JP2023522137A - 正極片、当該正極片を含む電気化学装置及び電子装置 - Google Patents
正極片、当該正極片を含む電気化学装置及び電子装置 Download PDFInfo
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- JP2023522137A JP2023522137A JP2021541563A JP2021541563A JP2023522137A JP 2023522137 A JP2023522137 A JP 2023522137A JP 2021541563 A JP2021541563 A JP 2021541563A JP 2021541563 A JP2021541563 A JP 2021541563A JP 2023522137 A JP2023522137 A JP 2023522137A
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- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 229940017219 methyl propionate Drugs 0.000 description 1
- 229940057061 mevalonolactone Drugs 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 150000003014 phosphoric acid esters Chemical class 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 1
- 229920005569 poly(vinylidene fluoride-co-hexafluoropropylene) Polymers 0.000 description 1
- 229920002312 polyamide-imide Polymers 0.000 description 1
- 229920006267 polyester film Polymers 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229920005614 potassium polyacrylate Polymers 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 239000002153 silicon-carbon composite material Substances 0.000 description 1
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 1
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 1
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 1
- 229910021384 soft carbon Inorganic materials 0.000 description 1
- 239000004759 spandex Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- WMOVHXAZOJBABW-UHFFFAOYSA-N tert-butyl acetate Chemical compound CC(=O)OC(C)(C)C WMOVHXAZOJBABW-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 description 1
- 125000001889 triflyl group Chemical group FC(F)(F)S(*)(=O)=O 0.000 description 1
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical compound COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910001928 zirconium 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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Abstract
Description
[化1]
Li1+xAaFeyMnzTivPO4-wSw (1)
式(1)において、-0.1<x<0.1、0<a<0.01、0≦y≦1、0≦z≦1、0.001<v<0.005、0≦w<0.05、AがNa又はKの少なくとも1つを含み、
[化2]
Li2+rNasM1+qO2+t (2)
式(2)において、-0.2<r<0.2、0<s<0.05、-0.1<q<0.1、0≦t<0.05、MがNi、Cu、Mn、Fe又はCoの少なくとも1つを含み、
当該正極片の圧縮密度(compaction density)がR g/cm3であり、即ち圧縮密度Rの単位がg/cm3であり、当該正極片の片面の面密度がQ g/1540.25mm2であり、即ち片面の面密度Qの単位がg/1540.25mm2であり、5.2≦R/Q≦13.5である、正極片を提供する。
以下、実施例及び比較例を挙げて本発明の実施形態をより具体的に説明する。各試験及び評価は、後述の方法に従って行われた。なお、「部」、「%」は、特に断りのない限り、質量基準である。
正極片の圧縮密度Rは、式R=m/vによって算出される。当式において、mは正極活物質層の質量であって、その単位はgであり、vは正極活物質層の体積であって、その単位はcm3である。ここで、体積vは正極活物質層の面積Arと正極活物質層の厚さとの積である。
正極片の片面の面密度Qは、式Q=1540.25m/Arにより算出される。当該式において、mは正極活物質層の質量であって、その単位はgであり、Arは正極活物質層の面積であって、その単位はmm2である。
第1の正極活物質及び第2の正極活物質のDv50、Dv90は、レーザー粒度計を用いて測定される。
60℃の条件で、リチウムイオン二次電池を1Cレートで3.6Vまで定電流充電し、次に電流が0.05C以下になるまで定電圧充電してから、1Cレートで2.5Vまで定電流放電する。これを1つの充放電サイクルとし、リチウムイオン二次電池の1回目のサイクルの放電容量を記録する。リチウムイオン二次電池を上記の方法で充放電サイクルを1000回行い、1000回目のサイクルの放電容量を記録して、容量維持率=1000回目のサイクルの放電容量/1回目のサイクルの放電容量によって、容量維持率を記録する。
25℃の条件で、リチウムイオン二次電池を0.2Cのレートで3.6Vまで定電流充電し、次に電流が0.05C以下になるまで定電圧充電し、その後30分間静置してから、更に、0.2Cレートで2.5Vまで定電流放電する。測定するによってリチウムイオン二次電池の0.2Cレートの放電容量を得る。
25℃の条件で、リチウムイオン二次電池を0.2Cレートで3.6Vまで定電流充電し、次に電流が0.05C以下になるまで定電圧充電し、その後30分間静置してから、更に、1Cレートで2.5Vまで定電流放電する。測定するによってリチウムイオン二次電池の1Cレートの放電容量を得る。
リチウムイオン二次電池の1Cレートの放電容量維持率(%)=1Cレートの放電容量/0.2Cレートの放電容量×100%。
25℃の条件で、リチウムイオン二次電池を0.2Cレートで3.6Vまで定電流充電し、次に電流が0.05C以下になるまで定電圧充電し、その後30分間静置してから、更に、0.2Cレートで2.5Vまで定電流放電し、リチウムイオン二次電池の0.2Cレートでの放電容量D0(Ah)及び放電プラットフォーム V0(V)を記録する。リチウムイオン電池の質量を秤量し、m0(kg)とする。
リチウムイオン二次電池のエネルギー密度は、エネルギー密度=D0×V0/m0によって算出される。
第2の正極活物質と、導電剤である導電性カーボンブラックと、粘着剤であるポリフッ化ビニリデン(PVDF)とを90:5:5の質量比で混合し、溶媒としてN-メチルピロリドン(NMP)を添加して、撹拌して固形分含有量が40%であるスラリーを調製し、ドクターブレードにより、集電体であるアルミニウム箔に、塗布層の厚さが100μmとなるように塗布し、真空乾燥器による乾燥を130℃で12h行った後、乾燥環境で打ち抜き機によって直径が1cmの円形片に切り出し、グローブボックス内でリチウム金属片を対電極とし、ceglard複合膜をセパレーターとして選択し、電解液を添加し組み立ててボタン型電池を得る。電解液はエチレンカーボネート(EC)と、メチルエチルカーボネート(EMC)と、ジエチルカーボネート(DEC)とを、30:50:20の質量比で混合して得られた有機溶液であり、電解液におけるリチウム塩の濃度は1.15mol/Lである。
本発明において、Wuhan Landian CT2001Aシステムを使用して充電比容量の測定を行う。第2の正極活物質を含む測定用ボタン型電池を25±3℃の雰囲気で30分間静置し、0.1C(グラムあたりの理論容量は400mAh/gとされる)レートで電圧が4.4Vになるまで定電流充電し、次に電流が0.025Cになるまで定電圧充電し、充電容量を記録する。
第2の正極活物質を含むボタン型電池の充電比容量=充電容量/第2の正極活物質の質量。
本発明において、Wuhan LandianCT2001Aシステムを使用して放電比容量の測定を行う。第2の正極活物質を含む測定用ボタン型電池を25±3℃の雰囲気で30分間静置し、0.1C(グラムあたりの理論容量は400mAh/gとされる)レートで電圧が4.4Vになるまで定電流充電し、次に電流が0.025Cになるまで定電圧充電し、5min静置してから、ボタン型電池は、更に、0.1Cでカットオフ電圧が2.5Vになるまで定電流放電し、初回放電容量を記録する。
第2の正極活物質を含むボタン型電池の放電比容量=放電容量/第2の正極活物質の質量。
第1の正極活物質であるLi0.998Na0.002Fe0.996Ti0.002PO4と、第2の正極活物質であるLi1.995Na0.005NiO2と、粘着剤であるPVDFと、導電剤であるカーボンブラックとを混合した。ここで、Li0.998Na0.002Fe0.996Ti0.002PO4と、Li1.995Na0.005NiO2と、PVDFと、導電性カーボンブラックとの質量比は93.6:2.8:2.1:1.5である。そして、溶媒としてNMPを添加し、真空で均一かつ透明な溶液になるまで撹拌することにより、固形分含有量が75%である正極スラリーを得た。正極スラリーを、厚さ10μmの正極集電体であるアルミニウム箔に均一に塗布し、130℃の条件で乾燥させ、塗布層の厚さが110μmである正極片を得た。以上のステップが完了した後、正極片の片面での塗布は完了した。その後、当該正極片の他の表面に対して、上記のステップを繰り返すことにより、両面に正極活物質が塗布された正極片を得た。塗布が完了した後、さらに冷間プレスを行い、正極片を74mm×867mmに裁断してタブを溶接した後、二次電池用正極片が得られた。
負極活物質であるグラファイトと、ナノレベルの導電性カーボンブラックと、スチレンブタジエンゴムと、カルボキシメチルセルロースナトリウムとを、95:2:1.5:1.5の質量比で混合し、溶媒として脱イオン水を添加して、固形分含有量が70%であるスラリーを調製して、均一に撹拌した。スラリーを集電体である銅箔に均一に塗布し、110℃の条件で乾燥させ、冷間プレスを行った後に、負極活物質層の厚さが150μmであり、かつ片面に活物質層が塗布された負極片を得た。以上のステップが完了した後、同様の方法で当該負極片の裏面に対して、これらのステップを行うことにより、両面で塗布された負極片を得た。塗布が完了した後、負極片を76mm×851mmに裁断し、タブを溶接した後、二次電池用負極片が得られた。
乾燥のアルゴン雰囲気において、有機溶媒であるエチレンカーボネートと、メチルエチルカーボネートと、ジエチルカーボネートとを、EC:EMC:DEC=30:50:20の質量比で混合して有機溶液を得た。そして、有機溶媒にリチウム塩であるヘキサフルオロリン酸リチウムを添加し溶解させ、均一に混合することで、リチウム塩の濃度が1.15mol/Lである電解液を得た。
厚さ14μmのポリプロピレン(PP)フィルム(Celgard社製)を使用した。
セパレータが正極片と負極片との間に介在して隔離の役割を果たすように、上記で調製された正極片、セパレーター、負極片を順に積層し、巻いて電極組立体を得た。電極組立体をアルミニウムプラスチック複合フィルム包装袋に入れて、80℃で水分を除去し、調製された電解液を注入し、真空封止、静置、フォーメーション、成形などの工程を行うことにより、リチウムイオン電池を得た。
<第2の正極活物質の調製>
適量のクエン酸を秤量してLi2NiO2に添加し(クエン酸とLi2NiO2との質量比が1:50である)、エタノールを溶媒として機械的に撹拌して混合し、1hの超音波分散を行って、混合溶液を得た。その後、水浴で撹拌して溶媒を揮発させ、乾燥生成物を得た後に窒素雰囲気で1回目の焼結を行い、焼結温度は350℃であり、焼結時間は4hであり、冷却後に上記生成物とアセチレンブラックとを十分に砕いて粉末にした(上記生成物とアセチレンブラックとの質量比は97:3である)。そして、不活性雰囲気で2回目の焼結を行い、焼結温度は600℃であり、焼結時間は8hであり、これにより、炭素被覆Li2NiO2の第2の正極活物質を得た。
<正極片の調製>、<負極片の調製>、<電解液の調製>、<セパレータの調製>、及び<リチウムイオン電池の調製>については、実施例1と同様である。
Claims (12)
- 正極集電体と、前記正極集電体の少なくとも1つの表面に設置された正極活物質層を含む正極片であって、
前記正極活物質層が、下記の式(1)で示される第1の正極活物質と、下記の式(2)で示される第2の正極活物質とを含み、
[化1]
Li1+xAaFeyMnzTivPO4-wSw (1)
式(1)において、-0.1<x<0.1、0<a<0.01、0≦y≦1、0≦z≦1、0.001<v<0.005、0≦w<0.05であり、AがNa又はKの少なくとも1つを含み、
[化2]
Li2+rNasM1+qO2+t (2)
式(2)において、-0.2<r<0.2、0<s<0.05、-0.1<q<0.1、0≦t<0.05であり、MがNi、Cu、Mn、Fe、又はCoのうちの少なくとも1を含み、
前記正極片の圧縮密度がR g/cm3であり、前記正極片の片面の面密度がQ g/1540.25mm2であり、かつR/Qが5.2≦R/Q≦13.5を満たす正極片。 - 前記正極片の圧縮密度Rが1.8<R<2.5を満たす、請求項1に記載の正極片。
- 前記正極片の片面の面密度Qが0.18<Q<0.34を満たす、請求項1に記載の正極片。
- 前記第1の正極活物質と前記第2の正極活物質との質量比が4:1~100:1である、請求項1に記載の正極片。
- 前記正極活物質層における前記第1の正極活物質の含有量が80wt%以上98wt%以下である、請求項4に記載の正極片。
- 前記第1の正極活物質の平均粒子径Dv50が0.5μm~3μmであり、前記第1の正極活物質の粒子径分布Dv90が4μm~10μmである、請求項1に記載の正極片。
- 前記第2の正極活物質の平均粒子径Dv50が6μm~18μmであり、前記第2の正極活物質の粒子径分布Dv90が15μm~32μmである、請求項1に記載の正極片。
- 前記第2の正極活物質がX≧300mAh/g、Y/X≦40%を満たし、
Xが前記第2の正極活物質の初回充電比容量であり、Yが前記第2の正極活物質の初回放電比容量である、請求項1に記載の正極片。 - 下記(a)~(e)のうちの少なくとも1つを満たす請求項1に記載の正極片、
(a)前記正極片が5.6≦R/Q≦12.0を満たし、
(b)前記第1の正極活物質と前記第2の正極活物質との質量比が9:1~99:1であり、
(c)前記正極活物質層における前記第1の正極活物質の含有量が85wt%~98wt%であり、
(d)前記第1の正極活物質の平均粒子径Dv50が0.8μm~2μmであり、前記第1の正極活物質の粒子径分布Dv90が5μm~8μmであり、
(e)前記第2の正極活物質の平均粒子径Dv50が10μm~16μmであり、前記第2の正極活物質の粒子径分布Dv90が18μm~30μmである。 - 前記正極活物質層が第1の正極活物質層と第2の正極活物質層とを含み、前記第1の正極活物質層が前記第1の正極活物質を含み、前記第2の正極活物質層が前記第2の正極活物質を含む、請求項1~9のいずれか1項に記載の正極片。
- 請求項1~10のいずれか1項に記載の正極片を含む電気化学装置。
- 請求項11に記載の電気化学装置を含む電子装置。
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