JP7458033B2 - 非水電解質二次電池およびこれに用いる電解液 - Google Patents
非水電解質二次電池およびこれに用いる電解液 Download PDFInfo
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- JP7458033B2 JP7458033B2 JP2020569411A JP2020569411A JP7458033B2 JP 7458033 B2 JP7458033 B2 JP 7458033B2 JP 2020569411 A JP2020569411 A JP 2020569411A JP 2020569411 A JP2020569411 A JP 2020569411A JP 7458033 B2 JP7458033 B2 JP 7458033B2
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- lithium
- electrolyte
- negative electrode
- secondary battery
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- CHHOPPGAFVFXFS-UHFFFAOYSA-M [Li+].[O-]S(F)(=O)=O Chemical compound [Li+].[O-]S(F)(=O)=O CHHOPPGAFVFXFS-UHFFFAOYSA-M 0.000 claims description 15
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- -1 lithium hexafluorophosphate Chemical compound 0.000 claims description 14
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Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
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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、通常、リチウム塩、溶媒および添加剤を含む。電解液には、様々な添加剤が含まれ得る。1,4-ジオキサンは溶媒もしくは添加剤に分類される。電解液において、リチウム塩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。
[LSXの調製]
二酸化ケイ素と炭酸リチウムとを原子比:Si/Liが1.05となるように混合し、混合物を950℃空気中で10時間焼成することにより、式:Li2Si2O5(u=0.5)で表わされるリチウムシリケートを得た。得られたリチウムシリケートは平均粒径10μmになるように粉砕した。
導電層を有するLSX粒子と黒鉛とを3:97の質量比で混合し、負極活物質として用いた。負極活物質と、ポリアクリル酸リチウムと、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。混合溶媒には、表1に示す割合でLFSIとLiPF6とを溶解させた。また、電解液に表1に示す含有量の1,4-ジオキサンを含ませるとともに、ジフルオロリン酸リチウムおよびフルオロスルホン酸リチウムをそれぞれ1質量%ずつ含ませた。
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、実施例1~3の電池A1~A3と、比較例1~3の電池B1~B3を得た。
作製後の各電池について、25℃の環境下で、0.3It(1620mA)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0.05Itになるまで定電圧充電した。20分の休止の後、0.5It(2700mA)の電流で電圧が2.5Vになるまで定電流放電を行った。この充放電を2回繰り返した。
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=50~95(SCANモード)
ジフルオロリン酸リチウムおよびフルオロスルホン酸リチウムの量を表1に示すように変化させたこと以外、実施例1と同様に電解液を調製し、実施例4~6の電池A4~A6を作製し、上記と同様に評価した。400サイクル後の電池から取り出した電解液の成分をガスクロマトグラフィー質量分析法(GCMS)において、実施例4,5ではフルオロスルホン酸リチウムが検出されず、実施例6ではジフルオロリン酸リチウムが検出されなかったが、その他は実施例1と概ね同じ結果であった。表2に、電池A1の容量維持率を100としたときの電池A4~A6の容量維持率の相対値を示す。
電解液の調製において、LFSIを用いず、その代わりに、リチウムビス(トリフルオロメチルスルホニル)イミド(LTFSI)を用いたこと以外、実施例1と同様に比較例4の電池B4を作製し、上記と同じ充放電条件で充放電回数を100サイクル繰り返した。1サイクル目の放電容量に対する100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。表3に、電池A1の100サイクル目の容量維持率を100としたときの電池B4の容量維持率の相対値を示す。
負極の作製において、LSXを用いず、黒鉛と、カルボキシメチルセルロースと、スチレン-ブタジエンゴム(SBR)とを、97.5:1:1.5の質量比で混合して負極スラリーを調製したこと以外、実施例1と同様に実施例7の電池A7を作製し、比較例4と同様に100サイクル目の容量維持率を評価した。表3に、電池A1の100サイクル目の容量維持率を100としたときの電池A7の容量維持率の相対値を示す。
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、負極および電解液を有し、
前記電解液が、リチウムビス(フルオロスルホニル)イミドおよび1,4-ジオキサンを含み、
前記電解液中の1,4-ジオキサンの含有量が、電解液の質量に対して0.01質量%以上5質量%以下である、非水電解質二次電池。 - 前記電解液が、更にヘキサフルオロリン酸リチウムを含み、
前記リチウムビス(フルオロスルホニル)イミドと前記ヘキサフルオロリン酸リチウムとの合計に対する前記リチウムビス(フルオロスルホニル)イミドの割合が、5質量%以上50質量%以下である、請求項1に記載の非水電解質二次電池。 - 前記電解液が、更にジフルオロリン酸リチウムを含み、
前記電解液の質量に対して前記ジフルオロリン酸リチウムの含有量が、2質量%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。 - 前記電解液における前記リチウムビス(フルオロスルホニル)イミドと前記ヘキサフルオロリン酸リチウムとの合計の濃度が、1mol/リットル以上2mol/リットル以下である、請求項1~3のいずれか1項に記載の非水電解質二次電池。
- 前記電解液が、更にフルオロスルホン酸リチウムを含み、
前記電解液の質量に対して前記フルオロスルホン酸リチウムの含有量が、2質量%以下である、請求項1~4のいずれか1項に記載の非水電解質二次電池。 - 前記負極が、シリケート相と、前記シリケート相内に分散したシリコン粒子と、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。
- リチウムビス(フルオロスルホニル)イミドおよび1,4-ジオキサンを含み、
1,4-ジオキサンの含有量が、電解液の質量に対して0.01質量%以上5質量%以下である、非水電解質二次電池用電解液。
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