JP2022529683A - 固体電解質複合体及びそれを含む全固体電池用電極 - Google Patents
固体電解質複合体及びそれを含む全固体電池用電極 Download PDFInfo
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Abstract
Description
本発明による固体電解質複合体は、固体電解質材料及びその表面を被覆する保護膜(passivation film)を含むものである。例えば、前記固体電解質複合体は、粒子状の固体電解質材料、及び前記固体電解質材料の表面を少なくとも一部または全部被覆する保護膜を有するコア-シェル構造を有する。
本発明は、上述した固体電解質複合体を含む電極及び前記電極を含む全固体電池を提供する。前記全固体電池は、正極、負極及び固体電解質膜を含む。本発明の一実施形態において、前記負極は負極活物質として炭素系材料を含むことができる。
(1)固体電解質複合体の製造
エチレンカーボネートとジエチルカーボネートとを1:1の体積比で混合し、そこにLiPF6を1M濃度になるように混合した(溶液1)。次いで、ビニレンカーボネートにLiPF6を1M濃度になるように混合した溶液2を用意した。溶液1と溶液2とを60:40の体積比で混合して溶液3を用意した。溶液3に開始剤(AIBN)を0.5wt%の濃度になるように投入した(溶液4)。次いで、溶液4にLAGP固体電解質粉末(Li1.5Al0.5Ge1.5(PO4)3)を10wt%の濃度で投入し、常温で一晩撹拌した(溶液5)。その後、溶液5を濾過し、固体電解質粉末を常温真空下で1次乾燥して残量の溶媒を除去した。次いで、熱処理(80℃)によって2次真空乾燥して電解質粉末の表面にコーティングされたビニレンカーボネートを重合させ、ポリビニレンカーボネート保護層が形成された固体電解質複合体を収得した。
黒鉛とカーボンブラックとポリフッ化ビニリデン(PVDF)と収得した固体電解質複合体とを80:1:4:15の重量比で混合した後、それを厚さ20μmの銅薄膜にドクターブレードを用いて塗布し、その結果物を60℃で4時間真空乾燥した。その後、真空乾燥の結果物をロールプレスを用いて圧延工程を行い、2mAh/cm2の電極ローディング、電極層の厚さが48μm、気孔度が22vol%である電極を収得した。
製造した負極を1.4875cm2の円形に打ち抜いて用意した。1.7671cm2の円形で切断したリチウム金属薄膜を対向電極として用意した。これら二つの電極の間に固体電解質膜(厚さ100μm)を介在させてコイン型ハーフセルを製造した。固体電解質膜としてはポリエチレンオキサイド(PEO)とLiTFSIとを[EO]/[Li+]=9:1(モル比)で混合したものを使用した。
(1)固体電解質複合体の製造
LAGP固体電解質粉末(Li1.5Al0.5Ge1.5(PO4)3)の代わりにLPS固体電解質粉末(Li2S-P2S5)を使用することを除き、実施例1と同じ方法で固体電解質複合体を収得した。
黒鉛とカーボンブラックとポリフッ化ビニリデン(PVDF)と前記固体電解質複合体とを67:1:2:30の重量比で混合したことを除き、実施例1と同じ方法で電極を収得した。収得した電極は、電極ローディングが2mAh/cm2、電極層の厚さが48μm、気孔度が22vol%であった。
実施例1と同じ方法でコイン型ハーフセルを製造した。
(1)負極の製作
黒鉛とカーボンブラックとポリフッ化ビニリデン(PVDF)とLAGP固体電解質粉末(Li1.5Al0.5Ge1.5(PO4)3)とを80:1:4:15の重量比で混合した後、それを厚さ20μmの銅薄膜にドクターブレードを用いて塗布し、結果物を60℃で4時間真空乾燥した。その後、真空乾燥の結果物をロールプレスを用いて圧延工程を行って、2mAh/cm2の電極ローディング、電極層の厚さが48μm、気孔度が22vol%である電極を収得した。
製造した負極を1.4875cm2の円形に打ち抜いて用意した。1.7671cm2の円形で切断したリチウム金属薄膜を対向電極として用意した。これら二つの電極の間に固体電解質層(厚さ100μm)を介在させてコイン型ハーフセルを製造した。固体電解質膜としてはポリエチレンオキサイド(PEO)とLiTFSIとを[EO]/[Li+]=9:1(モル比)で混合したものを使用した。
(1)負極の製作
LAGP固体電解質粉末(Li1.5Al0.5Ge1.5(PO4)3)の代わりにLPS固体電解質粉末(Li2S-P2S5)を使用し、黒鉛とカーボンブラックとポリフッ化ビニリデン(PVDF)とLPS固体電解質粉末とを67:1:2:30の重量比で混合したことを除き、比較例1と同じ方法で負極を収得した。収得した電極は電極ローディングが2mAh/cm2、電極層の厚さが48μm、気孔度が22vol%であった。
製造した負極を1.4875cm2の円形に打ち抜いて用意した。1.7671cm2の円形で切断したリチウム金属薄膜を対向電極として用意した。これら二つの電極の間に固体電解質層(厚さ100μm)を介在させてコイン型ハーフセルを製造した。固体電解質膜としてはポリエチレンオキサイド(PEO)とLiTFSIとを[EO]/[Li+]=9:1(モル比)で混合したものを使用した。
(1)固体電解質複合体の製造
アセトニトリルにポリエチレンオキサイド(PEO)とLiTFSIとを6:4の重量比で投入して混合した(溶液1)。溶液1に開始剤(AIBN)を0.5wt%の濃度になるように投入した(溶液2)。次いで、溶液2にLPS固体電解質粉末(Li2S-P2S5)を10wt%の濃度で投入し、常温で一晩撹拌した(溶液3)。その後、溶液3を濾過し、固体電解質粉末を常温真空下で1次乾燥して残量の溶媒を除去した。次いで、熱処理(80℃)によって2次真空乾燥し、電解質粉末の表面にPEO保護層が形成された固体電解質複合体を収得した。
黒鉛とカーボンブラックとポリフッ化ビニリデン(PVDF)と収得した固体電解質複合体とを67:1:2:30の重量比で混合した後、それを厚さ20μmの銅薄膜にドクターブレードを用いて塗布し、その結果物を60℃で4時間真空乾燥した。その後、真空乾燥の結果物をロールプレスを用いて圧延工程を行い、2mAh/cm2の電極ローディング、電極層の厚さが48μm、気孔度が22vol%である電極を収得した。
製造した負極を1.4875cm2の円形に打ち抜いて用意した。1.7671cm2の円形で切断したリチウム金属薄膜を対向電極として用意した。これら二つの電極の間に固体電解質膜(厚さ100μm)を介在させてコイン型ハーフセルを製造した。前記固体電解質膜としてはポリエチレンオキサイド(PEO)とLiTFSIとを[EO]/[Li+]=9:1(モル比)で混合したものを使用した。
各実施例及び比較例で製造した電池に対して下記の条件で充/放電を行い、初期効率を評価した。実験温度は常温(25℃)にした。
放電時:CCモードで1.5Vまで0.1Cで放電。
Claims (11)
- 粒子状の固体電解質材料と、前記固体電解質材料の表面の全部または少なくとも一部を被覆する保護膜と、を含み、前記保護膜は1×10-5S/cm以上のイオン伝導度を有し、1×10-9S/cm以下の電気伝導度を有する、固体電解質複合体。
- 前記保護膜は、厚さが10nm~1μmである、請求項1に記載の固体電解質複合体。
- 前記保護膜は、ポリビニレンカーボネート系高分子を含む、請求項1または2に記載の固体電解質複合体。
- 前記ポリビニレンカーボネート系高分子は、重合単位としてビニレンカーボネートを含む、請求項3に記載の固体電解質複合体。
- 前記ポリビニレンカーボネート系高分子は、重合単位としてビニレンカーボネート及び前記ビニレンカーボネートと重合可能な第2重合単位をさらに含み、前記第2重合単位は、アクリロニトリル、メチルメタクリレート、スチレン、ビニルピロリドン、ビニルアセテート、ビニルアルコール及び塩化ビニルから選択された1種または2種以上である、請求項4に記載の固体電解質複合体。
- 前記固体電解質材料は、高分子系固体電解質、酸化物系固体電解質及び硫化物系固体電解質から選択された1種以上を含む、請求項1から5のいずれか一項に記載の固体電解質複合体。
- 前記酸化物系固体電解質は、酸素(O)を含み、周期表の第1族または第2族に属する金属のイオン伝導性を有するものであり、LLTO系化合物、Li6La2CaTa2O12、Li6La2ANb2O12(AはCaまたはSr)、Li2Nd3TeSbO12、Li3BO2.5N0.5、Li9SiAlO8、LAGP系化合物、LATP系化合物、Li1+xTi2-xAlxSiy(PO4)3-y(0≦x≦1、0≦y≦1)、LiAlxZr2-x(PO4)3(0≦x≦1、0≦y≦1)、LiTixZr2-x(PO4)3(0≦x≦1、0≦y≦1)、LISICON系化合物、LIPON系化合物、ペロブスカイト系化合物、NASICON系化合物、LLZO系化合物、またはこれらのうち2種以上を含む、請求項6に記載の固体電解質複合体。
- 請求項1から7のいずれか一項に記載の固体電解質複合体、電極活物質及び導電材を含む全固体電池用電極。
- 請求項1から7のいずれか一項に記載の固体電解質複合体を含む全固体電池。
- 前記全固体電池は、負極、正極、及び前記負極と正極との間に介在された固体電解質膜を含み、前記負極及び正極の少なくとも一つが前記固体電解質複合体を含む、請求項9に記載の全固体電池。
- 請求項1に記載の固体電解質複合体を製造する方法であって、
(S1)粒子状の固体電解質材料の表面を保護層組成物で被覆する段階と、
(S2)前記被覆された固体電解質材料を重合反応に供する段階と、を含み、
前記保護層組成物はビニレンカーボネート、リチウム塩、重合開始剤及び非水系有機溶媒を含む、固体電解質複合体を製造する方法。
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EP3955360A1 (en) | 2022-02-16 |
US20220216512A1 (en) | 2022-07-07 |
WO2020214009A1 (ko) | 2020-10-22 |
EP3955360A4 (en) | 2022-07-13 |
CN113728482A (zh) | 2021-11-30 |
KR20200123032A (ko) | 2020-10-28 |
JP7282917B2 (ja) | 2023-05-29 |
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