JP6305059B2 - 電極材料の製造方法 - Google Patents
電極材料の製造方法 Download PDFInfo
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- JP6305059B2 JP6305059B2 JP2013528716A JP2013528716A JP6305059B2 JP 6305059 B2 JP6305059 B2 JP 6305059B2 JP 2013528716 A JP2013528716 A JP 2013528716A JP 2013528716 A JP2013528716 A JP 2013528716A JP 6305059 B2 JP6305059 B2 JP 6305059B2
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- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- YQOXCVSNNFQMLM-UHFFFAOYSA-N [Mn].[Ni]=O.[Co] Chemical compound [Mn].[Ni]=O.[Co] YQOXCVSNNFQMLM-UHFFFAOYSA-N 0.000 description 1
- 150000001241 acetals Chemical class 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000003570 air Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- XYLMUPLGERFSHI-UHFFFAOYSA-N alpha-Methylstyrene Chemical compound CC(=C)C1=CC=CC=C1 XYLMUPLGERFSHI-UHFFFAOYSA-N 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 150000004292 cyclic ethers Chemical class 0.000 description 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
- NKDDWNXOKDWJAK-UHFFFAOYSA-N dimethoxymethane Chemical compound COCOC NKDDWNXOKDWJAK-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- UIWXSTHGICQLQT-UHFFFAOYSA-N ethenyl propanoate Chemical compound CCC(=O)OC=C UIWXSTHGICQLQT-UHFFFAOYSA-N 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 125000005677 ethinylene group Chemical group [*:2]C#C[*:1] 0.000 description 1
- KLKFAASOGCDTDT-UHFFFAOYSA-N ethoxymethoxyethane Chemical compound CCOCOCC KLKFAASOGCDTDT-UHFFFAOYSA-N 0.000 description 1
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 description 1
- 229920000840 ethylene tetrafluoroethylene copolymer Polymers 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- 239000006232 furnace black Substances 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 229920001903 high density polyethylene Polymers 0.000 description 1
- 239000004700 high-density polyethylene Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 150000003949 imides Chemical class 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000006233 lamp black Substances 0.000 description 1
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229920001684 low density polyethylene Polymers 0.000 description 1
- 239000004702 low-density polyethylene Substances 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- CRVGTESFCCXCTH-UHFFFAOYSA-N methyl diethanolamine Chemical compound OCCN(C)CCO CRVGTESFCCXCTH-UHFFFAOYSA-N 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 229910001317 nickel manganese cobalt oxide (NMC) Inorganic materials 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 229910052756 noble gas Inorganic materials 0.000 description 1
- 150000002835 noble gases Chemical class 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 150000005677 organic carbonates Chemical class 0.000 description 1
- AHKZTVQIVOEVFO-UHFFFAOYSA-N oxide(2-) Chemical compound [O-2] AHKZTVQIVOEVFO-UHFFFAOYSA-N 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 150000003018 phosphorus compounds Chemical class 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920006267 polyester film Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920001195 polyisoprene Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920005629 polypropylene homopolymer Polymers 0.000 description 1
- 229920002620 polyvinyl fluoride Polymers 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 150000004756 silanes Chemical class 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 1
- 239000006234 thermal black Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- PJANXHGTPQOBST-UHFFFAOYSA-N trans-Stilbene Natural products C=1C=CC=CC=1C=CC1=CC=CC=C1 PJANXHGTPQOBST-UHFFFAOYSA-N 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- PJANXHGTPQOBST-VAWYXSNFSA-N trans-stilbene Chemical group C=1C=CC=CC=1/C=C/C1=CC=CC=C1 PJANXHGTPQOBST-VAWYXSNFSA-N 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/12—Manganates manganites or permanganates
- C01G45/1221—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof
- C01G45/1228—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type [MnO2]n-, e.g. LiMnO2, Li[MxMn1-x]O2
-
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/12—Manganates manganites or permanganates
-
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/12—Manganates manganites or permanganates
- C01G45/1221—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof
- C01G45/1242—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type [Mn2O4]-, e.g. LiMn2O4, Li[MxMn2-x]O4
-
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
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- 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
-
- 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
- C01G53/54—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese of the type [Mn2O4]-, e.g. Li(NixMn2-x)O4, Li(MyNixMn2-x-y)O4
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- H01M4/00—Electrodes
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- 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
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- 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
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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
- H01M4/621—Binders
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/621—Binders
- H01M4/622—Binders being polymers
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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Description
Mは、元素の周期律表の3〜12族の一以上の金属、例えば、Ti、V、Cr、Mn、Fe、Co、Ni、Zn、又はMoであり、好ましくはMn、Co、及びNiであり、
xは1〜2の範囲であり、
yは、2〜4の範囲であり、
zは0.5〜1.5の範囲である。
aは、0〜0.4の範囲であり、tは0〜0.4の範囲であり、
更に、他の変数は上述のように選択される。
R1は、異なっているか好ましくは同一であり、上述のC1−C6−アルキル基から選択され、
R3は、異なっているか好ましくは同一であり、水素、フェニル基、及びC1−C4−アルキル基から選択され、好ましくはメチル基又はエチル基である。
Mは、元素の周期律表の3〜12族の一以上の金属、例えば、Ti、V、Cr、Mn、Fe、Co、Ni、Zn、又はMoであり、好ましくはMn、Co、及びNiであり、
xは1〜2の範囲であり、
yは、2〜4の範囲であり、
zは0.5〜1.5の範囲であり、
複合酸化物の0.01〜1質量%の範囲が+3又は+5の酸化状態のリンに改質される電極材料を提供する。なお、この複合酸化物を、略して「本発明の改質された複合酸化物」とも記載する。
aは、0〜0.4の範囲であり、tは0〜0.4の範囲であり、
更に、他の変数は上述のように選択される。
60〜98質量%、好ましくは70〜96質量%の改質された本発明の複合酸化物と、
1〜20質量%、好ましくは2〜15質量%のバインダと、
1〜25質量%、好ましくは2〜20質量%の導電性炭素含有材料と、
を含む。
Yが、酸素及び硫黄から選択される場合、m=1、
Yが、窒素及びリンから選択される場合、m=2、並びに
Yが、炭素及びケイ素から選択される場合、mは3である。
I.1 リン化合物(P−1)を用いた複合酸化物1.1の処理
スピネル構造を有する10gのLiNi0.5Mn1.5O4を、10gのリン酸トリエチルO=P(OC2H5)3(P−1)に懸濁した。このようにして得られた懸濁液を、窒素下において60℃で1時間撹拌した。次いで、懸濁液をガラスフリットで濾過した。その後、こうして得られた複合酸化物を、回転式チューブ炉内において窒素下で160℃で1時間焼成し、その後、500℃で3時間焼成した。これにより、本発明にしたがって処理された複合酸化物MOx−1を得た。本発明に係る処理された複合酸化物のリン含有量を、0.030質量%と測定した。X線回折測定により、スピネル構造が維持されていたことが示された。
スピネル構造を有する10gのLiNi0.5Mn1.5O4を、10gのリン酸トリエチルO=P(OC2H5)3(P−1)に懸濁した。このようにして得られた懸濁液を、窒素下において60℃で1時間撹拌した。そして、懸濁液を、ロータリーエバポレーターを用いて、約2ミリバールの圧力、及び110℃の加熱浴温度で濃縮乾固した。その後、こうして得られた残留物を、回転式チューブ炉内において窒素下で160℃で1時間焼成し、その後、500℃で3時間焼成した。これにより、本発明にしたがって処理された複合酸化物MOx−1’を得た。本発明に係る処理された複合酸化物MOx−1’のリン含有量を、0.022質量%と測定した。X線回折測定により、スピネル構造が維持されていたことが示された。
スピネル構造を有する10gのLiNi0.5Mn1.5O4を、10gのリン酸トリエチルO=P(OC2H5)3(P−1)に懸濁した。このようにして得られた懸濁液を、窒素下において60℃で1時間撹拌した。次いで、懸濁液をガラスフリットで濾過した。その後、こうして得られた残留物を、マッフル炉内において窒素下で300℃で1時間焼成した。これにより、本発明にしたがって処理された複合酸化物MOx−1’’を得た。本発明に係る処理された複合酸化物MOx−1’’のリン含有量を、0.050質量%と測定した。X線回折測定により、スピネル構造が維持されていたことが示された。
層構造を有する10gのLi(Li0.20Ni0.17Co0.10Mn0.53)O2を、10gのリン酸トリエチルO=P(OC2H5)3(P−1)に懸濁した。このようにして得られた懸濁液を、窒素下において60℃で1時間撹拌した。次いで、懸濁液をガラスフリットで濾過した。その後、こうして得られた残留物を、マッフル炉内において大気下で300℃で1時間焼成した。これにより、本発明にしたがって処理された複合酸化物MOx−2を得た。本発明に係る処理された複合酸化物MOx−2のリン含有量を、0.130質量%と測定した。X線回折測定により、層構造が維持されていたことが示された。
スピネル構造を有する10gのLiNi0.5Mn1.5O4を、12gのエタノールに0.5gのリン酸トリエチルO=P(OC2H5)3(P−1)を溶解させた溶液中で懸濁した。このようにして得られた懸濁液を、窒素下において60℃で1時間撹拌した。次いで、懸濁液を、ロータリーエバポレーターを用いて、70℃の加熱浴温度において初めに約250ミリバールの圧力とし、その後、10ミリバールの圧力として、濃縮乾固した。そして、こうして得られた残留物を、回転式チューブ炉内において窒素下で300℃で1時間焼成し、その後、500℃で3時間焼成した。これにより、本発明にしたがって処理された複合酸化物MOx−1’’’を得た。本発明に係る処理された複合酸化物MOx−1’’’のリン含有量を、0.10質量%と測定した。X線回折測定により、スピネル構造が維持されていたことが示された。
スピネル構造を有する25gのLiNi0.5Mn1.5O4を、投入部及び該投入口に対して180°の位置に排出口を有する2リットルの球状のガラスロータリーに投入した。ガラスロータリー内を乾燥窒素で30分間パージし、その後、120℃となるまで10分間加熱した。そして、ガラスロータリーを1分あたり5回転の速度で回転させた。O=P(CH3)(OCH3)2(P−2)を5体積%の割合で含むガス流を一時間、ロータリー球にポンプで供給した。ガス流量を、1時間あたり10標準リットルのガスが流れるように調整した。その後、得られた粉末を、室温に冷却して熱風乾燥機に送った。そして、熱風乾燥機内において、空気下で、30分間加熱を行い、300℃で2時間の熱処理を行った。これにより、本発明にしたがって処理された複合酸化物MOx−1.1’’’’を得た。本発明に係る処理された複合酸化物MOx−1’’’’のリン含有量を、0.04質量%と測定した。X線回折測定により、スピネル構造が維持されていたことが示された。
使用材料:
導電性炭素含有材料:
炭素材料(C−1):カーボンブラック(62m2/gのBET表面積、Timcal社により「Super P Li」の名称で市販されている)
バインダ(BM.1):粉末状のフッ化ビニリデン及びヘキサフルオロプロペンコポリマー(Arkema 社により「Kynar Flex」(登録商標)の商品名で市販されている)、
試験セルを、本発明(実施例I.6)にしたがい処理された複合酸化物MOx−1.1’’’’から製造された正極材料を用いて製造した。なお、正極材料は、IIと同様にして、炭素材料(C−1)及びポリマーバインダ(BM.1)とともに粉末状にされている。これに対して、比較用セルを、スピネル構造を有する未改質のLiNi0.5Mn1.5O4を用いて同様の方法で製造した。
本発明の電気化学セルEZ.6を、25℃において、4.9V〜3.5Vの間で100サイクル充放電した。充放電電流は、正極材料において150mAh/gであった。100サイクル後の放電容量維持率を測定した。
EZ.6:98.0%
比較例:96.0パーセント
Claims (3)
- 一以上の酸素含有の有機硫黄化合物若しくは有機リン化合物、又は酸素含有の有機硫黄化合物若しくは有機リン化合物の対応するアルカリ金属塩若しくはアンモニウム塩を用いて、カチオンとしてのリチウム及び一以上の遷移金属を含有する複合酸化物を化学的に処理する工程、
を含み、
前記酸素含有の有機リン化合物が、O=P(OR1)3、O=PR3(OR1)2、O=P(R3)2(OR1)、O=P(R3)3、P(OR1)3、PR3(OR1)2から選ばれ、及び
前記酸素含有の有機硫黄化合物が、O2S(OR1)2、O2SR2(OR1)、O2S(R1)2、OS(OR1)2、OSR2(OR1)、OS(R1)2、S(OR1)2、SR2(OR1)、O2S(OR1)OH、O2SR2(OH)、OS(OR1)OH、又はOSR2(OH)から選ばれ、
及びR1は、C1−C6−アルキル基から選択され、
及びR2は、C1−C6−アルキル基から選択され、
R3は、水素、フェニル基、及びC1−C4−アルキル基から選択され、
前記複合酸化物は、一般式(I)、(Ia)及び(Ib)の化合物から選択され、
LizMxOy (I)
Li1+tM1−tO2 (Ia)
Li1+tM2−tO4−a (Ib):
ここで、一般式(I)の変数について、
Mは、元素の周期律表の3〜12族の一以上の金属であり、
xは1〜2の範囲であり、
yは、2〜4の範囲であり、
zは0.5〜1.5の範囲であり、
及び一般式(Ia)、(Ib)の変数について、
aは、0〜0.4の範囲であり、
tは、0〜0.4の範囲であり、
Mは、一般式(I)の定義と同様に定義され、
更に上記工程の後に、以下の工程、
未反応の有機硫黄化合物又は有機リン化合物、任意の副生成物、及び使用された任意の溶媒を除去する工程、
を含み、及び上記工程の後に、以下の工程、
300℃〜500℃で熱処理する工程、
を含み、及び
前記化学的に処理する工程において、前記複合酸化物が、炭素及びポリマーバインダから選択される他の一以上の電極構成成分と混合されて化学的に処理されることを特徴とする電極材料の製造方法。 - 一般式(I)の化合物のMx、及び一般式(Ia)の化合物のM 1−t が、Ni0.33Mn0.33Co0.33、Ni0.5Mn0.3Co0.2、Ni0.4Mn0.2Co0.4、Ni0.22Mn0.66Co0.12、Ni0.4Co0.3Mn0.3、Ni0.45Co0.1Mn0.45、Ni0.4Co0.1Mn0.5、及びNi0.5Co0.1Mn0.4から選択されることを特徴とする請求項1に記載の電極材料の製造方法。
- 前記酸素含有の有機硫黄化合物若しくは有機リン化合物、又はこれらのアルカリ金属塩若しくはアンモニウム塩を用いて、
気相又は液相中において、前記カチオンとしてのリチウム及び一以上の遷移金属を含有する複合酸化物を化学的に処理する請求項1又は2に記載の製造方法。
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