JP7182198B2 - 非水電解質二次電池、電解液及び非水電解質二次電池の製造方法 - Google Patents
非水電解質二次電池、電解液及び非水電解質二次電池の製造方法 Download PDFInfo
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- JP7182198B2 JP7182198B2 JP2019568956A JP2019568956A JP7182198B2 JP 7182198 B2 JP7182198 B2 JP 7182198B2 JP 2019568956 A JP2019568956 A JP 2019568956A JP 2019568956 A JP2019568956 A JP 2019568956A JP 7182198 B2 JP7182198 B2 JP 7182198B2
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- secondary battery
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- carboxylic acid
- negative electrode
- positive electrode
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Images
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Description
負極は、例えば、負極集電体と、負極集電体の表面に形成され、かつ負極活物質を含む負極合剤層とを具備する。負極合剤層は、負極合剤を分散媒に分散させた負極スラリーを、負極集電体の表面に塗布し、乾燥させることにより形成できる。乾燥後の塗膜を、必要により圧延してもよい。負極合剤層は、負極集電体の一方の表面に形成してもよく、両方の表面に形成してもよい。
正極は、例えば、正極集電体と、正極集電体の表面に形成された正極合剤層とを具備する。正極合剤層は、正極合剤を分散媒に分散させた正極スラリーを、正極集電体の表面に塗布し、乾燥させることにより形成できる。乾燥後の塗膜を、必要により圧延してもよい。正極合剤層は、正極集電体の一方の表面に形成してもよく、両方の表面に形成してもよい。
電解液は、リチウム塩およびカルボン酸の他に、溶媒を含む。電解液は、リチウム塩、カルボン酸、アルコールおよび溶媒とは異なる材料を添加剤として含み得るが、リチウム塩とカルボン酸とアルコールと溶媒との合計量は電解液の90質量%以上、更には95質量%以上を占めることが好ましい。
正極と負極との間には、セパレータを介在させることが望ましい。セパレータは、イオン透過度が高く、適度な機械的強度および絶縁性を備えている。セパレータとしては、微多孔薄膜、織布、不織布などを用いることができる。セパレータの材質としては、ポリプロピレン、ポリエチレンなどのポリオレフィンが好ましい。
[負極の作製]
黒鉛を負極活物質として用いた。負極活物質と、カルボキシメチルセルロースナトリウム(CMC-Na)と、スチレン-ブタジエンゴム(SBR)とを、97.5:1:1.5の質量比で混合し、水を添加した後、混合機(プライミクス社製、T.K.ハイビスミックス)を用いて攪拌し、負極スラリーを調製した。次に、銅箔の表面に1m2当りの負極合剤の質量が190gとなるように負極スラリーを塗布し、塗膜を乾燥させた後、圧延して、銅箔の両面に、密度1.5g/cm3の負極合剤層が形成された負極を作製した。
リチウムニッケル複合酸化物(LiNi0.8Co0.18Al0.02O2)と、アセチレンブラックと、ポリフッ化ビニリデンとを、95:2.5:2.5の質量比で混合し、N-メチル-2-ピロリドン(NMP)を添加した後、混合機(プライミクス社製、T.K.ハイビスミックス)を用いて攪拌し、正極スラリーを調製した。次に、アルミニウム箔の表面に正極スラリーを塗布し、塗膜を乾燥させた後、圧延して、アルミニウム箔の両面に、密度3.6g/cm3の正極合剤層が形成された正極を作製した。
溶媒には、エチレンカーボネート(EC)、ジメチルカーボネート(DMC)および酢酸メチル(MA)を20:70:10の体積比で含む混合溶媒を用いた。リチウム塩には、表1に示す割合で、LFSIとLiPF6とを併用した。得られた電解液に対し、表1に示す割合で、カルボン酸とメタノールとを含ませた。酢酸メチル(MA)は、純度99.9999%のものを使用した。
各電極にタブをそれぞれ取り付け、タブが最外周部に位置するように、セパレータを介して正極および負極を渦巻き状に巻回することにより電極群を作製した。電極群をアルミニウムラミネートフィルム製の外装体内に挿入し、105℃で2時間真空乾燥した後、非水電解液を注入し、外装体の開口部を封止して、電池A1~A7を得た。
溶媒に、エチレンカーボネート(EC)およびジメチルカーボネート(DMC)を20:80の体積比で含む混合溶媒を用い、表1に示す割合で、カルボン酸とメタノールを用いたこと以外、実施例1と同様に、実施例8の電池A8を作製した。
メタノールを用いなかったこと以外、実施例1と同様に、実施例9の電池A9を作製した。
溶媒に、エチレンカーボネート(EC)およびジメチルカーボネート(DMC)を20:80の体積比で含む混合溶媒を用いた。リチウム塩には、表1に示すように、比較例1、3ではLiPF6を単独で使用し、比較例2ではLFSIとLiPF6とを併用した。比較例1、2では、電解液にカルボン酸もメタノールも添加せず、比較例3では電解液にカルボン酸とメタノールを添加した。上記以外については、実施例と同様に、比較例1~3の電池B1~B3を作製した。
酢酸もメタノールも用いなかったこと以外、実施例1と同様に、比較例4の電池B4を作製した。
作製後の各電池について、25℃の環境下で、0.3It(800mA)の電流で電圧が4.2Vになるまで定電流充電を行い、その後、4.2Vの定電圧で電流が0.015It(40mA)になるまで定電圧充電した。その後、0.3It(800mA)の電流で電圧が2.75Vになるまで定電流放電を行った。
カラム:アジレントテクノロジー社製、HP-1(膜厚1.0μm×長さ60m)
カラム温度:50℃→110℃(5℃/min,12min hold)→250℃(5℃/min,7min hold)→300℃(10℃/min,20min hold)
スプリット比:1/50
線速度:29.2cm/s
注入口温度:270℃
注入量:0.5μL
インターフェース温度:230℃
質量範囲:m/z=30~400(SCANモード)、m/z=29,31,32,43,45,60(SIMモード)
分析により得られたカルボン酸の含有量およびアルコールの含有量(電解液全体に対する質量比)を、表2に示す。
評価1と同じ充放電条件で充放電を繰り返した。1サイクル目の放電容量に対する400サイクル目の放電容量の割合を、容量維持率として求めた。
2 正極リード
3 負極リード
4 電池ケース
5 封口板
6 負極端子
7 ガスケット
Claims (7)
- 正極、負極、前記正極と前記負極との間に介在するセパレータおよび電解液を有し、
前記電解液が、リチウム塩およびカルボン酸を含み、
前記リチウム塩が、リチウムビス(フルオロスルホニル)イミド:LiN(SO2F)2を含み、
前記電解液における前記カルボン酸の含有量が、前記電解液の質量に対して5ppm以上500ppm以下である、非水電解質二次電池。 - 前記電解液における前記リチウム塩の濃度が、1mol/リットル以上2mol/リットル以下である、請求項1に記載の非水電解質二次電池。
- 前記リチウム塩が、更にLiPF6を含み、
前記リチウム塩に占めるLiN(SO2F)2の割合が、7mol%以上60mol%以下である、請求項1または2に記載の非水電解質二次電池。 - 前記正極が、リチウムとニッケルとを含む複合酸化物を含み、
前記複合酸化物が、一般式:LiaNibM1-bO2で表される岩塩型結晶構造の層状化合物であり、
Mは、LiおよびNi以外の金属および/または半金属であり、
0.95≦a≦1.2、かつ0.6≦b≦1を満たす、請求項1~3のいずれか1項に記載の非水電解質二次電池。 - Mは、Na、Mg、Sc、Y、Mn、Fe、Co、Cu、Zn、Al、Cr、Pb、SbおよびBよりなる群から選択された少なくとも1種である、請求項4に記載の非水電解質二次電池。
- 前記カルボン酸が、酢酸を含む、請求項1~5のいずれか1項に記載の非水電解質二次電池。
- 25℃の環境下で、0.3Itの電流で電池電圧が4.2Vになるまで定電流充電を行い、その後、4.2Vの定電圧で電流が0.015Itになるまで定電圧充電を行い、その後、0.3Itの電流で電池電圧が2.75Vになるまで定電流放電を行い、充電と放電との間の休止期間を10分間とする充放電サイクル試験を行うとき、前記試験前の前記電解液における前記カルボン酸の含有量m1と、前記試験における5サイクル後の前記電解液における前記カルボン酸の含有量m2との比:m1/m2が、1以上である、請求項1~6のいずれか1項に記載の非水電解質二次電池。
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WO2017204213A1 (ja) | 2016-05-26 | 2017-11-30 | 日本電気株式会社 | リチウムイオン二次電池 |
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US20210050625A1 (en) | 2021-02-18 |
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