JP6388594B2 - 負極活物質、それを含むリチウム二次電池、及び該負極活物質の製造方法 - Google Patents
負極活物質、それを含むリチウム二次電池、及び該負極活物質の製造方法 Download PDFInfo
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Description
(半)金属酸化物とリチウムとを予め合金化するためのリチウム源は、リチウム金属、酸素を含まないリチウム塩、及び酸素を含むリチウム塩などに大別される。
図1は、本発明の一実施様態による負極活物質の構造形成を概略的に示した概念図である。
前記コア部の直径は、約0.05ないし約30μm、または約0.5ないし約15μmであり得る。
前記負極活物質は高い容量を有し、電池に使用される場合、サイクル特性及び体積膨張の制御能力に優れ、さらに初期効率が非常に高い。
選択的に、本発明によって注入される電解液は、通常の電解液に含まれる過充電防止剤などのような添加剤をさらに含み得る。
図2は、本発明の一実施様態による負極活物質の製造工程を示したフロー図である。以下、図2を参照して説明する。
コア部及びシェル部の詳細は、上述した負極活物質に関する記載と同様である。
(S2)段階において、前記(S1)段階で形成された複合体とリチウム金属粉末とを混合する。
前記(S1)段階で形成された複合体は、化学的混合方法、機械的混合方法、乾式混合方法などによってリチウム金属粉末と混合される。
前記(S2)段階で形成された複合体とリチウム金属粉末との混合物は、(半)金属酸化物‐Li合金を形成するために熱処理を必要とする。
(半)金属酸化物として平均粒径5μmのSiO 10gを回転管状炉に投入し、そこにアルゴンガスを0.5L/分で流した後、温度を5℃/分の速度で1,000℃まで昇温させた。前記回転管状炉を10rpm/分の速度で回転させながら、アルゴンガスを1.8L/分、アセチレンガスを0.3L/分で流して2時間熱処理することで、コア部としてのSiO表面にシェル部として導電性炭素物質がコーティングされたコア−シェル構造の複合体を製造した。ここで、シェル部の炭素含量は前記コア部100重量部を基準に5.3重量部であった。また、シェル部の厚さはTEM分析から40nmであることが観察された。前記製造された複合体をリチウム金属粉末と92:8の重量比で混合して混合物を形成した。
熱処理温度を600℃に調節したこと以外は、実施例1と同様の方法で負極活物質を製造した。
熱処理温度を1,000℃に調節したこと以外は、実施例1と同様の方法で負極活物質を製造した。
複合体とリチウム金属粉末との混合物に対する熱処理によるコア部のリチウム合金化を実施しないことを除き、実施例1と同様の方法で(半)金属酸化物粉末(SiO、D60=5μm)に炭素物質をコーティングすることでSiO/Cの負極活物質を製造した。
図4は、本発明の比較例1による負極活物質を撮影したSEM写真である。
図3及び図4を参照すれば、図面に示されたSEMイメージは実施例1と比較例1で使用されたLi‐SiO/CとSiO/Cのものであるが、外形的に大きい相違点は殆どないことが確認できる。
(半)金属酸化物粉末(SiO、D60=5μm)とリチウム金属粉末とを92:8の重量比で混合し、Ar雰囲気下、700℃で5時間熱処理することで、リチウムが合金化された複合体を製造した。前記複合体の組成を測定した結果、0.5<x<5であって、1<y<5の値を有することが確認できた。
実施例1、比較例1及び比較例2で製造された負極活物質と黒鉛とを15:85の重量比で混合した後、該混合物に導電材としてカーボンブラックとSBR/CMCとを94:2:2:2の重量比で混合した。これらを溶媒である蒸溜水に入れて混合し、均一な電極スラリーを製造した。前記電極スラリーを銅集電体の一面に65μmの厚さでコーティングし、乾燥及び圧延した後、必要な大きさに打ち抜いて負極を製造した。
正極としてリチウム金属を使用し、前記製造された負極と正極との間にポリオレフィンセパレータを介在させて電極組立体を製造した。
実施例1、比較例1及び比較例2で製造された負極活物質を使用して製造した前記製造例1のコイン型半電池に対し、下記の条件での一回目の充放電特性及び寿命特性を測定して、その結果を下記の表1に示した。
− 電池の充電:5mVまで定電流で充電した後、5mVで電流が0.005Cに達するまで定電圧で充電した。
− 電池の放電:1.0Vまで定電流で放電した。
− 50サイクル充電(lithiation)状態で終了したコインセルを分解し、DMCでリチウム塩などを除去した後、乾燥して厚さを測定し、次の式を用いて厚さ膨張率を計算した。
厚さ膨張率(%)=(50サイクル後の電極厚さ−初期電極厚さ)/初期電極厚さ × 100
上記式において、電極厚さは集電体の厚さを除いた活物質層のみの厚さである。
Claims (8)
- 負極活物質の製造方法であって、
前記負極活物質が、コア−シェル構造を備えてなり、
前記コア−シェル構造が、(半)金属酸化物‐Li合金を有するコア部と、及び、前記コア部の表面にコーティングされた炭素物質を含むシェル部とを備えてなり、
前記コア部が、下記(式)で表されるものであり、
前記負極活物質内に含まれた(半)金属の結晶粒の大きさが45nmないし150nmであることを特徴とするものであり、
(S1)(半)金属の酸化物を含むコア部の表面に、炭素物質を含むシェル部をコーティングすることでコア−シェル構造の複合体を形成する段階と、
(S2)前記複合体にリチウム金属粉末を混合して混合物を形成する段階と、
(S3)前記混合物を熱処理する段階とを含んでなり、
(半)金属酸化物‐Li合金であり、下記(式)で表されるコア部を有する前記負極活物質を得ることを含んでなる、負極活物質の製造方法。
MO x Li y (式)
〔上記式中、
Mは(半)金属であり、
0<x<1.5、
0<y<4である〕 - 前記(半)金属が、Si、Sn、Al、Sb、Bi、As、Ge、Pb、Zn、Cd、In、Ti、Ga及びこれらの合金からなる群より選択されたものであることを特徴とする、請求項1に記載の負極活物質の製造方法。
- 前記(半)金属酸化物が、SiO、SnO、及びSnO2からなる群より選択された一種の化合物又は二種の混合物であることを特徴とする、請求項1又は2に記載の負極活物質の製造方法。
- 前記コア部の直径が、0.05ないし30μmであることを特徴とする、請求項1〜3の何れか一項に記載の負極活物質の製造方法。
- 前記炭素物質が、結晶質炭素、非晶質炭素、又はこれらの混合物であることを特徴とする、請求項1〜4の何れか一項に記載の負極活物質の製造方法。
- 前記シェル部の炭素物質が、負極活物質の重量対比0.05ないし30重量%であることを特徴とする、請求項1〜5の何れか一項に記載の負極活物質の製造方法。
- 前記混合物の形成段階で、前記複合体とリチウム金属粉末との重量比は30:70ないし95:5であることを特徴とする、請求項1〜6の何れか一項に記載の負極活物質の製造方法。
- 前記(S3)の熱処理段階が、500℃ないし2,000℃の温度条件で行われることを特徴とする、請求項1〜7の何れか一項に記載の負極活物質の製造方法。
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PCT/KR2013/011033 WO2014084679A1 (ko) | 2012-11-30 | 2013-11-29 | 음극활물질, 이를 포함하는 리튬 이차전지 및 상기 음극활물질의 제조방법 |
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KR101720429B1 (ko) | 2014-09-18 | 2017-03-27 | 주식회사 엘지화학 | 실리콘-탄소나노튜브 복합체, 이의 제조방법, 이를 포함하는 리튬 이차 전지용 음극 활물질 및 이를 포함하는 리튬 이차 전지 |
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EP2840634A4 (en) | 2016-03-16 |
US9419276B2 (en) | 2016-08-16 |
CN104380507A (zh) | 2015-02-25 |
KR101591698B1 (ko) | 2016-02-04 |
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