JP2022529975A - 全固体電池用電解質膜及びそれを含む全固体電池 - Google Patents
全固体電池用電解質膜及びそれを含む全固体電池 Download PDFInfo
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- JP2022529975A JP2022529975A JP2021561994A JP2021561994A JP2022529975A JP 2022529975 A JP2022529975 A JP 2022529975A JP 2021561994 A JP2021561994 A JP 2021561994A JP 2021561994 A JP2021561994 A JP 2021561994A JP 2022529975 A JP2022529975 A JP 2022529975A
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- solid electrolyte
- solid
- electrolyte membrane
- state battery
- lithium
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Images
Classifications
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- H—ELECTRICITY
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/446—Composite material consisting of a mixture of organic and inorganic materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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Abstract
Description
1.電解質フィルムの製造
以下の方法で電解質フィルムを製造した。溶媒としてアセトニトリル(AN)にポリエチレンオキサイド(Mw=4,000,000g/mol)を溶かして4wt%の高分子溶液を用意した。このとき、リチウム塩としてLiTFSIを[EO]/[Li+]=18/1(モル比)になるように一緒に投入した。前記高分子溶液をPEO及びリチウム塩が十分に溶けるように60℃で一晩撹拌した。次いで、開始剤と硬化剤を含む添加剤溶液を用意した。硬化剤としてはポリエチレングリコールジアクリレート(PEGDA、Mw=575)、開始剤としては過酸化ベンゾイル(BPO)を使用し、PEGDAはPEO対比20wt%、BPOはPEGDA対比1wt%の量になるようにし、溶媒としてはアセトニトリルを使用した。前記添加剤溶液を投入した成分が十分に混合されるように約1時間撹拌した。その後、前記添加剤溶液を前記高分子溶液に添加し、二つの溶液を十分に混合した。混合した溶液を離型フィルムにドクターブレードを用いて塗布及びコーティングした。コーティングギャップは800μm、コーティング速度は20mm/minにした。前記溶液がコーティングされた離型フィルムをガラス板に移し、水平を維持しながら常温条件で一晩乾燥し、100℃で12時間真空乾燥した。このような方式で電解質フィルムをそれぞれ二枚収得した。収得されたそれぞれの電解質フィルムの厚さは約50μmであった。
次いで、Liデンドライトガイド物質として金ナノ粒子(シグマアルドリッチ社製、100nm粒径)を、追加的に精製せず、エタノールに分散して分散液を用意した。前記金ナノ粒子の含量は最終的に収得される固体電解質膜の重さ対比1wt%になるようにした。製造例1で用意した一枚の電解質フィルムの表面に前記分散液をスピンコーティングで塗布し、乾燥して溶媒を除去してガイド層を形成した。その後、製造例1で用意した残り一枚の電解質フィルムを前記ガイド層上に配置してラミネーションし、最終ガイド層が含まれた固体電解質膜を製造した。最終的に得られた固体電解質膜の厚さは約100μmであった。
スラリーを製作するため、電極活物質としてのNCM811(LiNi0.8Co0.1Mn0.1O2)、導電材としてのVGCF(気相法炭素繊維(vapor grown carbon fiber))及び高分子系固体電解質(PEO+LiTFSI、[EO]:[Li+]=18:1mol比)を80:3:17の重量比で混合し、アセトニトリルに投入して撹拌して電極スラリーを製造した。これを厚さ20μmのアルミニウム集電体にドクターブレードを用いて塗布し、その結果物を120℃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22%である電極を収得した。
製造された正極を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。二つの電極の間に収得した固体電解質層を介在させてコイン型ハーフセルを製造した。
Liデンドライトガイド物質の含量を2wt%にしたことを除き、実施例1と同じ方法で固体電解質膜を製造した。また、製造された固体電解質膜を用いて実施例1と同じ方法で電池を製造した。
実施例1の製造例1と同じ方法で固体電解質フィルムを三枚用意した。二枚の固体電解質フィルムの表面にガイド層を形成した。ガイド層の形成は実施例1の前記2.と同じ方法で行った。それぞれのガイド層が固体電解質フィルムの間に介在されるように三枚の固体電解質フィルムを積層しラミネーションして固体電解質膜を製造した。その断面構造は固体電解質フィルム/ガイド層/固体電解質フィルム/ガイド層/固体電解質フィルムが順次に積層された形態であった。このようにして製造された固体電解質膜を用いて実施例1の前記3.及び4.と同じ方法で全固体電池を製造した。
Liデンドライトガイド物質としての銀ナノ粒子(シグマアルドリッチ社製、100nm)の含量を2wt%にしたことを除き、実施例1と同じ方法で固体電解質膜を製造した。また、製造された固体電解質膜を用いて実施例1と同じ方法で電池を製造した。
Liデンドライトガイド物質を含まないことを除き、実施例1と同じ方法で固体電解質膜を製造した。また、製造された固体電解質膜を用いて実施例1と同じ方法で電池を製造した。
Liデンドライトガイド物質を含まないことを除き、実施例3と同じ方法で固体電解質膜を製造した。また、製造された固体電解質膜を用いて実施例1と同じ方法で電池を製造した。
それぞれの実施例及び比較例で製作された固体電解質膜を1.7671cm2の円形で切断した。これを二枚のステンレス鋼(SUS)の間に配置してコインセルを製作した。分析装置(VMP3、バイオロジック社製)を使用して60℃、振幅10mV及びスキャンレンジ500kHz~20MHzの条件で電気化学的インピーダンスを測定し、それに基づいてイオン伝導度を計算した。
実施例1~4及び比較例1、2で製造した電池に対し、60℃、0.05Cで充電及び放電を行って初期放電容量を評価した。
放電条件:CC(定電流)条件3V、(0.05C)
Claims (11)
- ガイド層を含む固体電解質膜であって、
前記固体電解質膜は、固体電解質材料及び金属粒子を含み、前記金属粒子はリチウムと合金化可能なものであり、
前記ガイド層は、前記固体電解質膜内に層状構造で配置され、前記金属粒子は前記ガイド層に含まれる、全固体電池用固体電解質膜。 - 前記金属粒子は、リチウム金属核生成過電位が100mV以下である、請求項1に記載の全固体電池用固体電解質膜。
- 前記固体電解質膜は、金属粒子としてAu、Ag、Pt、Zn、Mg、Al、Ni、Biまたはこれらのうち二つ以上を含む、請求項1または2に記載の全固体電池用固体電解質膜。
- 前記ガイド層は、厚さが1nm~1,000nmである、請求項1から3のいずれか一項に記載の全固体電池用固体電解質膜。
- 前記固体電解質材料は、高分子系固体電解質材料を含む、請求項1から4のいずれか一項に記載の全固体電池用固体電解質膜。
- 前記高分子系固体電解質材料は、高分子樹脂及びリチウム塩を含み、1×10-7S/cm以上のイオン伝導度を有する、請求項5に記載の全固体電池用固体電解質膜。
- 前記金属粒子は、粒径が1nm~5μmである、請求項1に記載の全固体電池用固体電解質膜。
- 前記金属粒子は、固体電解質膜100重量%に対して0.1wt%~20wt%の比率で含まれる、請求項1に記載の全固体電池用固体電解質膜。
- 請求項1から8のいずれか一項に記載の固体電解質膜を含む全固体電池。
- 前記全固体電池は、負極が負極活物質としてリチウム金属を含むか又は負極活物質なしに集電体のみからなる、請求項9に記載の全固体電池。
- 前記全固体電池は、負極、正極及び固体電解質膜を含み、前記固体電解質膜は負極と正極との間に介在され、前記負極及び正極の一つ以上は固体電解質材料を含み、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、硫化物系固体電解質またはこれらのうち二つ以上を含む、請求項9に記載の全固体電池。
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- 2019-04-19 KR KR1020190046310A patent/KR20200122904A/ko not_active Application Discontinuation
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2020
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- 2020-04-20 WO PCT/KR2020/005231 patent/WO2020214010A1/ko unknown
- 2020-04-20 CN CN202080029893.6A patent/CN113892205A/zh active Pending
- 2020-04-20 EP EP20791674.3A patent/EP3955362A4/en active Pending
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JP2014534553A (ja) * | 2011-09-27 | 2014-12-18 | シーメンス アクチエンゲゼルシヤフトSiemens Aktiengesellschaft | 蓄積部材および当該蓄積部材の製造方法 |
US20150118572A1 (en) * | 2013-10-29 | 2015-04-30 | Battery Energy Storage Systems-Technologies | Solid-state battery and methods of fabrication |
JP2019505074A (ja) * | 2016-02-03 | 2019-02-21 | コリア インスティテュート オブ インダストリアル テクノロジーKorea Institute Of Industrial Technology | Llzo固体電解質を含む全固体リチウム二次電池及びその製造方法 |
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US20220200097A1 (en) | 2022-06-23 |
KR20200122904A (ko) | 2020-10-28 |
WO2020214010A1 (ko) | 2020-10-22 |
EP3955362A1 (en) | 2022-02-16 |
CN113892205A (zh) | 2022-01-04 |
EP3955362A4 (en) | 2022-02-16 |
JP7263551B2 (ja) | 2023-04-24 |
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