JP6610552B2 - 非水電解質二次電池用正極及びそれを用いた非水電解質二次電池 - Google Patents
非水電解質二次電池用正極及びそれを用いた非水電解質二次電池 Download PDFInfo
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- JP6610552B2 JP6610552B2 JP2016551485A JP2016551485A JP6610552B2 JP 6610552 B2 JP6610552 B2 JP 6610552B2 JP 2016551485 A JP2016551485 A JP 2016551485A JP 2016551485 A JP2016551485 A JP 2016551485A JP 6610552 B2 JP6610552 B2 JP 6610552B2
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- Prior art keywords
- positive electrode
- lithium
- carbonate
- electrolyte secondary
- secondary battery
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000011255 nonaqueous electrolyte Substances 0.000 title claims description 35
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 71
- 229910001930 tungsten oxide Inorganic materials 0.000 claims description 71
- -1 carbonate compound Chemical class 0.000 claims description 69
- 229910021437 lithium-transition metal oxide Inorganic materials 0.000 claims description 56
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 50
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 50
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 31
- 239000011572 manganese Substances 0.000 claims description 24
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 22
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 21
- 229910001386 lithium phosphate Inorganic materials 0.000 claims description 9
- TWQULNDIKKJZPH-UHFFFAOYSA-K trilithium;phosphate Chemical compound [Li+].[Li+].[Li+].[O-]P([O-])([O-])=O TWQULNDIKKJZPH-UHFFFAOYSA-K 0.000 claims description 9
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
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- 229910052748 manganese Inorganic materials 0.000 claims description 3
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 2
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- 229910021446 cobalt carbonate Inorganic materials 0.000 claims description 2
- ZOTKGJBKKKVBJZ-UHFFFAOYSA-L cobalt(2+);carbonate Chemical compound [Co+2].[O-]C([O-])=O ZOTKGJBKKKVBJZ-UHFFFAOYSA-L 0.000 claims description 2
- 239000011656 manganese carbonate Substances 0.000 claims description 2
- 229940093474 manganese carbonate Drugs 0.000 claims description 2
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- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 claims description 2
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 claims description 2
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 claims description 2
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- 239000002245 particle Substances 0.000 description 54
- 239000007774 positive electrode material Substances 0.000 description 39
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- 230000006872 improvement Effects 0.000 description 4
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
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- 229910052739 hydrogen Chemical group 0.000 description 3
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- 239000010937 tungsten Substances 0.000 description 3
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- 229910013188 LiBOB Inorganic materials 0.000 description 2
- 229910013870 LiPF 6 Inorganic materials 0.000 description 2
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- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 2
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 2
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- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
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Images
Classifications
-
- 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
- H01M4/13—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
-
- 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
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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Description
本発明では、リチウム遷移金属酸化物の表面の少なくとも一部に酸化タングステンを有し、正極に混合した炭酸化合物が、酸化タングステンの表面の一部に接し、炭酸化合物と酸化タングステンとの間の界面が形成される。
負極としては、従来から用いられてきた負極を用いることができ、例えば、負極活物質と、結着剤とを水あるいは適当な溶媒で混合し、負極集電体に塗布し、乾燥し、圧延することにより得られる。負極集電体には、導電性を有する薄膜体、特に銅などの負極の電位範囲で安定な金属箔や合金箔、銅などの金属表層を有するフィルム等を用いることが好適である。結着剤としては、正極の場合と同様にポリテトラフルオロエチレン(PTFE)等を用いることもできるが、スチレンーブタジエン共重合体(SBR)又はこの変性体等を用いることが好ましい。結着剤は、カルボキシメチルセルロース(CMC)等の増粘剤と併用されてもよい。
非水電解質の溶媒としては、従来から使用されている、エチレンカーボネート、プロピレンカーボネート、ブチレンカーボネート、ビニレンカーボネート等の環状カーボネートや、ジメチルカーボネート、メチルエチルカーボネート、ジエチルカーボネート等の鎖状カーボネートを用いることができる。特に、高誘電率、低粘度、低融点の観点でリチウムイオン伝導度の高い非水系溶媒として、環状カーボネートと鎖状カーボネートとの混合溶媒を用いることが好ましい。また、この混合溶媒における環状カーボネートと鎖状カーボネートとの体積比は、2:8〜5:5の範囲に規制することが好ましい。
セパレータとしては、従来から用いられてきたセパレータを用いることができる。例えば、ポリプロピレン製やポリエチレン製のセパレータ、ポリプロピレン−ポリエチレンの多層セパレータや、セパレータの表面にアラミド系樹脂等の樹脂が塗布されたものを用いることができる。
(実験例1)
[正極活物質の作製]
まず、共沈により得られた[Ni0.50Co0.20Mn0.30](OH)2で表されるニッケルコバルトマンガン複合水酸化物を500℃で焼成して、ニッケルコバルトマンガン複合酸化物を得た。次に水酸化リチウムと上記で得たニッケルコバルトマンガン複合酸化物とを、リチウムと遷移金属全体とのモル比が1.15:1になるように、石川式らいかい乳鉢にて混合した。
上記正極活物質と導電剤としてのカーボンブラックと、結着剤としての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、正極活物質と導電剤と結着剤との質量比が92:5:3となるように秤量し、これらを混練して正極合剤スラリーを調製した。次いで、上記正極合剤スラリーを、アルミニウム箔からなる正極集電体の両面に塗布し、これを乾燥させた後、圧延ローラーにより圧延し、さらにアルミニウム製の集電タブを取り付けることにより、正極集電体の両面に正極合剤層が形成された正極極板を作製した。
正極極板を作製する際に、圧延ローラーより圧延した後、以下の条件で大気曝露を行ったこと以外は、電池A1と同様にして大気曝露した正極極板を用いた電池(電池B1)を作製した。
温度60℃、湿度50%の恒温恒湿槽に3日放置した。
正極活物質の作製において、Li1.07[Ni0.465Co0.186Mn0.279]O2からなる正極活物質粒子に対して、WO3を混合した以外は実験例1の場合と同様にして、三電極式試験セルを作製した。このようにして作製した電池を、以下、電池A2と称する。
正極活物質の作製において、Li1.07[Ni0.465Co0.186Mn0.279]O2を主成分とする正極活物質粒子に対して、炭酸リチウムを混合した以外は、実験例1の場合と同様にして、三電極式試験セルを作製した。このようにして作製した電池を、以下、電池A3と称する。
正極活物質の作製において、Li1.07[Ni0.465Co0.186Mn0.279]O2からなる正極活物質粒子に対して、WO3を混合した後に炭酸リチウムを混合した以外は、実験例1の場合と同様にして、三電極式試験セルを作製した。このようにして作製した電池を、以下、電池A4と称する。
正極活物質の作製において、Li1.07[Ni0.465Co0.186Mn0.279]O2からなる正極活物質粒子に対して、炭酸リチウムを混合した後にリン酸リチウムをさらに混合した以外は、実験例4の場合と同様にして、三電極式試験セルを作製した。このようにして作製した電池を、以下、電池A5と称する。
25℃の温度条件下において、0.2mA/cm2の電流密度で4.3V(vs.Li/Li+)まで定電流充電を行い、4.3V(vs. Li/Li+)の定電圧で電流密度が0.04mA/cm2になるまで定電圧充電を行い、初期充電容量を測定した。
上記で求めた初期充電容量のうち、大気曝露なし(大気曝露していない正極極板使用時)の電池の初期充電容量を「曝露なし初期充電容量」とし、大気曝露あり(大気曝露した正極極板使用時)の電池の初期充電容量を「曝露あり初期充電容量」とし、下記に示す式(1)に基づき、対応する電池の曝露なし初期充電容量と曝露あり初期充電容量の差から大気曝露による劣化充電容量を算出した。
大気曝露による劣化充電容量=曝露なし初期充電容量−曝露あり初期充電容量 (1)
(実験例6)
まず、共沈による得られた[Ni0.5Co0.20Mn0.30](OH)2で表されるニッケルコバルトマンガン複合水酸化物を500℃で焼成して、ニッケルコバルトマンガン複合酸化物を得た。次に水酸化リチウムと上記で得たニッケルコバルトマンガン複合酸化物とを、リチウムと、遷移金属全体とのモル比が1.2:1になるように、石川式らいかい乳鉢にて混合した。
正極活物質の作製において、Li1.07[Ni0.465Co0.186Mn0.279]O2からなる正極活物質粒子に対して、炭酸リチウムを混合した以外は、実験例6の場合と同様にして、三電極式試験セルを作製した。このようにして作製した電池を、以下、電池A8と称する。
正極活物質の作製において、Li1.07[Ni0.465Co0.186Mn0.279]O2にWO3を混合した後に炭酸リチウムを混合したこと以外は、実験例6と同様にして三電極式試験セルを作製した。このようにして作製した電池を、以下、電池A9と称する。
正極活物質の作製において、Li1.07[Ni0.465Co0.186Mn0.279]O2に炭酸リチウムを混合した後にリン酸リチウムをさらに混合した以外は、実験例9の場合と同様にして、三電極式試験セルを作製した。このようにして作製した電池を、以下、電池A10と称する。
12 対極(負極)
13 参照極
14 非水電解液
20 三電極式試験セル
31 炭酸リチウム
32 酸化タングステン
33 リチウムニッケルコバルトマンガン複合酸化物
Claims (10)
- リチウム遷移金属酸化物を含む非水電解質二次電池用正極であって、
リチウム遷移金属酸化物と、酸化タングステンと、炭酸化合物とを混合してなり、
前記リチウム遷移金属酸化物の表面の少なくとも一部に、酸化タングステンが点在して付着しており、
前記酸化タングステンの表面の一部に、混合した炭酸化合物が付着しており、
前記炭酸化合物は、前記酸化タングステンを介して前記リチウム遷移金属酸化物に接しており、
前記炭酸化合物は、炭酸リチウム、炭酸二水素リチウム、炭酸コバルト、炭酸ニッケル、炭酸マンガン、炭酸カリウムおよび炭酸二水素アンモニウムから選択される少なくとも一種である、非水電解質二次電池用正極。
- 前記炭酸化合物が、リチウム遷移金属酸化物に対して0.5質量%以上、5質量%以下含まれる請求項1に記載の非水電解質二次電池用正極。
- 前記炭酸化合物が炭酸リチウムである請求項1または2に記載の非水電解質二次電池用正極。
- 前記炭酸リチウムは、混合する量が正極中に含まれる炭酸リチウムの50質量%以上であることを特徴とする請求項3に記載の非水電解質二次電池用正極。
- 前記酸化タングステンがWO3である請求項1〜4のいずれかに記載の非水電解質二次電池用正極。
- 前記リチウム遷移金属酸化物は一般式Li1+xMaO2+b(式中、x、aおよびbは、x+a=1、−0.2<x≦0.2、−0.1≦b≦0.1の条件を満たし、MはNi、Co、Mn及びAlからなる群より少なくとも一種の元素を含む)で表される請求項1〜5のいずれかに記載の非水電解質二次電池用正極。
- リン酸化合物が含まれる請求項1〜6のいずれかに記載の非水電解質二次電池用正極。
- 前記酸化タングステンの表面の一部に、前記リン酸化合物を有する請求項7に記載の非水電解質二次電池用正極。
- 前記リン酸化合物が、リン酸リチウムである請求項7または8に記載の非水電解質二次電池用正極。
- 請求項1〜9のいずれかに記載の非水電解質二次電池用正極を用いた、非水電解質二次電池。
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JPWO2016051653A1 (ja) | 2017-07-13 |
US20170194628A1 (en) | 2017-07-06 |
CN106716685A (zh) | 2017-05-24 |
WO2016051653A1 (ja) | 2016-04-07 |
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