JP7434209B2 - 二次電池の製造方法、及び二次電池 - Google Patents
二次電池の製造方法、及び二次電池 Download PDFInfo
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- JP7434209B2 JP7434209B2 JP2021075083A JP2021075083A JP7434209B2 JP 7434209 B2 JP7434209 B2 JP 7434209B2 JP 2021075083 A JP2021075083 A JP 2021075083A JP 2021075083 A JP2021075083 A JP 2021075083A JP 7434209 B2 JP7434209 B2 JP 7434209B2
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- negative electrode
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- secondary battery
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Description
第1の実施形態によると、二次電池の製造方法が提供される。係る製造方法は、電池構造物を準備する工程と、処理電位調整状態を得る工程と、処理電位調整状態にした電池構造物を50℃以上90℃以下の範囲内の保持温度に保持する工程とを含む。電池構造物は、正極と、負極と、電解質とを具備する。正極は、リチウムニッケルコバルトマンガン複合酸化物を含む。負極は、ニオブチタン複合酸化物を含む。電解質は、粘度(η)が1cP以下である第1有機溶媒を1以上含有する。処理電位調整状態は、正極の正極電位をリチウムの酸化還元電位を基準に3.4 V以上3.9 V以下の範囲内に調整すること、及び負極の負極電位をリチウムの酸化還元電位を基準に1.5 V以上2.0 V以下の範囲内に調整することにより得られる。
正極は、正極活物質としてリチウムニッケルコバルトマンガン複合酸化物を含む。正極は、正極活物質を含有する正極活物質含有層を含み得る。正極は、正極集電体をさらに含み得る。
負極は、負極活物質としてニオブチタン複合酸化物を含む。負極は、負極活物質を含有する負極活物質含有層を含み得る。負極は、負極集電体をさらに含み得る。
電解質としては、例えば液状非水電解質又はゲル状非水電解質を用いることができる。液状非水電解質は、溶質としての電解質塩を有機溶媒等の液状溶媒に溶解することにより調製される。電解質塩の濃度は、0.5mol/L以上2.5mol/L以下であることが好ましい。
セパレータは、例えば、ポリエチレン(polyethylene;PE)、ポリプロピレン(polypropylene;PP)、セルロース、若しくはポリフッ化ビニリデン(polyvinylidene fluoride;PVdF)を含む多孔質フィルム、又は合成樹脂製不織布から形成される。安全性の観点からは、ポリエチレン又はポリプロピレンから形成された多孔質フィルムを用いることが好ましい。これらの多孔質フィルムは、一定温度において溶融し、電流を遮断することが可能なためである。
外装部材としては、例えば、ラミネートフィルムからなる容器、又は金属製容器を用いることができる。
負極端子は、負極に含まれるニオブチタン複合酸化物のLi吸蔵放出電位において電気化学的に安定であり、かつ導電性を有する材料から形成することができる。具体的には、負極端子の材料としては、銅、ニッケル、ステンレス若しくはアルミニウム、又は、Mg,Ti,Zn,Mn,Fe,Cu,及びSiからなる群より選択される少なくとも1種の元素を含むアルミニウム合金が挙げられる。負極端子の材料としては、アルミニウム又はアルミニウム合金を用いることが好ましい。負極端子は、負極集電体との接触抵抗を低減するために、負極集電体と同様の材料からなることが好ましい。
正極端子は、リチウムの酸化還元電位に対し3V以上4.5V以下の電位範囲(vs.Li/Li+)において電気的に安定であり、且つ導電性を有する材料から形成することができる。正極端子の材料としては、アルミニウム、或いは、Mg、Ti、Zn、Mn、Fe、Cu及びSiからなる群より選択される少なくとも1種の元素を含むアルミニウム合金が挙げられる。正極端子は、正極集電体との接触抵抗を低減するために、正極集電体と同様の材料から形成されることが好ましい。
活物質として含む化合物の結晶構造は、粉末X線回折(XRD:X-Ray diffraction)により確認することができる。例えば、負極活物質が含むニオブチタン複合酸化物および他の化合物の結晶構造や、正極活物質粒子が含むニッケル含有酸化物や他の化合物の結晶構造を、粉末X線回折測定によって確認することができる。粉末X線回折測定の装置としては、例えばRigaku社製SmartLab、又は、これと等価な機能を有する装置を用いる。測定条件は以下の通りとする:
X線源:Cuターゲット
出力:45kV 200mA
ソーラスリット:入射及び受光共に5°
ステップ幅(2θ):0.02deg
スキャン速度:20deg/分
半導体検出器:D/teX Ultra 250
試料板ホルダー:平板ガラス試料板ホルダー(厚さ0.5mm)
測定範囲:5°≦2θ≦90°。
ガスクロマトグラフィー-質量分析(Gas Chromatography - Mass Spectrometry;GC-MS)測定により電解質の組成および電解質中の成分の定量が可能である。電解質の溶媒の粘度は、回転式粘度計により測定することができる。
第2の実施形態によると、二次電池が提供される。当該二次電池は、第1の実施形態に係る製造方法によって製造された二次電池である。
以下に実施例を説明するが、実施形態は、以下に記載される実施例に限定されるものではない。
<正極の作製>
正極活物質としてリチウムニッケルコバルトマンガン複合酸化物LiNi0.5Co0.3Mn0.2O2、(NCM532)を100質量部と、導電剤としてアセチレンブラック5質量部と、結着剤としてポリフッ化ビニリデン(PVdF)5質量部とを、N-メチルピロリドン(NMP)に加えて混合してスラリーを調製した。このスラリーを、厚さ12μmのアルミニウム箔からなる集電体の両面に塗布した後、乾燥し、プレスすることにより、電極密度(集電体を除く)が3.2g/cm3の正極を作製した。
負極活物質として、単斜晶型ニオブチタン複合酸化物Nb2TiO7を100質量部と、導電剤としてアセチレンブラックを8質量部と、結着剤としてPVdFを8質量部とを、NMPに加えて混合してスラリーを調製した。このスラリーを、厚さ12μmのアルミニウム箔からなる集電体の片面に塗布した後、乾燥し、プレスすることにより、電極密度(集電体を除く)が2.6g/cm3の負極を作製した。
上記で作製した正極と、厚さ15μmのセルロースからなるセパレータと、上記で作製した負極と、セパレータとを、この順序で積層した後、負極が最外周に位置するように渦巻き状に捲回して電極群を作製した。これを90℃で加熱プレスすることにより、幅が58mmで、厚さが3.0mmの偏平状電極群を作製した。得られた電極群を、厚さが40μmのアルミニウム箔とそのアルミニウム箔の両面に形成されたポリプロピレン層とで構成された、厚さが0.1mmのラミネートフィルムからなる外装部材に収容し、120℃で24時間真空乾燥した。
アルゴン雰囲気下において、プロピレンカーボネート(PC)とメチルエチルカーボネート(MEC)とプロピオン酸エチル(EP)を体積比率1:1:1で混合し(第1溶媒(MEC+EP)の体積割合:66.7%)、混合溶媒を調製した。この混合溶媒に、六フッ化リン酸リチウム(LiPF6)を1.0モル/Lの濃度で溶解した。そこへ、1,3-プロパンスルトン(PS)を溶液全体に対し1質量%の割合になるようさらに加えて、液状非水電解質(電解液)を調製した。
室温(25℃)にて仮封止二次電池を電池電圧1.8 Vまで充電することで(SOC 10%)、正極電位を3.65V (vs. Li/Li+)及び負極電位を1.85V (vs. Li/Li+)にそれぞれ調整した。このように処理電位調整状態にした仮封止二次電池を、温度が80℃(保持温度、即ち、エージング温度)の恒温槽内で24時間(保持時間、即ち、エージング時間)加熱した。
加熱後、アルゴン雰囲気下において、仮封止したラミネートパック上部を開封した。その後、減圧することにより気体を排出し、ラミネートフィルムを密封して(本封止)、二次電池を得た。
下記表1及び表2に示すとおり電解質の組成および前処理条件を変更したことを除き、実施例1と同様の手順で二次電池の製造を行った。電解質の組成については、表1及び表2に示すように電解質溶媒の組成、並びにスルトン化合物の材料種および添加量を変更した。前処理条件については、処理電位調整状態を得るために調整した正極電位および負極電位、並びにエージングの温度および時間(保持温度および保持時間)を変更した。
<出力性能評価>
各実施例及び比較例で製造した二次電池の内部抵抗を測定した。内部抵抗が低い方が、より高い出力性能が得られることを示す。
各二次電池に対し、SOCが30%から80%になるような容量範囲において、70℃で充放電を1000サイクル行い、ガス発生量を測定した。
Claims (10)
- リチウムニッケルコバルトマンガン複合酸化物を含む正極と、ニオブチタン複合酸化物を含む負極と、粘度が1cP以下である第1有機溶媒を1以上含有する電解質とを具備する電池構造物を準備する工程と、
前記正極の正極電位をリチウムの酸化還元電位を基準に3.4 V以上3.9 V以下の範囲内に調整すること、及び前記負極の負極電位をリチウムの酸化還元電位を基準に1.5 V以上2.0 V以下の範囲内に調整することにより処理電位調整状態を得る工程と、
前記処理電位調整状態にある前記電池構造物を50℃以上90℃以下の範囲内の保持温度に保持する工程とを含む、
二次電池の製造方法。 - 前記電池構造物を前記処理電位調整状態に前記保持温度にて保持する工程は、6時間以上72時間以下で行う、請求項1に記載の二次電池の製造方法。
- 前記電解質は、前記第1有機溶媒を10%以上の体積割合で含有する、請求項1又は2に記載の二次電池の製造方法。
- 前記第1有機溶媒は、ジエチルカーボネート、メチルエチルカーボネート、及びプロピオン酸エチルからなる群より選択される1以上を含む、請求項1から3の何れか1項に記載の二次電池の製造方法。
- 前記電解質は、プロピレンカーボネートを含む第2有機溶媒を含有する、請求項1から4の何れか1項に記載の二次電池の製造方法。
- 前記電解質は、スルトン化合物をさらに含有する、請求項1から5の何れか1項に記載の二次電池の製造方法。
- 前記スルトン化合物は、1,3-プロパンスルトン、1,3-プロペンスルトン、1,4-ブタンスルトン、及び2,4-ブタンスルトンからなる群より選択される1以上を含む、請求項6に記載の二次電池の製造方法。
- 前記リチウムニッケルコバルトマンガン複合酸化物は、LixNi1-y-zCoyMnzO2で表され、0<x≦1、0<y<1、0<z<1、及びy+z<1である化合物を含む、請求項1から7の何れか1項に記載の二次電池の製造方法。
- 前記ニオブチタン複合酸化物は、LiaTi1-bM1bNb2-cM2cO7+δで表され、M1はZr,Si,及びSnからなる群より選択される少なくとも1つであり、M2はV,Ta,及びBiからなる群より選択される少なくとも1つであり、0≦a≦5、0≦b<1、0≦c<2、並びに-0.3≦δ≦0.3である化合物、及びLiaTi1-bM3b+cNb2-cO7-δで表され、M3はMg,Fe,Ni,Co,W,Ta,及びMoからなる群より選択される少なくとも1つであり、0≦a≦5、0≦b<1、0≦c<2、並びに-0.3≦δ≦0.3である化合物からなる群より選択される1以上の単斜晶型ニオブチタン複合酸化物を含む、請求項1から8の何れか1項に記載の二次電池の製造方法。
- 請求項1から9の何れか1項に記載の製造方法によって製造された、二次電池。
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JP2015149267A (ja) | 2013-03-14 | 2015-08-20 | 株式会社東芝 | 非水電解質電池及び電池パック |
JP2016035899A (ja) | 2014-07-31 | 2016-03-17 | 株式会社東芝 | 非水電解質電池及び電池パック |
JP2018160416A (ja) | 2017-03-23 | 2018-10-11 | 株式会社東芝 | 電極、非水電解質電池、電池パック及び車両 |
JP2019046688A (ja) | 2017-09-04 | 2019-03-22 | 株式会社豊田自動織機 | リチウムイオン二次電池の製造方法 |
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