JPWO2020184692A1 - 全固体電池用外装材、全固体電池及びその製造方法 - Google Patents
全固体電池用外装材、全固体電池及びその製造方法 Download PDFInfo
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Abstract
Description
少なくとも、基材層、バリア層、熱融着性樹脂層をこの順に備える積層体と、前記熱融着性樹脂層の前記基材層側とは反対側に設けられた絶縁層と、から構成された、全固体電池用外装材であり、
正極活物質層と、負極活物質層と、前記正極活物質層及び前記負極活物質層の間に積層された固体電解質層と、を含む単電池を少なくとも含む電池素子を、前記全固体電池用外装材により形成された包装体中に収容した全固体電池を平面視した場合に、前記絶縁層は、前記全固体電池の前記正極活物質層の全面を覆う位置に配置されている、全固体電池用外装材。
本開示の全固体電池用外装材10は、例えば図6から図9に示すように、少なくとも、基材層1、バリア層3、及び熱融着性樹脂層4をこの順に備える積層体Mと、熱融着性樹脂層4の基材層1側とは反対側に設けられた絶縁層11とから構成されている。全固体電池用外装材10において、基材層1が外層側になり、絶縁層11が内層側になる。全固体電池用外装材10と電池素子を用いて全固体電池を組み立てる際に、全固体電池用外装材10の熱融着性樹脂層4同士を対向させた状態で、周縁部を熱融着させることによって形成された空間に、電池素子が収容される。全固体電池用外装材10において、熱融着性樹脂層4の基材層1側とは反対側(すなわち、電池素子側)に絶縁層11が設けられる。ただし、絶縁層11は、少なくとも、熱融着性樹脂層4同士が熱融着される位置には設けられていない。
本開示の全固体電池用外装材10(以下、「外装材10」と表記することがある)が適用される全固体電池については、外装材10(積層体Mと絶縁層11を含む)を用いることを除いて、特に制限されない。すなわち、外装材10(積層体Mと絶縁層11を含む)以外の電池素子(電極、固体電解質、端子など)等については、全固体電池に適用されるものであれば特に制限されず、公知の全固体電池に使用されているものであってもよい。以下、本開示の全固体電池70を例にして、本開示の全固体電池用外装材10を全固体電池に適用する態様を具体的に説明する。
正極活物質層31は、少なくとも正極活物質を含有する層である。正極活物質層31は、正極活物質に加えて、必要に応じて、固体電解質材料、導電化材、結着材などをさらに含んでいてもよい。
正極集電体32を構成する材料としては、例えばステンレス鋼(SUS)、アルミニウム、ニッケル、鉄、チタン、カーボンなどが挙げられる。
負極活物質層21は、少なくとも負極活物質を含有する層である。負極活物質層21は、負極活物質に加えて、必要に応じて、固体電解質材料、導電化材、結着材などを含んでいてもよい。
負極集電体22を構成する材料としては、例えばステンレス鋼(SUS)、銅、ニッケル、カーボン等が挙げられる。
固体電解質層40は、固体電解質材料を含有する層である。固体電解質材料としては、例えば、硫化物固体電解質材料および酸化物固体電解質材料が挙げられる。
本開示の外装材10は、少なくとも、基材層1、バリア層3、熱融着性樹脂層4をこの順に備える積層体Mと、絶縁層11とから構成されている。絶縁層11は、熱融着性樹脂層4の基材層1側とは反対側に設けられている。以下、本開示の外装材10の積層体Mを構成する各層と絶縁層11について、詳述する。
本開示において、絶縁層11は、全固体電池の短絡を効果的に抑制するために、全固体電池を平面視した場合に、全固体電池の正極活物質層31の全面を覆うようにして設けられ、絶縁部材によって構成される層である。前述の通り、全固体電池70は、電池素子を全固体電池用外装材10により形成された包装体中に収容したものである。また、電池素子は、単電池50を少なくとも含んでいる。さらに、単電池50は、正極活物質層31と、負極活物質層21と、正極活物質層31及び負極活物質層21の間に積層された固体電解質層40とを含んでいる。
絶縁層11の突刺し強さは、JIS Z1707:1997の規定に準拠した方法により測定する。具体的には、23±2℃、相対湿度(50±5)%の測定環境において、中央に直径15mmの開口部を有する直径115mmの台と押さえ板で試験片を固定し、直径1.0mm、先端形状半径0.5mmの半円形の針を毎分50±5mmの速度で突き刺し、針が貫通するまでの最大応力を測定する。試験片の数は5個であり、その平均値を求める。なお、試験片の数が足りず5個測定できない場合は測定可能な数を測定し、その平均値を求める。
本開示において、基材層1は、全固体電池用外装材の基材としての機能を発揮させることなどを目的として積層体Mに設けられる層である。基材層1は、全固体電池用外装材の外層側に位置する。
本開示の全固体電池用外装材において、接着剤層2は、積層体Mの基材層1とバリア層3との接着性を高めることを目的として、必要に応じて、これらの間に設けられる層である。
着色層は、基材層1とバリア層3との間に必要に応じて設けられる層である(図示を省略する)。接着剤層2を有する場合には、基材層1と接着剤層2との間、接着剤層2とバリア層3との間に着色層を設けてもよい。また、基材層1の外側に着色層を設けてもよい。着色層を設けることにより、全固体電池用外装材を着色することができる。
全固体電池用外装材において、積層体Mのバリア層3は、少なくとも水分の浸入を抑止する層である。
1次イオン:ビスマスクラスターのダブルチャージイオン(Bi3 ++)
1次イオン加速電圧:30 kV
質量範囲(m/z):0〜1500
測定範囲:100μm×100μm
スキャン数:16 scan/cycle
ピクセル数(1辺):256 pixel
エッチングイオン:Arガスクラスターイオンビーム(Ar−GCIB)
エッチングイオン加速電圧:5.0 k
本開示の全固体電池用外装材において、積層体Mの熱融着性樹脂層4は、最内層に該当し、全固体電池の組み立て時に熱融着性樹脂層同士が熱融着して電池素子を密封する機能を発揮する層(シーラント層)である。
本開示の全固体電池用外装材において、積層体Mの接着層5は、バリア層3(又は耐腐食性皮膜)と熱融着性樹脂層4を強固に接着させるために、これらの間に必要に応じて設けられる層である。
本開示の外装材は、意匠性、耐傷性、成形性などの向上の少なくとも一つを目的として、必要に応じて、積層体Mの基材層1の上(基材層1のバリア層3とは反対側)に、表面被覆層6を備えていてもよい。表面被覆層6は、外装材を用いて全固体電池を組み立てた時に、外装材の最外層側に位置する層である。
基材層としてポリエチレンテレフタレートフィルム(12μm)/接着剤層(2液硬化型ウレタン接着剤(ポリオール化合物と芳香族イソシアネート化合物)、厚さ3μm)/二軸延伸ナイロンフィルム(厚さ15μm)が順に積層された積層フィルムを用意した。次に、基材層の二軸延伸ナイロンフィルム(厚さ15μm)の上に、アルミニウム箔(JIS H4160:1994 A8021H−O、厚さ40μm、両面にクロム酸を用いた耐腐食性皮膜が形成されている)からなるバリア層をドライラミネート法により積層させた。具体的には、アルミニウム箔の一方面に、2液硬化型ウレタン接着剤(ポリオール化合物と芳香族イソシアネート化合物)を塗布し、アルミニウム箔上に接着剤層(硬化後の厚み3μm)を形成した。次いで、アルミニウム箔上の接着剤層と二軸延伸ナイロンフィルムを積層した後、エージング処理を実施することにより、基材層/接着剤層/バリア層の積層体を作製した。次に、得られた積層体のバリア層の上に、接着層としての無水マレイン酸変性ポリプロピレン(厚さ40μm)と、熱融着性樹脂層としてのポリプロピレン(厚さ40μm)とを共押出しすることにより、バリア層上に接着層/熱融着性樹脂層を積層させた。次に、得られた積層体をエージングし、加熱することにより、ポリエチレンテレフタレートフィルム(12μm)/接着剤層(3μm)/二軸延伸ナイロンフィルム(15μm)/接着剤層(3μm)/バリア層(40μm)/接着層(40μm)/熱融着性樹脂層(40μm)がこの順に積層された積層体M1を得た。なお、絶縁層については、後述の通り、全固体電池を製造する際に、熱融着性樹脂層の内側に配置され、全固体電池用外装材となる。
基材層として、ポリエチレンテレフタレートフィルム(25μm)を用いたこと以外は、製造例1と同様にして、ポリエチレンテレフタレートフィルム(25μm)/接着剤層(3μm)/バリア層(40μm)/接着層(40μm)/熱融着性樹脂層(40μm)がこの順に積層された積層体M2を得た。
熱融着性樹脂層として、ポリブチレンテレフタレートフィルム(25μm)を用い、接着層として2液硬化型ウレタン接着剤(ポリオール化合物と芳香族イソシアネート化合物)を用いたドライラミネート法により、基材層/接着剤層/バリア層の積層体のバリア層の上に、ポリブチレンテレフタレートフィルムを積層したこと以外は、製造例1と同様にして、ポリエチレンテレフタレートフィルム(12μm)/接着剤層(3μm)/二軸延伸ナイロンフィルム(15μm)/接着剤層(3μm)/バリア層(40μm)/接着層(3μm)/熱融着性樹脂層(ポリブチレンテレフタレートフィルム 25μm)がこの順に積層された積層体M3を得た。
[実施例1]
図1の模式図に示すような全固体電池70を作製した。具体的には、露点マイナス50℃以下のドライ環境において、正極集電体32(厚み20μm)としてのアルミニウム合金箔の上に正極活物質層31(厚み100μm)としてのLiCoO2を積層した正極層30と、負極集電体22(厚み10μm)としてのSUS304箔の上に負極活物質層21(厚み120μm)としてのグラファイトを積層した負極層20とを、固体電解質層(Li2S:P2S5=75:25、厚み100μm)を介して積層して単電池50を作製した。なお、全固体電池を平面視した場合に、正極活物質層31は縦30mm×横30mm、正極集電体32は縦40mm×横35mm、負極活物質層21は縦32mm×横32mm、負極集電体22は縦40mm×横35mm、固体電解質層は縦32mm×横32mmである。次に、正極集電体32及び負極集電体22それぞれに端子60を接合した。
製造例1において、外装材(積層体M1)の絶縁層として、ポリエチレンテレフタレートフィルム(厚み5μm、融点265℃、表2の突き刺し強さ)を用いたこと以外は、実施例1と同様にして、全固体電池を作製した。
製造例1において、外装材(積層体M1)の絶縁層として、ポリエチレンテレフタレートフィルム(厚み25μm、融点265℃、表2の突き刺し強さ)を用いたこと以外は、実施例1と同様にして、全固体電池を作製した。
製造例1において、外装材(積層体M1)の絶縁層として、ポリフェニレンサルファイドフィルム(厚み16μm、融点290℃、表2の突き刺し強さ)を用いたこと以外は、実施例1と同様にして、全固体電池を作製した。
製造例1において、外装材(積層体M1)の絶縁層として、ポリエーテルエーテルケトンフィルム(厚み12μm、融点334℃、表2の突き刺し強さ)を用いたこと以外は、実施例1と同様にして、全固体電池を作製した。
製造例1において、外装材(積層体M1)の絶縁層として、ポリエチレンナフタレートフィルム(厚み25μm、融点265℃、表2の突き刺し強さ)を用いたこと以外は、実施例1と同様にして、全固体電池を作製した。
製造例1において、外装材(積層体M1)の絶縁層として、ポリブチレンテレフタレートフィルム(厚み15μm、融点260℃、表2の突き刺し強さ)を用いたこと以外は、実施例1と同様にして、全固体電池を作製した。
製造例1において、外装材(積層体M1)の絶縁層として、ポリブチレンテレフタレートフィルム(厚み25μm、融点260℃、表2の突き刺し強さ)を用いたこと以外は、実施例1と同様にして、全固体電池を作製した。
製造例1で製造した外装材(積層体M1)の代わりに、製造例2で製造した外装材(積層体M2)を用いたこと以外は、実施例1と同様にして、全固体電池を作製した。
製造例1で製造した外装材(積層体M1)の代わりに、製造例3で製造した外装材(積層体M3)を用いたこと以外は、実施例1と同様にして、全固体電池を作製した。実施例10で使用した外装材(積層体M3)は、熱融着性樹脂層としてポリブチレンテレフタレートフィルムが使用されており、厚みが薄い場合にも優れた耐熱性を発揮することができる。すなわち、外装材全体としての厚みを薄くして、優れた耐熱性を発揮することができる。
絶縁層11を用いなかったこと以外は、実施例1と同様にして、全固体電池を作製した。
絶縁層の突刺し強さは、JIS Z1707:1997の規定に準拠した方法により測定した。具体的には、23±2℃、相対湿度(50±5)%の測定環境において、中央に直径15mmの開口部を有する直径115mmの台と押さえ板で試験片を固定し、試験片の主面から、直径1.0mm、先端形状半径0.5mmの半円形の針を毎分50±5mmの速度で突き刺し、針が貫通するまでの最大応力を測定する。試験片の数は5個であり、その平均値を求めた。測定機器として、イマダ社製のZP−50N(フォースゲージ)及びイマダ社製のMX2−500N(測定スタンド)を用いた。
バリア層(アルミニウム合金箔)の表面に形成した耐腐食性皮膜の分析は、次のようにして行った。まず、バリア層と接着層との間を引き剥がした。この際、水や有機溶剤、酸やアルカリの水溶液などを利用せずに、物理的に剥離させた。バリア層と接着層との間を剥離した後には、バリア層の表面に接着層が残存していたため、残存している接着層をAr−GCIBによるエッチングで除去した。このようにして得られたバリア層の表面について、飛行時間型2次イオン質量分析法を用いて、バリア層保護膜の分析を行った。それぞれ、CrPO4 -、PO2 -、及びPO3 -に由来するピーク強度PCrPO4は3.8×104、PPO2は6.3×105、PPO3は1.0×106であった。
測定装置:ION−TOF社製 飛行時間型2次イオン質量分析装置TOF.SIMS5
(測定条件)
1次イオン:ビスマスクラスターのダブルチャージイオン(Bi3 ++)
1次イオン加速電圧:30 kV
質量範囲(m/z):0〜1500
測定範囲:100μm×100μm
スキャン数:16 scan/cycle
ピクセル数(1辺):256 pixel
エッチングイオン:Arガスクラスターイオンビーム(Ar−GCIB)
エッチングイオン加速電圧:5.0 kV
上記で得られた各全固体電池について、短絡の抑制効果を次のようにして行った。まず、正極活物質層31と同じサイズ(縦30mm×横30mm)のステンレス鋼板を2枚用意した。次に、全固体電池70を平面視した場合に、ステンレス鋼板が正極活物質層の全面を覆うようにして、全固体電池を上下から挟み込んだ。次に、120℃の環境において、上下のステンレス鋼板に100MPaの荷重を加え、この状態で24時間保持した。次に、全固体電池からステンレス鋼板を外し、正極端子と外装材のアルミニウム合金箔とをテスターに接続して導通を確認した。導通が確認されなかった場合を、短絡が抑制されていると評価(A)し、導通が確認された場合を、短絡が抑制されていないと評価(C)した。結果を表1に示す。
項1. 少なくとも、基材層、バリア層、熱融着性樹脂層をこの順に備える積層体と、前記熱融着性樹脂層の前記基材層側とは反対側に設けられた絶縁層と、から構成された、全固体電池用外装材であり、
正極活物質層と、負極活物質層と、前記正極活物質層及び前記負極活物質層の間に積層された固体電解質層と、を含む単電池を少なくとも含む電池素子を、前記全固体電池用外装材により形成された包装体中に収容した、全固体電池を平面視した場合に、前記絶縁層は、前記全固体電池の前記正極活物質層の全面を覆う位置に配置されている、全固体電池用外装材。
項2. 前記絶縁層の融点が200℃以上である、項1に記載の全固体電池用外装材。
項3. 正極活物質層と、負極活物質層と、前記正極活物質層及び前記負極活物質層の間に積層された固体電解質層と、を含む単電池を少なくとも含む電池素子が、全固体電池用外装材により形成された包装体中に収容された全固体電池であって、
前記全固体電池用外装材は、少なくとも、基材層、バリア層、熱融着性樹脂層をこの順に備える積層体と、前記熱融着性樹脂層の前記基材層側とは反対側に設けられた絶縁層と、から構成されており、
前記全固体電池を平面視した場合に、前記絶縁層は、前記全固体電池の正極活物質層の全面を覆う位置に配置されている、全固体電池。
項4. 正極活物質層と、負極活物質層と、前記正極活物質層及び前記負極活物質層の間に積層された固体電解質層と、を含む単電池を少なくとも含む電池素子を、全固体電池用外装材により形成された包装体中に収容する収容工程を備えており、
前記全固体電池用外装材は、少なくとも、基材層、バリア層、熱融着性樹脂層をこの順に備える積層体と、前記熱融着性樹脂層の前記基材層側とは反対側に設けられた絶縁層と、から構成されており、
前記全固体電池用外装材の前記絶縁層は、前記全固体電池を平面視した場合に、前記全固体電池の前記正極活物質層の全面を覆う位置に配置する、全固体電池の製造方法。
項5. 全固体電池の外装材に設けられる絶縁層を構成する絶縁部材であって、
前記外装材は、少なくとも、基材層、バリア層、熱融着性樹脂層をこの順に備える積層体から構成されており、
前記絶縁層は、前記熱融着性樹脂層の基材層側とは反対側に設けられ、
前記絶縁層は、前記全固体電池を平面視した場合に、前記全固体電池の正極活物質層の全面を覆うようにして設けられる、絶縁部材。
2 接着剤層
3 バリア層
4 熱融着性樹脂層
5 接着層
6 表面被覆層
10 全固体電池用外装材
11 絶縁層
20 負極層
21 負極活物質層
22 負極集電体
30 正極層
31 正極活物質層
32 正極集電体
40 固体電解質層
50 単電池
60 端子
70 全固体電池
M 積層体
Claims (7)
- 少なくとも、基材層、バリア層、熱融着性樹脂層をこの順に備える積層体と、前記熱融着性樹脂層の前記基材層側とは反対側に設けられた絶縁層と、から構成された、全固体電池用外装材であり、
正極活物質層と、負極活物質層と、前記正極活物質層及び前記負極活物質層の間に積層された固体電解質層と、を含む単電池を少なくとも含む電池素子を、前記全固体電池用外装材により形成された包装体中に収容した全固体電池を平面視した場合に、前記絶縁層は、前記全固体電池の前記正極活物質層の全面を覆う位置に配置されている、全固体電池用外装材。 - 前記絶縁層の融点が200℃以上である、請求項1に記載の全固体電池用外装材。
- 前記バリア層の表面に形成された、耐腐食性皮膜を有している、請求項1又は2に記載の全固体電池用外装材。
- 前記耐腐食性皮膜について、飛行時間型2次イオン質量分析法を用いて分析した場合に、CrPO4 -に由来するピーク強度PCrPO4に対するPO3 -に由来するピーク強度PPO3の比PPO3/CrPO4が、6以上120以下の範囲内にある、請求項1〜3のいずれかに記載の全固体電池用外装材。
- 前記積層体は、前記熱融着性樹脂層側から前記基材層側に突出した形状の凹部を有しており、
前記凹部に、前記絶縁層が配置されている、請求項1〜4のいずれかに記載の全固体電池用外装材。 - 正極活物質層と、負極活物質層と、前記正極活物質層及び前記負極活物質層の間に積層された固体電解質層と、を含む単電池を少なくとも含む電池素子が、全固体電池用外装材により形成された包装体中に収容された全固体電池であって、
前記全固体電池用外装材は、少なくとも、基材層、バリア層、熱融着性樹脂層をこの順に備える積層体と、前記熱融着性樹脂層の前記基材層側とは反対側に設けられた絶縁層と、から構成されており、
前記全固体電池を平面視した場合に、前記絶縁層は、前記全固体電池の正極活物質層の全面を覆う位置に配置されている、全固体電池。 - 正極活物質層と、負極活物質層と、前記正極活物質層及び前記負極活物質層の間に積層された固体電解質層と、を含む単電池を少なくとも含む電池素子を、全固体電池用外装材により形成された包装体中に収容する収容工程を備えており、
前記全固体電池用外装材は、少なくとも、基材層、バリア層、熱融着性樹脂層をこの順に備える積層体と、前記熱融着性樹脂層の前記基材層側とは反対側に設けられた絶縁層と、から構成されており、
前記全固体電池用外装材の前記絶縁層は、前記全固体電池を平面視した場合に、前記全固体電池の前記正極活物質層の全面を覆う位置に配置する、全固体電池の製造方法。
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