JP2020536038A - 硫黄−炭素複合体の製造方法 - Google Patents
硫黄−炭素複合体の製造方法 Download PDFInfo
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- JP2020536038A JP2020536038A JP2020519362A JP2020519362A JP2020536038A JP 2020536038 A JP2020536038 A JP 2020536038A JP 2020519362 A JP2020519362 A JP 2020519362A JP 2020519362 A JP2020519362 A JP 2020519362A JP 2020536038 A JP2020536038 A JP 2020536038A
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- sulfur
- carbon
- phase
- lithium
- positive electrode
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- 229910052712 strontium Inorganic materials 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
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- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- BDZBKCUKTQZUTL-UHFFFAOYSA-N triethyl phosphite Chemical compound CCOP(OCC)OCC BDZBKCUKTQZUTL-UHFFFAOYSA-N 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
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Abstract
Description
(a)多孔性炭素材を乾燥する段階;及び(b)多孔性炭素材に硫黄を混合してボールミリング(ball milling)工程でミキシング(mixing)した後、熱処理する段階;を含む硫黄−炭素複合体の製造方法を提供する。
そこで、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、ロシキーアイト相(Rosickyite phase)の硫黄を硫黄−炭素複合体に担持させる硫黄−炭素複合体の製造方法を提供する。
本発明の硫黄−炭素複合体は、製造時に特定の条件で乾燥された多孔性炭素材を、特定の条件で混合した後、熱処理を行うことによって、硫黄−炭素複合体の多孔性炭素材の内側及び外側の表面のうち少なくとも一部に含まれた硫黄の相(phase)がロシキーアイト相(Rosickyite phase)に変化するようになり、これにより、本発明の硫黄−炭素複合体はロシキーアイト相(Rosickyite phase)の硫黄を含むことになる。
本発明で提示する硫黄−炭素複合体は、リチウム二次電池の正極活物質として好適に使用が可能であり、特に、正極内に硫黄化合物を含むリチウム−硫黄電池用正極活物質として用いることができる。
本発明の一実施例として、リチウム二次電池は前述した正極;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;前記正極と正極との間に介在される分離膜;及び前記正極、正極、及び分離膜に含浸されており、リチウム塩と有機溶媒を有する電解質を含むことができる。特に、前記リチウム二次電池は、正極内に硫黄化合物を含むリチウム−硫黄電池であってもよい。
硫黄−炭素複合体の製造
[実施例1]
カーボンナノチューブ4.5gを130℃の真空オーブンで12時間熱処理した。乾燥されたカーボンナノチューブの水分含有量をMETROHM 860 KF Coulometer機器を使用して測定した結果、30ppmであった。
未乾燥のカーボンナノチューブの水分含有量を実施例1と同様の方法で測定した結果、200ppmであった。乾燥されないカーボンナノチューブ4.5gを硫黄(Aldrich社のα−硫黄(sulfur))10.5gと、実施例1と同様の方法のボールミリング工程でミキシング(mixing)した後、155℃のオーブンで30分間熱処理して硫黄−炭素複合体を製造した。
比較例1と同一のカーボンナノチューブ1.5gを硫黄(Aldrich社のα−硫黄(sulfur))3.5gと乳鉢ミキシング(mixing)した後、155℃のオーブンで30分間熱処理して硫黄−炭素複合体を製造した。
前記実施例及び比較例において、カーボンナノチューブの水分含有量の定量方法は、電量(Coulometric)方式を使用した。これは、カールフィッシャー(Karl Fischer)反応を基礎としたもので、試料中の水分量は、ヨウ素(Iodine)を生成するために利用される電子のモル(mole)数から計算される。Faraday法則によれば、電解反応によって1モル(mole)の化学種を生成するのに必要な電気量は96485C/molであり、これは、1mAの電気量を100秒間供給したとき、1.03μmolのI2が生成されるということである。このように生成されたI2はカールフィッシャー(Karl Fischer)反応に参加することになり、生成されるI2がμmol単位で微量の水分結晶が可能である。したがって、ヨウ素(Iodine)を作成するとき、使われる電流を測定し、この電流値から水分量を決定した。
実施例1及び比較例1〜2で製造された硫黄−炭素複合体に対し、X線回折分析(X−ray Diffraction Spectroscopy,Mettler−Toledo,TGA2)分析を実施し、その結果を図1に示した。
実施例1及び比較例1〜2で製造された硫黄−炭素複合体を用いて、硫黄−炭素複合体:導電材:バインダー=90:5:5の重量比で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。このとき、導電材としてカーボンブラックを、バインダーとしてはスチレンブタジエンゴム、カルボキシメチルセルロースを用いた。製造された電極を50℃のオーブンで一晩(overnight)乾燥し、リチウム−硫黄電池用正極を製造した。
Claims (9)
- (a)多孔性炭素材を乾燥する段階と;
(b)前記多孔性炭素材に硫黄を混合してボールミリング(ball milling)工程でミキシング(mixing)した後、熱処理する段階と;
を含む硫黄−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より選ばれた1種以上である、請求項1に記載の硫黄−炭素複合体の製造方法。
- 前記(a)段階の乾燥は、100℃〜150℃の温度で6時間〜36時間行う、請求項1に記載の硫黄−炭素複合体の製造方法。
- 前記(b)段階のボールミリング工程は100〜500rpmで、30分〜5時間行う、請求項1に記載の硫黄−炭素複合体の製造方法。
- 前記(b)段階の熱処理は、130℃〜170℃の温度で行う、請求項1に記載の硫黄−炭素複合体の製造方法。
- 前記(b)段階において、前記硫黄と前記多孔性炭素材を9:1〜5:5の重量比で混合する、請求項1に記載の硫黄−炭素複合体の製造方法。
- 前記(b)段階で混合される前記硫黄と前記多孔性炭素材との混合物の重量が10g以上である、請求項1に記載の硫黄−炭素複合体の製造方法。
- 前記硫黄−炭素複合体内にロシキーアイト相(Rosickyite phase)の硫黄を0超過10重量%未満で含む、請求項1に記載の硫黄−炭素複合体の製造方法。
- 前記硫黄−炭素複合体内にα−相(phase)の硫黄及びβ−相(phase)の硫黄の内の少なくとも1つを更に含む、請求項8に記載の硫黄−炭素複合体の製造方法。
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EP3670449A1 (en) | 2020-06-24 |
JP6952892B2 (ja) | 2021-10-27 |
EP3670449B1 (en) | 2024-08-07 |
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