JP6672278B2 - 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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- JP6672278B2 JP6672278B2 JP2017517000A JP2017517000A JP6672278B2 JP 6672278 B2 JP6672278 B2 JP 6672278B2 JP 2017517000 A JP2017517000 A JP 2017517000A JP 2017517000 A JP2017517000 A JP 2017517000A JP 6672278 B2 JP6672278 B2 JP 6672278B2
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- lithium
- active material
- positive electrode
- electrode active
- secondary battery
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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
- 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
- 238000005259 measurement Methods 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- PYLWMHQQBFSUBP-UHFFFAOYSA-N monofluorobenzene Chemical compound FC1=CC=CC=C1 PYLWMHQQBFSUBP-UHFFFAOYSA-N 0.000 description 1
- 150000002823 nitrates Chemical class 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
- 230000001151 other effect Effects 0.000 description 1
- 150000003891 oxalate salts Chemical class 0.000 description 1
- 239000011301 petroleum pitch Substances 0.000 description 1
- 239000011295 pitch Substances 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 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
- 239000001008 quinone-imine dye Substances 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
- 238000007086 side reaction Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000002153 silicon-carbon composite material Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000007581 slurry coating method Methods 0.000 description 1
- 229910021384 soft carbon Inorganic materials 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 239000000243 solution Substances 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
- 238000006277 sulfonation reaction Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 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
- 239000002733 tin-carbon composite material Substances 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
- 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
- 239000011701 zinc Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- PAPBSGBWRJIAAV-UHFFFAOYSA-N ε-Caprolactone Chemical compound O=C1CCCCCO1 PAPBSGBWRJIAAV-UHFFFAOYSA-N 0.000 description 1
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- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
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- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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Description
本出願は、2014年10月2日付韓国特許出願第2014−0133383号及び2015年10月1日付韓国特許出願第2015−0138716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。
本発明は、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に関する。
これに伴い、現在活発に研究/開発されて用いられているリチウム二次電池用正極活物質は層状構造のLiCoO2である。LiCoO2は、合成が容易で、寿命特性を含めた電気化学的性能に優れて最も多く用いられているが、構造的な安定性が低いため、電池の高容量化技術に適用されるには限界がある。
第1リチウムコバルト酸化物を含むコア、及び
前記コアの表面上に位置する表面改質層を含み、
前記表面改質層は、コアの表面上に不連続的に分布するリチウム化合物、及び前記リチウム化合物に接触するか、または隣接して分布するLi/Coのモル比が1未満である第2リチウムコバルト酸化物を含み、そして
前記リチウム化合物は、Ti、W、Zr、Mn、Mg、P、Ni、Al、Sn、V、Cr及びMoからなる群より選択されるいずれか一つまたは2以上のリチウム反応性元素を含むものであるリチウム二次電池用正極活物質を提供する。
第1リチウムコバルト酸化物を含むコア;及び
前記コアの表面上に位置する表面改質層を含み、
前記表面改質層は、コアの表面上に不連続的に分布するリチウム化合物、及び前記リチウム化合物に接触するか、または隣接して分布するLi/Coのモル比が1未満である第2リチウムコバルト酸化物を含み、そして
前記リチウム化合物は、Ti、W、Zr、Mn、Mg、P、Ni、Al、Sn、V、Cr及びMoからなる群より選択されるいずれか一つまたは2以上のリチウム反応性元素を含む。
LiaCoMxO2 (1)
(前記化学式(1)で、Mはドーピング元素としてW、Mo、Zr、Ti、Mg、Ta、Al、Fe、V、Cr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、1≦a≦1.2であり、0≦x≦0.02である。)
Li1−bCoM’yO2 (2)
(前記化学式(2)で、b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<b≦0.05で、0≦y≦0.02であり、M’はドーピング元素として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む)
Li2CO3粉末及びCo3O4粉末を、Li/Coモル比が1.02になるようにする量で混合した後、750℃で20時間の間1次熱処理して第1リチウムコバルト酸化物を製造した。
表面処理剤としてP粉末を、リチウムコバルト酸化物の100重量部に対し0.25重量部の量で用いることを除き、前記製造例1と同様の方法で行って正極活物質を製造した。
表面処理剤としてMn(OH2)を、リチウムコバルト酸化物の100重量部に対し0.3重量部の量で用いることを除き、前記製造例1と同様の方法で行って正極活物質を製造した。
表面処理剤としてAl2O3を、リチウムコバルト酸化物の100重量部に対し0.05重量部の量で用いることを除き、前記製造例1と同様の方法で行って正極活物質を製造した。
Li2CO3粉末及びCo3O4粉末を、Li/Coモル比が1になるようにする量で乾式で混合し、追加的にW2O3粉末を、Li 1モルに対してW金属の含量が0.001モルになるようにする量で添加、混合した後、900℃で20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第2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5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。
Li2TiO3をNMPに溶解させて製造したスラリーにLiCoO2を含浸した後に乾燥し、350℃で熱処理し、表面にLi2TiO3のコーティング層がTi濃度基準0.001重量部の含量で形成されたLiCoO2系負極活物質(平均粒径:12μm)を製造した。
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(TEM)及びエダックス(EDS)を利用して活物質粒子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粒子に対し、アトムプローブトモグラフィー(atom probe tomography、APT)を利用して粒子の表面側におけるリチウムの分布を観察した。その結果を図1に示した。
前記製造例1から4で製造した正極活物質に対するTEM−EDS分析を介し、表面改質層内に生成されたリチウム化合物の種類、及びリチウムと反応した元素の含量を確認した。その結果を下記表2にそれぞれ示した。
前記製造例1で製造した正極活物質において、コアを形成する第1リチウムコバルト酸化物と、表面改質層内に含まれているリチウム欠損の第2リチウムコバルト酸化物とに対し、透過電子回折分析器を利用して結晶構造をそれぞれ観察した。その結果を図2に示した。
前記製造例1及び比較例1で製造した正極活物質を利用してコインセル(Li金属の負極を使用)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3に示した。
前記製造例1及び比較例1で製造した正極活物質を利用してコインセル(Li金属の負極を使用)を製造し、常温(25℃)で0.1C/0.1Cの条件で充放電時に率特性を測定し、その結果を下記図4に示した。
前記実施例1から4、及び比較例1、2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 (21)
- 第1リチウムコバルト酸化物を含むコア、及び
前記コアの表面上に位置する表面改質層を含み、
前記表面改質層は、コアの表面上に不連続的に分布するリチウム化合物、及び前記リチウム化合物に接触するか、または隣接して分布するLi/Coのモル比が1未満である第2リチウムコバルト酸化物を含み、そして
前記リチウム化合物は、Ti、W、Zr、Mn、Mg、P、Ni、Sn、V、Cr及びMoからなる群より選択されるいずれか一つまたは2以上のリチウム反応性元素のリチウム酸化物であるリチウム二次電池用正極活物質。 - 前記リチウム反応性元素は、正極活物質の総重量に対し50ppmから50,000ppmの含量で含まれ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。
- 前記リチウム化合物は、Li2TiO3、Li4Ti5O12、Li3PO4、Li2MnO3、及びLiMn2O4からなる群より選択されるいずれか一つ、またはこれらのうち2以上の混合物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。
- 前記リチウム化合物は、前記コアの表面上にアイランド(island)形態で分布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。
- 前記コアに含まれる前記第1リチウムコバルト酸化物は、下記化学式(1)の化合物を含み、
前記表面改質層に含まれる前記第2リチウムコバルト酸化物は、下記化学式(2)の化合物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。
LiaCoMxO2 (1)
Li1−bCoM’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、Fe、V、Cr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、1≦a≦1.2、0<b≦0.05、0≦x≦0.02及び0≦y≦0.02である。) - 前記第1リチウムコバルト酸化物は、層状結晶構造を有し、
前記第2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。 - 前記コア内リチウムの濃度は、表面改質層内に含まれるリチウムの濃度より高く、
前記コアと表面改質層の界面からコアの中心に行くほど、リチウムが漸進的に増加する濃度勾配で分布し、
前記化学式(1)で、aは、1≦a≦1.2の範囲内でコアの中心に行くほど増加するものである請求項5に記載のリチウム二次電池用正極活物質。 - 前記コア内リチウムの濃度は、表面改質層内に含まれるリチウムの濃度より高く、
前記リチウムは、コア及び表面改質層それぞれの領域内で一つの濃度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。 - 前記コアと表面改質層は、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。
- 3から50μmの平均粒径(D50)を有する単一構造体のものである請求項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1≦Li/Coモル比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を製造する段階;及び
前記第1リチウムコバルト酸化物を、リチウム反応性元素を含む表面処理剤と混合した後、2次熱処理して前記第1リチウムコバルト酸化物の表面上に位置する表面改質層を形成する段階を含み、
前記表面改質層は、前記第1リチウムコバルト酸化物の表面上に不連続的に分布するリチウム化合物、及び前記リチウム化合物に接触するか、または隣接して分布するLi/Coのモル比が1未満である第2リチウムコバルト酸化物を含み、
前記リチウム化合物は、Ti、W、Zr、Mn、Mg、P、Ni、Sn、V、Cr及びMoからなる群より選択されるいずれか一つまたは2以上のリチウム反応性元素のリチウム酸化物である、リチウム二次電池用正極活物質の製造方法。 - 前記表面処理剤は、正極活物質内のリチウム反応性金属の含量が50から50,000ppmになるようにする量で用いら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1次熱処理は、750℃から900℃の温度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2次熱処理は、400℃から1100℃の温度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。
- 請求項1から請求項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16に記載の正極を含むリチウム二次電池。
- 請求項17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18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19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20に記載の電池パック。
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