JP7337432B2 - 電解質組成物、電解質シート及び二次電池 - Google Patents
電解質組成物、電解質シート及び二次電池 Download PDFInfo
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- JP7337432B2 JP7337432B2 JP2020507835A JP2020507835A JP7337432B2 JP 7337432 B2 JP7337432 B2 JP 7337432B2 JP 2020507835 A JP2020507835 A JP 2020507835A JP 2020507835 A JP2020507835 A JP 2020507835A JP 7337432 B2 JP7337432 B2 JP 7337432B2
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- KTQDYGVEEFGIIL-UHFFFAOYSA-N n-fluorosulfonylsulfamoyl fluoride Chemical compound FS(=O)(=O)NS(F)(=O)=O KTQDYGVEEFGIIL-UHFFFAOYSA-N 0.000 description 1
- 229920003052 natural elastomer Polymers 0.000 description 1
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- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
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- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- JUJWROOIHBZHMG-UHFFFAOYSA-O pyridinium Chemical compound C1=CC=[NH+]C=C1 JUJWROOIHBZHMG-UHFFFAOYSA-O 0.000 description 1
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- 229910052708 sodium Inorganic materials 0.000 description 1
- BAZAXWOYCMUHIX-UHFFFAOYSA-M sodium perchlorate Chemical compound [Na+].[O-]Cl(=O)(=O)=O BAZAXWOYCMUHIX-UHFFFAOYSA-M 0.000 description 1
- 229910001488 sodium perchlorate Inorganic materials 0.000 description 1
- 229910001495 sodium tetrafluoroborate Inorganic materials 0.000 description 1
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- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0565—Polymeric materials, e.g. gel-type or solid-type
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Description
N(SO2CmF2m+1)(SO2CnF2n+1)- (1)
[m及びnは、それぞれ独立に0~5の整数を表す。]
図1は、第1実施形態に係る二次電池を示す斜視図である。図1に示すように、二次電池1は、正極、負極及び電解質層から構成される電極群2と、電極群2を収容する袋状の電池外装体3とを備えている。正極及び負極には、それぞれ正極集電タブ4及び負極集電タブ5が設けられている。正極集電タブ4及び負極集電タブ5は、それぞれ正極及び負極が二次電池1の外部と電気的に接続可能なように、電池外装体3の内部から外部へ突き出している。
[FSI]-:N(SO2F)2 -、ビス(フルオロスルホニル)イミドアニオン
[TFSI]-:N(SO2CF3)2 -、ビス(トリフルオロメタンスルホニル)イミドアニオン
[BOB]-:B(O2C2O2)2 -、ビスオキサレートボラートアニオン
[f3C]-:C(SO2F)3 -、トリス(フルオロスルホニル)カルボアニオン
N(SO2CmF2m+1)(SO2CnF2n+1)- (1)
[式(1)中、m及びnは、それぞれ独立に0~5の整数を表す。m及びnは、互いに同一でも異なっていてもよく、好ましくは互いに同一である。]
次に、第2実施形態に係る二次電池について説明する。図5は、第2実施形態に係る二次電池における電極群の一実施形態を示す模式断面図である。図5に示すように、第2実施形態における二次電池が第1実施形態における二次電池と異なる点は、電極群2Bが、バイポーラ電極16を備えている点である。すなわち、電極群2Bは、正極6と、第1の電解質層7と、バイポーラ電極16と、第2の電解質層7と、負極8とをこの順に備えている。
<実施例1>
マトリクスポリマであるフッ化ビニリデンとヘキサフルオロピレンとのコポリマ(PVDF-HFP)を30質量部と、酸化物粒子であるSiO2粒子(製品名:AEROSIL OX50、日本アエロジル株式会社製)を20質量部と、電解質塩であるリチウムビス(フルオロスルホニル)イミド(Li[FSI])を1.5mol/Lの濃度で溶解させたN-メチル-N-プロピルピロリジニウムビス(フルオロスルホニル)イミド(Py13-FSI)(以下、電解質塩を溶解させたイオン液体の組成を表す際に、「リチウム塩の濃度/リチウム塩の種類/イオン液体の種類」のように表記することがある。)を50質量部と、セルロース繊維(平均長さ50μm、平均繊維径0.1μm)を0.4質量部とを、分散媒である1-メチル-2-ピロリドン(NMP)に分散させ、電解質組成物を含むスラリを調製した。このスラリをポリエチレンテレフタレート製の基材(製品名:テオネックスR-Q51、帝人デュポンフィルム株式会社製、厚さ38μm)上にアプリケータを用いて塗布した。塗布したスラリを80℃で1時間加熱乾燥することにより、分散媒を揮発させて、電解質シートを得た。得られた電解質シートにおける電解質層の厚さは、25±5μmであった。
実施例1の電解質シートにおいて、セルロース繊維の含有量を1.0質量部に変更した以外は、実施例1と同様の方法により電解質シートを作製した。
正極と負極を想定した銅箔を2枚用意した。上述した実施例1~2の電解質シートから基材を剥離し、電解質層を2枚の銅箔の間に挟持させた3層サンプルをそれぞれ作製した。3層サンプルでは、電解質層が2枚の銅箔を絶縁するように(銅箔同士が接触しないように)各層を配置した。
作製した3層サンプルについて、釘刺し模擬試験装置を用いた釘刺し模擬試験を実施した。釘刺し模擬試験装置としては、半田こて(FX-600、白光株式会社製)を、上下に昇降可能な可動部を有するスタンドによりこて先を床面に対し略垂直に下に向けて固定したものを用いた。試験に先立ち、3層サンプルに0.1Vの電圧を印加して、約10秒経過後に、電流がほぼ底値になることを確認した。その後、図6に示すように、2枚の銅箔18,18間に電解質層7が挟持された3層サンプル19を、こて20の先の下に設置し、3層サンプル19に対して、200℃に加熱したこて20の先を3層サンプル19の積層方向に差込み、約3秒間保持した。このとき、銅箔の貫通孔が3mmになるように、こて20の先の差し込み深さDを、0.5mmとした。そして、こて20の先を差し込んだ状態で、2枚の銅箔18,18間の電流を記録した。その後、こて20の先を3層サンプル19の上方に引き抜いた。こて20の先を差し込んだ3秒間の電流の最大値から、以下の式(7)により3層サンプル19の絶縁抵抗を計算した。なお、絶縁抵抗が1kΩ以上であれば、短絡が十分に抑制されているといえる。
絶縁抵抗(Ω)=電圧(V)÷3秒間の最大電流(A) (7)
(正極の作製)
層状型リチウム・ニッケル・マンガン・コバルト複合酸化物(正極活物質)78.5質量部と、アセチレンブラック(導電剤、製品名:HS-100、デンカ株式会社製)5質量部と、フッ化ビニリデンとヘキサフルオロプロピレンとのコポリマ溶液(固形分12質量%)2.5質量部と、イオン液体(1.5mol/L/Li[FSI]/Py13-FSI)を14質量部と、を混合して正極合剤スラリを調製した。この正極合剤スラリを正極集電体(厚さ15μmのアルミニウム箔)上の両面に塗工量125g/m2で塗工し、加熱乾燥させた。この電極をプレスすることにより、合剤密度2.7g/cm3に調整した。これを合剤層のサイズが82mm×112mmとなるように打抜き、正極とした。
黒鉛(負極活物質、日立化成株式会社製)80.4質量部と、炭素繊維(導電剤、製品名:VGCF-H、昭和電工株式会社製)0.6質量部と、フッ化ビニリデンとヘキサフルオロプロピレンのコポリマ溶液(固形分12質量%)5質量部と、イオン液体(1.5mol/L/Li[FSI]/Py13-FSI)を14質量部と、を混合して負極合剤スラリを調製した。この負極合剤スラリを集電体(厚さ10μmの銅箔)上の両面に塗工量60g/m2で塗工し、加熱乾燥させた。この電極をプレスすることにより、合剤密度1.8g/cm3に調整した。これを合剤層のサイズが86mm×116mmとなるように打抜き、負極とした。
正極、負極、実施例1で作製した電解質シートから得られる電解質層を用いて評価用電池を作製した。負極、電解質層、正極をこの順に重ね、負極9枚、電解質層16枚、正極8枚を多積層した電極群を作製した。電極群の正極にAlタブを、負極にNiタブを超音波溶接し、この電極群をアルミラミネートで封止し、評価用電池とした。
実施例2の電解質シートから得られる電解質層を用いた以外は、実施例3と同様の方法により評価用電池を作製した。
作製した評価用電池について、釘刺し試験を実施した。釘刺し試験を実施する前に、評価用電池は、充放電装置(東洋システム株式会社製)を用いて以下の充放電条件の下で充電した。
(1)0.1Cの定電流で終止電圧4.2Vまで充電した後、終止電圧4.2Vで充電総時間が15時間又は充電電流0.02Cとなるまで定電圧充電する定電流定電圧(CCCV)充電を行った後、0.1Cで終止電圧2.7Vまで定電流(CC)放電するサイクルを3サイクル行い、初期化した。なお、Cとは「電流値(A)/電池容量(Ah)」を意味する。
(2)次いで、0.1Cの定電流で終止電圧4.2Vまで充電した後、終止電圧4.2Vで充電総時間が15時間又は充電電流0.02Cとなるまで定電圧充電するCCCV充電を行った。
電圧の低下率(%)=(試験後(5秒後)の電圧-試験後(600秒後)の電圧)/試験後(5秒後)の電圧×100
Claims (10)
- マトリクスポリマと、
リチウム塩、ナトリウム塩、カルシウム塩及びマグネシウム塩からなる群より選ばれる少なくとも1種の電解質塩と、
酸化物粒子と、
繊維と、
イオン液体と、
を含有し、
前記繊維は、セルロース繊維及びポリアクリロニトリル系樹脂繊維のうちのいずれか一つであり、
前記繊維の平均長さは、前記酸化物粒子の平均粒径以上である、電解質組成物。 - 前記マトリクスポリマは、四フッ化エチレン及びフッ化ビニリデンからなる群より選ばれる第1の構造単位を有する、請求項1に記載の電解質組成物。
- 前記マトリクスポリマを構成する構造単位の中に、前記第1の構造単位と、ヘキサフルオロプロピレン、アクリル酸、マレイン酸、エチルメタクリレート、及びメチルメタクリレートからなる群より選ばれる第2の構造単位とが含まれる、請求項2に記載の電解質組成物。
- 前記電解質塩は、イミド系リチウム塩を含む、請求項1~3のいずれか一項に記載の電解質組成物。
- 前記イオン液体は、アニオン成分として、下記式(1)で表されるアニオン成分の少なくとも1種を含有する、請求項1~4のいずれか一項に記載の電解質組成物。
N(SO2CmF2m+1)(SO2CnF2n+1)- (1)
[m及びnは、それぞれ独立に0~5の整数を表す。] - 前記イオン液体は、カチオン成分として、鎖状四級オニウムカチオン、ピペリジニウムカチオン、ピロリジニウムカチオン、ピリジニウムカチオン、及びイミダゾリウムカチオンからなる群より選ばれる少なくとも1種を含有する、請求項1~5のいずれか一項に記載の電解質組成物。
- 基材と、
前記基材上に設けられ、請求項1~6のいずれか一項に記載の電解質組成物で形成された電解質層と、を備える電解質シート。 - 前記繊維の平均繊維径は前記電解質層の厚さ以下である、請求項7に記載の電解質シート。
- 正極と、
負極と、
前記正極及び前記負極の間に設けられ、請求項1~6のいずれか一項に記載の電解質組成物で形成された電解質層と、を備える、二次電池。 - 前記繊維の平均繊維径は前記電解質層の厚さ以下である、請求項9に記載の二次電池。
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JP2004111229A (ja) | 2002-09-19 | 2004-04-08 | National Institute Of Advanced Industrial & Technology | ポリマー電解質支持体およびリチウム二次電池 |
WO2011037060A1 (ja) | 2009-09-24 | 2011-03-31 | コニカミノルタホールディングス株式会社 | 電解質組成物、及びリチウムイオン二次電池 |
JP2011192568A (ja) | 2010-03-16 | 2011-09-29 | Konica Minolta Holdings Inc | 電解質組成物、および二次電池 |
US20170222244A1 (en) | 2016-02-03 | 2017-08-03 | Samsung Electronics Co., Ltd. | Solid electrolyte and lithium battery comprising the solid electrolyte |
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