JP2023047565A - 全固体電池 - Google Patents
全固体電池 Download PDFInfo
- Publication number
- JP2023047565A JP2023047565A JP2021156540A JP2021156540A JP2023047565A JP 2023047565 A JP2023047565 A JP 2023047565A JP 2021156540 A JP2021156540 A JP 2021156540A JP 2021156540 A JP2021156540 A JP 2021156540A JP 2023047565 A JP2023047565 A JP 2023047565A
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- Prior art keywords
- solid electrolyte
- solid
- electrode layer
- negative electrode
- nonwoven fabric
- Prior art date
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- 239000007784 solid electrolyte Substances 0.000 claims abstract description 129
- 239000004745 nonwoven fabric Substances 0.000 claims abstract description 65
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- 239000002203 sulfidic glass Substances 0.000 claims description 22
- 150000003839 salts Chemical class 0.000 claims description 6
- 150000004678 hydrides Chemical class 0.000 claims description 5
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- 229910052736 halogen Inorganic materials 0.000 description 4
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- ZXMGHDIOOHOAAE-UHFFFAOYSA-N 1,1,1-trifluoro-n-(trifluoromethylsulfonyl)methanesulfonamide Chemical compound FC(F)(F)S(=O)(=O)NS(=O)(=O)C(F)(F)F ZXMGHDIOOHOAAE-UHFFFAOYSA-N 0.000 description 2
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- 229910001228 Li[Ni1/3Co1/3Mn1/3]O2 (NCM 111) Inorganic materials 0.000 description 2
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- QECVIPBZOPUTRD-UHFFFAOYSA-N N=S(=O)=O Chemical group N=S(=O)=O QECVIPBZOPUTRD-UHFFFAOYSA-N 0.000 description 2
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- 241000156302 Porcine hemagglutinating encephalomyelitis virus Species 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 239000006230 acetylene black Substances 0.000 description 2
- SLSPYQCCSCAKIB-UHFFFAOYSA-N bis(1,1,2,2,2-pentafluoroethylsulfonyl)azanide Chemical compound FC(F)(F)C(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)C(F)(F)F SLSPYQCCSCAKIB-UHFFFAOYSA-N 0.000 description 2
- NVIANCROYQGROD-UHFFFAOYSA-N bis(fluorosulfonyl)azanide Chemical compound FS(=O)(=O)[N-]S(F)(=O)=O NVIANCROYQGROD-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
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- 229910052746 lanthanum Inorganic materials 0.000 description 2
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- GGYPIUANQNUBOE-UHFFFAOYSA-N n-(trifluoromethylsulfonyl)sulfamoyl fluoride Chemical compound FC(F)(F)S(=O)(=O)NS(F)(=O)=O GGYPIUANQNUBOE-UHFFFAOYSA-N 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
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- 239000002002 slurry Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical class C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 1
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- 229920000181 Ethylene propylene rubber Polymers 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000002227 LISICON Substances 0.000 description 1
- 229910000733 Li alloy Inorganic materials 0.000 description 1
- 229910004043 Li(Ni0.5Mn1.5)O4 Inorganic materials 0.000 description 1
- 229910001216 Li2S Inorganic materials 0.000 description 1
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 1
- 229910011281 LiCoPO 4 Inorganic materials 0.000 description 1
- 229910010707 LiFePO 4 Inorganic materials 0.000 description 1
- 229910015643 LiMn 2 O 4 Inorganic materials 0.000 description 1
- 229910014689 LiMnO Inorganic materials 0.000 description 1
- 229910013290 LiNiO 2 Inorganic materials 0.000 description 1
- 229910013086 LiNiPO Inorganic materials 0.000 description 1
- 229910008291 Li—B—O Inorganic materials 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- RWRDLPDLKQPQOW-UHFFFAOYSA-O Pyrrolidinium ion Chemical compound C1CC[NH2+]C1 RWRDLPDLKQPQOW-UHFFFAOYSA-O 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- ZMZDMBWJUHKJPS-UHFFFAOYSA-M Thiocyanate anion Chemical compound [S-]C#N ZMZDMBWJUHKJPS-UHFFFAOYSA-M 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 239000004760 aramid Substances 0.000 description 1
- 229920003235 aromatic polyamide Polymers 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical class C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 description 1
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- 150000001767 cationic compounds Chemical class 0.000 description 1
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- 150000001875 compounds Chemical class 0.000 description 1
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- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
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- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
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- 230000012447 hatching Effects 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- ZMZDMBWJUHKJPS-UHFFFAOYSA-N hydrogen thiocyanate Natural products SC#N ZMZDMBWJUHKJPS-UHFFFAOYSA-N 0.000 description 1
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- 239000007788 liquid Substances 0.000 description 1
- 239000001989 lithium alloy Substances 0.000 description 1
- 239000004750 melt-blown nonwoven Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
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- 229920001778 nylon Polymers 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
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- 238000012360 testing method Methods 0.000 description 1
- 125000005207 tetraalkylammonium group Chemical group 0.000 description 1
- 125000005497 tetraalkylphosphonium group Chemical group 0.000 description 1
- 238000013519 translation Methods 0.000 description 1
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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
- H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
- H01M10/0562—Solid materials
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/51—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof
- D06M11/53—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with hydrogen sulfide or its salts; with polysulfides
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- D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/11—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
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- D06M11/52—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with selenium, tellurium, polonium or their compounds; with sulfur, dithionites or compounds containing sulfur and halogens, with or without oxygen; by sulfohalogenation with chlorosulfonic acid; by sulfohalogenation with a mixture of sulfur dioxide and free halogens
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Abstract
Description
本開示における電極構造体は、正極層と、負極層と、上記正極層および上記負極層の間に配置された固体電解質層と、を有する。また、電極構造体は、正極層および負極層が対向する対向部を有する。厚さ方向に沿った平面視において、対向部の形状は、長辺および短辺を有する矩形である。対向部の平面視形状は、典型的には長方形である。また、短辺の長さに対する長辺の長さの割合は、通常、1.5以上であり、2.0以上であってもよく、2.5以上であってもよい。一方、短辺の長さに対する長辺の長さの割合は、例えば20以下であり、15以下であってもよい。
本開示における固体電解質層は、正極層および負極層の間に配置される層である。固体電解質層は、不織布と、上記不織布の内部に配置された固体電解質と、を含有する。
不織布は、通常、複数の繊維を有し、複数の繊維の間に空隙が形成されている。また、複数の繊維は、繊維方向に沿って延びている。複数の繊維は、繊維方向に沿って、直線的に延びていてもよく、蛇行またはジグザグに延びていてもよい。繊維の材料としては、例えば、ポリエステル系樹脂、ポリオレフィン系樹脂、ポリアミド系樹脂等の樹脂が挙げられる。ポリエステル系樹脂としては、例えば、ポリエチレンテレフタレート(PET)が挙げられる。ポリオレフィン系樹脂としては、例えば、ポリエチレン(PE)、ポリプロピレン(PP)が挙げられる。ポリアミド系樹脂としては、例えばナイロン、アラミドが挙げられる。また、繊維の材料としてガラスを用いてもよい。すなわち、不織布は、ガラス繊維不織布であってもよい。不織布を構成する繊維の繊維径および繊維長は、特に限定されない。
固体電解質層は、不織布の内部に配置された固体電解質を含有する。固体電解質層は、固体電解質を1種のみ含有していてもよく、2種以上含有していてもよい。固体電解質としては、例えば、硫化物固体電解質、酸化物固体電解質、水素化物固体電解質、ハロゲン化物固体電解質、窒化物固体電解質等の無機固体電解質が挙げられる。硫化物固体電解質は、アニオン元素の主成分として、硫黄(S)を含有することが好ましい。酸化物固体電解質は、アニオン元素の主成分として、酸素(O)を含有することが好ましい。水素化物固体電解質は、アニオン元素の主成分として、水素(H)を含有することが好ましい。ハロゲン化物固体電解質は、アニオンの主成分として、ハロゲン(X)を含有することが好ましい。窒化物固体電解質は、アニオン元素の主成分として、窒素(N)を含有することが好ましい。
固体電解質層は、バインダーを含有していてもよく、含有していなくてもよい。バインダーとしては、例えば、ブタジエンゴム、水素化ブタジエンゴム、スチレンブタジエンゴム(SBR)、水素化スチレンブタジエンゴム、ニトリルブタジエンゴム、水素化ニトリルブタジエンゴム、エチレンプロピレンゴム等のゴム系バインダー;ポリフッ化ビニリデン(PVDF)、ポリフッ化ビニリデン-ポリヘキサフルオロプロピレン共重合体(PVDF-HFP)、ポリテトラフルオロエチレン、フッ素ゴム等のフッ化物系バインダーが挙げられる。固体電解質層におけるバインダーの割合は、固体電解質100重量部に対して、例えば、0重量部以上3重量部以下である。
正極層は、少なくとも正極活物質を含有する層であり、必要に応じて、固体電解質、導電材およびバインダーの少なくとも一つを含有していてもよい。正極活物質としては、例えば、酸化物活物質が挙げられる。酸化物活物質としては、例えば、LiCoO2、LiMnO2、LiNiO2、LiVO2、LiNi1/3Co1/3Mn1/3O2等の岩塩層状型活物質、LiMn2O4、Li4Ti5O12、Li(Ni0.5Mn1.5)O4等のスピネル型活物質、LiFePO4、LiMnPO4、LiNiPO4、LiCoPO4等のオリビン型活物質が挙げられる。
負極層は、少なくとも負極活物質を含有する層であり、必要に応じて、固体電解質、導電材およびバインダーの少なくとも一つを含有していてもよい。負極活物質としては、例えば、金属リチウム、リチウム合金等のLi系活物質;グラファイト、ハードカーボン、ソフトカーボン等の炭素系活物質;チタン酸リチウム等の酸化物系活物質;Si単体、Si合金、酸化ケイ素等のSi系活物質が挙げられる。
電極構造体は、正極層、固体電解質層および負極層を有する。ここで、正極層、固体電解質層および負極層のセットを発電単位とした場合、電極構造体は、発電単位を1つのみ有していてもよく、2つ以上有していてもよい。電極構造体が2つ以上の発電単位を有する場合、それらの発電単位は、直列接続されていてもよく、並列接続されていてもよい。
本開示における全固体電池は、電極構造体を少なくとも収納する外装体を有していてもよい。外装体としては、例えば、ラミネート型外装体、ケース型外装体が挙げられる。
(正極の作製)
正極活物質として、レーザー回折・散乱法に基づいて測定される平均粒子径(D50)が5μmであるLiNi1/3Co1/3Mn1/3O2粉体を使用した。次に、ゾルゲル法を用いて、正極活物質の表面にLiNbO3を被覆した。また、硫化物固体電解質として、レーザー回折・散乱法に基づいて測定される平均粒子径(D50)が2.5μmである15LiBr・10LiI・75(0.75Li2S・0.25P2S5)ガラスセラミックスを使用した。
負極活物質として、レーザー回折・散乱法に基づいて測定される平均粒子径(D50)が5μmであるSi粉末を使用した。また、硫化物固体電解質として、レーザー回折・散乱法に基づいて測定される平均粒子径(D50)が2.5μmである15LiBr・10LiI・75(0.75Li2S・0.25P2S5)ガラスセラミックスを使用した。
硫化物固体電解質として、レーザー回折・散乱法に基づいて測定される平均粒子径(D50)が2.5μmである15LiBr・10LiI・75(0.75Li2S・0.25P2S5)ガラスセラミックスを使用した。また、バインダーとして、SBR系バインダーを使用した。
転写部材を、7.5cm×5.1cmの長方形に切り出した。この際、繊維方向(MD方向)が長方形の長辺と平行となるように、転写部材を切り出した。また、負極構造体を7.5cm×5.1cmの長方形に切り出した。また、正極構造体を、7.3cm×4.9cmの長方形に切り出した。
転写部材および負極構造体を、8.6cm×4.5cmの長方形に切り出し、正極構造体を、8.4cm×4.3cmの長方形に切り出したこと以外は、実施例1と同様にして全固体電池を得た。
転写部材および負極構造体を、9.7cm×4.0cmの長方形に切り出し、正極構造体を、9.5cm×3.8cmの長方形に切り出したこと以外は、実施例1と同様にして全固体電池を得た。
転写部材および負極構造体を、10.7cm×3.6cmの長方形に切り出し、正極構造体を、10.5cm×3.4cmの長方形に切り出したこと以外は、実施例1と同様にして全固体電池を得た。
転写部材および負極構造体を、12.2cm×3.2cmの長方形に切り出し、正極構造体を、12.0cm×3.0cmの長方形に切り出したこと以外は、実施例1と同様にして全固体電池を得た。
繊維方向(MD方向)が長方形の短辺と平行となるように、転写部材を切り出したこと以外は、実施例5と同様にして全固体電池を得た。
転写部材および負極構造体を、6.2cm×6.2cmの長方形に切り出し、正極構造体を、6.0cm×6.0cmの正方形に切り出したこと以外は、実施例1と同様にして全固体電池を得た。
実施例1~5および比較例1、2で作製した全固体電池を用いて、サイクル試験を行った。測定は、以下の手順で行った。まず、全固体電池を、100MPaの圧力で拘束し、電流レート36mAで、4.5VまでCCCV充電した(電流カット値:0.36mA)。次に、電流レート36mAで、3.0VまでCCCV放電した(電流カット値:0.36mA)。この充放電を100サイクル行い、容量維持率を求めた。その結果を表1に示す。
容量維持率(%)=100サイクル目の放電容量/1サイクル目の放電容量×100
2…負極層
3…固体電解質層
4…正極集電体
5…負極集電体
10…電極構造体
100…全固体電池
Claims (8)
- 正極層と、負極層と、前記正極層および前記負極層の間に配置された固体電解質層と、を有する電極構造体を備える全固体電池であって、
前記電極構造体は、前記正極層および前記負極層が対向する対向部を有し、
厚さ方向に沿った平面視において、前記対向部の形状は、長辺および短辺を有する矩形であり、
前記短辺の長さに対する前記長辺の長さの割合が、1.5以上であり、
前記固体電解質層は、不織布と、前記不織布の内部に配置された固体電解質と、を含有し、
前記平面視において、前記対向部における長手方向と、前記不織布における繊維方向との角度が、0°以上30°以下である、全固体電池。 - 前記角度が、0°以上10°以下である、請求項1に記載の全固体電池。
- 前記不織布における空隙率が、70%以上90%以下である、請求項1または請求項2に記載の全固体電池。
- 前記不織布において、前記繊維方向の引張強度が、前記繊維方向に直交する方向の引張強度より大きい、請求項1から請求項3までのいずれかの請求項に記載の全固体電池。
- 前記固体電解質が、無機固体電解質である、請求項1から請求項4までのいずれかの請求項に記載の全固体電池。
- 前記無機固体電解質が、硫化物固体電解質、酸化物固体電解質および水素化物固体電解質の少なくとも一種である、請求項5に記載の全固体電池。
- 前記固体電解質が、25℃で固体の溶融塩である、請求項1から請求項4までのいずれかの請求項に記載の全固体電池。
- 前記固体電解質が、柔粘性結晶固体電解質である、請求項1から請求項4までのいずれかの請求項に記載の全固体電池。
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