JP6517330B2 - リチウム二次電池用正極活物質、この製造方法及びこれを含むリチウム二次電池 - Google Patents
リチウム二次電池用正極活物質、この製造方法及びこれを含むリチウム二次電池 Download PDFInfo
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- JP6517330B2 JP6517330B2 JP2017517259A JP2017517259A JP6517330B2 JP 6517330 B2 JP6517330 B2 JP 6517330B2 JP 2017517259 A JP2017517259 A JP 2017517259A JP 2017517259 A JP2017517259 A JP 2017517259A JP 6517330 B2 JP6517330 B2 JP 6517330B2
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- lithium
- positive electrode
- active material
- electrode active
- cobalt oxide
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- SIAPCJWMELPYOE-UHFFFAOYSA-N lithium hydride Chemical compound [LiH] SIAPCJWMELPYOE-UHFFFAOYSA-N 0.000 description 1
- 229910000103 lithium hydride Inorganic materials 0.000 description 1
- HSZCZNFXUDYRKD-UHFFFAOYSA-M lithium iodide Inorganic materials [Li+].[I-] HSZCZNFXUDYRKD-UHFFFAOYSA-M 0.000 description 1
- 229910002102 lithium manganese oxide Inorganic materials 0.000 description 1
- QEXMICRJPVUPSN-UHFFFAOYSA-N lithium manganese(2+) oxygen(2-) Chemical class [O-2].[Mn+2].[Li+] QEXMICRJPVUPSN-UHFFFAOYSA-N 0.000 description 1
- 229910000686 lithium vanadium oxide Inorganic materials 0.000 description 1
- 229910021437 lithium-transition metal oxide Inorganic materials 0.000 description 1
- ACFSQHQYDZIPRL-UHFFFAOYSA-N lithium;bis(1,1,2,2,2-pentafluoroethylsulfonyl)azanide Chemical compound [Li+].FC(F)(F)C(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)C(F)(F)F ACFSQHQYDZIPRL-UHFFFAOYSA-N 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- PYLWMHQQBFSUBP-UHFFFAOYSA-N monofluorobenzene Chemical compound FC1=CC=CC=C1 PYLWMHQQBFSUBP-UHFFFAOYSA-N 0.000 description 1
- 239000002077 nanosphere Substances 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 150000005181 nitrobenzenes Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000011301 petroleum pitch Substances 0.000 description 1
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- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- YGSFNCRAZOCNDJ-UHFFFAOYSA-N propan-2-one Chemical compound CC(C)=O.CC(C)=O YGSFNCRAZOCNDJ-UHFFFAOYSA-N 0.000 description 1
- 229920001384 propylene homopolymer Polymers 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 239000002296 pyrolytic carbon Substances 0.000 description 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
- 239000001008 quinone-imine dye Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000004627 regenerated cellulose Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 229910021435 silicon-carbon complex Inorganic materials 0.000 description 1
- 239000011867 silicon-carbon complex material Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910021384 soft carbon Inorganic materials 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical class O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 239000006234 thermal black Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000005011 time of flight secondary ion mass spectroscopy Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
- 238000004841 transmission electron microscopy energy-dispersive X-ray spectroscopy Methods 0.000 description 1
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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Description
本出願は、2014年10月2日付韓国特許出願第2014−0133474号及び2015年10月1日付韓国特許出願第2015−0138717号に基づいた優先権の利益を主張し、当該韓国特許出願の文献に開示されている全ての内容は本明細書の一部として含まれる。
[化学式1]
Li1−aCoMxO2 (1)
前記化学式(1)で、a及びxは、それぞれ独立的な酸化物組成元素の原子分率であって、0<a≦0.05であり、xは0≦x≦0.02である。
[化学式2]
Li1−aCoMxO2 (1)
[化学式3]
LibCoM’yO2 (2)
(前記化学式(1)及び(2)で、
M及びM’は、それぞれ独立的にW、Mo、Zr、Ti、Mg、Ta、Al、Fe、V、Cr、Ba、Ca及びNbからなる群より選択されるいずれか一つまたは2以上の金属元素を含み、
a、b、x及びyは、それぞれ独立的な酸化物組成元素の原子分率であって、0<a≦0.05、1≦b≦1.2、0≦x≦0.02及び0≦y≦0.02である。)
前記化学式(1)において0<a≦0.05及び1≦b≦1.2の条件を同時に満たす場合、aが0.05を超過するか、またはbが1.2を超過する場合の活物質に比べ、リチウム欠損構造の形成に伴う率特性改善の効果が10%以上さらに改善可能である。また、リチウム欠損構造を形成していないリチウムコバルト酸化物(LiCOO2)に比べては、率特性改善の効果が最大30%まで改善可能である。
Li2CO3粉末及びCo3O4粉末を、Li/Coモル比が0.95になるようにする量で混合した後、900℃で10時間の間1次熱処理を行った。結果として収得した粉末を粉砕及び分級してリチウム欠損の第1リチウムコバルト酸化物の粒子を製造した。
Li2CO3粉末及びCo3O4粉末を、Li/Coモル比が0.95になるようにする量で混合した後、900℃で10時間の間1次熱処理した。結果として収得した粉末を粉砕及び分級してリチウム欠損の第1リチウムコバルト酸化物の粒子を製造した。
Li2CO3粉末及びCo3O4粉末を、Li/Coモル比が0.95になるようにする量で混合した後、900℃で10時間の間1次熱処理した。結果として収得した粉末を粉砕及び分級してリチウム欠損の第1リチウムコバルト酸化物の粒子を製造した。
前記製造例1から3で製造した正極活物質をそれぞれ利用してリチウム二次電池を製造した。
正極活物質としてLiCoO2(平均粒径:12μm)を用いることを除き、前記実施例1と同様の方法で行ってリチウム二次電池を製造した。
前記製造例1で製造した正極活物質に対し、X線光電子分光器(X−ray photoelectron spectroscopy、XPS)を利用して活物質の表面から内部までの深さプロファイル(depth profile)に応じたLi/Coのモル比の変化を観察した。その結果を下記表1に示した。
前記製造例1で製造した正極活物質に対し、透過電子顕微鏡を利用して活物質表面側と内部での結晶構造とをそれぞれ観察した。その結果を図1に示した。
前記製造例1で製造した正極活物質を利用してコインセル(Li金属負極を使用)を製造し、常温(25℃)で0.1C/0.1Cの条件で充放電を行った後、初期充放電特性を評価した。その結果を下記図2に示した。
前記実施例1及び比較例1で製造したリチウム二次電池に対し、下記のような方法で電池特性を評価した。
Claims (22)
- リチウムコバルト酸化物の粒子を含み、
前記リチウムコバルト酸化物の粒子は、粒子の内部にLi/Coのモル比が1未満であるリチウム欠損のリチウムコバルト酸化物を含み、
前記リチウムコバルト酸化物の粒子は、
下記化学式(1)の第1リチウムコバルト酸化物を含むコア部;及び
前記コア部の表面上に位置し、下記化学式(2)の第2リチウムコバルト酸化物を含むシェル部のコア−シェル構造を有するものであるリチウム二次電池用正極活物質。
[化学式1]
Li 1−a CoM x O 2 (1)
[化学式2]
Li b CoM’ y O 2 (2)
(前記化学式(1)及び(2)で、M及びM’は、それぞれ独立的にW、Mo、Zr、Ti、Mg、Ta、Al、Fe、V、Cr、Ba、Ca及びNbからなる群より選択されるいずれか一つまたは2以上の金属元素を含み、a、b、x及びyは、0<a≦0.05、1≦b≦1.2、0≦x≦0.02及び0≦y≦0.02である。) - 前記リチウム欠損のリチウムコバルト酸化物は、空間群がFd−3mに属し、キュービック型結晶構造を有するものである請求項1に記載のリチウム二次電池用正極活物質。
- 前記第1リチウムコバルト酸化物は空間群がFd−3mに属し、キュービック型結晶構造を有し、
前記第2リチウムコバルト酸化物は層状結晶構造を有するものである請求項1に記載のリチウム二次電池用正極活物質。 - 前記コア部は、リチウムコバルト酸化物の粒子の中心から表面までの距離に対し、0%から99%の距離に該当する領域であるものである請求項1に記載のリチウム二次電池用正極活物質。
- 前記コア部とシェル部は、1:0.01から1:0.1の厚さ比を有するものである請求項1に記載のリチウム二次電池用正極活物質。
- 前記コア部及びシェル部は、それぞれ独立的にリチウムコバルト酸化物粒子の中心に行くほど減少する濃度勾配で分布するリチウムを含むものである請求項1に記載のリチウム二次電池用正極活物質。
- 前記コア部内でのリチウムの濃度勾配の傾斜度と、シェル部内でのリチウムの濃度勾配の傾斜度とは、互いに同一であるか、または互いに異なる傾斜度の値を有するものである請求項1に記載のリチウム二次電池用正極活物質。
- 前記コア部及びシェル部の少なくとも一つは、当該領域内で一つの濃度値で存在するリチウムを含むものである請求項1に記載のリチウム二次電池用正極活物質。
- 前記リチウムコバルト酸化物粒子の表面から中心に行くほどリチウムが漸進的に減少する濃度勾配で分布し、
前記化学式(1)及び(2)で、aは、0<a≦0.05の範囲内で粒子の中心に行くほど増加し、bは、1≦b≦1.2の範囲内で粒子の中心に行くほど減少するものである請求項1に記載のリチウム二次電池用正極活物質。 - 3から50μmの平均粒径を有する単一構造体(monolith)であるものである請求項1に記載のリチウム二次電池用正極活物質。
- 充電及び放電に伴う電圧プロファイルの測定時、4.0Vから4.2Vの電圧区間で変曲点を有するものである請求項1に記載のリチウム二次電池用正極活物質。
- コバルト原料物質及びリチウム原料物質を0<Li/Coモル比<1になるようにする量で混合した後、1次熱処理して第1リチウムコバルト酸化物の粒子を準備する段階、及び
前記第1リチウムコバルト酸化物の粒子に対し、コバルト原料物質及びリチウム原料物質を1≦Li/Coモル比になるようにする量で混合した後、2次熱処理する段階
を含むリチウム二次電池用正極活物質の製造方法であって、
前記リチウム二次電池用正極活物質は、
リチウムコバルト酸化物の粒子を含み、
前記リチウムコバルト酸化物の粒子は、粒子の内部にLi/Coのモル比が1未満であるリチウム欠損のリチウムコバルト酸化物を含むものである、リチウム二次電池用正極活物質の製造方法。 - 前記第1リチウムコバルト酸化物の粒子の準備段階で、コバルト原料物質及びリチウム原料物質の混合時にW、Mo、Zr、Ti、Mg、Ta、Al、Fe、V、Cr、Ba、Ca及びNbからなる群より選択されるいずれか一つまたは2以上の金属元素含有の原料物質を添加する工程をさらに含む請求項12に記載のリチウム二次電池用正極活物質の製造方法。
- 前記第1リチウムコバルト酸化物の粒子の準備段階は、コバルト原料物質及びリチウム原料物質を0.95≦Li/Coモル比<1になるようにする量で混合した後、800℃から1100℃で熱処理して行われるものである請求項12に記載のリチウム二次電池用正極活物質の製造方法。
- 前記2次熱処理は、800℃から1100℃で行われるものである請求項12に記載のリチウム二次電池用正極活物質の製造方法。
- 前記第1リチウムコバルト酸化物に対するコバルト原料物質及びリチウム原料物質の混合時にW、Mo、Zr、Ti、Mg、Ta、Al、Fe、V、Cr、Ba、Ca及びNbからなる群より選択されるいずれか一つまたは2以上の金属元素含有の原料物質を添加する工程をさらに含む請求項12に記載のリチウム二次電池用正極活物質の製造方法。
- 請求項1から11のいずれか一項に記載の正極活物質を含むリチウム二次電池用正極。
- 請求項17に記載の正極を含むリチウム二次電池。
- 請求項18に記載のリチウム二次電池を単位セルで含む電池モジュール。
- 請求項19に記載の電池モジュールを含む電池パック。
- 中大型デバイスの電源として用いられるものである請求項20に記載の電池パック。
- 前記中大型デバイスが、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電気自動車及び電力貯蔵用システムからなる群より選択されるものである請求項21に記載の電池パック。
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