JP7196304B2 - リチウム-硫黄二次電池 - Google Patents
リチウム-硫黄二次電池 Download PDFInfo
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Description
[数式1]
[数式1]
[数式2]
[数式3]
[数式4]
VはLi/Li+に対する放電公称電圧(V)で、
SC factorは前記数式1によって定義された値と同一で、
Cは0.1Cレート(rate)で放電する時の放電容量(mAh/g)で、
Dは電解液の密度(g/cm3)である。)。
[実施例1]
比表面積が2000m2/g以上で、気孔体積が1.2cm3/g以上の微小多孔性炭素材と硫黄(S8)を3:1の重量比で均一に混合し、乳鉢混合(mortar mixing)で粉砕した後、155℃のオーブンで30分間置いて硫黄-炭素複合体を製造した。
正極の製造条件を変更して正極活物質層の空隙率が54%、正極活物質層の単位面積当たり硫黄の質量が4.6mg/cm2、これに基づいて計算されたSC factor値が0.85の正極を製造したことを除いては、実施例1と同様の方法でリチウム-硫黄二次電池を製造した。
正極の製造条件を変更して正極活物質層の空隙率が53%、正極活物質層の単位面積当たり硫黄の質量が3.8mg/cm2、これに基づいて計算されたSC factor値が0.72の正極を製造したことを除いては、実施例1と同様の方法でリチウム-硫黄二次電池を製造した。製造された電池の充放電は25℃で行った。
正極の製造条件を変更してカーボンナノチューブと硫黄(S8)を3:1の重量比で均一に混合し、乳鉢混合(mortar mixing)で粉砕した後、155℃のオーブンで30分間置いて製造した硫黄-炭素複合体と、比表面積が150m2/g以上であるカーボンナノチューブとグラフェンを9:1の重量比で混合した形態の導電材を使用し、これによって正極のエネルギー密度が5.45mAh/cm2、正極活物質層の空隙率が68%、正極活物質層の単位面積当たり硫黄の質量が4.54mg/cm2、これに基づいて計算されたSC factor値が0.668の正極を製造したことを除いては、実施例1と同様の方法でリチウム-硫黄二次電池を製造した。製造された電池の充放電は45℃で行った。
電解液の製造条件を変更してジエチレングリコールジメチルエーテルと1,3-ジオキソラン(DECDME:DOL=6:4(体積比))からなる有機溶媒に1M LiFSI、1重量%のLiNO3を溶解させて製造された電解液を使用したことを除いては、実施例3と同様の方法でリチウム-硫黄二次電池を製造した。
正極の製造条件を変更して導電材で気相成長炭素繊維(VGCF)を使用し、正極のエネルギー密度が5.67mAh/cm2、正極活物質層の空隙率は68%、正極活物質層の単位面積当たり硫黄の質量は4.73mg/cm2で、これに基づいて計算されたSC factor値が0.700の正極を製造したことを除いては、実施例4と同様の方法でリチウム-硫黄二次電池を製造した。
実施例1ないし3及び比較例1で製造された電池を充放電測定装置を利用して1.0から3.6Vまでの容量を測定した。この時、得られた結果は図1ないし図4に示す。
前記実施例4及び比較例2で製造した正極の表面形状を走査電子顕微鏡(Scanning Electron Microscope、SEM)を利用して観察した。この時、得られた結果を下記図5及び図6に示す。
実施例4及び比較例2で製造された電池を充放電測定装置を利用して1.0から3.6Vまでの容量を測定した。また、0.1C、0.2Cレート(rate)CCで順次放電するサイクルを行って放電容量を測定した(CC:一定電流(Constant Current))。この時、得られた結果は図7ないし図10に示す。
Claims (20)
- 正極、負極、分離膜及び電解液を含むリチウム-硫黄二次電池であって、
前記正極は微小多孔性炭素材及び硫黄を含む硫黄-炭素複合体を含み、
前記正極は、下記数式1で表されるSC factor値が0.45以上であり、
前記電解液は溶媒及びリチウム塩を含み、
前記溶媒は、下記数式2で表されるDV 2 factor値が1.75以下である第1溶媒及びフッ素化されたエーテル系溶媒である第2溶媒を含む、リチウム-硫黄二次電池:
[数式1]
Pは正極内の正極活物質層の空隙率(%)で、
Lは正極内の正極活物質層の単位面積当たり硫黄の質量(mg/cm2)で、
αは10(定数)である。)
[数式2]
DVは単位体積当たり双極子モーメント(D・mol/L)で、
μは溶媒の粘度(cP、25℃)で、
γは100(定数)である。)。 - 前記微小多孔性炭素材は平均直径が1ないし10nmの気孔を含む、請求項1に記載のリチウム-硫黄二次電池。
- 前記微小多孔性炭素材は比表面積が500ないし4500m2/gである、請求項1または2に記載のリチウム-硫黄二次電池。
- 前記微小多孔性炭素材は空隙率が10ないし90%である、請求項1から3のいずれか一項に記載のリチウム-硫黄二次電池。
- 前記微小多孔性炭素材は気孔体積が0.8ないし5cm3/gである、請求項1から4のいずれか一項に記載のリチウム-硫黄二次電池。
- 前記硫黄は、無機硫黄、Li2Sn(n≧1)、ジスルフィド化合物、有機硫黄化合物及び炭素-硫黄ポリマーからなる群から選択される1種以上を含む、請求項1から5のいずれか一項に記載のリチウム-硫黄二次電池。
- 前記硫黄は前記硫黄-炭素複合体の全体重量を基準にして50ないし90重量%で含まれる、請求項1から6のいずれか一項に記載のリチウム-硫黄二次電池。
- 前記高い比表面積の炭素材は比表面積が100ないし500m2/gである、請求項8に記載のリチウム-硫黄二次電池。
- 前記高い比表面積の炭素材は、カーボンナノチューブ、グラフェン、カーボンブラック及び炭素繊維からなる群から選択される1種以上を含む、請求項8または9に記載のリチウム-硫黄二次電池。
- 前記高い比表面積の炭素材は、カーボンナノチューブ及びグラフェンを0:10ないし10:0の重量比で混合したものである、請求項8から10のいずれか一項に記載のリチウム-硫黄二次電池。
- 前記高い比表面積の炭素材は、正極活物質スラリーの全体重量を基準にして0.01ないし30重量%で含まれる、請求項8から11のいずれか一項に記載のリチウム-硫黄二次電池。
- 前記第1溶媒はDV2 factor値が1.5以下である、請求項1または8に記載のリチウム-硫黄二次電池。
- 前記第1溶媒は、プロピオニトリル、ジメチルアセトアミド、ジメチルホルムアミド、ガンマ-ブチロラクトン、トリエチルアミン及び1-ヨードプロパンからなる群から選択される1種以上を含む、請求項1、8、13または14に記載のリチウム-硫黄二次電池。
- 前記第2溶媒は、1H,1H,2´H,3H-デカフルオロジプロピルエーテル、ジフルオロメチル2,2,2-トリフルオロエチルエーテル、1,2,2,2-テトラフルオロエチルトリフルオロメチルエーテル、1,1,2,3,3,3-ヘキサフルオロプロピルジフルオロメチルエーテル、ペンタフルオロエチル2,2,2-トリフルオロエチルエーテル及び1H,1H,2´H-パーフルオロジプロピルエーテルからなる群から選択される1種以上を含む、請求項1、8、13または14に記載のリチウム-硫黄二次電池。
- 前記溶媒は前記溶媒の全体重量を基準にして第1溶媒を1ないし50重量%で含む、請求項1、8、13または14に記載のリチウム-硫黄二次電池。
- 前記溶媒は、前記溶媒の全体重量を基準にして第2溶媒を50ないし99重量%で含む、請求項1、8、13または14に記載のリチウム-硫黄二次電池。
- 前記溶媒は、第1溶媒と第2溶媒を3:7ないし1:9の重量比で含む、請求項1、8、13または14に記載のリチウム-硫黄二次電池。
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