JP5465173B2 - 炭素がコーティングされたリン酸マンガンリチウムカソード材料 - Google Patents
炭素がコーティングされたリン酸マンガンリチウムカソード材料 Download PDFInfo
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- JP5465173B2 JP5465173B2 JP2010515635A JP2010515635A JP5465173B2 JP 5465173 B2 JP5465173 B2 JP 5465173B2 JP 2010515635 A JP2010515635 A JP 2010515635A JP 2010515635 A JP2010515635 A JP 2010515635A JP 5465173 B2 JP5465173 B2 JP 5465173B2
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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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- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
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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
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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
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
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- H—ELECTRICITY
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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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- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Description
表1は、検討中の種々の材料を集めている。
表2は、測定サンプルのラマンバンド及び文献との比較をまとめている。バンドの帰属:ν2 a V4−PO4の対称及び非対称の変角、ν1 a ν3−PO4の対称及び非対称の伸縮;強度:vw−非常に弱い、w−弱い、m−中程度、s−強い。
最初のステップでは、純粋なLiMnPO4(703061−P)を従来技術より公知の方法によって調製した。例えば、国際公開第2007/049815号には、優れた結晶性及び高純度を有するLiMnPO4の製造方法が開示されている。方法の別の例は、国際公開第2007/113624号に開示されており、純粋なLiMnPO4の「ポリオール」合成が記載されている。
LiMnPO4をカーボンブラック20重量%とともにアルゴン下で単純に粉砕することによってLiMnPO4/炭素複合材料(サンプルA)を調製し、次に230℃で終夜乾燥させた。
本発明による材料のマイクロラマン分析を、ペルチェ冷却CCD検出器が接続されたマルチチャネルのレニショー・イン・バイア・リフレックス(Renishaw In Via Reflex)分光計上で行った。励起は、ダイオードレーザーの785nm線、又はAr+レーザーの514.5nm線で行った。サンプルは、100〜3700cm−1の波数シフトで2cm−1のスペクトル分解能においてスキャンした。較正は、520.2cm−1においてSiモードを使用して行った。各ラマンスペクトルのスキャンパラメーターは、通常10秒とし、10(純粋サンプルの場合)から30(アセチレンブラックを有するサンプルの場合)のスキャンを、より良い信号対ノイズ比を得るために各実験ごとに蓄積した。スペクトルの再現性をチェックするために、同じサンプルの異なる領域上で複数のスポット解析を行った。
本発明に記載される材料を使用して、カソード電極を作製した。LiMnPO4/C材料(90重量%)と、ポリ(フッ化ビニリデン)(PVdF)バインダー(5重量%)及びアセチレンブラック(5重量%)とのN−メチルピロリドン(NMP)スラリーをアルミニウム集電体上にテープキャスティングすることによって、電気化学的試験用の電極を作製した。真空下160℃で乾燥させた後、電極を、厚さ50〜60μmで23mmφの円板に圧縮し、活性物質充填量は8mg/cm2であった。Li金属箔を対電極として使用し、微孔質ポリマーセパレーター(Celgard 2400(商標))及びプロピレンカーボネート(PC)とエチレンカーボネート(EC)と炭酸ジメチル(DMC)との溶媒混合物(体積比1:1:3)中に1M LiPF6を含有する液体電解質混合物を使用して、セルをSwagelok(商標)取付具中で組み立てた。LiMnPO4電極の電気化学的性質は、Arbin BT 2000電気化学測定システムを使用して、低電流条件での充電/放電及びサイクリックボルタンメトリーによって測定した。
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Claims (8)
- 化学式C/LiMnPO4又はC/LiMn1−xZxPO4(式中、Z=Fe、Co、Ni、Mg、Ca、Al、Zr、V、Ti、x=0.01〜0.3)を有する、電気活性な炭素でコーティングされた材料であって、酸化マンガン界面層をLiMnPO4材料、LiMn1−xZxPO4材料のそれぞれと、炭素層との間に含み、前記酸化マンガン界面層が湿潤条件下での高エネルギー粉砕によるLiMnPO4 又はLiMn 1−x Z x PO 4 (式中、Z=Fe、Co、Ni、Mg、Ca、Al、Zr、V、Ti、x=0.01〜0.3)の酸化によって調製されることを特徴とする材料。
- 前記酸化マンガン界面層が、Mn3O4(ハウスマンナイト)、β−MnO2(パイロルサイト)、MnO(マンガノサイト)、MnOOH(グロウタイト)又はMn 1.85 O・6H2O(バーネサイト)のいずれかである、請求項1に記載の材料。
- 酸化マンガン濃度が、前記電気活性な炭素でコーティングされた材料に対して、0.01〜5%である、請求項1又は2に記載の材料。
- 含水率が0.5〜20%である、請求項1に記載の材料。
- 前記高エネルギー粉砕されるステップにおいてLiOH溶液が前記湿潤条件下に加えられる、請求項1に記載の材料。
- 130℃〜300℃の加熱処理をさらに含む、請求項1から5のいずれか一項に記載の材料。
- 請求項1から6のいずれか一項に記載の材料を含む、充電式電池。
- (a)アノード、カソード、並びに前記アノード及びカソードと接触し、それらを分離する電解質と、(b)前記カソードと電子的に接触しているカソード集電体と、(c)前記アノードと電子的に接触しているアノード集電体とを含み、前記アノード及びカソードの少なくとも1つが請求項1に記載の材料を含む、電気化学デバイス。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP07112490A EP2015382A1 (en) | 2007-07-13 | 2007-07-13 | Carbon coated lithium manganese phosphate cathode material |
EP07112490.3 | 2007-07-13 | ||
PCT/IB2008/052678 WO2009010895A1 (en) | 2007-07-13 | 2008-07-03 | Carbon coated lithium manganese phosphate cathode material |
Publications (2)
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JP2010533354A JP2010533354A (ja) | 2010-10-21 |
JP5465173B2 true JP5465173B2 (ja) | 2014-04-09 |
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JP2010515635A Expired - Fee Related JP5465173B2 (ja) | 2007-07-13 | 2008-07-03 | 炭素がコーティングされたリン酸マンガンリチウムカソード材料 |
Country Status (9)
Country | Link |
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US (1) | US8357468B2 (ja) |
EP (2) | EP2015382A1 (ja) |
JP (1) | JP5465173B2 (ja) |
KR (1) | KR101542060B1 (ja) |
CN (1) | CN101803075B (ja) |
AT (1) | ATE522941T1 (ja) |
CA (1) | CA2699999C (ja) |
TW (1) | TWI449248B (ja) |
WO (1) | WO2009010895A1 (ja) |
Families Citing this family (35)
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JP4991706B2 (ja) * | 2005-06-06 | 2012-08-01 | ダウ グローバル テクノロジーズ エルエルシー | リチウム再充電可能電気化学セル |
US7964118B2 (en) * | 2005-09-21 | 2011-06-21 | Kanto Denka Kogyo Co., Ltd. | Positive electrode active material and method of producing the same and nonaqueous electrolyte battery having positive electrode containing positive electrode active material |
JP5113081B2 (ja) * | 2006-02-14 | 2013-01-09 | ダウ グローバル テクノロジーズ エルエルシー | リチウム二次電池用リチウムマンガンリン酸塩正極材料 |
EP1901388A1 (en) * | 2006-09-14 | 2008-03-19 | High Power Lithium S.A. | Overcharge and overdischarge protection in lithium-ion batteries |
TWI466370B (zh) * | 2008-01-17 | 2014-12-21 | A123 Systems Inc | 鋰離子電池的混合式金屬橄欖石電極材料 |
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CA2699999C (en) | 2016-05-24 |
TW200913354A (en) | 2009-03-16 |
TWI449248B (zh) | 2014-08-11 |
KR20100048994A (ko) | 2010-05-11 |
ATE522941T1 (de) | 2011-09-15 |
WO2009010895A1 (en) | 2009-01-22 |
JP2010533354A (ja) | 2010-10-21 |
EP2015382A1 (en) | 2009-01-14 |
EP2210300B1 (en) | 2011-08-31 |
EP2210300A1 (en) | 2010-07-28 |
CA2699999A1 (en) | 2009-01-22 |
US8357468B2 (en) | 2013-01-22 |
CN101803075A (zh) | 2010-08-11 |
US20100178562A1 (en) | 2010-07-15 |
KR101542060B1 (ko) | 2015-08-06 |
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