JP2022543762A - 二次電池用正極活物質の製造方法 - Google Patents
二次電池用正極活物質の製造方法 Download PDFInfo
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- JP2022543762A JP2022543762A JP2022505618A JP2022505618A JP2022543762A JP 2022543762 A JP2022543762 A JP 2022543762A JP 2022505618 A JP2022505618 A JP 2022505618A JP 2022505618 A JP2022505618 A JP 2022505618A JP 2022543762 A JP2022543762 A JP 2022543762A
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- Prior art keywords
- active material
- additive
- positive electrode
- electrode active
- lithium
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- 239000007774 positive electrode material Substances 0.000 title claims abstract description 64
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims description 16
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 99
- 239000000654 additive Substances 0.000 claims abstract description 87
- 230000000996 additive effect Effects 0.000 claims abstract description 74
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 56
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 55
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 41
- 238000010304 firing Methods 0.000 claims abstract description 40
- 239000002243 precursor Substances 0.000 claims abstract description 28
- 150000001875 compounds Chemical class 0.000 claims abstract description 20
- 239000011572 manganese Substances 0.000 claims abstract description 16
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 12
- 239000010941 cobalt Substances 0.000 claims abstract description 12
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 claims abstract description 12
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910021437 lithium-transition metal oxide Inorganic materials 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 11
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims abstract description 7
- 150000002739 metals Chemical class 0.000 claims abstract description 7
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052796 boron Inorganic materials 0.000 claims abstract description 5
- 238000005245 sintering Methods 0.000 claims description 50
- 239000002245 particle Substances 0.000 claims description 32
- 239000006182 cathode active material Substances 0.000 claims description 26
- -1 NaCO3 Chemical compound 0.000 claims description 22
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 18
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- 239000002994 raw material Substances 0.000 claims description 9
- 238000001354 calcination Methods 0.000 claims description 7
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims description 7
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
- 239000001095 magnesium carbonate Substances 0.000 claims description 5
- 235000014380 magnesium carbonate Nutrition 0.000 claims description 5
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 5
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 5
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 claims description 3
- 235000010216 calcium carbonate Nutrition 0.000 claims description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 3
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 claims description 3
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 3
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 3
- 238000010298 pulverizing process Methods 0.000 claims description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 2
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims 2
- 230000000052 comparative effect Effects 0.000 description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 18
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- 239000002131 composite material Substances 0.000 description 15
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- 229910000314 transition metal oxide Inorganic materials 0.000 description 12
- 239000004020 conductor Substances 0.000 description 11
- 239000000463 material Substances 0.000 description 11
- 239000011163 secondary particle Substances 0.000 description 10
- 239000002904 solvent Substances 0.000 description 10
- 239000011230 binding agent Substances 0.000 description 9
- 239000007773 negative electrode material Substances 0.000 description 8
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- 239000010408 film Substances 0.000 description 7
- 239000011164 primary particle Substances 0.000 description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- 239000003960 organic solvent Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 5
- 229920001577 copolymer Polymers 0.000 description 5
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 229910001416 lithium ion Inorganic materials 0.000 description 5
- 229910003002 lithium salt Inorganic materials 0.000 description 5
- 159000000002 lithium salts Chemical class 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 4
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 4
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- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 4
- 229910002651 NO3 Inorganic materials 0.000 description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 4
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- 150000004820 halides Chemical class 0.000 description 4
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- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 3
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- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 239000004698 Polyethylene Substances 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 3
- KFDQGLPGKXUTMZ-UHFFFAOYSA-N [Mn].[Co].[Ni] Chemical compound [Mn].[Co].[Ni] KFDQGLPGKXUTMZ-UHFFFAOYSA-N 0.000 description 3
- 229910021383 artificial graphite Inorganic materials 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000003660 carbonate based solvent Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
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- 229910052723 transition metal Inorganic materials 0.000 description 3
- 150000003624 transition metals Chemical class 0.000 description 3
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
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- SEVNKUSLDMZOTL-UHFFFAOYSA-H cobalt(2+);manganese(2+);nickel(2+);hexahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mn+2].[Co+2].[Ni+2] SEVNKUSLDMZOTL-UHFFFAOYSA-H 0.000 description 2
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- AMXOYNBUYSYVKV-UHFFFAOYSA-M lithium bromide Chemical compound [Li+].[Br-] AMXOYNBUYSYVKV-UHFFFAOYSA-M 0.000 description 2
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- 150000005678 chain carbonates Chemical class 0.000 description 1
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- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 description 1
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 description 1
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- 150000004862 dioxolanes Chemical class 0.000 description 1
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
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- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical class [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 1
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- 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
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- VLXXBCXTUVRROQ-UHFFFAOYSA-N lithium;oxido-oxo-(oxomanganiooxy)manganese Chemical compound [Li+].[O-][Mn](=O)O[Mn]=O VLXXBCXTUVRROQ-UHFFFAOYSA-N 0.000 description 1
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- PPNAOCWZXJOHFK-UHFFFAOYSA-N manganese(2+);oxygen(2-) Chemical class [O-2].[Mn+2] PPNAOCWZXJOHFK-UHFFFAOYSA-N 0.000 description 1
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- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 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
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- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- BDZBKCUKTQZUTL-UHFFFAOYSA-N triethyl phosphite Chemical compound CCOP(OCC)OCC BDZBKCUKTQZUTL-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
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- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- PAPBSGBWRJIAAV-UHFFFAOYSA-N ε-Caprolactone Chemical compound O=C1CCCCCO1 PAPBSGBWRJIAAV-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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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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- H01M4/525—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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Abstract
Description
本発明は、二次電池用正極活物質の製造方法に関する。
本発明は、ニッケル、コバルト、およびマンガンを含み、全金属中でニッケルを60モル%以上含有する正極活物質前駆体を用意するステップと、前記正極活物質前駆体、リチウム原料ソース、第1焼成添加剤、第2焼成添加剤、および第3焼成添加剤を混合し、一次焼成してリチウム遷移金属酸化物を形成するステップと含み、前記第1焼成添加剤はリチウム含有化合物であり、前記第2焼成添加剤は炭酸イオン含有化合物であり、前記第3焼成添加剤はボロン含有化合物であることを特徴とする、正極活物質の製造方法を提供する。
先ず、ニッケル(Ni)、コバルト(Co)、およびマンガン(Mn)を含み、全金属中でニッケル(Ni)で60モル%以上含有する正極活物質前駆体を用意する。
[化学式1]
[NiaCobMncMd](OH)2
例えば、前記ニッケル-コバルト-マンガン前駆体は、ニッケル含有原料物質、コバルト含有原料物質、およびマンガン含有原料物質を含む遷移金属溶液に、アンモニウムカチオン含有錯体形成剤および塩基性化合物を添加し共沈反応させて製造されてもよい。
一方、前記共沈反応は、窒素またはアルゴンなどの不活性雰囲気下で、40℃~70℃の温度で行われてもよい。
前記リチウム原料ソースとしては、リチウム含有硫酸塩、硝酸塩、酢酸塩、炭酸塩、シュウ酸塩、クエン酸塩、ハライド、水酸化物、またはオキシ水酸化物などが用いられてもよく、水に溶解可能な限り、特に限定されない。具体的に、前記リチウムソースは、Li2CO3、LiNO3、LiNO2、LiOH、LiOH・H2O、LiH、LiF、LiCl、LiBr、LiI、CH3COOLi、Li2O、Li2SO4、CH3COOLi、またはLi3C6H5O7などであってもよく、これらの何れか1つまたは2つ以上の混合物が用いられてもよい。
前記焼成は、大気(Air)または酸素(O2)雰囲気下で行ってもよい。
前記粉砕および水洗は、特に制限されず、性能が劣化しない範囲内で、当該技術分野で周知の方法により行われてもよい。
本発明の他の一実施形態によると、上記のように製造された正極活物質を含む二次電池用正極およびリチウム二次電池を提供する。
具体的に、前記正極は、正極集電体と、前記正極集電体上に形成され、前記正極活物質を含む正極活物質層とを含む。
この際、前記導電材は、電極に導電性を付与するために用いられるものであり、構成される電池において、化学変化を引き起こさず電子伝導性を有するものであれば特に制限されずに使用可能である。具体的な例としては、天然黒鉛や人造黒鉛などの黒鉛;カーボンブラック、アセチレンブラック、ケッチェンブラック、チャンネルブラック、ファーネスブラック、ランプブラック、サーマルブラック、炭素繊維などの炭素系物質;銅、ニッケル、アルミニウム、銀などの金属粉末または金属繊維;酸化亜鉛、チタン酸カリウムなどの導電性ウィスカー;酸化チタンなどの導電性金属酸化物;またはポリフェニレン誘導体などの導電性高分子などが挙げられ、この中の1種の単独または2種以上の混合物が用いられてもよい。前記導電材は、通常、正極活物質層の総重量に対して1~30重量%で含まれてもよい。
前記負極集電体は、電池に化学的変化を誘発せず且つ高い導電性を有するものであれば特に制限されず、例えば、銅、ステンレススチール、アルミニウム、ニッケル、チタン、焼成炭素、銅やステンレススチールの表面に炭素、ニッケル、チタン、銀などで表面処理したもの、アルミニウム‐カドミウム合金などが用いられてもよい。また、前記負極集電体は通常3~500μmの厚さを有してもよく、正極集電体と同様に、前記集電体の表面に微細な凹凸を形成して負極活物質の結合力を強化させてもよい。例えば、フィルム、シート、箔、網、多孔質体、発泡体、不織布体などの多様な形態で用いられてもよい。
また、前記バインダーおよび導電材は、先ほど正極において説明したものと同様であってもよい。
前記有機溶媒としては、電池の電気化学的反応に関与するイオンが移動可能な媒質の役割を行うことができるものであれば特に制限されずに用いられてもよい。具体的に、前記有機溶媒としては、メチルアセテート(methyl acetate)、エチルアセテート(ethyl acetate)、γ‐ブチロラクトン(γ‐butyrolactone)、ε‐カプロラクトン(ε‐caprolactone)などのエステル系溶媒;ジブチルエーテル(dibutyl ether)またはテトラヒドロフラン(tetrahydrofuran)などのエーテル系溶媒;シクロヘキサノン(cyclohexanone)などのケトン系溶媒;ベンゼン(benzene)、フルオロベンゼン(fluorobenzene)などの芳香族炭化水素系溶媒;ジメチルカーボネート(dimethylcarbonate、DMC)、ジエチルカーボネート(diethylcarbonate、DEC)、メチルエチルカーボネート(methylethylcarbonate、MEC)、エチルメチルカーボネート(ethylmethylcarbonate、EMC)、エチレンカーボネート(ethylene carbonate、EC)、プロピレンカーボネート(propylene carbonate、PC)などのカーボネート系溶媒;エチルアルコール、イソプロピルアルコールなどのアルコール系溶媒;R‐CN(RはC2~C20の直鎖状、分岐状、または環状構造の炭化水素基であり、二重結合芳香環またはエーテル結合を含んでもよい。)などのニトリル類;ジメチルホルムアミドなどのアミド類;1,3‐ジオキソランなどのジオキソラン類;またはスルホラン(sulfolane)類などが用いられてもよい。この中でもカーボネート系溶媒が好ましく、電池の充放電性能を高めることができる高いイオン伝導度および高誘電率を有する環状カーボネート(例えば、エチレンカーボネートまたはプロピレンカーボネートなど)と、低粘度の直鎖状カーボネート系化合物(例えば、エチルメチルカーボネート、ジメチルカーボネート、またはジエチルカーボネートなど)との混合物がより好ましい。この場合、環状カーボネートと鎖状カーボネートは、約1:1~約1:9の体積比で混合して用いることが、優れた電解液性能を示すことができる。
正極活物質前駆体Ni0.8Co0.1Mn0.1(OH)2にLi/Metal(Ni、Co、Mn)のモル比が1.05になるようにリチウムソースLiOHを添加し、正極活物質前駆体100重量部に対して焼成添加剤の全含量が5重量部になるように、第1焼成添加剤としてLiOHを2重量部、第2焼成添加剤としてMgCO3を1重量部、および第3焼成添加剤としてB2O3を2重量部で添加した後に混合した。熱処理のために混合された粉末をアルミナルツボに投入した。その後、800℃、酸素雰囲気下で20時間焼成してリチウム遷移金属酸化物を製造した。その後、粉砕および水洗、乾燥工程を経た粉末を700℃、大気(Air)雰囲気下で熱処理し、単一粒子形態を有する正極活物質を得た。
正極活物質前駆体100重量部に対して焼成添加剤の全含量が5重量部になるように、第1焼成添加剤としてLiFを2重量部、第2焼成添加剤としてCaCO3を1重量部、および第3焼成添加剤としてH3BO3を2重量部で添加したことを除いては、実施例1と同様に実施して正極活物質を製造した。
正極活物質前駆体100重量部に対して焼成添加剤の全含量が5重量部になるように、第1焼成添加剤としてLiOHを3重量部、第2焼成添加剤としてMgCO3を1重量部、および第3焼成添加剤としてB2O3を1重量部で添加したことを除いては、実施例1と同様に実施して正極活物質を製造した。
焼成添加剤として、第1焼成添加剤であるLiOHのみを正極活物質前駆体100重量部に対して5重量部で混合したこと(第2および第3焼成添加剤は混合しない)を除いては、実施例1と同様に実施して正極活物質を製造した。
焼成添加剤として、第2焼成添加剤であるMgCO3のみを正極活物質前駆体100重量部に対して5重量部で混合したこと(第1および第3焼成添加剤は混合しない)を除いては、実施例1と同様に実施して正極活物質を製造した。
焼成添加剤として、第3焼成添加剤であるB2O3のみを正極活物質前駆体100重量部に対して5重量部で混合したこと(第1および第2焼成添加剤は混合しない)を除いては、実施例1と同様に実施して正極活物質を製造した。
焼成添加剤として、第1焼成添加剤であるLiOHおよび第3焼成添加剤であるB2O3を正極活物質前駆体100重量部に対してそれぞれ2.5重量部で混合したこと(第2焼成添加剤は混合しない)を除いては、実施例1と同様に実施して正極活物質を製造した。
第1、第2、および第3焼成添加剤を混合せず、900℃、酸素雰囲気下で20時間焼成してリチウム遷移金属酸化物を製造したことを除いては、実施例1と同様に実施して正極活物質を製造した。
前記実施例1~3および比較例1~5で製造された正極活物質を走査型電子顕微鏡(SEM)で拡大観察した写真を図1~図8に示した。
前記実施例1~3、比較例1~4で製造されたそれぞれの正極活物質、カーボンブラック導電材、およびPVDFバインダーをN-メチルピロリドン溶媒中で重量比として96:2:2の割合で混合して正極合材(粘度:5000mPa・s)を製造し、それをアルミニウム集電体の一面に塗布した後、130℃で乾燥後に圧延して正極を製造した。
負極としては、リチウムメタルを用いた。
前記実施例1~3、比較例1~5で製造されたそれぞれの正極活物質を用いて、リチウム二次電池フルセル(full cell)を製造した。実験例2と同様に製造するが、負極は、負極活物質として黒鉛(graphite)、カーボンブラック導電材、およびPVDFバインダーをN‐メチルピロリドン溶媒中で重量比として96:2:2の割合で混合して負極合材を製造し、それを銅集電体の一面に塗布した後、130℃で乾燥後に圧延して製造した。
製造されたリチウム二次電池(half cell)に対して、45℃でCCCVモードで0.2C、4.2Vになるまで充電し、CCモードで0.2Cで放電させ、その後、45℃でCCCVモードで0.7Cで4.2Vになるまで充電し、0.5Cの定電流で3Vまで放電して300回の充放電実験を行った際の容量維持率を測定した。その結果を下記表2に示した。
前記実施例1、比較例5で製造されたそれぞれの正極活物質を用いて、実験例2と同様に製造されたリチウム二次電池コインハーフセル(coin half cell)に対してSOC 10%にて1C放電時10秒常温抵抗を測定し、その結果を下記表3に示した。
Claims (10)
- ニッケル、コバルト、およびマンガンを含み、全金属中でニッケルを60モル%以上含有する正極活物質前駆体を用意するステップと、
前記正極活物質前駆体、リチウム原料ソース、第1焼成添加剤、第2焼成添加剤、および第3焼成添加剤を混合し、一次焼成してリチウム遷移金属酸化物を形成するステップとを含み、
前記第1焼成添加剤はリチウム含有化合物であり、
前記第2焼成添加剤は炭酸イオン含有化合物であり、
前記第3焼成添加剤はボロン含有化合物である、二次電池用正極活物質の製造方法。 - 前記第1焼成添加剤は、LiOH、Li2CO3、Li2O、およびLiFからなる群から選択された1つ以上である、請求項1に記載の二次電池用正極活物質の製造方法。
- 前記第2焼成添加剤は、BaCO3、NaCO3、MgCO3、およびCaCO3からなる群から選択された1つ以上である、請求項1に記載の二次電池用正極活物質の製造方法。
- 前記第3焼成添加剤は、B2O3およびH3BO3からなる群から選択された1つ以上である、請求項1に記載の二次電池用正極活物質の製造方法。
- 前記一次焼成は、650℃~850℃で行われる、請求項1に記載の二次電池用正極活物質の製造方法。
- 前記リチウム遷移金属酸化物は、単一粒子形態に形成される、請求項1に記載の二次電池用正極活物質の製造方法。
- 前記第1焼成添加剤、前記第2焼成添加剤、および前記第3焼成添加剤の全含量100重量部に対して、前記第1焼成添加剤は30~60重量部、前記第2焼成添加剤は10~40重量部、前記第3焼成添加剤は10~40重量部で含まれる、請求項1に記載の二次電池用正極活物質の製造方法。
- 前記第1焼成添加剤、前記第2焼成添加剤、および前記第3焼成添加剤の全含量は、前記正極活物質前駆体100重量部に対して0.5~15重量部で含まれる、請求項1に記載の二次電池用正極活物質の製造方法。
- 前記一次焼成後、前記リチウム遷移金属酸化物を粉砕および水洗後に600~750℃で二次焼成するステップをさらに含む、請求項1に記載の二次電池用正極活物質の製造方法。
- 前記正極活物質前駆体は、全金属中でニッケルを80モル%以上含有する、請求項1に記載の二次電池用正極活物質の製造方法。
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