JP7062166B2 - 硫黄-炭素複合体、その製造方法及びこれを含むリチウム二次電池 - Google Patents
硫黄-炭素複合体、その製造方法及びこれを含むリチウム二次電池 Download PDFInfo
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Description
多孔性炭素材;及び
前記多孔性炭素材の内部及び表面の少なくとも一部に硫黄がコーティングされた硫黄-炭素複合体において、
前記硫黄-炭素複合体の気孔体積が0.180ないし0.300cm3/gで、
前記硫黄-炭素複合体の平均気孔サイズが40.0ないし70.0nmである、硫黄-炭素複合体を提供する。
(a)1nmないし1μmの粒径を有する硫黄と多孔性炭素材をヘンシェルミキサーで混合する段階;及び
(b)前記混合された硫黄と多孔性炭素材を乾燥する段階;を含む硫黄-炭素複合体の製造方法を提供する。
ここで、本発明では硫黄-炭素複合体と電解液との反応性及びリチウム-硫黄電池の容量及び効率特性の改善効果を確保するために、多孔性炭素材の内部及び表面に硫黄がコーティングされた硫黄-炭素複合体を提供する。前記多孔性炭素材の内部は、多孔性炭素材の気孔内部を含む意味である。
本発明の硫黄-炭素複合体は、(a)1nmないし1μmの粒径を有する硫黄と多孔性炭素材をヘンシェルミキサーで混合する段階;及び(b)前記混合された硫黄と多孔性炭素材を乾燥する段階;を通じて製造される。
本発明で提示する硫黄-炭素複合体は、リチウム-硫黄電池の正極活物質として好ましく使用可能である。
本発明の一実施例として、リチウム-硫黄電池は上述したリチウム-硫黄電池用正極;負極活物質としてリチウム金属またはリチウム合金を含む負極;前記正極と負極の間に介在される分離膜;及び前記負極、正極及び分離膜に含浸され、リチウム塩と有機溶媒を含む電解質を含むことができる。
硫黄-炭素複合体の製造
[実施例1]
1Lのヘンシェルミキサーに硫黄78g、炭素30gを入れて1500rpmで1時間混合した。前記硫黄と炭素の混合物を155℃のオーブンで30分乾燥して硫黄-炭素複合体を製造した。
1L容器に5mm直径のZrO2ボール270g、硫黄23.4g、炭素9gを入れて、200rpmで3分間ボールミルして硫黄と炭素を混合した。以後、前記混合物を155℃のオーブンで30分間加熱して硫黄-炭素複合体を製造した。
(SEM分析及び粒度分析結果)
実施例1及び比較例1で製造した硫黄-炭素複合体を走査電子顕微鏡(SEM、S-4800、HITACHI)で撮影し、これを図2及び図3に示す。
実施例1及び比較例1で製造した硫黄-炭素複合体の気孔の大きさ、比表面積及び気孔体積を窒素吸着装備(BELSorp、BEL)を利用して測定し、表2及び図4に示す。
(電池の製造)
実施例1及び比較例1で製造した硫黄-炭素複合体:バインダー(poly(lithium acrylate)(LiPAA)/polyvinyl alcohol(PVA)を6.5:0.5で混合):導電材(Vapor Grown Carbon Fiber(VGCF))を88:7:5の重量比で混合してスラリーを製造した後、20μm厚さのアルミニウムホイルの集電体にコーティングして電極を製造した。
Claims (16)
- 多孔性炭素材;及び
前記多孔性炭素材の内部及び表面の中の少なくとも一部に硫黄がコーティングされた硫黄-炭素複合体において、
前記硫黄-炭素複合体の気孔体積が0.180ないし0.300cm3/gであり、
前記硫黄-炭素複合体の平均気孔サイズが40.0ないし70.0nmである、硫黄-炭素複合体。 - 前記硫黄-炭素複合体の気孔体積が0.200ないし0.250cm3/gであり、
前記硫黄-炭素複合体の平均気孔サイズが50.0ないし65.0nmである、請求項1に記載の硫黄-炭素複合体。 - 前記多孔性炭素材の直径が100nmないし50μmである、請求項1または2に記載の硫黄-炭素複合体。
- 前記硫黄-炭素複合体は、硫黄と多孔性炭素材が7.5:2.5ないし4:6の重量比で含まれる、請求項1から3のいずれか一項に記載の硫黄-炭素複合体。
- 前記多孔性炭素材は、グラファイト、グラフェン、カーボンブラック、カーボンナノチューブ、炭素繊維及び活性炭素からなる群から選択された1種以上である、請求項1から4のいずれか一項に記載の硫黄-炭素複合体。
- 請求項1から5のいずれか一項に記載の硫黄-炭素複合体を含む、リチウム-硫黄電池用正極。
- (a)1nmないし1μmの粒径を有する硫黄と多孔性炭素材をミキサーで混合する段階;及び
(b)前記混合された硫黄と多孔性炭素材を乾燥する段階;を含み、
前記(b)段階の乾燥は、130℃ないし180℃のオーブンで15分ないし2時間乾燥する、硫黄-炭素複合体の製造方法。 - 前記ミキサーによる混合は500ないし3000rpmの速度で混合する、請求項7に記載の硫黄-炭素複合体の製造方法。
- 前記ミキサーによる混合は15分ないし3時間混合する、請求項7または8に記載の硫黄-炭素複合体の製造方法。
- 前記硫黄-炭素複合体は、その粒度分布でd90が100ないし140μmで、d10が7ないし15μmで、d50が30ないし70μmである、請求項7から9のいずれか一項に記載の硫黄-炭素複合体の製造方法。
- 前記硫黄-炭素複合体は、その粒度分布でd90が110ないし130μmで、d10が8ないし12μmで、d50が40ないし60μmである、請求項7から10のいずれか一項に記載の硫黄-炭素複合体の製造方法。
- 前記多孔性炭素材は、グラファイト、グラフェン、カーボンブラック、カーボンナノチューブ、炭素繊維及び活性炭素からなる群から選択された1種以上である、請求項7から11のいずれか一項に記載の硫黄-炭素複合体の製造方法。
- 前記(b)段階の乾燥は、130ないし155℃のオーブンで15分ないし30分乾燥する、請求項7から12のいずれか一項に記載の硫黄-炭素複合体の製造方法。
- 前記硫黄-炭素複合体は、硫黄と多孔性炭素材が7.5:2.5ないし4:6の重量比で含まれる、請求項7から13のいずれか一項に記載の硫黄-炭素複合体の製造方法。
- 前記ミキサーが、ヘンシェルミキサーである、請求項7から14のいずれか一項に記載の硫黄-炭素複合体の製造方法。
- 請求項6に記載の正極;負極;及び電解質;を含むリチウム-硫黄電池。
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PCT/KR2018/012662 WO2019103326A2 (ko) | 2017-11-24 | 2018-10-24 | 황-탄소 복합체, 그의 제조방법 및 이를 포함하는 리튬 이차전지 |
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US20210143407A1 (en) * | 2018-09-28 | 2021-05-13 | Lg Chem, Ltd. | Sulfur-carbon composite and manufacturing method therefor |
KR102225821B1 (ko) | 2019-08-06 | 2021-03-10 | 고려대학교 산학협력단 | 양극 활물질 제조 방법 및 양극 활물질 |
KR102293240B1 (ko) * | 2019-11-29 | 2021-08-26 | 한국과학기술연구원 | 고용량의 황이 담지된 이차전지용 전극 소재 및 그 제조 방법 |
US20230050935A1 (en) * | 2020-09-21 | 2023-02-16 | Lg Energy Solution, Ltd. | Positive electrode slurry, positive electrode manufactured using same, and lithium-sulfur battery comprising same |
DE102020131233A1 (de) * | 2020-11-25 | 2022-05-25 | Netzsch Trockenmahltechnik Gmbh | Verfahren zur herstellung eines homogenisierten gemischs aus kohlenstoff, schwefel und ptfe |
US11496056B2 (en) * | 2021-03-10 | 2022-11-08 | Excelsys Technologies Ltd. | Parallel branched resonant converter |
WO2023075554A1 (ko) * | 2021-10-29 | 2023-05-04 | 주식회사 엘지에너지솔루션 | 황-탄소 복합체를 포함하는 양극 및 이를 포함하는 리튬 이온 이차 전지 |
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