JP2014526783A - 電池用正極 - Google Patents
電池用正極 Download PDFInfo
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- JP2014526783A JP2014526783A JP2014530764A JP2014530764A JP2014526783A JP 2014526783 A JP2014526783 A JP 2014526783A JP 2014530764 A JP2014530764 A JP 2014530764A JP 2014530764 A JP2014530764 A JP 2014530764A JP 2014526783 A JP2014526783 A JP 2014526783A
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- Prior art keywords
- coating
- core
- electrode
- active material
- coated
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- 238000000576 coating method Methods 0.000 claims abstract description 98
- 239000011248 coating agent Substances 0.000 claims abstract description 92
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- 238000010438 heat treatment Methods 0.000 claims abstract description 30
- 239000007772 electrode material Substances 0.000 claims abstract description 21
- 230000015556 catabolic process Effects 0.000 claims abstract description 5
- 238000006731 degradation reaction Methods 0.000 claims abstract description 5
- 150000001875 compounds Chemical class 0.000 claims description 92
- 239000000463 material Substances 0.000 claims description 67
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- 125000004432 carbon atom Chemical group C* 0.000 claims description 38
- 238000000034 method Methods 0.000 claims description 29
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- 238000004519 manufacturing process Methods 0.000 claims description 6
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- 125000002080 perylenyl group Chemical group C1(=CC=C2C=CC=C3C4=CC=CC5=CC=CC(C1=C23)=C45)* 0.000 claims description 5
- 239000011368 organic material Substances 0.000 claims description 3
- 125000001624 naphthyl group Chemical group 0.000 claims 3
- 125000005582 pentacene group Chemical group 0.000 claims 3
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- 239000007774 positive electrode material Substances 0.000 abstract description 17
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- NQRACBRRMUBSDA-UHFFFAOYSA-N 17-azahexacyclo[10.9.2.02,7.03,19.08,23.015,22]tricosa-1(21),2(7),3,5,8,10,12(23),13,15(22),19-decaene-16,18-dione Chemical compound C12=CC=C3C=CC=C4C5=CC=CC=6C(=CC=C(C1=C34)C56)C(NC2=O)=O NQRACBRRMUBSDA-UHFFFAOYSA-N 0.000 description 2
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- GRSMWKLPSNHDHA-UHFFFAOYSA-N Naphthalic anhydride Chemical compound C1=CC(C(=O)OC2=O)=C3C2=CC=CC3=C1 GRSMWKLPSNHDHA-UHFFFAOYSA-N 0.000 description 2
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- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
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- DXHQCBHTNBRZJT-UHFFFAOYSA-N n-(1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-heptadecafluorooctyl)aniline Chemical compound FC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)NC1=CC=CC=C1 DXHQCBHTNBRZJT-UHFFFAOYSA-N 0.000 description 2
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 description 2
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- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
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- 239000013022 formulation composition Substances 0.000 description 1
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- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 1
- QRRKXCPLJGPVHN-UHFFFAOYSA-N hexabenzocoronene Chemical compound C12C(C(=C34)C(=C56)C7=C89)=C%10C7=C7C%11=CC=CC7=C8C=CC=C9C5=CC=CC6=C3C=CC=C4C1=CC=CC2=C1C%10=C%11C=CC1 QRRKXCPLJGPVHN-UHFFFAOYSA-N 0.000 description 1
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- CPABIEPZXNOLSD-UHFFFAOYSA-N lithium;oxomanganese Chemical compound [Li].[Mn]=O CPABIEPZXNOLSD-UHFFFAOYSA-N 0.000 description 1
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- H01B1/12—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances organic substances
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Abstract
Description
材料および合成方法
炭素フッ化物活性材料は、中程度のエネルギーで炭素前駆体とともにミルに供され、ついで後アニールされた。炭素前駆体は、KJ600(カーボンブラック)、PEG、PVDFおよびショ糖を含んでいた。炭素前駆体量は5wt%であった。アニール条件は、450℃と600℃で、2および6時間であった。
方法は、次の変更を除けば、例1と同一であった:ポリビニリデンフッ化物が炭素前駆体として使用された;炭素前駆体量は3つの条件であった(1、3、5wt%);アニール条件は、450℃と500℃で、3、6および12時間であった。
材料および合成方法
すべての反応は、高純度アルゴンを充てんされたグローブボックス(M-Braun,O2および湿分<0.1ppm)中で行われた。特に特定がなければ、材料は市販源から得られたものであり(たとえば、Sigma-Aldrich, Advanced Research Chemicals Inc., およびAlfa Aesar)、さらなる精製なしで用いられた。
CFx、LMO、およびLMNO粒子がミル処理により導電性炭素材料で被覆された。ミル容器は、ベース正極材料、導電性炭素被覆前駆体材料および溶媒を充てんされた。導電性炭素被覆前駆体材料は0〜5wt%の範囲で充てんされた。容器は密封され、ついでその内容物はミルされた。ミル後に、溶媒は約60℃で蒸発され、そしてある態様において、試料はN2流通下にアニールされた。
被覆CFx粒子の場合において、電極は、活性材料85%、バインダー材料11%、および導電性添加剤4%の配合組成で、次の配合法に従って、調製された:約200mgのPVDF(Sigma Aldrich)が10mLのNMP(Sigma Aldrich)に夜通し溶解された。約72.7mgの導電性添加剤が、その溶液に添加され、数時間撹拌された。約154mgの被覆CFx固体が、この溶液1mLに添加され、夜通し撹拌された。約100μLのスラリーをステンレス鋼カレントコレクター上に落下させて、150℃で約1時間、乾燥することにより、薄膜がキャスト形成された。乾燥薄膜は、冷却され、ついで1トン/cm2の圧力で押圧された。さらに電極は、真空下、150℃で12時間乾燥され、ついで電池組み立てのためにグローブボックスに運ばれた。
被覆LMO、LMNOおよびOLO粒子の場合において、電極は、活性材料85%、バインダー材料7.5%、および導電性添加剤7.5%の配合組成で、次の配合法に従って、調製された:約198mgのPVDF(Sigma Aldrich)および約198mgのSuper P Li(Timcal)が15mLのNMP(Sigma Aldrich)に夜通し溶解された。約150mgの被覆LMO、LMNOまたはOLO固体が、この溶液1mLに添加され、夜通し撹拌された。約66μLのスラリーをステンレス鋼カレントコレクター上に落下させて、150℃で約1時間、乾燥することにより、薄膜がキャスト形成された。乾燥薄膜は、冷却され、ついで1トン/cm2の圧力で押圧された。さらに電極は、真空下、150℃で12時間乾燥され、ついで電池組み立てのためにグローブボックスに運ばれた。
すべての電池は、特に特定がなければ、高純度アルゴンを充てんされたグローブボックス(M-Braun,O2および湿分<0.1ppm)中で組み立てられた。
例1および2により作製された電気化学的セルは、種々の試験方法により試験された。被覆された電極のない電気化学的セルと比較して、ある電気化学的セルは性能の増加を示した。
一次セルとして設計された電極およびセルは、0.1Cおよび1Cで一定の電流放電プロトコールを用いて30℃で電気化学的に特徴付けられた。
二次セルとして設計された電極およびセルは、次のプロトコールを用いて室温(〜23℃)で、電気化学的に特徴付けられた:(1)セルは、1サイクルで条件づけられ、そこでは、充電および放電がC/20のC−レートで生じ、電流がC/100に達するまで、定電流、定電圧放電を含む;(2)セルは、各C−レートでの3時間の無不可保持時間を伴う、種々のC−レート(2C、1C、0.5C、0.1C)の段階を経て、充電容量維持率を試験された。LMO活性材料について、充電電圧は4.5Vであった。LMNO活性材料について、充電電圧は4.95Vであった。セルは、各C−レートの間、3時間の無負荷保持時間を伴う、種々のC−レート(2C、1C、0.5C、0.1C)の段階を経て、放電された;(3)セルは、3時間の無負荷保持時間を含む、C/10のC−レートでサイクルされて過リチオ化相を生成する;ならびに(4)セルは、段階(2)のように、再度試験された。
CFx正極を有し、例3および4にしたがって組み立てられた一次セルは、例6にしたがって試験された。0.1C放電試験の正極は、(1)未被覆CFx活性材料;(2)PVDF前駆体材料を用いて堆積された炭素被覆を有し、黒鉛化方法により被覆されたCFx活性材料;および(3)ペンタセンで被覆されたCFx活性材料、からなっていた。図7は、ペンタセン被覆試料における動作電圧の改良を示す。
CFx正極を有し、例3および4にしたがって組み立てられた一次セルは、例6にしたがって試験された。1C放電試験の正極は、(1)未被覆CFx活性材料;(2)MWCNTで被覆されたCFx活性材料;(3)ペンタセンで被覆されたCFx活性材料;ならびに(4)MWCNTおよびペンタセンの混合物で被覆されたCFx活性材料からなっていた。図8は、ペンタセン被覆試料およびペンタセン/MWCNT試料の動作電圧および電圧遅延の改良を示す。
CFx正極を有し、例3および4にしたがって組み立てられた一次セルは、例6にしたがって試験された。1C放電試験の正極は、(1)未被覆CFx活性材料;(2)7,7,8,8−テトラシアノキノジメタンで被覆されたCFx活性材料;(3)テトラチアフルバレンで被覆されたCFx活性材料;ならびに(4)テトラチアフルバレンと7,7,8,8−テトラシアノキノジメタンの混合物で被覆されたCFx活性材料からなっていた。図9は、テトラチアフルバレンと7,7,8,8−テトラシアノキノジメタンの混合物被覆試料の動作電圧および電圧遅延の改良を示す。
二次セルは、例3および4にしたがって組み立てられた。試験の正極は、(1)未被覆LMO活性材料;(2)未被覆LMNO活性材料;(3)ルブレンで被覆されたLMO活性材料;(4)ルブレンで被覆されたLMNO活性材料;(5)N,N−ジオクチル−3,4,9,10−ペリレンジカルボキシイミドで被覆されたLMO活性材料;ならびに(6)N,N−ジオクチル−3,4,9,10−ペリレンジカルボキシイミドで被覆されたLMNO活性材料からなっていた。図10(A)(LMO)および10(B)(LMNO)は、被覆試料の高C−レートでの容量維持率の改良を示す。
電極およびセルは、次のプロトコールを用いて37℃で、電気化学的に特徴付けられた:電力測定のために所定の放電深さで、高電流パルスを伴う0.01Cバックグラウンド放電。パルスは、10秒間、2mA/cm2で実施され、ついで10秒間、OCV(無負荷電圧)を実施した。パルスは4パルスのセットで行われ、セルは、第1パルスの前および第4パルスの後に、1お時間OCVで休止された。図11は、放電深さ80%における、最良の炭素被覆CFxのパルス電力向上を示す。
Claims (20)
- 固有の導電度を有する被覆用化合物を活性電極材料と一緒にして混合物を形成すること;
その混合物を加熱して、導電性に被覆された活性電極材料を形成すること、ここでその混合物は活性電極材料の劣化を制限する時間および温度で加熱される;
その導電性に被覆された活性電極材料を、バインダー材料および導電性添加剤と混合して、電極形成用混合物を形成すること;ならびに
その電極形成用混合物を加熱して電極を形成すること;
を含む電気化学的セル用の電極の製造方法。 - 被覆用化合物が有機材料である請求項1に記載の方法。
- 被覆用化合物が複合コアを含み、そこでは炭素原子の少なくとも90%はspまたはsp2混成されている請求項1に記載の方法。
- 被覆用化合物が、炭素原子の少なくとも90%はspまたはsp2混成されている化合物である請求項1に記載の方法。
- 被覆用化合物が複合コアを含み、そこでは炭素原子の100%はspまたはsp2混成されている請求項1に記載の方法。
- 被覆用化合物が450℃未満で加熱される請求項1〜5のいずれか1項に記載の方法。
- 被覆用化合物が0〜6時間の範囲の時間、加熱される請求項1〜6のいずれか1項に記載の方法。
- 被覆用化合物がナフタレンコアを含む請求項1〜7のいずれか1項に記載の方法。
- 被覆用化合物がペンタセンコアを含む請求項1〜7のいずれか1項に記載の方法。
- 被覆用化合物がペリレンコアを含む請求項1〜7のいずれか1項に記載の方法。
- 活性電極材料;
バインダー材料;ならびに
固有導電性の被覆、ここで被覆は活性電極材料に付着される、
を含む電気化学的セル用の電極。 - 固有導電性の被覆が、複合コアを含む有機被覆用化合物から形成される請求項11に記載の電極。
- 固有導電性の被覆が、複合コアを含む有機被覆用化合物から形成され、ここで炭素原子の少なくとも90%はspまたはsp2混成されている請求項11に記載の電極。
- 複合コアが、ナフタレンコア、ペンタセンコア、ペリレンコア、アンスラセンコア、およびそれらの組み合わせからなる群より選ばれる請求項12に記載の電極。
- 正極活性電極材料と固有有機導電体の粒子を混合すること;ならびに
その混合物を正極活性電極材料の劣化を制限する時間および温度で加熱すること;
を含む活性電極材料の被覆粒子の製造方法。 - 時間が6時間未満であり、かつ温度が450℃未満である請求項15に記載の方法。
- 時間が6時間未満であり、かつ温度が350℃未満である請求項16に記載の方法。
- 時間が6時間未満であり、かつ温度が250℃未満である請求項16に記載の方法。
- 固有有機導電体が複合コアを含み、そこでは炭素原子の少なくとも90%はspまたはsp2混成されている請求項15に記載の方法。
- 複合コアが、ナフタレンコア、ペンタセンコア、ペリレンコア、アンスラセンコア、およびそれらの組み合わせからなる群より選ばれる請求項19に記載の方法。
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WO2014144167A1 (en) | 2013-03-15 | 2014-09-18 | Wildcat Discovery Technologies, Inc. | High energy materials for a battery and methods for making and use |
US9093703B2 (en) | 2013-03-15 | 2015-07-28 | Wildcat Discovery Technologies, Inc. | High energy materials for a battery and methods for making and use |
WO2014144179A1 (en) | 2013-03-15 | 2014-09-18 | Wildcat Discovery Technologies, Inc. | High energy materials for a battery and methods for making and use |
US9159994B2 (en) | 2013-03-15 | 2015-10-13 | Wildcat Discovery Technologies, Inc. | High energy materials for a battery and methods for making and use |
US8916062B2 (en) | 2013-03-15 | 2014-12-23 | Wildcat Discovery Technologies, Inc. | High energy materials for a battery and methods for making and use |
US20150044569A1 (en) * | 2013-08-07 | 2015-02-12 | Rutgers, The State University Of New Jersey | High energy cathode materials for primary batteries |
US10431823B2 (en) * | 2014-08-04 | 2019-10-01 | National Institute For Materials Science | Method for manufacturing base material powder having carbon nano-coating layer, method for manufacturing MgB2 superconductor using the method, MgB2 superconductor, method for manufacturing positive electrode material for lithium ion battery, lithium ion battery, and method for manufacturing photocatalyst |
CN104485441B (zh) * | 2014-12-29 | 2016-09-14 | 上海应用技术学院 | 一种四元金属磷酸盐锂离子电池正极材料及其制备方法 |
US10903483B2 (en) | 2015-08-27 | 2021-01-26 | Wildcat Discovery Technologies, Inc | High energy materials for a battery and methods for making and use |
US20180269476A1 (en) * | 2015-09-11 | 2018-09-20 | Umicore | Lithium Metal Oxide Material, the Use Thereof in a Positive Electrode of a Secondary Battery and a Method for Preparing such a Lithium Metal Oxide Material |
US20170133661A1 (en) * | 2015-11-09 | 2017-05-11 | Wildcat Discovery Technologies, Inc. | High energy cathode material |
CN109786756A (zh) * | 2019-01-09 | 2019-05-21 | 上海交通大学 | 一种制备柔性锂离子电池电极的方法及其应用 |
CN110444766B (zh) * | 2019-08-14 | 2021-09-21 | 创普斯(深圳)新能源科技有限公司 | 一种三元正极极片及提高正极极片高温循环性能的方法 |
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CN103814464A (zh) | 2014-05-21 |
JP6247211B2 (ja) | 2017-12-13 |
US20130065126A1 (en) | 2013-03-14 |
EP2756533A1 (en) | 2014-07-23 |
WO2013040101A1 (en) | 2013-03-21 |
EP2756533A4 (en) | 2015-05-06 |
WO2013040101A4 (en) | 2013-05-23 |
US9397339B2 (en) | 2016-07-19 |
CN103814464B (zh) | 2018-04-17 |
KR20140075678A (ko) | 2014-06-19 |
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