JP4944648B2 - 非水電解液二次電池用負極 - Google Patents
非水電解液二次電池用負極 Download PDFInfo
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- JP4944648B2 JP4944648B2 JP2007069923A JP2007069923A JP4944648B2 JP 4944648 B2 JP4944648 B2 JP 4944648B2 JP 2007069923 A JP2007069923 A JP 2007069923A JP 2007069923 A JP2007069923 A JP 2007069923A JP 4944648 B2 JP4944648 B2 JP 4944648B2
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Images
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
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- C—CHEMISTRY; METALLURGY
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- C25D5/18—Electroplating using modulated, pulsed or reversing current
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- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
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- C25D7/00—Electroplating characterised by the article coated
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Description
前記活物質層をその厚み方向に仮想的に二等分したときに、二分割された活物質層のうち、負極表面に近い側における前記金属材料の量が、負極表面から遠い側における前記金属材料の量よりも少ないことを特徴とする非水電解液二次電池用負極を提供するものである。
活物質の粒子を含むスラリーを集電体上に塗布して塗膜を形成し、
前記塗膜を有する集電体を、リチウム化合物の形成能の低い金属材料を含むめっき浴中に浸漬して、第1の電流密度で電解めっきを進行させて該塗膜中に金属材料を析出させ、
次いで第1の電流密度よりも高い第2の電流密度で電解めっきを進行させる非水電解液二次電池用負極の製造方法を提供するものである。
・ピロリン酸銅三水和物:85〜120g/l
・ピロリン酸カリウム:300〜600g/l
・硝酸カリウム:15〜65g/l
・浴温度:45〜60℃
・電流密度:1〜7A/dm2
・pH:アンモニア水とポリリン酸を添加してpH7.1〜9.5になるように調整する。
・硫酸ニッケル:100〜250g/l
・塩化アンモニウム:15〜30g/l
・ホウ酸:15〜45g/l
・浴温度:45〜60℃
・電流密度:1〜7A/dm2
・pH:25重量%アンモニア水:100〜300g/lの範囲でpH8〜11となるように調整する。
このアルカリニッケル浴と前述のピロリン酸銅浴とを比べると、ピロリン酸銅浴を用いた場合の方が活物質層12内に適度な空隙が形成される傾向があり、負極の長寿命化を図りやすいので好ましい。
(1)前記のスラリーの塗布によって形成された塗膜の単位面積当たりの重量を測定し、粒子12aの重量及び結着剤の重量を、スラリーの配合比から算出する。
(2)電解めっき後の単位面積当たりの重量変化から、析出しためっき金属種の重量を算出する。
(3)電解めっき後、負極の断面をSEM観察することで、活物質層12の厚みを求める。
(4)活物質層12の厚みから、単位面積当たりの活物質層12の体積を算出する。
(5)粒子12aの重量、結着剤の重量、めっき金属種の重量と、それぞれの配合比から、それぞれの体積を算出する。
(6)単位面積当たりの活物質層12の体積から、粒子12aの体積、結着剤の体積、めっき金属種の体積を減じて、空隙の体積を算出する。
(7)このようにして算出された空隙の体積を、単位面積当たりの活物質層12の体積で除し、それに100を乗じた値を空隙率(%)とする。
厚み18μmの電解銅箔からなる集電体を室温で30秒間酸洗浄した。処理後、15秒間純水洗浄した。集電体上にSiの粒子を含むスラリーを膜厚15μmになるように塗布し塗膜を形成した。スラリーの組成は、粒子:スチレンブタジエンラバー(結着剤):アセチレンブラック=100:1.7:2(重量比)であった。Siの粒子の平均粒径D50は2μmであった。平均粒径D50は、日機装(株)製のマイクロトラック粒度分布測定装置(No.9320−X100)を使用して測定した。
・ピロリン酸銅三水和物:105g/l
・ピロリン酸カリウム:450g/l
・硝酸カリウム:30g/l
・P比:7.7
・浴温度:50℃
・電流密度:1A/dm2
・pH:アンモニア水とポリリン酸を添加してpH8.2になるように調整した。
電流密度1A/dm2の条件下に塗膜の厚み方向全域にわたって銅の浸透めっきを行う以外は実施例1と同様にして比較例1の負極を得た。また電流密度7.5A/dm2の条件下に塗膜の厚み方向全域にわたって銅の浸透めっきを行う以外は実施例1と同様にして比較例2の負極を得た。
実施例及び比較例で得られた負極について、活物質層全体の単位面積当たりのCuの重量及びSiの重量を、ICP発光分析装置を用いて測定した。また、活物質層の縦断面を切り出し、Cu及びSiそれぞれの表面側活物質層及び集電体側活物質層における分布比をエネルギー分散型X線分析(EDX)装置(EDAX製のPegasus system)によって測定した。これらの測定結果から表面側活物質層及び集電体側活物質層それぞれについて単位面積当たりのCuの重量及びSiの重量を求めた。結果を表1に示す。なお、EDX装置による測定条件は以下のとおりである。
・加速電圧 5kV
・測定対象元素 C、O、F、Cu、Si、P
(これらの元素の合計を100重量%とする)
・解像度 512×400
・フレーム 64
・ドリフト補正 オン
〔密着性の評価〕
密着性評価にはJIS Z 1522に規定の幅12mmの透明粘着テープを用いた。テープの新しい接着面を長さ50mm以上指圧によって気泡が残らないように圧着し、10秒後、負極に直角の方向にすばやくテープを引き剥がした。集電体と活物質層とが剥離しなかった場合を密着性良好と、集電体と活物質層とが剥離している場合を密着性不良と判断した。以上の試験を実施例及び比較例で得られた負極についてそれぞれ20回行い、密着性良好であった回数を試験回数(20回)で除し、100を乗じた値を密着性の評価(%)とした。
11 集電体
12 活物質層
12a 活物質の粒子
13 リチウム化合物の形成能の低い金属材料
15 塗膜
Claims (8)
- 活物質の粒子を含む活物質層を備え、該粒子の表面の少なくとも一部がリチウム化合物の形成能の低い金属材料で被覆されていると共に、該金属材料で被覆された該粒子どうしの間に空隙が形成されている非水電解液二次電池用負極であって、
前記活物質層をその厚み方向に仮想的に二等分したときに、二分割された活物質層のうち、負極表面に近い側における前記金属材料の量が、負極表面から遠い側における前記金属材料の量よりも少ないことを特徴とする非水電解液二次電池用負極。 - 仮想的に二分割された活物質層のうち、負極表面に近い側における前記粒子/前記金属材料の重量比が、負極表面から遠い側における前記粒子/前記金属材料の重量比よりも大きい請求項1記載の非水電解液二次電池用負極。
- 前記粒子が、前記活物質層の厚み方向にわたってほぼ均一に分布している請求項1又は2記載の非水電解液二次電池用負極。
- 仮想的に二分割された活物質層のうち、負極表面に近い側における前記粒子の表面を被覆する前記金属材料の厚みが、負極表面から遠い側における前記粒子の表面を被覆する前記金属材料の厚みよりも小さい請求項1ないし3の何れかに記載の非水電解液二次電池用負極。
- 前記金属材料が、前記活物質層の厚み方向全域にわたって前記粒子の表面に存在している請求項1ないし4の何れかに記載の非水電解液二次電池用負極。
- pH7.1〜11のめっき浴を用いた電解めっきによって前記粒子の表面を前記金属材料で被覆してある請求項1ないし5の何れかに記載の非水電解液二次電池用負極。
- 請求項1ないし6の何れかに記載の非水電解液二次電池用負極を備えた非水電解液二次電池。
- 活物質の粒子を含むスラリーを集電体上に塗布して塗膜を形成し、
前記塗膜を有する集電体を、リチウム化合物の形成能の低い金属材料を含むめっき浴中に浸漬して、第1の電流密度で電解めっきを進行させて該塗膜中に金属材料を析出させ、
次いで第1の電流密度よりも高い第2の電流密度で電解めっきを進行させる非水電解液二次電池用負極の製造方法。
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JP2007069923A JP4944648B2 (ja) | 2006-06-30 | 2007-03-19 | 非水電解液二次電池用負極 |
US12/306,990 US20090191463A1 (en) | 2006-06-30 | 2007-04-18 | Negative electrode for nonaqueous secondary battery |
KR1020087030704A KR101047782B1 (ko) | 2006-06-30 | 2007-04-18 | 비수전해액 이차전지용 음극 |
DE112007001610T DE112007001610T5 (de) | 2006-06-30 | 2007-04-18 | Negative Elektrode für eine nicht-wässerige Sekundärbatterie |
PCT/JP2007/058414 WO2008001539A1 (fr) | 2006-06-30 | 2007-04-18 | Électrode négative pour accumulateur à électrolyte non aqueux |
CN2007800248823A CN101485013B (zh) | 2006-06-30 | 2007-04-18 | 非水电解液二次电池用负极 |
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JP5651547B2 (ja) * | 2011-06-29 | 2015-01-14 | 日立オートモティブシステムズ株式会社 | リチウムイオン二次電池 |
JP5904071B2 (ja) * | 2012-09-18 | 2016-04-13 | 株式会社豊田自動織機 | 蓄電装置、及び電極の製造方法 |
US9627722B1 (en) | 2013-09-16 | 2017-04-18 | American Lithium Energy Corporation | Positive temperature coefficient film, positive temperature coefficient electrode, positive temperature coefficient separator, and battery comprising the same |
HUE049590T2 (hu) | 2014-11-25 | 2020-09-28 | American Lithium Energy Corp | Újratölthetõ akkumulátor belsõ áramhatárolóval és árammegszakítóval |
CN105406050B (zh) | 2015-12-31 | 2018-11-02 | 深圳市贝特瑞新能源材料股份有限公司 | 一种复合硅负极材料、制备方法和用途 |
WO2018052077A1 (ja) * | 2016-09-15 | 2018-03-22 | 日本電気株式会社 | リチウムイオン二次電池 |
WO2019023683A1 (en) * | 2017-07-28 | 2019-01-31 | American Lithium Energy Corporation | ANTI-CORROSION COATING FOR BATTERY CURRENT COLLECTOR |
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- 2007-04-18 CN CN2007800248823A patent/CN101485013B/zh not_active Expired - Fee Related
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DE112007001610T5 (de) | 2009-04-30 |
KR20090018137A (ko) | 2009-02-19 |
US20090191463A1 (en) | 2009-07-30 |
KR101047782B1 (ko) | 2011-07-07 |
CN101485013B (zh) | 2011-11-02 |
JP2008034348A (ja) | 2008-02-14 |
WO2008001539A1 (fr) | 2008-01-03 |
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