含有於分子內或分子間反應性官能基彼此反應而生成之反應產物。
藉由將如前述之本發明之電極合劑糊劑,流延或塗布於以鋁、銅、鎳、鐵、鈦、鈷等之金屬箔或由它們的組合構成的合金箔製得之導電性的集電體上,並加熱處理來去除溶劑,可製造電極,該合金箔由。加熱處理,宜在使電極合劑糊劑含有的聚醯亞胺系樹脂熔融並使形成電極活性物質等之電極合劑層的成分一體化的同時,可使集電體與電極合劑層黏接之條件進行。具體而言,宜於所使用的聚醯亞胺系樹脂之熔點以上、350℃以下的溫度,更宜於加壓下進行熱處理。為了抑制固體電解質等之電極、及電池含有的成分之分解而得到具有良好特性的電極、及鋰離子二次電池等之電化學元件,通常加熱處理的溫度宜為350℃以下。 [實施例]
以下藉由實施例及比較例更具體地說明本發明,但本發明並不限定於這些實施例。
以下呈現以下的例子中使用的特性之測定方法。 <熔點測定方法(DSC法)> 使用示差掃描量熱計DSC-50(島津製作所),以20℃/min由室温(25℃)進行升溫至500℃,並測定熔點。 <附著性測試(百格測試法)> 附著性測試依JIS K 5600-5-6為準進行。又,藉由目視評估,依評估基準(3)為準以分類0~分類5(數字愈小愈強固地附著)呈現。
針對以下例子中使用之化合物的縮寫進行説明。 ODPA:4,4’-氧基二苯二甲酸二酐、 s-BPDA:3,3’,4,4’-聯苯四羧酸二酐、 a-BPDA:2,3’,3,4’-聯苯四羧酸二酐、 PMDA:苯均四酸二酐、 PEPA:4-苯乙炔基苯二甲酐、 PETA:苯乙炔基偏苯三甲酸酐、 PPD:對苯二胺、 MPD:間苯二胺、 ODA:4,4’-二胺基二苯醚、 TPE-R:1,3-雙(4-胺基苯氧基)苯、 DMD:癸二胺、 HMD:己二胺、 NMP:N-甲基-2-吡咯啶酮、 PVdF:聚偏二氟乙烯、 SBR:苯乙烯-丁二烯橡膠。
[實施例1] 使用s-BPDA作為酸酐、DMD作為二胺(s-BPDA:DMD=1:1(莫耳比)),於NMP中,於180℃聚合12小時,得到醯亞胺化反應完結之聚醯亞胺溶液。將該溶液分散於水中,分濾析出的聚醯亞胺。將水洗及分濾重複3次,並將回收而得的聚醯亞胺於150℃乾燥24小時,得到電極用黏合劑樹脂。該樹脂之熔點為190℃。 於3g之得到的電極用黏合劑樹脂中添加7g之矽粉末及90g之己烷並混練,製備成電極合劑糊劑。將該糊劑塗佈於銅箔,於常壓、氮氣環境下之熱風乾燥機於120℃加熱處理60分鐘後,於250℃進行熱壓並製作出電極。針對該電極進行附著性測試的結果,附著性為分類0。
[實施例2] 於實施例1中得到的3g之電極用黏合劑樹脂中添加1g之羧甲基纖維素、7g之矽粉末及90g之水並混練,製備電極合劑糊劑。除了使用該糊劑以外與實施例1同樣進行而製作電極。針對該電極進行附著性測試的結果,附著性為分類0。
[實施例3] 除了將酸酐變更為ODPA以外與實施例1同樣進行而得到電極用黏合劑樹脂。該樹脂之熔點為150℃。除了使用該電極用黏合劑樹脂以外與實施例1同樣進行而製作電極。針對該電極進行附著性測試的結果,附著性為分類0。
[實施例4] 使用a-BPDA及PEPA作為酸酐、TPE-R及MPD作為二胺(a-BPDA:PEPA:TPE-R:MPD=1:2:1:1(莫耳比)),除此之外與實施例1同樣進行而得到電極用黏合劑樹脂。該樹脂之熔點為175℃。除了使用該電極用黏合劑樹脂以外與實施例1同樣進行而製作電極。針對該電極進行附著性測試的結果,附著性為分類0。
[實施例5] 使用ODPA及PETA作為酸酐、HMD作為二胺(ODPA:PETA:HMD=1:2:2(莫耳比)),除此之外與實施例1同樣進行而得到電極用黏合劑樹脂。該樹脂之熔點為170℃。除了使用該電極用黏合劑樹脂以外與實施例1同樣進行而製作電極。針對該電極進行附著性測試的結果,附著性為分類0。
[實施例6] 使用ODPA、s-BPDA及PETA作為酸酐、ODA、PPD作為二胺(ODPA:s-BPDA:PETA:ODA:PPD=5:5:20:14:6(莫耳比)),除此之外與實施例1同樣進行而得到電極用黏合劑樹脂。該樹脂之熔點為250℃。除了使用該電極用黏合劑樹脂以外與實施例1同樣進行而製作電極。針對該電極進行附著性測試的結果,附著性為分類0。
[比較例1] 使用s-BPDA作為酸酐、PPD作為二胺,於NMP中,於180℃聚合12小時,得到醯亞胺化完結之聚醯亞胺NMP分散溶液。分濾析出的聚醯亞胺後,重複實施3次水洗及分濾,將回收的聚醯亞胺於150℃乾燥24小時而得到聚醯亞胺粉末。測定了該樹脂之熔點,但未觀測到熔點。 於得到的3g之聚醯亞胺粉末中添加7g之矽粉末及90g之己烷並混練,製備電極合劑糊劑。將該糊劑塗佈於銅箔,於常壓、氮氣環境下之熱風乾燥機於120℃加熱處理60分鐘後,於350℃進行熱壓,但電極合劑層與銅箔未黏接,因而無法製作電極。
[比較例2] 使用PMDA作為酸酐、ODA作為二胺,於NMP中,於180℃聚合12小時,得到醯亞胺化完結之聚醯亞胺NMP分散溶液。分濾析出的聚醯亞胺後,重複實施3次水洗及分濾,將回收的聚醯亞胺於150℃乾燥24小時而得到聚醯亞胺粉末。測定了該樹脂之熔點,但未觀測到熔點。 於得到的3g之聚醯亞胺粉末中添加7g之矽粉末及90g之己烷並混練,製備電極合劑糊劑。將該糊劑塗佈於銅箔,於常壓、氮氣環境下之熱風乾燥機於120℃加熱處理60分鐘後,於350℃進行熱壓,但電極合劑層與銅箔未黏接,因而無法製作電極。
[比較例3] 於3g之PVdF中添加7g之矽粉末及90g之己烷並混練,製備電極合劑糊劑。將該糊劑塗佈於銅箔,於常壓、氮氣環境下之熱風乾燥機於120℃加熱處理60分鐘後,於250℃進行熱壓並製作電極。針對該電極進行附著性測試的結果,附著性為分類5,黏接性非常差。
[比較例4] 於3g之SBR中添加7g之矽粉末及90g之己烷並混練,製備電極合劑糊劑。將塗佈了該糊劑之銅箔,於常壓、氮氣環境下之熱風乾燥機於120℃加熱處理60分鐘後,於250℃進行熱壓並製作電極。針對該電極進行附著性測試的結果,附著性為分類4,黏接性差。
Claims (15)
- 一種電極用黏合劑樹脂,係由熔點為300℃以下之聚醯亞胺系樹脂構成。
- 如申請專利範圍第1項之電極用黏合劑樹脂,其中,該聚醯亞胺系樹脂含有聚醯亞胺,該聚醯亞胺係由四羧酸成分與二胺成分獲得且四羧酸成分或二胺成分之至少一方含有50莫耳%以上之脂肪族化合物。
- 如申請專利範圍第2項之電極用黏合劑樹脂,其中,該聚醯亞胺係由下列化學式(1)表示之結構單元1種以上構成,式中,R1 係具有1個或2個芳香環之4價基,R2 係碳數1~20之2價伸烷基。
- 如申請專利範圍第3項之電極用黏合劑樹脂,其中,該化學式(1)中的R1 係選自由下列化學式(2)~(5)之4價基構成的群組中之1種以上;。
- 如申請專利範圍第1項之電極用黏合劑樹脂,其中,該聚醯亞胺系樹脂含有加成反應性醯亞胺寡聚物,該加成反應性醯亞胺寡聚物於平均聚合度為50以下之醯亞胺寡聚物之至少一邊的末端具有加成反應基。
- 如申請專利範圍第5項之電極用黏合劑樹脂,其中,該加成反應基為苯乙炔基、或含有乙炔鍵之基。
- 如申請專利範圍第6項之電極用黏合劑樹脂,其中,該加成反應性醯亞胺寡聚物係下列化學式(6)表示之加成反應性醯亞胺寡聚物,式中,R3 係選自由具有1個或2個芳香環之4價基構成之群組中之1種以上,R4 係選自由碳數1~20之2價烴基構成之群組中之1種以上,R5 係含有乙炔鍵之1價基,n係1~15之整數;在此,各結構單元含有的R3 及R4 可為相同亦可為不同。
- 一種電極用黏合劑樹脂組成物,包含如申請專利範圍1至7項中任一項之電極用黏合劑樹脂。
- 一種電極合劑糊劑,包含如申請專利範圍1至7項中任一項之電極用黏合劑樹脂、電極活性物質、及溶劑。
- 如申請專利範圍第9項之電極合劑糊劑,其中,該溶劑為非極性溶劑。
- 如申請專利範圍第9或10項之電極合劑糊劑,更包含固體電解質。
- 一種電極之製造方法,其特徵為包括下列步驟: 將如申請專利範圍9至11項中任一項之電極合劑糊劑塗佈於由金屬箔構成之集電體的表面;及, 將已塗佈之電極合劑糊劑以該電極合劑糊劑含有之聚醯亞胺系樹脂之熔點以上、350℃以下的溫度進行熱處理。
- 一種電極,具有電極合劑層,該電極合劑層含有如申請專利範圍1至7項中任一項之電極用黏合劑樹脂、及電極活性物質。
- 如申請專利範圍第13項之電極,其中,該電極合劑層形成於由金屬箔構成之集電體的表面。
- 如申請專利範圍第13或14項之電極,其中,該電極合劑層更含有固體電解質。
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KR (2) | KR102010209B1 (zh) |
CN (1) | CN109643803B (zh) |
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2018
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- 2018-08-06 JP JP2018558360A patent/JP6516076B1/ja active Active
- 2018-08-06 US US16/640,196 patent/US20200172731A1/en active Pending
- 2018-08-06 WO PCT/JP2018/029406 patent/WO2019039254A1/ja unknown
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US20200172731A1 (en) | 2020-06-04 |
JP2019117796A (ja) | 2019-07-18 |
JPWO2019039254A1 (ja) | 2019-11-07 |
KR102627227B1 (ko) | 2024-01-22 |
KR102010209B1 (ko) | 2019-08-12 |
JP7489224B2 (ja) | 2024-05-23 |
CN109643803B (zh) | 2020-04-17 |
JP6516076B1 (ja) | 2019-05-22 |
JP7042765B2 (ja) | 2022-03-28 |
EP3514869B1 (en) | 2023-10-04 |
KR20190022504A (ko) | 2019-03-06 |
JP2023113663A (ja) | 2023-08-16 |
CN109643803A (zh) | 2019-04-16 |
EP3514869A4 (en) | 2020-03-18 |
WO2019039254A1 (ja) | 2019-02-28 |
KR20200034943A (ko) | 2020-04-01 |
EP3514869A1 (en) | 2019-07-24 |
JP2020115474A (ja) | 2020-07-30 |
TWI791038B (zh) | 2023-02-01 |
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