JP5907682B2 - リチウム2次電池の正極保護膜用組成物、前記正極保護膜を含むリチウム2次電池およびその製造方法 - Google Patents
リチウム2次電池の正極保護膜用組成物、前記正極保護膜を含むリチウム2次電池およびその製造方法 Download PDFInfo
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- JP5907682B2 JP5907682B2 JP2011174685A JP2011174685A JP5907682B2 JP 5907682 B2 JP5907682 B2 JP 5907682B2 JP 2011174685 A JP2011174685 A JP 2011174685A JP 2011174685 A JP2011174685 A JP 2011174685A JP 5907682 B2 JP5907682 B2 JP 5907682B2
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- positive electrode
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- unsubstituted
- protective film
- borate
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- 230000001681 protective effect Effects 0.000 title claims description 39
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- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 20
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- 125000004185 ester group Chemical group 0.000 description 1
- 239000004210 ether based solvent Substances 0.000 description 1
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 229910052730 francium Inorganic materials 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 229910021385 hard carbon Inorganic materials 0.000 description 1
- 125000004404 heteroalkyl group Chemical group 0.000 description 1
- 125000000592 heterocycloalkyl group Chemical group 0.000 description 1
- 125000000717 hydrazino group Chemical group [H]N([*])N([H])[H] 0.000 description 1
- 125000005638 hydrazono group Chemical group 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- CTAPFRYPJLPFDF-UHFFFAOYSA-O hydron;1,2-oxazole Chemical class C=1C=[NH+]OC=1 CTAPFRYPJLPFDF-UHFFFAOYSA-O 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- KQNPFQTWMSNSAP-UHFFFAOYSA-N isobutyric acid Chemical compound CC(C)C(O)=O KQNPFQTWMSNSAP-UHFFFAOYSA-N 0.000 description 1
- CTAPFRYPJLPFDF-UHFFFAOYSA-N isoxazole Chemical class C=1C=NOC=1 CTAPFRYPJLPFDF-UHFFFAOYSA-N 0.000 description 1
- 239000003273 ketjen black Substances 0.000 description 1
- 239000005453 ketone based solvent Substances 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 229910000686 lithium vanadium oxide Inorganic materials 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000006051 mesophase pitch carbide Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 229940017219 methyl propionate Drugs 0.000 description 1
- 229940057061 mevalonolactone Drugs 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- 239000011255 nonaqueous electrolyte Substances 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- GHZRKQCHJFHJPX-UHFFFAOYSA-N oxacycloundecan-2-one Chemical compound O=C1CCCCCCCCCO1 GHZRKQCHJFHJPX-UHFFFAOYSA-N 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 125000005429 oxyalkyl group Chemical group 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920005735 poly(methyl vinyl ketone) Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 229940058401 polytetrafluoroethylene Drugs 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 229920000973 polyvinylchloride carboxylated Polymers 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- DOKHEARVIDLSFF-UHFFFAOYSA-N prop-1-en-1-ol Chemical group CC=CO DOKHEARVIDLSFF-UHFFFAOYSA-N 0.000 description 1
- 229940090181 propyl acetate Drugs 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229910021384 soft carbon Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical class O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- ZUHZGEOKBKGPSW-UHFFFAOYSA-N tetraglyme Chemical compound COCCOCCOCCOCCOC ZUHZGEOKBKGPSW-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 229910052725 zinc 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
また、前記組成物から形成された正極保護膜を含むリチウム2次電池を提供する。
また、本発明の他の具現例は、前記リチウム2次電池の製造方法を提供する。
前記エステル含有高分子化合物は、置換または非置換されたカルボキシレート含有高分子化合物、置換または非置換された(メタ)アクリレート含有高分子およびこれらの組み合わせより選択される一つを含んでも良い。
本明細書で別途の定義がない限り「ヘテロ」とは、N、O、SおよびPより選択されたヘテロ原子を1〜3個含有したことを意味する。
図1は、本発明の一具現例によるリチウム2次電池を示す概略図であり、図2は、図1のリチウム2次電池の一部分を拡大して示した概略図である。
図1および図2を参照すれば、本発明の一具現例によるリチウム2次電池100は、正極114、正極114と対向する負極112、正極114と負極112との間に配置されているセパレータ113、正極114とセパレータ113との間に位置する正極保護膜115および正極114、負極112およびセパレータ113を含浸する電解液(図示せず)を含む電極群と、前記電極群を内蔵している電池容器120および前記電池容器120を密封する密封部材140を含む。
集電体は、アルミニウム箔などを使用しても良いが、これに限定されるのではない。
正極活物質層は、正極活物質、バインダーおよび導電剤を含む。
正極活物質は、リチウムが可逆的にインターカレーションおよびデインターカレーションすることができる化合物であれば特に制限されず、具体的にリチウム(Li)とコバルト(Co)、マンガン(Mn)、ニッケル(Ni)およびこれらの組み合わせより選択される金属の複合酸化物であっても良い。
バインダーは、正極活物質粒子間の凝集力を高めると同時に正極活物質が集電体上に良好に接着されるようにする。バインダーは、正極活物質の化学的特性に影響を与えると共に、接着性を有する物質であれば特に限定されない。
バインダーは、正極活物質層の総含量に対して約4〜20重量%で含まれても良い。
セパレータ113は、単一膜または多層膜であっても良く、例えば、ポリエチレン、ポリプロピレン、ポリビニリデンフルオライドおよびこれらの組み合わせで作られても良い。
正極保護膜115は、正極114およびセパレータ113の表面に正極保護膜用組成物を塗布して形成しても良い。
高分子化合物は、エステル含有高分子化合物、フッ素系高分子化合物およびこれらの組み合わせより選択される一つであっても良い。
イオン性液体は、陽イオンと陰イオンを含み、常温で液体特性を示す塩(salt)である。
前記高分子化合物、前記イオン性液体および前記溶媒を含む組成物は、溶液形態で製造されて正極114およびセパレータ113の表面で正極保護膜115として形成されても良い。
このような正極保護膜115は、高分子化合物とボレート系陰イオンが結合して形成された高分子ネットワークがマンガンのような遷移金属イオンをトラップしながら高温で正極活物質をなす遷移金属イオンが電解液に溶出されることを抑制することができる。
集電体は、銅箔、ニッケル箔、ステレンス鋼箔、チタニウム箔、ニッケル発泡体(foam)、伝導性金属が塗布された高分子基材などで作られても良いが、これに限定されるのではない。
負極活物質は、リチウムイオンを可逆的にインターカレーションおよびデインターカレーションすることができる化合物であれば特に制限されず、具体的に炭素系負極活物質、リチウムと合金化することができる化合物、遷移金属酸化物、リチウムをドープおよび脱ドープすることができる化合物、リチウムと可逆的に反応することができる化合物およびこれらの組み合わせからなる群より選択されても良い。
バインダーおよび導電剤は、前述したとおりである。
前記非水性有機溶媒は、電池の電気化学的反応に関与するイオンが移動することができる媒質の役割を果たす。前記非水性有機溶媒としては、カーボネート系、エステル系、エーテル系、ケトン系、アルコール系および非プロトン性溶媒より選択されても良い。
まず、前述したように高分子化合物、ボレート系陰イオンを有するイオン性液体および溶媒を混合して正極保護膜用組成物を準備する。
その後、正極114、負極112およびセパレータ113をそれぞれ準備した後、正極114およびセパレータ113の一面に前記正極保護膜用組成物を塗布する。
次に、正極保護膜115が形成された正極114およびセパレータ113を向き合うように配置した後、これを約100℃で熱圧着して正極保護膜115を一体化する。
次に、図1に示すように正極114、負極112およびセパレータ113を含む電極群を形成する。
以下、実施例を通じて前述した本発明の具現例をより詳細に説明する。但し、下記の実施例は単に説明の目的のためのものであり、本発明の範囲を制限するものではない。
<正極保護膜用組成物の製造>
ポリ(ビニリデンフルオライド−ヘキサフルオロプロピレン)(PVdF−HFP、HFP含量5モル%)3重量%、リチウムビス(オキサラト)ボレート(LiBOB)7重量%およびエチルメチルカーボネート(EMC)90重量%を混合して正極保護膜用組成物を製造する。
LiMn2O490重量%、ポリ(ビニリデンフルオライド−ヘキサフルオロプロピレン)(P(VdF−HFP))5重量%およびアセチレンブラック5重量%をN−メチルピロリドンの中で混合して正極スラリーを製造し、この正極スラリーをAl箔に塗布して正極を準備した。また、負極活物質として人造黒鉛を使用し、セパレータとしてポリエチレン材質のフィルムを使用した。
正極保護膜を形成しないことを除いては、実施例1と同様な方法でリチウム2次電池を製造した。
前記正極およびセパレータの一面に前記正極保護膜用組成物の代わりに酸化アルミニウム(Al2O3)でコーティングしたことを除いては、実施例1と同様な方法でリチウム2次電池を製造した。
前述した方法で製造されたリチウム2次電池を60℃で1Cで50回充放電した後、電解液にマンガンイオン(Mn2+)が溶出される程度を測定した。
その結果は表1のとおりである。
以上で本発明の好適な実施例について詳細に説明したが、本発明の権利範囲はこれに限定されるのではなく、次の特許請求の範囲で定義している本発明の基本概念を利用した当業者の多様な変形および改良形態も本発明の権利範囲に属する。
112…正極
114…負極
113…セパレータ
115…正極保護膜
120…電池容器
140…密封部材
Claims (3)
- 正極、
前記正極と対向する負極、
前記正極と負極との間に位置するセパレータ、
前記正極と前記セパレータとの間に位置する正極保護膜、および
前記正極、負極、およびセパレータに含浸する電解液
を含み、
前記正極保護膜は、高分子化合物および前記高分子化合物に結合されているボレート系陰イオンのイオン性液体を含み、
前記ボレート系陰イオンは、ビス(オキサラト)ボレート(BOB)、ジフルオロオキサラトボレート(FOB)、ビス(マロナト)ボレート(BMB)、ビス(ペルフルオロピナコラト)ボレート(BPFPB)およびこれらの組み合わせより選択される陰イオンであり、
前記高分子化合物は、ポリ(ビニリデンフルオライド−ヘキサフルオロプロピレン)であり、
前記高分子化合物と前記イオン性液体との重量の比が、3:7〜20:1であり、
前記正極は、遷移金属を含有する正極活物質を含む、
リチウム2次電池。 - 高分子化合物、ボレート系陰イオンを有するイオン性液体および溶媒を混合して正極保護膜用組成物を準備する段階であって、前記高分子化合物、前記イオン性液体、および前記溶媒は、前記正極保護膜用組成物の総含量に対して、それぞれ1〜20重量%、1〜10重量%、および70〜98重量%の含量で含まれ、且つ、前記高分子化合物と前記イオン性液体との重量の比が、3:7〜20:1である、段階、
正極およびセパレータのうちの少なくとも一つの表面に前記正極保護膜用組成物を塗布する段階、および
前記正極、前記セパレータ、負極、および電解液を含む電極群を形成する段階
を含み、
前記ボレート系陰イオンは、ビス(オキサラト)ボレート(BOB)、ジフルオロオキサラトボレート(FOB)、ビス(マロナト)ボレート(BMB)、ビス(ペルフルオロピナコラト)ボレート(BPFPB)およびこれらの組み合わせより選択される陰イオンであり、
前記高分子化合物は、ポリ(ビニリデンフルオライド−ヘキサフルオロプロピレン)であり、
前記正極は、遷移金属を含有する正極活物質を含む、
リチウム2次電池の製造方法。 - 前記正極保護膜用組成物を塗布する段階後に、前記正極保護膜用組成物を介して前記正極およびセパレータを熱圧着する段階をさらに含む、請求項2に記載のリチウム2次電池の製造方法。
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