JPWO2016136179A1 - 非水電解質二次電池 - Google Patents
非水電解質二次電池 Download PDFInfo
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- JPWO2016136179A1 JPWO2016136179A1 JP2017501895A JP2017501895A JPWO2016136179A1 JP WO2016136179 A1 JPWO2016136179 A1 JP WO2016136179A1 JP 2017501895 A JP2017501895 A JP 2017501895A JP 2017501895 A JP2017501895 A JP 2017501895A JP WO2016136179 A1 JPWO2016136179 A1 JP WO2016136179A1
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- Prior art keywords
- lithium
- rare earth
- transition metal
- particles
- metal oxide
- Prior art date
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- 229910052744 lithium Inorganic materials 0.000 claims abstract description 110
- -1 rare earth compounds Chemical class 0.000 claims abstract description 99
- 229910000314 transition metal oxide Inorganic materials 0.000 claims abstract description 93
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 90
- 239000011164 primary particle Substances 0.000 claims abstract description 87
- 239000011163 secondary particle Substances 0.000 claims abstract description 82
- 239000007774 positive electrode material Substances 0.000 claims abstract description 55
- IGILRSKEFZLPKG-UHFFFAOYSA-M lithium;difluorophosphinate Chemical compound [Li+].[O-]P(F)(F)=O IGILRSKEFZLPKG-UHFFFAOYSA-M 0.000 claims abstract description 27
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- 238000004220 aggregation Methods 0.000 claims abstract description 8
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- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims description 8
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 claims description 8
- 229910017052 cobalt Inorganic materials 0.000 claims description 5
- 239000010941 cobalt Substances 0.000 claims description 5
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- XFULIUKARWFBDF-UHFFFAOYSA-K erbium(3+);phosphate Chemical compound [Er+3].[O-]P([O-])([O-])=O XFULIUKARWFBDF-UHFFFAOYSA-K 0.000 description 1
- AKFFNTKRAYWFRN-UHFFFAOYSA-N ethyl 5-(trifluoromethyl)-1h-pyrazole-3-carboxylate Chemical compound CCOC(=O)C=1C=C(C(F)(F)F)NN=1 AKFFNTKRAYWFRN-UHFFFAOYSA-N 0.000 description 1
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Classifications
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
-
- 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
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
-
- 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
-
- 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
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
- H01M10/0567—Liquid materials characterised by the additives
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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Abstract
Description
正極は、例えば金属箔等の正極集電体と、正極集電体上に形成された正極活物質層とで構成される。正極集電体には、アルミニウムなどの正極の電位範囲で安定な金属の箔、当該金属を表層に配置したフィルム等を用いることができる。正極合材層は、正極活物質の他に、導電材及び結着材を含むことが好適である。正極は、例えば正極集電体上に正極活物質、導電材、及び結着材等を含む正極合材スラリーを塗布し、塗膜を乾燥させた後、圧延して正極合材層を集電体の両面に形成することにより作製できる。
負極は、例えば金属箔等からなる負極集電体と、当該集電体上に形成された負極合材層とで構成される。負極集電体には、銅などの負極の電位範囲で安定な金属の箔、当該金属を表層に配置したフィルム等を用いることができる。負極合材層は、負極活物質の他に、結着材を含むことが好適である。負極は、例えば負極集電体上に負極活物質、結着材等を含む負極合材スラリーを塗布し、塗膜を乾燥させた後、圧延して負極合材層を集電体の両面に形成することにより作製できる。
セパレータには、イオン透過性及び絶縁性を有する多孔性シートが用いられる。多孔性シートの具体例としては、微多孔薄膜、織布、不織布等が挙げられる。セパレータの材質としては、ポリエチレン、ポリプロピレン等のポリオレフィン樹脂、セルロースなどが好適である。セパレータは、セルロース繊維層及びポリオレフィン樹脂等の熱可塑性樹脂繊維層を有する積層体であってもよい。また、ポリエチレン層及びポリプロピレン層を含む多層セパレータであってもよく、セパレータの表面にアラミド樹脂等が塗布されたものを用いてもよい。
非水電解質は、非水溶媒と、非水溶媒に溶解した溶質とを含む。非水溶媒には、例えばエステル類、エーテル類、ニトリル類、ジメチルホルムアミド等のアミド類、ヘキサメチレンジイソシアネート等のイソシアネート類及びこれらの2種以上の混合溶媒等を用いることができる。非水溶媒は、これら溶媒の水素の少なくとも一部をフッ素等のハロゲン原子で置換したハロゲン置換体を含有していてもよい。
(実験例1)
[正極活物質の作製]
LiOHと、共沈により得られたNi0.91Co0.06Al0.03(OH)2で表されるニッケルコバルトアルミニウム複合水酸化物を500℃で熱処理して得られた酸化物とを、Liと遷移金属全体とのモル比が1.05:1になるように、石川式らいかい乳鉢にて混合した。次に、この混合物を酸素雰囲気中にて760℃で20時間熱処理後に粉砕することにより、平均二次粒径が約15μmのLi1.05Ni0.91Co0.06Al0.03O2で表されるリチウムニッケルコバルトアルミニウム複合酸化物(リチウム含有遷移金属酸化物)の粒子を得た。
上記正極活物質粒子に、カーボンブラックと、ポリフッ化ビニリデンを溶解させたN−メチル−2−ピロリドン溶液とを、正極活物質粒子と導電材と結着材との質量比が100:1:1となるように秤量し、T.K.ハイビスミックス(プライミクス社製)を用いてこれらを混練して正極合材スラリーを調製した。
負極活物質である人造黒鉛と、CMC(カルボキシメチルセルロースナトリウム)と、SBR(スチレン−ブタジエンゴム)とを、100:1:1の質量比で水溶液中において混合し、負極合材スラリーを調製した。次に、この負極合材スラリーを銅箔からなる負極集電体の両面に均一に塗布した後、塗膜を乾燥させ、圧延ローラーにより圧延し、集電体にニッケル製の集電タブを取り付けた。これにより、負極集電体の両面に負極合材層が形成された負極極板を作製した。なお、この負極における負極活物質の充填密度は1.75g/cm3であった。
エチレンカーボネート(EC)と、メチルエチルカーボネート(MEC)と、ジメチルカーボネート(DMC)とを、2:2:6の体積比で混合した混合溶媒に対して、六フッ化リン酸リチウム(LiPF6)を1.3モル/リットルの濃度となるように、溶解させた後、当該混合溶媒に対してビニレンカーボネート(VC)を2.0質量%の濃度で溶解させた。さらにこの混合溶媒に対してジフルオロリン酸リチウムを0.07モル/リットルの濃度になるようにそれぞれ溶解させ、非水電解液を調製した。
このようにして得た正極および負極を、これら両極間にセパレータを配置して渦巻き状に巻回した後、巻き芯を引き抜いて渦巻状の電極体を作製した。次に、この渦巻状の電極体を押し潰して、扁平型の電極体を得た。この後、この偏平型の電極体と上記非水電解液とを、アルミニウムラミネート製の外装体内に挿入し、電池A1を作製した。なお、当該電池のサイズは、厚み3.6mm×幅35mm×長さ62mmであった。また、当該非水電解質二次電池を4.20Vまで充電し、3.0Vまで放電したときの放電容量は950mAhであった。
非水電解液の調整時にジフルオロリン酸リチウムを溶解させなかったこと以外は、上記実験例1と同様にして電池A2を作製した。
正極活物質の作製において、懸濁液に硫酸エルビウム塩水溶液を加えている間の懸濁液のpHを9で一定に保持したこと以外は、上記実験例1と同様にして正極活物質を作製し、当該正極活物質を用いて電池A3を作製した。なお、上記懸濁液のpHを9に調整するために、適宜10質量%の水酸化ナトリウム水溶液を加えた。
非水電解液の調整時にジフルオロリン酸リチウムを溶解させなかったこと以外は、上記実験例3と同様にして電池A4を作製した。
正極活物質の作製において、硫酸エルビウム塩水溶液を加えず、リチウム含有遷移金属酸化物の二次粒子表面に水酸化エルビウムを付着させなかったこと以外は、上記実験例1と同様にして正極活物質を作製し、当該正極活物質を用いて電池A5を作製した。
非水電解液の調整時にジフルオロリン酸リチウムを溶解させなかったこと以外は、上記実験例5と同様にして電池A6を作製した。
上述のようにして作製した電池A1〜A6の各電池について、下記条件で充放電サイクル前及び100サイクル後のDCRの測定を行った。
SOC100%まで475mAの電流で充電した後、SOCが100%に到達した電池電圧で電流値が30mAとなるまで定電圧充電を行った。充電終了後120分間休止した時点の開放電圧(OCV:Open Circuit Voltage)を測定し、475mAで0.5秒間放電を行い、放電0.5秒後の電圧を測定した。下記式(1)によりサイクル前のDCR(SOC100%)を測定した。
DCR(Ω)
=(120分休止後のOCV(V) − 放電0.5秒後の電圧(V))/(電流値(A))・・・(1)
・充電条件
475mAの電流で電池電圧が4.2V(正極電位はリチウム基準で4.3V)となるまで定電流充電を行い、電池電圧が4.2Vに達した後は、4.2Vの定電圧で電流値が30mAとなるまで定電圧充電を行った。
・放電条件
950mAの定電流で電池電圧が3.0Vとなるまで定電流放電を行った。
・休止条件
上記充電と放電の間の休止間隔は10分間とした。
上述した、サイクル前のDCRの測定と同様の方法で、100サイクル後のDCR値測定を行った。なお、充放電サイクル試験とサイクル後のDCR測定の間の休止時間は10分間とした。DCR測定、充放電サイクル試験ともに25℃の恒温槽内で行った。
下記式(2)により100サイクル後のDCR上昇率を算出した。結果を表1に示す。
DCR上昇率(SOC100%)
=(100サイクル後のDCR(SOC100%)/(サイクル前のDCR(SOC100%)×100 ・・・(2)
上記実験例においては、希土類元素としてエルビウムを用いたが、第2実験例では、希土類元素として、サマリウム、ネオジムを用いた場合について検討した。
正極活物質の作製において、硫酸エルビウム塩水溶液の代わりに、硫酸サマリウム溶液を用いた以外は、上記実験例1と同様にして正極活物質を作製し、当該正極活物質を用いて電池A7を作製した。サマリウム化合物の付着量を誘導結合プラズマイオン化(ICP)発光分析法により測定したところ、サマリウム元素換算で、リチウムニッケルコバルトアルミニウム複合酸化物に対して0.13質量%であった。
正極活物質の作製において、硫酸エルビウム塩水溶液の代わりに、硫酸ネオジム溶液を用いた以外は、上記実験例1と同様にして正極活物質を作製し、当該正極活物質を用いて電池A8を作製した。ネオジム化合物の付着量を誘導結合プラズマイオン化(ICP)発光分析法により測定したところ、ネオジム元素換算で、リチウムニッケルコバルトアルミニウム複合酸化物に対して0.13質量%であった。
Claims (6)
- 正極と、負極と、非水電解質とを備えた非水電解質二次電池であって、
前記正極の正極活物質は、
リチウム含有遷移金属酸化物の一次粒子が凝集して形成された二次粒子と、
希土類化合物の一次粒子が凝集して形成された二次粒子と、
を含み、
前記希土類化合物の二次粒子は、前記リチウム含有遷移金属酸化物の二次粒子の表面において、隣接する前記一次粒子間に形成された凹部に付着し、且つ当該凹部において隣接し合う前記一次粒子の両方に付着しており、
前記非水電解質は、ジフルオロリン酸リチウムを含む、非水電解質二次電池。 - 前記希土類化合物を構成する希土類元素が、ネオジム、サマリウム及びエルビウムから選ばれる少なくとも1種の元素である、請求項1に記載の非水電解質二次電池。
- 前記希土類化合物が、水酸化物及びオキシ水酸化物から選ばれる少なくとも1種の化合物である、請求項1又は2に記載の非水電解質二次電池。
- 前記リチウム含有遷移金属酸化物に占めるニッケルの割合が、リチウムを除く金属元素の総モル量に対して80モル%以上である、請求項1〜3の何れか1項に記載の非水電解質二次電池。
- 前記非水電解質に含まれる前記ジフルオロリン酸リチウムの濃度は、0.01M以上0.25M以下である、請求項1〜4の何れか1項に記載の非水電解質二次電池。
- 前記リチウム含有遷移金属酸化物中に占めるコバルトの割合が、リチウムを除く金属元素の総モル量に対して7モル%以下である、請求項1〜5の何れか1項に記載の非水電解質二次電池。
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CN107004897B (zh) | 2020-02-07 |
CN107004897A (zh) | 2017-08-01 |
US20170331158A1 (en) | 2017-11-16 |
WO2016136179A1 (ja) | 2016-09-01 |
JP6633049B2 (ja) | 2020-01-22 |
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