JP5381330B2 - 電極合剤、電極および非水電解質二次電池 - Google Patents
電極合剤、電極および非水電解質二次電池 Download PDFInfo
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- JP5381330B2 JP5381330B2 JP2009127497A JP2009127497A JP5381330B2 JP 5381330 B2 JP5381330 B2 JP 5381330B2 JP 2009127497 A JP2009127497 A JP 2009127497A JP 2009127497 A JP2009127497 A JP 2009127497A JP 5381330 B2 JP5381330 B2 JP 5381330B2
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- secondary battery
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- aqueous electrolyte
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Classifications
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
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- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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Description
すなわち本発明は、下記の発明を提供する。
<1>平均粒径が1μm以下のリチウムニッケルマンガン複合金属酸化物と、導電剤と、過充電防止剤とを有することを特徴とする電極合剤。
<2>リチウムニッケルマンガン複合金属酸化物が、以下の式(1)で表される前記<1>記載の電極合剤。
Liz(Ni1-x-yMnxMy)O2 (1)
(ここで、xは0を超え1未満の範囲の値であり、yは0以上1未満の範囲の値であり、x+yは0を超え1未満の範囲の値であり、zは、0.5以上1.5以下の範囲の値である。Mは、Co、Al、B、Ti、MgおよびFeからなる群より選ばれる1種以上を表す。)
<3>過充電防止剤が、芳香族化合物である前記<1>または<2>記載の電極合剤。
<4>過充電防止剤が、アラミド、ポリエーテル、ポリスルホンおよびポリエーテルスルホンからなる群より選ばれる1種以上である前記<1>〜<3>のいずれかに記載の電極合剤。
<5>導電剤が、炭素材料である前記<1>〜<4>のいずれかに記載の電極合剤。
<6>さらに、結着剤および/または有機溶媒を有する前記<1>〜<5>のいずれかに記載の電極合剤。
<7>粘度が2000mPa・s以上10000mPa・s以下の範囲である前記<6>記載の電極合剤。
<8>前記<1>〜<7>のいずれかに記載の電極合剤を有する電極。
<9>正極、リチウムイオンをドープ・脱ドープすることのできる負極、セパレータおよび非水電解液を有し、該正極が前記<8>記載の電極である非水電解質二次電池。
<10>非水電解液が過充電防止剤を有する前記<9>記載の非水電解質二次電池。
<11>非水電解液における過充電防止剤が、芳香族化合物である前記<10>記載の非水電解質二次電池。
<12>非水電解液における過充電防止剤が、ジフェニルエーテル、ジフェニルエーテル誘導体、ジフェニルスルホンおよびジフェニルスルホン誘導体からなる群より選ばれる1種以上である前記<10>または<11>記載の非水電解質二次電池。
<13>セパレータが、耐熱多孔層と多孔質フィルムとが積層されてなる積層フィルムからなる前記<9>〜<12>のいずれかに記載の非水電解質二次電池。
Liz(Ni1-x-yMnxMy)O2 (1)
(ここで、xは0を超え1未満の範囲の値であり、yは0以上1未満の範囲の値であり、x+yは0を超え1未満の範囲の値であり、zは、0.5以上1.5以下の範囲の値である。Mは、Co、Al、B、Ti、MgおよびFeからなる群より選ばれる1種以上を表す。)
(1)Ni、Mn、Clおよび必要に応じてMを含有する水溶液とアルカリとを接触させて共沈物スラリーを得る工程。
(2)該共沈物スラリーから、共沈物を得る工程。
(3)該共沈物とリチウム化合物、必要に応じて不活性溶融剤とを混合して得られる混合物を、900℃未満の温度で保持して焼成してリチウムニッケルマンガン複合金属酸化物を得る工程。
(2´)該共沈物スラリーを固液分離後、洗浄、乾燥して、共沈物を得る工程。
(ここで、R1、R2は、それぞれ独立に、C=O−NH、OおよびSO2からなる群より選ばれる1種を表す。nは、3以上100000以下の範囲の値である。)
(ここで、R3、R4は、それぞれ独立に、H、CH3およびO−CH3からなる群より選ばれる1種を表す。)
リチウム複合金属酸化物の粉末X線回折測定は株式会社リガク製RINT2500TTR型を用いて行った。測定は、リチウム複合金属酸化物を専用の基板に充填し、CuKα線源を用いて、回折角2θ=10°〜90°の範囲にて行い、粉末X線回折図形を得た。
粉末1gを窒素雰囲気中150℃、15分間乾燥した後、マイクロメトリックス製フローソーブII2300を用いて測定した。
粉末を塩酸に溶解させた後、誘導結合プラズマ発光分析法(SPS3000、以下ICP−AESと呼ぶことがある)を用いて測定した。
リチウム複合金属酸化物を構成する粒子をサンプルステージ上に貼った導電性シート上に載せ、日本電子株式会社製JSM−5510を用いて、加速電圧が20kVの電子線を照射してSEM観察を行った。粒子の粒子径の平均値は、SEM観察により得られた画像(SEM写真)から任意に50個の粒子を抽出し、それぞれの粒子径を測定し、それらの平均値を算出することにより求めた。
ポリプロピレン製ビーカー内で、蒸留水200mlに、水酸化カリウム83.88gを添加、攪拌により溶解し、水酸化カリウムを完全に溶解させ、水酸化カリウム水溶液(アルカリ水溶液)を調製した。また、ガラス製ビーカー内で、蒸留水200mlに、塩化ニッケル(II)六水和物15.68g、塩化マンガン(II)四水和物を13.66g、塩化鉄(II)四水和物2.982gとしたを添加、攪拌により溶解し、ニッケル−マンガン−鉄混合水溶液を得た。前記水酸化カリウム水溶液を攪拌しながら、これに前記ニッケル−マンガン−鉄混合水溶液を滴下することにより、共沈物が生成し、共沈物スラリーを得た。次いで、共沈物スラリーについて、ろ過・蒸留水洗浄を行い、100℃で乾燥させて共沈物P1を得た。該共沈物P1のSEM観察における一次粒子の粒子径は、その平均値が0.05μmであり、BET比表面積は63m2/gであった。また、P1の組成分析の結果、Ni:Mn:Feのモル比は0.44:0.46:0.10であった。
結着剤としてポリフッ化ビニリデン(PVdF)を用い、有機溶媒としてN−メチル−2−ピロリドン(NMP)を用いて、結着剤を有機溶媒に溶解させて、結着剤溶液を作製した。ここでは、NMP90重量部にPVdF10重量部を溶解させた。
過充電防止剤1として、アラミドを用いた。有機溶媒であるNMP90重量部にアラミド10重量部を溶解させて、過充電防止剤溶液1を作製した。
過充電防止剤2として、ポリエーテルスルホン(PES)を用いた。有機溶媒であるNMP90重量部にPES10重量部を溶解させて、過充電防止剤溶液2を作製した。
上記で得られたリチウムニッケルマンガン複合金属酸化物を用い、該酸化物85重量部と、導電剤(アセチレンブラックと黒鉛を9:1で混合したもの)を10重量部、結着剤を4重量部、過充電防止剤を1重量部およびNMP45重量部を混合、混練して、さらに、NMPを添加して、粘度を5000mPa・sに調整して、電極合剤1を得た。この電極合剤1を、ドクターブレード法により厚み15μmのアルミニウム箔からなる集電体上に両面に塗布し、60℃、2時間乾燥後、更に150℃、10時間真空乾燥させてNMPを揮発させた後、圧延した。乾燥後の電極合剤塗工量は15.0mg/cm2であった。このようにして電極合剤が集電体に塗布された電極1を得た。
結着剤、過充電防止剤1のそれぞれを、3重量部、2重量部とした以外は電極1と同様にして、電極2を得た。
過充電防止剤1にかえて過充電防止剤2を用いた以外は電極1と同様にして、電極3を得た。
過充電防止剤1にかえて過充電防止剤2を用いた以外は、電極2と同様にして、電極4を得た。
結着剤を5重量部とし、過充電防止剤を使用しないこと以外は電極1と同様にして、電極5を得た。
負極材料として、平均粒径が10μmの炭素材料(大阪ガスケミカル(株)製MCMB)と、上記結着剤溶液を用いて、負極材料90重量部と結着剤10重量部を混合、混練して、さらに、NMPを添加して、粘度を5000mPa・sに調整して、負極合剤を得た。この負極合剤を、ドクターブレード法により厚み10μmの銅箔からなる集電体上に両面に塗布し、60℃、2時間乾燥後、更に150℃、10時間真空乾燥させてNMPを揮発させた後、圧延した。乾燥後の負極合材塗工量は7.5mg/cm2であった。このようにして負極合剤が集電体に塗布された負極を得た。
エチレンカーボネート(EC)とジメチルカーボネート(DMC)とエチルメチルカーボネート(EMC)をEC:DMC:EMC=30:35:35(体積比)で混合させてなる混合溶媒に、LiPF6を1モル/リットルになるように溶解して、電解液1を作製した。
非水電解液1に過充電防止剤であるジフェニルエーテルを5重量部添加して、電解液2を作製した。
非水電解液1に過充電防止剤であるジフェニルエーテルを20重量部添加して、電解液3を作製した。
上記の電極1を正極として用いて、該正極と負極とを、ポリプロピレン製多孔質セパレータを介して積層、巻回し、電池サイズ長さ62mm、幅35mm、厚さ3.6mmの電極群を作製した。これをアルミラミネート製の電池ケースに収容し、上記の電解液1を注液してから、電池ケース上部を熱封口して、電池1を作製した。
正極として上記の電極2を用いた以外は、電池1と同様にして電池2を得た。
正極として上記の電極3を用いた以外は、電池1と同様にして電池3を得た。
正極として上記の電極4を用いた以外は、電池1と同様にして電池4を得た。
正極として上記の電極5を用いた以外は、電池1と同様にして電池5を得た。
電解液1にかえて電解液2を用いた以外は、電池1と同様にして電池6を得た。
電解液1にかえて電解液2を用いた以外は、電池5と同様にして電池7を得た。
電解液1にかえて電解液3を用いた以外は、電池5と同様にして電池8を得た。
作製した電池1〜8を室温で10時間放置して、電極に電解液を十分含浸させた。次に室温において0.2Cのレートで4.2Vまで定電流充電してから4.2Vで定電圧充電する定電流定電圧充電を8時間行った後、0.2Cのレートで3.0Vまで放電する定電流放電を行うことで初期充放電を行い、初期放電容量を測定し、過充電防止剤を有する電極合剤を用いた電池1、2、3、4および6においても、電池5と比べて初期放電容量が低下しないことを確認した。
初期充放電を行った電池1〜8を室温において0.2Cのレートで4.2Vまで定電流充電してから4.2Vで定電圧充電する定電流定電圧充電を8時間行った後、10Cのレートで3.0Vまで放電する定電流放電を行うことで、出力特性評価を行った結果、過充電防止剤を有する電極合剤を用いた電池1、2、3、4および6においても、電池5と比べて、出力特性が低下しないことがわかった。また、電池8においては、出力特性が大きく低下した。なお、出力特性は、次の式により評価した。
放電容量維持率(%)=10Cのレートにおける放電容量/初期放電容量×100
初期充放電後、電池1〜8を室温において2Cのレートで定電流充電して、初期放電容量の200%の容量を電池に充電したところ、電池1、2、3、4、6および8は、膨れが確認されなかった一方で、電池7は電池中央部に約2mmの膨れが認められ、電池5は、電池中央部に5mmの膨れが認められた。これらの膨れは、過充電による電解液の分解反応によるものと推定している。
(1)塗工液の製造
NMP4200gに塩化カルシウム272.7gを溶解した後、パラフェニレンジアミン132.9gを添加して完全に溶解させた。得られた溶液に、テレフタル酸ジクロライド243.3gを徐々に添加して重合し、パラアラミドを得て、さらにNMPで希釈して、濃度2.0重量%のパラアラミド溶液(A)を得た。得られたパラアラミド溶液100gに、アルミナ粉末(a)2g(日本アエロジル社製、アルミナC、平均粒子径0.02μm)とアルミナ粉末(b)2g(住友化学株式会社製スミコランダム、AA03、平均粒子径0.3μm)とをフィラーとして計4g添加して混合し、ナノマイザーで3回処理し、さらに1000メッシュの金網で濾過、減圧下で脱泡して、スラリー状塗工液(B)を製造した。パラアラミドおよびアルミナ粉末の合計重量に対するアルミナ粉末(フィラー)の重量は、67重量%となる。
多孔質フィルムとしては、ポリエチレン製多孔質膜(膜厚12μm、透気度140秒/100cc、平均孔径0.1μm、空孔率50%)を用いた。厚み100μmのPETフィルムの上に上記ポリエチレン製多孔質膜を固定し、テスター産業株式会社製バーコーターにより、該多孔質膜の上にスラリー状塗工液(B)を塗工した。PETフィルム上の塗工された該多孔質膜を一体にしたまま、貧溶媒である水中に浸漬させ、パラアラミド多孔質膜(耐熱多孔層)を析出させた後、溶媒を乾燥させて、耐熱多孔層と多孔質フィルムとが積層された積層フィルム1を得た。積層フィルム1の厚みは16μmであり、パラアラミド多孔質膜(耐熱多孔層)の厚みは4μmであった。積層フィルム1の透気度は180秒/100cc、空孔率は50%であった。積層フィルム1における耐熱多孔層の断面を走査型電子顕微鏡(SEM)により観察をしたところ、0.03μm〜0.06μm程度の比較的小さな微細孔と0.1μm〜1μm程度の比較的大きな微細孔とを有することがわかった。尚、積層フィルムの評価は以下の方法で行った。
(A)厚み測定
積層フィルムの厚み、多孔質フィルムの厚みは、JIS規格(K7130−1992)に従い、測定した。また、耐熱多孔層の厚みとしては、積層フィルムの厚みから多孔質フィルムの厚みを差し引いた値を用いた。
(B)ガーレー法による透気度の測定
積層フィルムの透気度は、JIS P8117に基づいて、株式会社安田精機製作所製のデジタルタイマー式ガーレー式デンソメータで測定した。
(C)空孔率
得られた積層フィルムのサンプルを一辺の長さ10cmの正方形に切り取り、重量W(g)と厚みD(cm)を測定した。サンプル中のそれぞれの層の重量(Wi(g))を求め、Wiとそれぞれの層の材質の真比重(真比重i(g/cm3))とから、それぞれの層の体積を求めて、次式より空孔率(体積%)を求めた。
空孔率(体積%)=100×{1−(W1/真比重1+W2/真比重2+・・+Wn/真比重n)/(10×10×D)}
Claims (7)
- 過充電防止剤を含む非水電解液、正極、リチウムイオンをドープ・脱ドープすることのできる負極およびセパレータを有し、該正極が、平均粒径が1μm以下のリチウムニッケルマンガン複合金属酸化物と、導電剤と、芳香族化合物であって、アラミド、ポリエーテル、ポリスルホンおよびポリエーテルスルホンからなる群より選ばれる1種以上である過充電防止剤とを有する電極である非水電解質二次電池。
- リチウムニッケルマンガン複合金属酸化物が、以下の式(1)で表される請求項1記載の非水電解質二次電池。
Liz(Ni1-x-yMnxMy)O2 (1)
(ここで、xは0を超え1未満の範囲の値であり、yは0以上1未満の範囲の値であり、x+yは0を超え1未満の範囲の値であり、zは、0.5以上1.5以下の範囲の値である。Mは、Co、Al、B、Ti、MgおよびFeからなる群より選ばれる1種以上を表す。) - 導電剤が、炭素材料である請求項1または2記載の非水電解質二次電池。
- さらに、正極に、結着剤を有する請求項1〜3のいずれかに記載の非水電解質二次電池。
- 非水電解液における過充電防止剤が、芳香族化合物である請求項1〜4のいずれかに記載の非水電解質二次電池。
- 非水電解液における過充電防止剤が、ジフェニルエーテル、ジフェニルエーテル誘導体、ジフェニルスルホンおよびジフェニルスルホン誘導体からなる群より選ばれる1種以上である請求項1〜5のいずれかに記載の非水電解質二次電池。
- セパレータが、耐熱多孔層と多孔質フィルムとが積層されてなる積層フィルムからなる請求項1〜6のいずれかに記載の非水電解質二次電池。
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JP2009127497A JP5381330B2 (ja) | 2009-05-27 | 2009-05-27 | 電極合剤、電極および非水電解質二次電池 |
EP10780684A EP2437334A1 (en) | 2009-05-27 | 2010-05-26 | Electrode mix, electrode, and non-aqueous electrolyte secondary battery |
PCT/JP2010/059299 WO2010137730A1 (ja) | 2009-05-27 | 2010-05-26 | 電極合剤、電極および非水電解質二次電池 |
CN201080022731.6A CN102449820B (zh) | 2009-05-27 | 2010-05-26 | 电极合剂、电极以及非水电解质二次电池 |
US13/322,373 US20120082883A1 (en) | 2009-05-27 | 2010-05-26 | Electrode mix, electrode, and non-aqueous electrolyte secondary battery |
KR1020117030685A KR101678712B1 (ko) | 2009-05-27 | 2010-05-26 | 전극 합제, 전극 및 비수전해질 이차 전지 |
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JP2009127497A JP5381330B2 (ja) | 2009-05-27 | 2009-05-27 | 電極合剤、電極および非水電解質二次電池 |
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US (1) | US20120082883A1 (ja) |
EP (1) | EP2437334A1 (ja) |
JP (1) | JP5381330B2 (ja) |
KR (1) | KR101678712B1 (ja) |
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JP5433529B2 (ja) * | 2010-08-25 | 2014-03-05 | 株式会社日立製作所 | リチウムイオン二次電池 |
JP5920638B2 (ja) * | 2011-05-02 | 2016-05-18 | トヨタ自動車株式会社 | 非水電解質二次電池 |
US10361431B2 (en) * | 2012-03-30 | 2019-07-23 | Nec Corporation | Lithium ion secondary battery |
CN108417891A (zh) * | 2017-02-10 | 2018-08-17 | 中信国安盟固利动力科技有限公司 | 一种防过充锂离子电解液及由其制备的锂离子电池 |
CN108365223A (zh) * | 2018-02-10 | 2018-08-03 | 中国科学院苏州纳米技术与纳米仿生研究所南昌研究院 | 一种用于锂离子电池正极材料的碳纳米管导电剂及其制备方法 |
CN116722101A (zh) * | 2018-12-26 | 2023-09-08 | 株式会社Lg新能源 | 包含草酸的正极浆料、其制备方法、正极和二次电池 |
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JP4525649B2 (ja) * | 1997-02-05 | 2010-08-18 | 住友化学株式会社 | リチウム二次電池用正極およびリチウム二次電池 |
JP2002050345A (ja) * | 2000-08-07 | 2002-02-15 | Mitsubishi Chemicals Corp | リチウム二次電池用正極材料、リチウム二次電池用正極及びリチウム二次電池 |
WO2002073718A1 (fr) * | 2001-03-14 | 2002-09-19 | Yuasa Corporation | Matiere active pour electrode positive et accumulateur a electrolyte non aqueux comportant ladite matiere |
JP2003007303A (ja) * | 2001-06-22 | 2003-01-10 | Sony Corp | 非水電解質電池 |
JP4380664B2 (ja) * | 2002-07-24 | 2009-12-09 | 三菱化学株式会社 | 非水系電解液二次電池および非水系電解液 |
EP1705736B1 (en) * | 2003-12-15 | 2015-08-26 | Mitsubishi Chemical Corporation | Nonaqueous electrolyte secondary battery |
JP2005268206A (ja) * | 2004-02-16 | 2005-09-29 | Sony Corp | 正極合剤、非水電解質二次電池およびその製造方法 |
JP4608943B2 (ja) * | 2004-05-19 | 2011-01-12 | パナソニック株式会社 | 非水電解質リチウム二次電池 |
JP5403845B2 (ja) * | 2004-07-06 | 2014-01-29 | 三菱化学株式会社 | 非水系電解液及びそれを用いたリチウム二次電池 |
US20080118833A1 (en) * | 2004-11-19 | 2008-05-22 | Atsushi Ueda | Non-Aqueous Electrolyte Secondary Battery |
KR100773247B1 (ko) * | 2005-04-20 | 2007-11-05 | 주식회사 엘지화학 | 향상된 과충전 안전성의 리튬 이차전지 |
JP4934999B2 (ja) * | 2005-06-27 | 2012-05-23 | 三菱化学株式会社 | 非水系電解液及び非水系電解液電池 |
CN101292380B (zh) * | 2005-10-21 | 2010-08-11 | 阿尔特尔纳米技术公司 | 锂离子电池 |
JP2007200795A (ja) * | 2006-01-30 | 2007-08-09 | Matsushita Electric Ind Co Ltd | リチウムイオン二次電池 |
JP5332121B2 (ja) * | 2006-04-21 | 2013-11-06 | 住友化学株式会社 | 正極活物質粉末 |
KR101386330B1 (ko) * | 2006-04-21 | 2014-04-17 | 스미또모 가가꾸 가부시끼가이샤 | 정극 활물질 분말 |
JP5095121B2 (ja) * | 2006-04-28 | 2012-12-12 | パナソニック株式会社 | 非水電解質二次電池用セパレータおよび非水電解質二次電池 |
JP2008307893A (ja) * | 2007-05-14 | 2008-12-25 | Sumitomo Chemical Co Ltd | 積層多孔質フィルム |
JP4740415B2 (ja) * | 2007-05-25 | 2011-08-03 | 株式会社日立製作所 | 電気自動車或いはハイブリッド自動車用リチウム二次電池 |
JP4943242B2 (ja) * | 2007-06-20 | 2012-05-30 | ソニー株式会社 | リチウムイオン二次電池 |
JP5481786B2 (ja) * | 2007-07-03 | 2014-04-23 | 住友化学株式会社 | リチウム複合金属酸化物 |
JP2009099418A (ja) * | 2007-10-17 | 2009-05-07 | Hitachi Vehicle Energy Ltd | リチウム二次電池用正極材料及びこれを用いたリチウム二次電池 |
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- 2010-05-26 CN CN201080022731.6A patent/CN102449820B/zh active Active
- 2010-05-26 KR KR1020117030685A patent/KR101678712B1/ko active IP Right Grant
- 2010-05-26 US US13/322,373 patent/US20120082883A1/en not_active Abandoned
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JP2010277756A (ja) | 2010-12-09 |
WO2010137730A1 (ja) | 2010-12-02 |
CN102449820A (zh) | 2012-05-09 |
KR101678712B1 (ko) | 2016-11-23 |
EP2437334A1 (en) | 2012-04-04 |
CN102449820B (zh) | 2014-09-03 |
US20120082883A1 (en) | 2012-04-05 |
KR20120027380A (ko) | 2012-03-21 |
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