JP6256001B2 - 二次電池の製造方法 - Google Patents
二次電池の製造方法 Download PDFInfo
- Publication number
- JP6256001B2 JP6256001B2 JP2013522544A JP2013522544A JP6256001B2 JP 6256001 B2 JP6256001 B2 JP 6256001B2 JP 2013522544 A JP2013522544 A JP 2013522544A JP 2013522544 A JP2013522544 A JP 2013522544A JP 6256001 B2 JP6256001 B2 JP 6256001B2
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- JP
- Japan
- Prior art keywords
- positive electrode
- secondary battery
- cyclic
- lithium
- additive
- Prior art date
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Description
(正極に対する添加剤の還元分解電位以下の電位の印加工程)
本実施形態に係る二次電池の製造方法では、まず、添加剤を含む前処理用電解液中で、該添加剤が還元分解される電位以下の電位を正極に印加する。
次に、添加剤を含む前処理用電解液中で、該添加剤が還元分解される電位以下の電位を印加された前記正極と、負極とを備える二次電池を組み立てる。
本実施形態に係る二次電池は、添加剤が還元分解されることにより形成される皮膜を備え、正極活物質としてスピネル構造のリチウム含有複合酸化物を含む正極と、負極と、を備える。本実施形態に係る二次電池は、前記本実施形態に係る二次電池の製造方法により製造することができる。本実施形態に係る二次電池は、高いサイクル特性を示す。
(負極の作製)
負極活物質として、平均粒径が20μm、平均アスペクト比が1.4、比表面積が1m2/gの塊状人造黒鉛粉末と、結着剤としてアクリル変性樹脂(商品名:LSR−7、日立化成工業(株)製)と、カーボンブラックとを固形分質量比で96:3:1の割合でN−メチルピロリドン(NMP)中に均一に分散させてスラリーを作製した。このスラリーを負極集電体となる厚さ15μmの銅箔上に塗布後、125℃にて10分間NMPを蒸発させることにより負極活物質層を形成し、プレスすることによって片面塗布した負極を作製した。乾燥後の単位面積当たりの負極合剤量は0.008g/cm2とした。なお、前記結着剤は、ニトリル基含有単量体由来の繰り返し単位を80質量%以上含んだアクリル変性樹脂である。
正極活物質として平均粒径10μmのLiMn2O4粉末と、結着剤としてPVDFと、導電助剤として炭素質粉末とを質量比を92:4:4でNMP中に均一に分散させてスラリーを作製した。そのスラリーを正極集電体となる厚み20μmのアルミ箔上に塗布後、125℃にて10分間NMPを蒸発させることにより正極活物質層を形成し、正極とした。乾燥後の単位面積当たりの正極合剤量は0.025g/cm2とした。
EC:DEC=30:70(体積%)の混合溶媒に、電解質として1mol/LのLiPF6を溶解させた溶液を電解液Rとした。これに添加剤として、MMDSを1質量%混合した溶液を電解液Aとした。
作製した正極と負極とを各々5cm(幅)×6.0cm(長さ)に切り出した。このうち、一辺の5cm×1cmはタブを接続するための未塗布部であって、活物質層は5cm×5cmである。アルゴン雰囲気のグローブボックス内で、予めアルゴン置換した電解液Aをテフロン(登録商標)容器にいれ、これに前記正極(W)、リチウム電極(C)及びリチウム電極(R)を挿入し、3極セルを組んだ。ポテンショスタットにより、正極(W)に対し1.3Vの電位を1秒印加し、10秒休止する操作を1800回繰り返した。これにより、正極(W)の表面に皮膜を形成した。なお、正極(W)の表面にMMDSの還元分解による皮膜が形成されていることは、XPSにより正極(W)の表面元素組成が変化していることを観察することにより確認した。
正極(W)を前記電解液から取り出し、DECですすいだ。次に幅5mm、長さ3cm、厚み0.1mmのアルミ製の正極タブを正極未塗布部に長さ1cmで超音波溶接した。同様に、正極タブと同サイズのニッケル製の負極タブを負極未塗布部に超音波溶接した。
作製したラミネート型二次電池についてサイクル試験を行った。具体的には、60mAの定電流で4.2Vまで充電した後、合計で2.5時間の4.2V定電圧充電を行ってから、60mAで3.0Vまで定電流放電する充放電サイクルを500回繰り返した。初回放電容量に対する500サイクル後の放電容量の比率を容量維持率(%)として求めた。試験温度は、高温環境化での劣化試験及び加速試験を目的として、60℃とした。結果を表1に示す。
実施例1の電解液Rに、添加剤としてVCを1質量%混合したものを電解液Bとし、正極への皮膜形成において、電解液Aに代わりに電解液Bを用いた。また、正極への皮膜形成において、正極(W)に間欠印加する電位を1.5Vとした。それ以外は実施例1と同様の操作を行った。結果を表1に示す。
実施例1の電解液Rに、添加剤としてLiBOBを1質量%混合したものを電解液Cとし、正極への皮膜形成において、電解液Aに代わりに電解液Cを用いた。また、正極への皮膜形成において、正極(W)に間欠印加する電位を1.5Vとした。それ以外は実施例1と同様の操作を行った。結果を表1に示す。
正極活物質として平均粒径10μmのLiMn2O4粉末と平均粒径10μmのLiNiO2粉末の混合物(LiMn2O4とLiNiO2との混合比(質量比):90/10)を用いた。それ以外は実施例1と同様の操作を行った。結果を表1に示す。
正極への皮膜形成において正極(W)に電位を印加する際、間欠印加を行わず、正極(W)の電位を1.3Vに調整し、30分保持することで正極(W)の表面に皮膜を形成した。それ以外は実施例1と同様の操作を行った。結果を表1に示す。
正極への皮膜形成において、電解液Aの代わりに電解液Rを用いたこと以外は実施例1と同様の操作を行った。結果を表1に示す。
正極への皮膜形成において、正極(W)に電位を印加せずに30分放置した以外は実施例1と同様の操作を行った。結果を表1に示す。
正極への皮膜形成において、電解液Aに代わりに電解液Rを用いたこと以外は比較例2と同様の操作を行った。結果を表1に示す。
正極活物質として平均粒径10μmのLiMn2O4粉末と平均粒径10μmのLiNiO2粉末の混合物(LiMn2O4とLiNiO2との混合比(質量比):90/10)を用いた。それ以外は比較例2と同様の操作を行った。結果を表1に示す。
負極活物質としてリチウム金属を用い、これを銅箔に蒸着したものを負極として用いた。また、該負極と同一の電極を参照電極として用いた。正極には実施例1において作製した皮膜形成前の正極を用いた。
2 作用極(正極)
3 皮膜
4 参照極
5 前処理用電解液
6 ポテンショスタット
11 正極活物質層
12 負極活物質層
13 正極集電体
14 負極集電体
15 セパレータ
16 ラミネート外装体
17 負極タブ
18 正極タブ
Claims (8)
- 添加剤を含む前処理用電解液中で、該添加剤が還元分解される電位以下の電位を正極に印加して、正極表面に皮膜を形成する工程と、
前記工程の後に前記正極と、負極とを備える二次電池を組み立てる工程と、を含む二次電池の製造方法であって、
前記添加剤が環状ジスルホン酸エステル、環状スルホン酸エステル、環状スルホン、環状ハロゲン化カーボネート、不飽和カーボネート、酸無水物、環状イミド、リチウムビスオキサレートボレート、ジフルオロ[オキソラト−O,O’]ホウ酸リチウム、サルファイト、不飽和エステル、グリコリド及びシアノフランからなる群から選択される少なくとも1種である二次電池の製造方法。 - 前記正極に含まれる正極活物質がスピネル構造のリチウム含有複合酸化物である請求項1に記載の二次電池の製造方法。
- 前記添加剤が還元分解される電位以下の電位を正極に印加する工程において、正極に電位を間欠印加する請求項2に記載の二次電池の製造方法。
- 前記負極が備える負極集電体が銅を含む請求項1から3のいずれか1項に記載の二次電池の製造方法。
- 前記二次電池が二次電池用電解液を備え、該二次電池用電解液が環状ジスルホン酸エステル、環状スルホン酸エステル、環状スルホン、環状ハロゲン化カーボネート、不飽和カーボネート、酸無水物、環状イミド、リチウムビスオキサレートボレート、ジフルオロ[オキソラト−O,O’]ホウ酸リチウム、サルファイト、不飽和エステル、グリコリド及びシアノフランからなる群から選択される少なくとも1種の添加剤を含む請求項1から4のいずれか1項に記載の二次電池の製造方法。
- 添加剤Aが還元分解されることにより形成される皮膜を備えかつ正極活物質としてスピネル構造のリチウム含有複合酸化物を含む正極と、
添加剤Bが還元分解されることにより形成される皮膜を備える負極と、を備える二次電池であって、
前記添加剤Aが環状ジスルホン酸エステル、環状スルホン酸エステル、環状スルホン、環状ハロゲン化カーボネート、不飽和カーボネート、酸無水物、環状イミド、リチウムビスオキサレートボレート、ジフルオロ[オキソラト−O,O’]ホウ酸リチウム、サルファイト、不飽和エステル、グリコリド及びシアノフランからなる群から選択される少なくとも1種であり、
前記二次電池が二次電池用電解液を備え、該二次電池用電解液が環状ジスルホン酸エステル、環状スルホン酸エステル、環状スルホン、環状ハロゲン化カーボネート、不飽和カーボネート、酸無水物、環状イミド、リチウムビスオキサレートボレート、ジフルオロ[オキソラト−O,O’]ホウ酸リチウム、サルファイト、不飽和エステル、グリコリド及びシアノフランからなる群から選択される少なくとも1種の前記添加剤Bを含む二次電池。 - 前記負極が備える負極集電体が銅を含む請求項6に記載の二次電池。
- 前記添加剤Aと前記添加剤Bとが異なる添加剤である請求項6又は7に記載の二次電池。
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JP2000268857A (ja) * | 1999-03-18 | 2000-09-29 | Toyota Central Res & Dev Lab Inc | リチウムイオン二次電池 |
JP2005259641A (ja) * | 2004-03-15 | 2005-09-22 | Mitsubishi Heavy Ind Ltd | リチウム二次電池用の電解液、電極、リチウム二次電池およびそれらの製造方法 |
JP2009164082A (ja) * | 2008-01-10 | 2009-07-23 | Sanyo Electric Co Ltd | 非水電解質二次電池及びその製造方法 |
JP5421220B2 (ja) * | 2010-11-01 | 2014-02-19 | 日本電気株式会社 | 二次電池用電解液および二次電池 |
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