JP2016525778A - 寿命特性に優れたリチウムコバルト系複合酸化物及びそれを含む二次電池用正極活物質 - Google Patents
寿命特性に優れたリチウムコバルト系複合酸化物及びそれを含む二次電池用正極活物質 Download PDFInfo
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- JP2016525778A JP2016525778A JP2016529726A JP2016529726A JP2016525778A JP 2016525778 A JP2016525778 A JP 2016525778A JP 2016529726 A JP2016529726 A JP 2016529726A JP 2016529726 A JP2016529726 A JP 2016529726A JP 2016525778 A JP2016525778 A JP 2016525778A
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- Prior art keywords
- composite oxide
- lithium
- lithium cobalt
- positive electrode
- secondary battery
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000007774 positive electrode material Substances 0.000 title claims description 14
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- 239000013078 crystal Substances 0.000 claims abstract description 22
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- 239000000126 substance Substances 0.000 claims abstract description 12
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- 239000010941 cobalt Substances 0.000 claims abstract description 10
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 10
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- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims abstract description 3
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- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
上記式中、0.95≦x≦1.15、0<y≦0.3、0≦z≦0.2であり、
Aは、Al、Mg、Ti、Zr、Sr、W、Nb、Mo、Ga、及びNiからなる群から選択される1種以上の元素である。
Coソース、Mnソース、Liソースを乾式で十分に混合し、Li:Co:Mn:Oがモル比で1.03:0.9982:0.0018:2である混合物を得た。前記混合物を900〜1200℃で5〜20時間焼成して得られた焼成物を粉砕、分級して、Li1.03Co0.9989Mn0.0011O2で表されるリチウムコバルト系複合酸化物を得た。
Coソース、Mnソース、Liソースを乾式で十分に混合し、Li:Co:Mn:Oがモル比で1.03:0.9969:0.0031:2である混合物を得た。前記混合物を900〜1200℃で5〜20時間焼成して得られた焼成物を粉砕、分級して、Li1.03Co0.9982Mn0.0018O2で表されるリチウムコバルト系複合酸化物を得た。
Coソース、Mnソース、Liソースを乾式で十分に混合し、Li:Co:Mn:Oがモル比で1.03:0.9957:0.0043:2である混合物を得た。前記混合物を900〜1200℃で5〜20時間焼成して得られた焼成物を粉砕、分級して、Li1.03Co0.9975Mn0.0025O2で表されるリチウムコバルト系複合酸化物を得た。
Coソース、Mnソース、Liソースを乾式で十分に混合し、Li:Co:Mn:Oがモル比で1.03:0.9933:0.0067:2である混合物を得た。前記混合物を900〜1200℃で5〜20時間焼成して得られた焼成物を粉砕、分級して、Li1.03Co0.9960Mn0.0040O2で表されるリチウムコバルト系複合酸化物を得た。
Coソース、Mnソース、Liソースを乾式で十分に混合し、Li:Co:Mn:Oがモル比で1.03:0.9519:0.0481:2である混合物を得た。前記混合物を900〜1200℃で5〜20時間焼成して得られた焼成物を粉砕、分級して、Li1.03Co0.9550Mn0.0450O2で表されるリチウムコバルト系複合酸化物を得た。
Coソース、Mnソース、Mgソース、Liソースを乾式で十分に混合し、Li:Co:Mn:Mg:Oがモル比で1.03:0.9988:0.0011:0.0001:2である混合物を得た。前記混合物を900〜1200℃で5〜20時間焼成して得られた焼成物を粉砕、分級して、Li1.03Co0.9988Mn0.0011Mg0.0001O2で表されるリチウムコバルト系複合酸化物を得た。
Coソース、Mnソース、Mgソース、Liソースを乾式で十分に混合し、Li:Co:Mn:Mg:Oがモル比で1.03:0.9986:0.0011:0.0003:2である混合物を得た。前記混合物を900〜1200℃で5〜20時間焼成して得られた焼成物を粉砕、分級して、Li1.03Co0.9986Mn0.0011Mg0.0003O2で表されるリチウムコバルト系複合酸化物を得た。
CoソースとLiソースを乾式で十分に混合し、Li:Co:Oがモル比で1.03:1:2である混合物を得た。前記混合物を900〜1200℃で5〜20時間焼成して得られた焼成物を粉砕、分級して、Li1.03CoO2で表されるリチウムコバルト系複合酸化物を得た。
前記実施例1、4及び比較例1のリチウムコバルト系複合酸化物のサンプルを準備し、各サンプルに対するX線回折(XRD)パターンを、銅ターゲットのX線チューブ及び回折されたビームモノクロメータを装着したジーメンスD500回折器を使用して各電圧に応じて収集した。十分に厚く、広いので、X線ビームによって照射される体積が一定となるようにする平らな四角形粉末−ベッドとしてサンプルを製造した。このデータを文献[A.C.Larson and R.B.Von Dreele、“General Structure Analysis System(GSAS)”、Los Alamos National Laboratory Report LAUR 86−748(2000)]で記述されたリートベルト精製プログラムのGSASを使用して、単位セルの格子定数を計算した。その結果を下記表1に示した。
実施例1〜3及び比較例1でそれぞれ製造されたリチウムコバルト系複合酸化物を使用し、リチウムコバルト系複合酸化物:導電材(Denka black):バインダー(PVdF)の量が95:2.5:2.5になるように計量した後、NMPに入れ、ミキシング(mixing)して、正極合剤を製造し、20μmの厚さのアルミニウムホイルに前記正極合剤を200μmの厚さにコーティングした後、圧延及び乾燥して、正極を製造した。
製造されたリチウム二次電池を3.0Vから4.4Vの電圧領域で0.1Cで充放電したとき、初期容量及び効率を測定し、その結果を下記表2に示した。
製造されたリチウム二次電池を25℃のチャンバーで、3.0Vから4.4Vの電圧領域で0.1Cで1回充放電した後、0.5C充電、1C放電を行いながら50回の間寿命特性を測定し、45℃のチャンバーで3.0Vから4.5Vの電圧領域で0.1Cで1回充放電した後、0.5C充電、1C放電を行いながら50回の間充放電を行いながら寿命特性を測定した。その結果を下記表2、及び図1乃至図10に示した。
製造されたリチウム二次電池を3.0Vから4.4Vの電圧領域でレート特性テストを行い、0.1Cの容量対比各C−rateによる容量で計算して、下記表2、及び図11に示した。
実施例1、6、及び7でそれぞれ製造されたリチウムコバルト系複合酸化物を使用し、リチウムコバルト系複合酸化物:導電材(Denka black):バインダー(PVdF)の量が95:2.5:2.5になるように計量した後、NMPに入れ、ミキシング(mixing)して、正極合剤を製造し、20μmの厚さのアルミニウムホイルに前記正極合剤を200μmの厚さにコーティングした後、圧延及び乾燥して、正極を製造した。
Claims (16)
- リチウム、コバルト、マンガンを含んでおり、下記化学式1で表されるリチウムコバルト系複合酸化物であって、理論容量の50%以上の充電状態(State of Charge:SOC)でO3相(O3phase)の単一相結晶構造を維持することを特徴とする、リチウムコバルト系複合酸化物:
LixCo1−y−zMnyAzO2 (1)
上記式中、0.95≦x≦1.15、0<y≦0.3、0≦z≦0.2であり、
Aは、Al、Mg、Ti、Zr、Sr、W、Nb、Mo、Ga、及びNiからなる群から選択される1種以上の元素である。 - 前記リチウムコバルト系複合酸化物は、脱リチウム化が50%以上進行した状態でO3相の単一相結晶構造を維持することを特徴とする、請求項1に記載のリチウムコバルト系複合酸化物。
- 前記リチウムコバルト系複合酸化物は、4.35V以上の作動電圧下で、O3相の単一相結晶構造を維持することを特徴とする、請求項1に記載のリチウムコバルト系複合酸化物。
- 前記リチウムコバルト系複合酸化物は、4.35V以上〜4.5V以下の作動電圧下で、O3相の単一相結晶構造を維持することを特徴とする、請求項3に記載のリチウムコバルト系複合酸化物。
- 前記yは、0.0001≦y≦0.2であることを特徴とする、請求項1に記載のリチウムコバルト系複合酸化物。
- 前記zは、0<z≦0.2であることを特徴とする、請求項1に記載のリチウムコバルト系複合酸化物。
- 前記AはMgであることを特徴とする、請求項1に記載のリチウムコバルト系複合酸化物。
- 前記リチウムコバルト系複合酸化物の平均粒径は0.5μm〜30μmであることを特徴とする、請求項1に記載のリチウムコバルト系複合酸化物。
- 請求項1に記載のリチウムコバルト系複合酸化物を含むことを特徴とする、正極活物質。
- 請求項9に記載の正極活物質を含むことを特徴とする、二次電池用正極合剤。
- 請求項10に記載の二次電池用正極合剤が集電体上に塗布されていることを特徴とする、二次電池用正極。
- 請求項11に記載の二次電池用正極を含むことを特徴とする、リチウム二次電池。
- 請求項12に記載のリチウム二次電池を単位電池として含むことを特徴とする、電池モジュール。
- 請求項12に記載のリチウム二次電池を含むことを特徴とする、デバイス。
- 請求項13に記載の電池モジュールを含むことを特徴とする、デバイス。
- 前記デバイスは、携帯電話、タブレットコンピュータ、ノートパソコン、電気自動車、ハイブリッド電気自動車、プラグ-インハイブリッド自動車、又は電力貯蔵装置であることを特徴とする、請求項14又は15に記載のデバイス。
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CN105431970B (zh) | 2019-08-02 |
EP3016185A4 (en) | 2017-03-08 |
EP3016185A1 (en) | 2016-05-04 |
CN105431970A (zh) | 2016-03-23 |
KR101587055B1 (ko) | 2016-01-20 |
TWI521781B (zh) | 2016-02-11 |
US10505190B2 (en) | 2019-12-10 |
WO2015026121A1 (ko) | 2015-02-26 |
JP6321801B2 (ja) | 2018-05-09 |
EP3016185B1 (en) | 2019-04-03 |
TW201523990A (zh) | 2015-06-16 |
KR20150021008A (ko) | 2015-02-27 |
US20160181609A1 (en) | 2016-06-23 |
US10964943B2 (en) | 2021-03-30 |
US20190148727A1 (en) | 2019-05-16 |
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