JP2022513681A - 正極活物質、前記正極活物質を含む正極及びリチウム二次電池 - Google Patents
正極活物質、前記正極活物質を含む正極及びリチウム二次電池 Download PDFInfo
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- JP2022513681A JP2022513681A JP2021531030A JP2021531030A JP2022513681A JP 2022513681 A JP2022513681 A JP 2022513681A JP 2021531030 A JP2021531030 A JP 2021531030A JP 2021531030 A JP2021531030 A JP 2021531030A JP 2022513681 A JP2022513681 A JP 2022513681A
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- Prior art keywords
- positive electrode
- active material
- electrode active
- nickel
- lithium
- Prior art date
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- 239000007774 positive electrode material Substances 0.000 title claims abstract description 118
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 66
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 61
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 93
- 229910021437 lithium-transition metal oxide Inorganic materials 0.000 claims abstract description 54
- KFDQGLPGKXUTMZ-UHFFFAOYSA-N [Mn].[Co].[Ni] Chemical compound [Mn].[Co].[Ni] KFDQGLPGKXUTMZ-UHFFFAOYSA-N 0.000 claims abstract description 52
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 47
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 27
- 229910052751 metal Inorganic materials 0.000 claims abstract description 26
- 239000000126 substance Substances 0.000 claims abstract description 19
- 239000002184 metal Substances 0.000 claims abstract description 16
- 229910052796 boron Inorganic materials 0.000 claims abstract description 13
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 11
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 11
- 229910052742 iron Inorganic materials 0.000 claims abstract description 11
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 11
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 11
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 11
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 9
- 229910052785 arsenic Inorganic materials 0.000 claims abstract description 8
- 229910052793 cadmium Inorganic materials 0.000 claims abstract description 8
- 229910052737 gold Inorganic materials 0.000 claims abstract description 8
- 229910052738 indium Inorganic materials 0.000 claims abstract description 8
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 8
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 26
- 239000002245 particle Substances 0.000 claims description 12
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 11
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 11
- 239000006227 byproduct Substances 0.000 claims description 3
- -1 lithium transition metal Chemical class 0.000 abstract description 26
- 229910052723 transition metal Inorganic materials 0.000 abstract description 21
- 238000004519 manufacturing process Methods 0.000 abstract description 16
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- 230000000052 comparative effect Effects 0.000 description 24
- 239000010936 titanium Substances 0.000 description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 22
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- 229910017052 cobalt Inorganic materials 0.000 description 18
- 239000010941 cobalt Substances 0.000 description 18
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 18
- 239000011572 manganese Substances 0.000 description 18
- 238000000034 method Methods 0.000 description 18
- 239000000203 mixture Substances 0.000 description 18
- 239000007773 negative electrode material Substances 0.000 description 17
- 150000003624 transition metals Chemical class 0.000 description 17
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 16
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical group [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 16
- 239000007864 aqueous solution Substances 0.000 description 16
- 239000010410 layer Substances 0.000 description 16
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- 239000011777 magnesium Substances 0.000 description 12
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 10
- 239000011248 coating agent Substances 0.000 description 10
- 229910052799 carbon Inorganic materials 0.000 description 9
- 239000008151 electrolyte solution Substances 0.000 description 9
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- 239000011701 zinc Substances 0.000 description 9
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 8
- 239000011247 coating layer Substances 0.000 description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 229910052802 copper Inorganic materials 0.000 description 7
- 239000010949 copper Substances 0.000 description 7
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- SOXUFMZTHZXOGC-UHFFFAOYSA-N [Li].[Mn].[Co].[Ni] Chemical compound [Li].[Mn].[Co].[Ni] SOXUFMZTHZXOGC-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
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- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 6
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 5
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- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
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- IPZJQDSFZGZEOY-UHFFFAOYSA-N dimethylmethylene Chemical compound C[C]C IPZJQDSFZGZEOY-UHFFFAOYSA-N 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 150000004862 dioxolanes Chemical class 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
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- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Chemical group CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 239000004210 ether based solvent Substances 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
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- 229920001519 homopolymer Polymers 0.000 description 1
- 239000001863 hydroxypropyl cellulose Substances 0.000 description 1
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 239000003273 ketjen black Substances 0.000 description 1
- 239000005453 ketone based solvent Substances 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 description 1
- 229910002102 lithium manganese oxide Inorganic materials 0.000 description 1
- 229910000686 lithium vanadium 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
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 description 1
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- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
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- 238000002156 mixing Methods 0.000 description 1
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- 150000002823 nitrates Chemical class 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
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- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- CIBMHJPPKCXONB-UHFFFAOYSA-N propane-2,2-diol Chemical compound CC(C)(O)O CIBMHJPPKCXONB-UHFFFAOYSA-N 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
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- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 239000001008 quinone-imine dye Substances 0.000 description 1
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- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
- PAPBSGBWRJIAAV-UHFFFAOYSA-N ε-Caprolactone Chemical compound O=C1CCCCCO1 PAPBSGBWRJIAAV-UHFFFAOYSA-N 0.000 description 1
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- C01G53/50—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese of the type [MnO2]n-, e.g. Li(NixMn1-x)O2, Li(MyNixMn1-x-y)O2
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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Abstract
Description
本出願は、2018年11月30日付韓国特許出願第10-2018-0152743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。
本発明による二次電池用正極活物質は、リチウムを除いた金属の総モル数に対して、60モル%以上のニッケルを含むニッケル-コバルト-マンガン系リチウム遷移金属酸化物を含み、前記ニッケル-コバルト-マンガン系リチウム遷移金属酸化物は、ドーピング元素M1(前記ドーピング元素M1は、Alを含む金属元素である)及びドーピング元素M2(前記ドーピング元素M2は、Mg、La、Ti、Zn、B、W、Ni、Co、Fe、Cr、V、Ru、Cu、Cd、Ag、Y、Sc、Ga、In、As、Sb、Pt、Au及びSiからなる群から選択された1種以上の金属元素である)によりドーピングされたものであり、前記ニッケル-コバルト-マンガン系リチウム遷移金属酸化物は、ドーピング元素M1を100から10,000ppmで含み、ドーピング元素M1及びM2が50:50から99:1の重量比で含まれたものである。
Li1+a[NixCoyMnzM1 wM2 v]O2
前記化学式1中、前記M1は、ニッケル-コバルト-マンガン系リチウム遷移金属酸化物内の遷移金属サイト(site)に置換されたドーピング元素であり、Alを含む金属元素であってよい。
1.0≦(A1/A0)≦1.8
前記式1中、前記A1は、前記正極活物質を相対湿度(Relative Humidity、RH)60%、25℃の環境で1日間放置した後に測定した正極活物質の表面に存在する炭酸リチウムの含量であり、前記A0は、正極活物質の前記放置前に測定した正極活物質の表面に存在する炭酸リチウムの初期含量である。
一方、前記正極活物質は、市販のニッケル-コバルト-マンガン系リチウム遷移金属酸化物を購入して用いるか、当該技術分野で知られているニッケル-コバルト-マンガン系リチウム遷移金属酸化物の製造方法により製造されたものであってよい。
次に、本発明によるリチウム二次電池用正極に対して説明する。
また、本発明は、前記正極を含む電気化学素子を製造できる。前記電気化学素子は、具体的に、電池、キャパシター等であってよく、より具体的には、リチウム二次電池であってよい。
実施例1
NiSO4、CoSO4、MnSO4、AlCl3、MgCl2、TiCl4及びLaCl3を、ニッケル:コバルト:マンガン:アルミニウム:マグネシウム:ランタニウム:チタニウムのモル比が8:1:1:0.03:0.004:0.004:0.002となる量でイオン交換水の中に溶かし、0.01Mの遷移金属水溶液を準備した。
NiSO4、CoSO4、MnSO4、AlCl3及びMgCl2をニッケル:コバルト:マンガン:アルミニウム:マグネシウムのモル比が8:1:1:0.03:0.004となる量でイオン交換水の中に溶かして遷移金属水溶液を準備し、これを用いることを除いては、前記実施例1と同一の方法で正極活物質を製造した。
NiSO4、CoSO4、MnSO4、AlCl3及びLaCl3をニッケル:コバルト:マンガン:アルミニウム:ランタニウムのモル比が8:1:1:0.03:0.002となる量でイオン交換水の中に溶かして遷移金属水溶液を準備し、これを用いることを除いては、前記実施例1と同一の方法で正極活物質を製造した。
NiSO4、CoSO4、MnSO4、AlCl3及びTiCl4をニッケル:コバルト:マンガン:アルミニウム:チタニウムのモル比が8:1:1:0.03:0.004となる量でイオン交換水の中に溶かして遷移金属水溶液を準備し、これを用いることを除いては、前記実施例1と同一の方法で正極活物質を製造した。
NiSO4、CoSO4、MnSO4、AlCl3、MgCl2及びLaCl3をニッケル:コバルト:マンガン:アルミニウム:マグネシウム:ランタニウムのモル比が8:1:1:0.03:0.004:0.002となる量でイオン交換水の中に溶かして遷移金属水溶液を準備し、これを用いることを除いては、前記実施例1と同一の方法で正極活物質を製造した。
NiSO4、CoSO4、MnSO4、AlCl3、MgCl2及びTiCl4をニッケル:コバルト:マンガン:アルミニウム:マグネシウム:チタニウムのモル比が8:1:1:0.03:0.004:0.004となる量でイオン交換水の中に溶かして遷移金属水溶液を準備し、これを用いることを除いては、前記実施例1と同一の方法で正極活物質を製造した。
NiSO4、CoSO4、MnSO4、AlCl3、TiCl4及びLaCl3をニッケル:コバルト:マンガン:アルミニウム:チタニウム:ランタニウムのモル比が8:1:1:0.03:0.004:0.002となる量でイオン交換水の中に溶かして遷移金属水溶液を準備し、これを用いることを除いては、前記実施例1と同一の方法で正極活物質を製造した。
NiSO4、CoSO4及びMnSO4をニッケル:コバルト:マンガンのモル比が8:1:1となる量でイオン交換水の中に溶かして遷移金属水溶液を準備し、これを用いることを除いては、前記実施例1と同一の方法で正極活物質を製造した。
NiSO4、CoSO4、MnSO4及びAlCl3をニッケル:コバルト:マンガン:アルミニウムのモル比が8:1:1:0.03となる量でイオン交換水の中に溶かして遷移金属水溶液を準備し、これを用いることを除いては、前記実施例1と同一の方法で正極活物質を製造した。
NiSO4、CoSO4、MnSO4、MgCl2、TiCl4及びLaCl3をニッケル:コバルト:マンガン:マグネシウム:ランタニウム:チタニウムのモル比が8:1:1:0.004:0.004:0.002となる量でイオン交換水の中に溶かして遷移金属水溶液を準備し、これを用いることを除いては、前記実施例1と同一の方法で正極活物質を製造した。
NiSO4、CoSO4、MnSO4、AlCl3、MgCl2、TiCl4及びLaCl3をニッケル:コバルト:マンガン:アルミニウム:マグネシウム:ランタニウム:チタニウムのモル比が8:1:1:0.01:0.01:0.01:0.01となる量でイオン交換水の中に溶かして0.01Mの遷移金属水溶液を準備し、これを用いることを除いては、前記実施例1と同一の方法で正極活物質を製造した。
前記実施例1~7及び比較例1~4で製造した正極活物質の吸湿量を評価した。
実施例1~6及び比較例1、2、4で製造した正極活物質の表面に存在する残留リチウムの含量を測定するため、pH meterとしてpH metromhを用いて、pH滴定(pH titration)を行った。具体的に、実施例1~7及び比較例1~4で製造した正極活物質粉末10gと、蒸溜水100mLを撹拌した。前記溶液に0.1NのHCl溶液を加えながら、pH滴定を行った。
前記実施例1~3、5、比較例1~4で製造した正極活物質を用いてリチウム二次電池を製造した後、前記二次電池の容量特性を比べた。
実施例1~6及び比較例1、2、4で製造した正極活物質の表面に存在する残留リチウムの含量を測定するため、pH meterとしてpH metromhを用いて、pH滴定(pH titration)を行った。具体的に、実施例1~6及び比較例1、2、4で製造した正極活物質粉末10gと、蒸溜水100mLを撹拌した。前記溶液に0.1NのHCl溶液を加えながら、pH滴定を行った。
Claims (9)
- リチウムを除いた金属の総モル数に対して、60モル%以上のニッケルを含むニッケル-コバルト-マンガン系リチウム遷移金属酸化物を含み、
前記ニッケル-コバルト-マンガン系リチウム遷移金属酸化物は、ドーピング元素M1(前記ドーピング元素M1は、Alを含む金属元素である)及びドーピング元素M2(前記ドーピング元素M2は、Mg、La、Ti、Zn、B、W、Ni、Co、Fe、Cr、V、Ru、Cu、Cd、Ag、Y、Sc、Ga、In、As、Sb、Pt、Au及びSiからなる群から選択された1種以上の金属元素である)によりドーピングされたものであり、
前記ニッケル-コバルト-マンガン系リチウム遷移金属酸化物は、ドーピング元素M1を100から10,000ppmで含み、
ドーピング元素M1及びM2が50:50から99:1の重量比で含まれている、正極活物質。 - 前記リチウム遷移金属酸化物は、下記化学式1で表されるものである、請求項1に記載の正極活物質。
[化学式1]
Li1+a[NixCoyMnzM1 wM2 v]O2
前記化学式1中、
M1は、Alを含む金属元素であり、
M2は、Mg、La、Ti、Zn、B、W、Ni、Co、Fe、Cr、V、Ru、Cu、Cd、Ag、Y、Sc、Ga、In、As、Sb、Pt、Au及びSiからなる群から選択された1種以上の金属元素であり、
0≦a≦0.3、0.60≦x<1、0<y<0.35、0<z<0.35、0<w≦0.01、0<v≦0.005である。 - 前記M2は、Mg、La、及びTiからなる群から選択された1種以上の金属元素である、請求項1に記載の正極活物質。
- 前記化学式1中、w≧vであり、1≦w/v≦15である、請求項2に記載の正極活物質。
- 前記正極活物質は、下記式1を満たすものである、請求項1に記載の正極活物質。
[式1]
1.0≦(A1/A0)≦1.8
前記A1は、前記正極活物質を相対湿度(Relative Humidity、RH)60%、25℃の環境で1日間放置した後に測定した正極活物質の表面に存在する炭酸リチウムの含量であり、前記A0は、正極活物質の前記放置前に測定した正極活物質の表面に存在する炭酸リチウムの初期含量である。 - 前記正極活物質を相対湿度(Relative Humidity、RH)60%、25℃の環境で1日間放置した後に前記正極活物質の表面に存在する水酸化リチウム及び炭酸リチウムのうち少なくとも何れか一つを含むリチウム副産物の総含量は、正極活物質の総重量100重量部に対して0.5重量部以下である、請求項5に記載の正極活物質。
- 前記正極活物質の平均粒径(D50)は、8から15μmである、請求項1に記載の正極活物質。
- 正極集電体、前記正極集電体上に形成される正極活物質層を含み、
前記正極活物質層は、請求項1から請求項7の何れか一項に記載の正極活物質を含むものである、正極。 - 請求項8に記載の正極を含むリチウム二次電池。
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