JP2021520041A - 正極活物質の洗浄方法、それを含む正極活物質の製造方法、及びそれにより製造された正極活物質 - Google Patents
正極活物質の洗浄方法、それを含む正極活物質の製造方法、及びそれにより製造された正極活物質 Download PDFInfo
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- JP2021520041A JP2021520041A JP2020560153A JP2020560153A JP2021520041A JP 2021520041 A JP2021520041 A JP 2021520041A JP 2020560153 A JP2020560153 A JP 2020560153A JP 2020560153 A JP2020560153 A JP 2020560153A JP 2021520041 A JP2021520041 A JP 2021520041A
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- positive electrode
- active material
- electrode active
- transition metal
- metal oxide
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- 229910021385 hard carbon Inorganic materials 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000012535 impurity Substances 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
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 239000003273 ketjen black Substances 0.000 description 1
- 150000004715 keto acids Chemical class 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000006233 lamp black Substances 0.000 description 1
- 238000007561 laser diffraction method Methods 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910000625 lithium cobalt 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
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000011302 mesophase pitch Substances 0.000 description 1
- 239000002905 metal composite material Substances 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
- 150000002825 nitriles Chemical class 0.000 description 1
- 150000005181 nitrobenzenes Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229920005569 poly(vinylidene fluoride-co-hexafluoropropylene) Polymers 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 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
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- CIBMHJPPKCXONB-UHFFFAOYSA-N propane-2,2-diol Chemical compound CC(C)(O)O CIBMHJPPKCXONB-UHFFFAOYSA-N 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-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
- 238000012827 research and development Methods 0.000 description 1
- 238000000926 separation method 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
- 229910021384 soft carbon Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 229920005608 sulfonated EPDM Polymers 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000002335 surface treatment layer Substances 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
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000002733 tin-carbon composite material Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- BDZBKCUKTQZUTL-UHFFFAOYSA-N triethyl phosphite Chemical compound CCOP(OCC)OCC BDZBKCUKTQZUTL-UHFFFAOYSA-N 0.000 description 1
- RIUWBIIVUYSTCN-UHFFFAOYSA-N trilithium borate Chemical compound [Li+].[Li+].[Li+].[O-]B([O-])[O-] RIUWBIIVUYSTCN-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 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
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/40—Nickelates
- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
- C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
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- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- H01M4/02—Electrodes composed of, or comprising, active material
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- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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Abstract
Description
本出願は、2018年5月4日付け韓国特許出願第10−2018−0051714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た全ての内容は本明細書の一部として含まれる。
(1)Ni、Co、及びMnを含み、Ni組成が60モル%以上のリチウム複合遷移金属酸化物を準備する段階と、
(2)前記リチウム複合遷移金属酸化物を水に投入する段階と、
(3)前記リチウム複合遷移金属酸化物が投入された水に弱酸を添加し、pHを7から10の範囲に調節する段階と、を含む、正極活物質の洗浄方法を提供する。
(1)Ni、Co、及びMnを含み、Ni組成が60モル%以上のリチウム複合遷移金属酸化物を準備する段階と、
(2)前記リチウム複合遷移金属酸化物を水に投入する段階と、
(3)前記リチウム複合遷移金属酸化物が投入された水に弱酸を添加し、pHを7から10の範囲に調節する段階と、を含む。
段階(1)では、Ni、Co、及びMnを含み、Ni組成が60モル%以上のリチウム複合遷移金属酸化物を準備する。
LiNiaCobMncMdO2
(a≧0.6であり、0<b<0.25、0<c<0.25、0≦d≦0.2、a+b+c+d=1であり、Mは、W、Cu、Fe、V、Cr、Ti、Zr、Zn、Al、In、Ta、Y、In、La、Sr、Ga、Sc、Gd、Sm、Ca、Ce、Nb、Mg、B、及びMoからなる群から選択される1種以上のドーピング元素である)
段階(2)では、前記リチウム複合遷移金属酸化物の洗浄のために、水にこれを投入する。
前記リチウム複合遷移金属酸化物を水に投入した後には、これに弱酸を添加してpHを7から10の範囲に調節する。
50gのNMC(811)正極活物質を50gの水に浸して2分間掻きまぜた後、10%(w/w)P2O5水溶液をpH7になるまで1.25g投入した。これを2分間さらに掻きまぜた後、減圧フィルターを用いて2分間水を除去してから真空オーブンで乾燥し、前記正極活物質の洗浄を完了した。
前記実施例1で水の量を25gに変更したことを除いては、実施例1と同一の方法により正極活物質の洗浄を完了した。
前記実施例1で10%(w/w)P2O5水溶液をpH9になるまで0.75g投入したことを除いては、実施例1と同一の方法により正極活物質の洗浄を完了した。
50gのNMC(811)正極活物質を50gの水に浸して2分間掻きまぜた後、20%(w/w)P2O5水溶液をpH7になるまで投入した。これを5分間さらに掻きまぜた後、減圧フィルターを用いて2分間水を除去してから真空オーブンで乾燥し、前記正極活物質の洗浄を完了した。
前記実施例1で10%(w/w)P2O5水溶液の代わりに0.1モル%のクエン酸(C6H8O7)水溶液をpH7になるまで投入したことを除いては、実施例1と同一の方法により正極活物質の洗浄を完了した。
50gのNMC(811)正極活物質を50gの水に浸して5分間掻きまぜた後、減圧フィルターを用いて2分間水を除去してから真空オーブンで乾燥し、前記正極活物質の洗浄を完了した。
50gのNMC(811)正極活物質を25gの水に浸して5分間掻きまぜた後、減圧フィルターを用いて2分間水を除去してから真空オーブンで乾燥し、前記正極活物質の洗浄を完了した。
50gのNMC(811)正極活物質を50gの水に浸して2分間掻きまぜた後、20%(w/v)HCl水溶液をpH7になるまで投入した。これを5分間さらに掻きまぜた後、減圧フィルターを用いて2分間水を除去してから真空オーブンで乾燥し、前記正極活物質の洗浄を完了した。
50gのNMC(811)正極活物質を50gの水に浸して2分間掻きまぜた後、3%(w/v)HCl水溶液をpH7になるまで投入した。これを5分間さらに掻きまぜた後、減圧フィルターを用いて2分間水を除去してから真空オーブンで乾燥し、前記正極活物質の洗浄を完了した。
前記実施例1から5及び比較例1から4でそれぞれ洗浄が完了した正極活物質に対し、Mettler Toledo社製の888 titrando機器を用いてOH−イオンとCO3 2−イオンの量を滴定するワルダー滴定(Warder titration)方法によりリチウム副産物の含量を測定し、下記表1に示した。
前記実施例1から5及び比較例1から4でそれぞれ洗浄が完了した正極活物質を、導電材としてカーボンブラック(carbon black)及びバインダーとしてポリビニリデンジフルオリド(PVdF)と、97.5:1:1.5の重量比で溶媒であるN−メチル−2−ピロリドン(NMP)に添加し、正極スラリーをそれぞれ製造した。
前記実験例2で製造された実施例4及び比較例3でそれぞれ洗浄が完了した正極活物質を用いて製造されたコイン型の半電池を、45℃で0.33Cに充電・放電して放電容量を測定し、また、放電60秒間の電圧降下を測定してセル抵抗を測定した。これを1から50サイクル繰り返し行い、その結果を下記表3に示した。
Claims (14)
- (1)Ni、Co、及びMnを含み、Ni組成が60モル%以上のリチウム複合遷移金属酸化物を準備する段階と、
(2)前記リチウム複合遷移金属酸化物を水に投入する段階と、
(3)前記リチウム複合遷移金属酸化物が投入された水に弱酸を添加し、pHを7から10の範囲に調節する段階と、を含む正極活物質の洗浄方法。 - 前記リチウム複合遷移金属酸化物は、Ni、Co、及びMnを含み、Ni組成が80モル%以上である、請求項1に記載の正極活物質の洗浄方法。
- 前記リチウム複合遷移金属酸化物は、下記化学式1で表される、請求項1に記載の正極活物質の洗浄方法。
[化学式1]
LiNiaCobMncMdO2
(a≧0.6であり、0<b<0.25、0<c<0.25、0≦d≦0.2、a+b+c+d=1であり、Mは、W、Cu、Fe、V、Cr、Ti、Zr、Zn、Al、In、Ta、Y、In、La、Sr、Ga、Sc、Gd、Sm、Ca、Ce、Nb、Mg、B、及びMoからなる群から選択される1種以上のドーピング元素である) - 前記段階(2)において、前記水の含量は、前記リチウム複合遷移金属酸化物100重量部を基準に30重量部から150重量部である、請求項1から3のいずれか一項に記載の正極活物質の洗浄方法。
- 前記弱酸は、五酸化リン(P2O5)、リン酸、酢酸、シュウ酸、クエン酸及びホウ酸からなる群から選択された1種以上である、請求項1から4のいずれか一項に記載の正極活物質の洗浄方法。
- 前記弱酸を添加する過程は、五酸化リン(P2O5)粉末、クエン酸粉末、又はこれらの混合物を前記リチウム複合遷移金属酸化物が投入された水に投入して行われる、請求項1から4のいずれか一項に記載の正極活物質の洗浄方法。
- 請求項1から6のいずれか一項に記載の正極活物質の洗浄方法を含む、正極活物質の製造方法。
- リチウム複合遷移金属酸化物の表面にコーティング層を形成する段階をさらに含む、請求項7に記載の正極活物質の製造方法。
- リチウム複合遷移金属酸化物及び前記リチウム複合遷移金属酸化物の表面に存在するリチウム副産物を含み、
前記リチウム副産物は、前記リチウム複合遷移金属酸化物の全体モル数を基準に0.3モル%から0.41モル%で含まれ、Li2CO3及びLiOHを1:1.8から1:3のモル比で含む、正極活物質。 - 前記リチウム複合遷移金属酸化物は、表面に前記リチウム複合遷移金属酸化物の全体モル数を基準に0.05モル%から0.14モル%のLi2CO3を含む、請求項9に記載の正極活物質。
- 前記リチウム複合遷移金属酸化物は、表面に前記リチウム複合遷移金属酸化物の全体モル数を基準に0.15モル%から0.27モル%のLiOHを含む、請求項9または10に記載の正極活物質。
- 前記正極活物質は、前記リチウム複合遷移金属酸化物の表面に1種以上の金属元素又は半金属元素を含むコーティング層を含む、請求項9から11のいずれか一項に記載の正極活物質。
- 請求項9から12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13に記載のリチウム二次電池用正極を含むリチウム二次電池。
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