JP7460258B2 - 正極活物質前駆体及びその製造方法 - Google Patents
正極活物質前駆体及びその製造方法 Download PDFInfo
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- JP7460258B2 JP7460258B2 JP2023506317A JP2023506317A JP7460258B2 JP 7460258 B2 JP7460258 B2 JP 7460258B2 JP 2023506317 A JP2023506317 A JP 2023506317A JP 2023506317 A JP2023506317 A JP 2023506317A JP 7460258 B2 JP7460258 B2 JP 7460258B2
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- active material
- positive electrode
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- 239000011294 coal tar pitch Substances 0.000 description 1
- 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
- CKFRRHLHAJZIIN-UHFFFAOYSA-N cobalt lithium Chemical compound [Li].[Co] CKFRRHLHAJZIIN-UHFFFAOYSA-N 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 150000004292 cyclic ethers Chemical class 0.000 description 1
- 125000000753 cycloalkyl group Chemical group 0.000 description 1
- 238000009831 deintercalation Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 150000004862 dioxolanes Chemical class 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000010294 electrolyte impregnation Methods 0.000 description 1
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000011357 graphitized carbon fiber Substances 0.000 description 1
- 229910021385 hard carbon Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 150000004677 hydrates Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 150000002461 imidazolidines Chemical class 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 239000005453 ketone based solvent Substances 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical class [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 1
- 229910002102 lithium manganese oxide Inorganic materials 0.000 description 1
- QEXMICRJPVUPSN-UHFFFAOYSA-N lithium manganese(2+) oxygen(2-) Chemical class [O-2].[Mn+2].[Li+] QEXMICRJPVUPSN-UHFFFAOYSA-N 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
- URIIGZKXFBNRAU-UHFFFAOYSA-N lithium;oxonickel Chemical class [Li].[Ni]=O URIIGZKXFBNRAU-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011656 manganese carbonate Substances 0.000 description 1
- 235000006748 manganese carbonate Nutrition 0.000 description 1
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 1
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 description 1
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 description 1
- ISPYRSDWRDQNSW-UHFFFAOYSA-L manganese(II) sulfate monohydrate Chemical compound O.[Mn+2].[O-]S([O-])(=O)=O ISPYRSDWRDQNSW-UHFFFAOYSA-L 0.000 description 1
- GEYXPJBPASPPLI-UHFFFAOYSA-N manganese(III) oxide Inorganic materials O=[Mn]O[Mn]=O GEYXPJBPASPPLI-UHFFFAOYSA-N 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002931 mesocarbon microbead Substances 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 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
- 239000011301 petroleum pitch Substances 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 229920005569 poly(vinylidene fluoride-co-hexafluoropropylene) Polymers 0.000 description 1
- 239000004584 polyacrylic acid Substances 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
- 229920006254 polymer film Polymers 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000000047 product Substances 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
- 230000009257 reactivity Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000007789 sealing 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
- 229910001388 sodium aluminate Inorganic materials 0.000 description 1
- 229910021384 soft carbon Inorganic materials 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical class O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000002733 tin-carbon composite material Substances 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
- 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
Images
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Description
[M1 aM2 bM3 cM4 d](OH)2
[化学式2]
[M1 aM2 bM3 cM4 d]O・OH
先ず、本発明に係る正極活物質前駆体について説明する。
[M1 aM2 bM3 cM4 d](OH)2
[化学式2]
[M1 aM2 bM3 cM4 d]O・OH
次に、本発明に係る正極活物質前駆体の製造方法について説明する。
先ず、M1金属を含む第1金属溶液、M2金属を含む第2金属溶液、及びM3金属を含む第3金属溶液をそれぞれ準備する。
第1金属溶液、第2金属溶液、及び第3金属溶液が準備されると、前記第1金属溶液、アンモニウム陽イオン錯体形成剤、及び塩基性化合物を混合して反応溶液を形成し、沈澱反応によりM1金属の水酸化物又はオキシ水酸化物粒子を形成する。
前記第2段階により反応溶液中にM1金属の水酸化物又はオキシ水酸化物粒子が十分に形成されると、第1金属溶液の供給を中断し、M2金属を含む第2金属溶液を投入し、沈澱反応を進行させ、M1金属及びM2金属の水酸化物又はオキシ水酸化物粒子を形成する。
前記第3段階により反応溶液中にM1金属及びM2金属の水酸化物又はオキシ水酸化物粒子が十分に形成されると、第2金属溶液の供給を中断し、第3金属溶液を投入し、沈澱反応を進行させ、M1金属、M2金属、及びM3金属の水酸化物又はオキシ水酸化物粒子を形成する。
一方、必須なものではないが、前記正極活物質前駆体の製造方法は、M4金属を含む第4金属溶液を準備する段階、及び前記第4金属溶液を反応溶液に投入して沈澱反応を進行する段階をさらに含んでよい。
前記のような方法により製造された本発明の正極活物質をリチウム原料物質と混合した後、焼成して正極活物質を製造することができる。
次に、本発明に係る電気化学素子について説明する。本発明に係る電気化学素子は、前述した本発明の正極を含むものであって、前記電気化学素子は、具体的には、電池、キャパシターなどであってよく、より具体的には、リチウム二次電池であってよい。
(1)第1段階
NiSO4を蒸留水に投入して、2.4M濃度の第1金属溶液を準備した。
反応器に脱イオン水を入れた後、窒素ガスを反応器にパージングして水中の溶存酸素を除去し、反応器内を非酸化雰囲気に組成した。前記反応器に8.0MのNaOH溶液と5.1MのNH4OH水溶液とを投入してpH12.0の反応母液を準備し、前記第1金属溶液を3.8L/hrの速度で、NaOH水溶液を2.3L/hr、NH4OH水溶液を0.54L/hrの速度でそれぞれ投入して、28.8時間沈澱反応を進行した。この際、反応溶液のpHは、11.6を維持した。
その後、第1金属溶液の投入を中断し、pHセンサー連動方式でNaOHを投入して反応溶液のpHを11.4に調節した後、第2金属溶液を3.8L/hrの速度で、NaOH水溶液を2.3L/hr、NH4OH水溶液を0.5L/hrの速度でそれぞれ投入して、9.6時間沈澱反応を進行した。
その後、第2金属溶液の投入を中断し、pHセンサー連動方式でNaOHを投入して反応溶液のpHを10.8~11.0範囲に調節した後、第3金属溶液を3.8L/hrの速度で、NaOH水溶液を2.3L/hr、NH4OH水溶液を0.54L/hrの速度でそれぞれ投入し、9.6時間沈澱反応を進行して、[Ni0.6Co0.2Mn0.2](OH)2組成を有する正極活物質前駆体を製造した。
(1)第1段階
NiSO4を蒸留水に投入して、2.4M濃度の第1金属溶液を準備した。
反応器に脱イオン水を入れた後、窒素ガスを反応器にパージングして水中の溶存酸素を除去し、反応器内を非酸化雰囲気に組成した。前記反応器に8.0MのNaOH溶液と5.1MのNH4OH水溶液とを投入してpH12.0の反応母液を準備し、前記第1金属溶液を3.8L/hrの速度で、NaOH水溶液を2.3L/hr、NH4OH水溶液を0.54L/hrの速度でそれぞれ投入して、43.2時間沈澱反応を進行した。この際、反応pHは、11.6を維持した。
その後、第1金属溶液の投入を中断し、pHセンサー連動方式でNaOHを投入して反応溶液のpHを11.4に調節した後、第2金属溶液を3.8L/hrの速度で、NaOH水溶液を2.3L/hr、NH4OH水溶液を0.54L/hrの速度でそれぞれ投入して、2.4時間沈澱反応を進行した。
その後、第2金属溶液の投入を中断し、pHセンサー連動方式でNaOHを投入して反応溶液のpHを10.8~11.0に調節した後、第3金属溶液を3.8L/hrの速度で、NaOH水溶液を2.3L/hr、NH4OH水溶液を0.54L/hrの速度でそれぞれ投入し、2.4時間沈澱反応を進行して、[Ni0.9Co0.05Mn0.05](OH)2組成を有する正極活物質前駆体を製造した。
(1)第1段階
NiSO4を蒸留水に投入して、2.4M濃度の第1金属溶液を準備した。
反応器に脱イオン水を入れた後、窒素ガスを反応器にパージングして水中の溶存酸素を除去し、反応器内を非酸化雰囲気に組成した。前記反応器に8.0MのNaOH溶液と5.1MのNH4OH水溶液とを投入してpH12.0の反応母液を準備し、前記第1金属溶液を3.8L/hrの速度で、NaOH水溶液を2.3L/hr、NH4OH水溶液を0.54L/hrの速度でそれぞれ投入して、43.2時間沈澱反応を進行した。この際、反応pHは、11.6を維持した。
その後、第1金属溶液の投入を中断し、pHセンサー連動方式でNaOHを投入して反応溶液のpHを10.8~11.0に調節した後、第2金属溶液を3.8L/hrの速度で、NaOH水溶液を2.3L/hr、NH4OH水溶液を0.54L/hrの速度でそれぞれ投入して、2.4時間沈澱反応を進行した。
その後、第2金属溶液の投入を中断し、pHセンサー連動方式でNaOHを投入して反応溶液のpHを11.4に調節した後、第3金属溶液を3.8L/hrの速度で、NaOH水溶液を2.3L/hr、NH4OH水溶液を0.54L/hrの速度でそれぞれ投入し、2.4時間沈澱反応を進行して、[Ni0.9Mn0.05Co0.05](OH)2組成を有する正極活物質前駆体を製造した。
NiSO4、CoSO4、及びMnSO4をニッケル:コバルト:マンガンのモル比が60:20:20になるようにする量で蒸留水中で混合して、2.4M濃度の金属溶液を準備した。
NiSO4、CoSO4、及びMnSO4をニッケル:コバルト:マンガンのモル比が90:5:5になるようにする量で蒸留水中で混合して、2.4M濃度の金属溶液を準備した。
実施例1~3の正極活物質前駆体の製造時に、第2段階、第3段階、及び第4段階後に反応溶液から正極活物質前駆体粒子をサンプリングした後、ICP分析により正極活物質前駆体粒子内の遷移金属中のニッケル、コバルト、マンガン金属の濃度(mol%)を測定し、その結果を下記[表1]に示した。
実施例1及び比較例1により製造された正極活物質前駆体の金属元素分布を確認するために、SEM-EDS分析(S-4800、Hitachi社)を行い、その結果を下記[表2]に示した。
X線回折分析機(Rikaku社)を用いて、実施例2、3及び比較例2で製造した正極活物質前駆体粒子のXRDパターンを測定した後、測定されたXRDパターンから(100)面及び(001)面のピーク半価幅を得て、シェラー(Scherrer)式を用いて各結晶面における結晶粒の大きさを計算した。測定結果は下記表3に示した。
実施例1、実施例2、及び比較例1により製造された正極活物質前駆体のそれぞれとLiOH・H2Oを、Li:遷移金属のモル比が1.05:1になるように混合し、酸素雰囲気下において805℃で13時間焼成して正極活物質を製造した。
20 第2領域
Claims (16)
- 下記化学式1又は下記化学式2で表される組成を有する正極活物質前駆体であって、
前記正極活物質前駆体の粒子の中心部に形成され、全遷移金属中のM1金属のモル比が90モル%以上の第1領域と、
前記第1領域の上部に形成され、全遷移金属中のM2金属のモル比が90モル%以上の第2領域と、
前記第2領域の上部に形成され、全遷移金属中のM3金属のモル比が90モル%以上の第3領域と、を含む正極活物質前駆体:
[化学式1]
[M1 aM2 bM3 cM4 d](OH)2
[化学式2]
[M1 aM2 bM3 cM4 d]O・OH
前記[化学式1]及び[化学式2]で、
前記M1、M2、及びM3は、それぞれ独立して、Ni、Co、及びMnからなる群から選択され、前記M1、M2、及びM3が互いに異なり、
前記M4は、B、Mg、Ca、Al、Ti、V、Cr、Fe、Zn、Ga、Y、Zr、Nb、Mo、Ta及びWからなる群から選択される1種以上であり、
0<a<1、0<b<1、0<c<1、0≦d<1であり、a+b+c+d=1である。 - 前記正極活物質前駆体は、前記第1領域と第2領域の境界面、前記第2領域と第3領域の境界面、及び第3領域の上部のうちの少なくとも一つに形成され、M4金属を含む第4領域をさらに含む、請求項1に記載の正極活物質前駆体。
- 前記第1領域、第2領域、及び第3領域のうちの少なくとも一つ以上にM4金属を含む、請求項1または2に記載の正極活物質前駆体。
- 前記[化学式1]及び[化学式2]で、0.5≦a<1、0<b<0.4、0<c<0.4、0≦d<0.1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前駆体。
- 前記[化学式1]及び[化学式2]で、0.6≦a<1、0<b<0.3、0<c<0.3、0≦d<0.1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前駆体。
- 前記M1金属はNiであり、前記M2金属はMnであり、前記M3金属はCoである、請求項1から5のいずれか一項に記載の正極活物質前駆体。
- 前記M1金属はNiであり、前記M2金属はCoであり、前記M3金属はMnである、請求項1から5のいずれか一項に記載の正極活物質前駆体。
- 前記M4金属はAlである、請求項1から7のいずれか一項に記載の正極活物質前駆体。
- 前記正極活物質前駆体は、(100)結晶面における結晶粒の大きさが30nm以上である、請求項1から8のいずれか一項に記載の正極活物質前駆体。
- 前記正極活物質前駆体は、(001)結晶面における結晶粒の大きさ(C(001))に対する(100)結晶面における結晶粒の大きさ(C(100))の比率C(100)/C(001)が3.5~6.0である、請求項1から9のいずれか一項に記載の正極活物質前駆体。
- M1金属を全金属中の90モル%以上に含む第1金属溶液、M2金属を全金属中の90モル%以上に含む第2金属溶液、及びM3金属を全金属中の90モル%以上に含む第3金属溶液をそれぞれ準備する第1段階と、
前記第1金属溶液、アンモニウム陽イオン錯体形成剤、及び塩基性化合物を混合して反応溶液を形成し、沈澱反応によりM1金属の水酸化物又はオキシ水酸化物粒子を形成する第2段階と、
前記M1金属の水酸化物又はオキシ水酸化物粒子を含む反応溶液に第2金属溶液を投入し、沈澱反応によりM1金属及びM2金属の水酸化物又はオキシ水酸化物粒子を形成する第3段階と、
前記M1金属及びM2金属の水酸化物又はオキシ水酸化物粒子を含む反応溶液に第3金属溶液を投入し、沈澱反応によりM1金属、M2金属及びM3金属の水酸化物又はオキシ水酸化物粒子を形成する第4段階と、を含み、
前記M1、M2、及びM3は、それぞれ独立して、Ni、Co、及びMnからなる群から選択され、前記M1、M2、及びM3が互いに異なる正極活物質前駆体の製造方法。 - M4金属を全金属中の90モル%以上に含む第4金属溶液を準備する段階と、
前記第2段階と第3段階との間、前記第3段階と第4段階との間、及び第4段階後のうちの少なくとも一つに前記第4金属溶液を投入して沈澱反応させる段階と、をさらに含み、
前記M4金属は、M4はB、Mg、Ca、Al、Ti、V、Cr、Fe、Zn、Ga、Y、Zr、Nb、Mo、Ta及びWからなる群から選択される1種以上である、請求項11に記載の正極活物質前駆体の製造方法。 - 前記第1金属溶液、第2金属溶液、及び第3金属溶液のうちの少なくとも一つがM4金属を全遷移金属中の10モル%以下に含み、
前記M4金属は、M4はB、Mg、Ca、Al、Ti、V、Cr、Fe、Zn、Ga、Y、Zr、Nb、Mo、Ta及びWからなる群から選択される1種以上である、請求項11に記載の正極活物質前駆体の製造方法。 - 前記M1金属はNi、M2金属はMn、M3金属はCoであり、
前記第2段階における反応溶液のpHが11.4~11.8であり、
前記第3段階における反応溶液のpHは11.0以下であり、
前記第4段階における反応溶液のpHは11.0~11.4である、請求項11に記載の正極活物質前駆体の製造方法。 - 前記M1金属はNi、M2金属はCo、M3金属はMnであり、
前記第2段階における反応溶液のpHが11.4~11.8であり、
前記第3段階における反応溶液のpHは11.0~11.4であり、
前記第4段階における反応溶液のpHは11.0以下である、請求項11に記載の正極活物質前駆体の製造方法。 - 請求項1~10のいずれか一項に記載の正極活物質前駆体とリチウム原料物質の焼成品である正極活物質。
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