JP2022521364A - リチウム二次電池用分離膜及びこれを含むリチウム二次電池 - Google Patents
リチウム二次電池用分離膜及びこれを含むリチウム二次電池 Download PDFInfo
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- JP2022521364A JP2022521364A JP2021532465A JP2021532465A JP2022521364A JP 2022521364 A JP2022521364 A JP 2022521364A JP 2021532465 A JP2021532465 A JP 2021532465A JP 2021532465 A JP2021532465 A JP 2021532465A JP 2022521364 A JP2022521364 A JP 2022521364A
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- Prior art keywords
- lithium
- secondary battery
- lithium secondary
- molybdenum disulfide
- sulfur
- Prior art date
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- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims abstract description 88
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Images
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Abstract
Description
前記コーティング層は欠陥を含む二硫化モリブデンを含むリチウム二次電池用分離膜を提供する。
(a)欠陥を含む二硫化モリブデンを製造する段階
(b)前記欠陥を含む二硫化モリブデンを含むコーティング用組成物を製造する段階及び
(c)前記コーティング用組成物を多孔性基材の少なくとも一面に塗布する段階を含む。
(a‐1)モリブデン前駆体及び硫黄前駆体を水系溶媒に溶解して混合溶液を製造する段階;
(a‐2)前記混合溶液を水熱合成して二硫化モリブデンを形成する段階、及び
(a‐3)前記段階(a‐2)で形成された二硫化モリブデンを乾燥する段階を含むことができる。
以下、本発明を理解しやすくするために好ましい実施例を提示するが、下記実施例は本発明を例示するものに過ぎず、本発明の範疇及び技術思想の範囲内で多様な変更及び修正が可能であることは当業者にとって明白であり、このような変形及び修正が添付の特許請求範囲に属することも当然である。
[製造例1]
ヘプタモリブデン酸アンモニウム((NH4)6Mo7O24・4H2O)、純正化学(junsei chemical)社製)0.82g及びチオウレア(CH4N2S、シグマアルドリッチ(sigma aldrich)社製)1.54gを脱イオン水20mlに投入し、30分間激しく撹拌して均一な混合溶液を製造した(Mo:S=1:4.3のモル比)。
[実施例1]
(1)分離膜製造
多孔性基材で20μmのポリエチレン(気孔度68%)フィルムを準備した。
正極活物質で硫黄‐炭素複合体(S/C 7:3の重量部)を90重量部、導電材でデンカブラックを5重量部、バインダーでスチレンブタジエンゴム/カルボキシメチルセルロース(SBR/CMC 7:3)5重量部を投入し、ミキシングして正極スラリー組成物を製造した。
電池製造時に分離膜のコーティング層を正極と対面するように配置したことを除いては、前記実施例1と同様に行ってリチウム二次電池を製造した。
分離膜にコーティング層を形成せず、多孔性基材をそのまま使ったことを除いては、前記実施例1と同様に行ってリチウム二次電池を製造した。
分離膜の製造時、製造例1で得られた欠陥を含む二硫化モリブデンの代わりに、欠陥がない二硫化モリブデン(defect‐free MoS2、シグマアルドリッチ社製)を同一含量で溶解させたコーティング用組成物を使用してコーティング層を形成したことを除いては、前記実施例1と同様に行ってリチウム二次電池を製造した。
製造例1で製造した欠陥を含む二硫化モリブデンに対して、走査電子顕微鏡(scanning electron microscope;SEM)及び高分解能透過電子顕微鏡(high resolution transmission electron microscopy;HR‐TEM)で観察した。走査電子顕微鏡は日立(hitachi)社のS‐4800を、高分解能透過電子顕微鏡は日本電子(JEOL)社のJEM‐2100Fを利用した。この時、得られた結果は図1及び2に示す。
製造例1による欠陥を含む二硫化モリブデンに対し、X‐線回折(X‐ray diffraction、XRD)パターンを測定した。前記実験に利用されたXRD装置は、固体相検出機で1.5418Å Cu‐Kα X‐線波長を使うRigaku MiniFlex 600X‐線回折分析装備であった。この時、得られた結果を図3に示す。
製造例1による欠陥を含む二硫化モリブデン及び比較例2で使用した欠陥のない二硫化モリブデンに対し、エネルギー分散型X‐線分光(Energy Dispersive X‐ray Spectrometer、EDS)分析を行った。前記実験に利用されたEDS装置は、日本電子(JEOL)社のJSM‐7610Fであった。この時、得られた結果は表1と図4及び5に示す。
製造例1による欠陥を含む二硫化モリブデンと、従来リチウム‐ポリスルフィド吸着物質で使われる炭素ナノチューブのリチウムポリスルフィド(Li2S6)溶液に対する吸光度を測定した。前記吸光度を測定する時、UV‐Vis分光器(UV‐Vis spectrophotometer)はAgilent社のAgilent 8453を利用した。測定された吸光度が低いほどリチウムポリスルフィドに対する吸着効果が優れることを意味し、この時、得られた結果を図6に示す。
実施例1で製造した分離膜に対し、走査電子顕微鏡(scanning electron microscope;SEM)で観察した。走査電子顕微鏡は日立(hitachi)社のS‐4800を利用した。この時、得られた結果は図7に示す。
前記実施例及び比較例で製造された電池を0.1Cの電流密度で放電と充電を3回繰り返した後、0.2Cの電流密度で放電と充電を3回行った後、0.5Cの放電と0.3Cの充電を行いながら放電容量及びクーロン効率を測定して電池の寿命特性を評価した。この時、得られた結果を図8に示す。
Claims (10)
- 多孔性基材;及び
前記多孔性基材の少なくとも一面に形成されたコーティング層を含み、
前記コーティング層は欠陥(defect)を含む二硫化モリブデンを含む、リチウム二次電池用分離膜。 - 前記欠陥を含む二硫化モリブデンはナノシート形状である、請求項1に記載のリチウム二次電池用分離膜。
- 前記欠陥を含む二硫化モリブデンは厚さが1ないし20nmである、請求項2に記載のリチウム二次電池用分離膜。
- 前記欠陥を含む二硫化モリブデンは結晶性である、請求項1~3のいずれか一項に記載のリチウム二次電池用分離膜。
- 前記欠陥を含む二硫化モリブデンは、X線回折(XRD)を測定する時、回折角度(2θ)が14.0±0.2゜、33.1±0.2゜、39.4±0.2゜及び58.7±0.2゜の範囲でそれぞれ示される回折ピークを含む、請求項4に記載のリチウム二次電池用分離膜。
- 前記欠陥は、点欠陥、線欠陥及び面欠陥からなる群から選択される1種以上である、請求項1~5のいずれか一項に記載のリチウム二次電池用分離膜。
- 前記コーティング層は厚さが0.1ないし10μmである、請求項1~6のいずれか一項に記載のリチウム二次電池用分離膜。
- 前記コーティング層はリチウム二次電池の負極に対面して配置される、請求項1~7のいずれか一項に記載のリチウム二次電池用分離膜。
- 正極;負極;これらの間に介在される分離膜及び電解質を含むリチウム二次電池において、
前記分離膜は請求項1~8のいずれか一項に記載の分離膜を含むリチウム二次電池。 - 前記正極は、硫黄元素及び硫黄系化合物からなる群から選択される1種以上を正極活物質で含む、請求項9に記載のリチウム二次電池。
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