JP6841156B2 - 蓄電装置およびその製造方法ならびにイオン伝導性材料の製造方法 - Google Patents
蓄電装置およびその製造方法ならびにイオン伝導性材料の製造方法 Download PDFInfo
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- JP6841156B2 JP6841156B2 JP2017098535A JP2017098535A JP6841156B2 JP 6841156 B2 JP6841156 B2 JP 6841156B2 JP 2017098535 A JP2017098535 A JP 2017098535A JP 2017098535 A JP2017098535 A JP 2017098535A JP 6841156 B2 JP6841156 B2 JP 6841156B2
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Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Paints Or Removers (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Conductive Materials (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Description
2(−CO−OH) + P2O5 → (−CO−O−PO(OH))2O
2(−CO−OH) + P2O5 + H2O → 2(−CO−O−PO(OH)2)
また、上記の反応が例えばエタノール溶媒中で進行するのであれば、例えば下記の反応式のとおり、反応が進行すると考えられる。
2(−CO−OH) + P2O5 + 4EtOH → 2(−CO−O−PO(OEt)2) + 3H2O
2(COO−PO(OH)2) + CaCO3 → −COO−PO(OH)−O−Ca−O−PO(OH)−OCO− + H2CO3
2(−COO−PO(OEt)2) + Ca(OH)2 → −COO−PO(OEt)−O−Ca−O−PO(OEt)−OCO− + 2EtOH
以下、蓄電装置の代表例であるリチウムイオン二次電池についての説明を通じて、本発明の電極及び本発明の電極を具備する本発明の蓄電装置の説明をする。
3CaSi2+6HCl → Si6H6+3CaCl2
Si6H6 → 6Si+3H2↑
例えば、正極と負極とでセパレータを挟持して電極体とする。電極体は、正極、セパレータ及び負極を重ねた積層型、又は、正極、セパレータ及び負極の積層体を捲いた捲回型のいずれの型にしても良い。正極の集電体および負極の集電体から外部に通ずる正極端子および負極端子までを、集電用リード等を用いて接続した後に、電極体に電解液を加えてリチウムイオン二次電池とするとよい。
ポリアクリル酸(重量平均分子量250000、和光純薬工業株式会社)0.5質量部を4.5質量部のエタノールに溶解したポリアクリル酸溶液を調製した。また、0.985質量部の五酸化二リンを2質量部のエタノールに溶解した五酸化二リン溶液を調製した。ポリアクリル酸溶液に五酸化二リン溶液を滴下して、その後、2時間撹拌し、実施例1の溶液を調製した。なお、エタノールは、含水量が100ppm以下のものを用いた。
なお、実施例1の溶液においては、ポリアクリル酸を構成するアクリル酸モノマーのモル数と五酸化二リンのモル数の比が1:1である。換言すると、(使用するカルボン酸基含有ポリマーにおけるカルボン酸基のモル数)/(使用する5価のリン化合物におけるリンのモル数)の値が1/2である。
3gの実施例1の溶液に対して、第2族元素化合物である水酸化カルシウム粉末15mgを添加して、60℃で撹拌した。徐々に水酸化カルシウムが溶液に溶解していく様子が観察された。水酸化カルシウムが溶解した溶液を実施例2の溶液とした。なお、通常、水酸化カルシウムはエタノールに溶解しないので、上述した観察の様子は、水酸化カルシウムが反応した結果が反映されたと考えられる。
ポリアクリル酸(重量平均分子量250000、和光純薬工業株式会社)0.5質量部を4.5質量部のエタノールに溶解したポリアクリル酸溶液を調製した。ポリアクリル酸溶液をアルミニウム箔の表面に膜状に塗布し、次いで、加熱してエタノールを除去することで、膜状の比較例1のイオン伝導性材料を製造した。
実施例1、実施例2及び比較例1のイオン伝導性材料について、複素交流インピーダンス測定装置を用いて、イオン伝導度を測定した。結果を表1に示す。表1から、実施例1及び実施例2のイオン伝導性材料は、比較例1のイオン伝導性材料と比較して、著しく優れたイオン伝導性を示したことがわかる。
赤外分光光度計を用いて、実施例1、実施例2及び比較例1のイオン伝導性材料の赤外吸収スペクトルを測定した。実施例1の赤外吸収スペクトルを図1に、実施例2の赤外吸収スペクトルを図2に、比較例1の赤外吸収スペクトルを図3に、それぞれ示す。図1〜図3の横軸は波数(cm−1)であり、縦軸は強度である。
これらの結果から、実施例1のイオン伝導性材料は、カルボン酸基とP2O5が反応して生成した、−CO−O−PO構造を含有するといえる。さらに、図1の赤外吸収スペクトルには、C−H結合に由来するピークが2900〜3000cm−1に観察された点、及び、O−H結合に由来する3300cm−1付近のピークがほとんど観察されなかった点を併せて考察すると、実施例1のイオン伝導性材料は、−CO−O−PO(OEt)2構造を含有するといえる。
実施例1の溶液を用いて、実施例1−Pの正極及びリチウムイオン二次電池を以下のとおり製造した。
ポリアクリル酸(重量平均分子量250000、和光純薬工業株式会社)0.5質量部を4.5質量部のエタノールに溶解したポリアクリル酸溶液を調製した。実施例1の溶液に替えて、当該ポリアクリル酸溶液を用いた以外は、実施例1−Pと同様の方法で、比較例1−Pの正極及びリチウムイオン二次電池を製造した。
0.985質量部の五酸化二リンを2質量部のエタノールに溶解した五酸化二リン溶液を調製した。実施例1の溶液に替えて、当該五酸化二リン溶液を用いた以外は、実施例1−Pと同様の方法で、比較例2−Pの正極及びリチウムイオン二次電池を製造した。
実施例1の溶液を用いずに、実施例1−Pの正極前駆体を比較例3−Pの正極として用いた以外は、実施例1−Pと同様の方法で、比較例3−Pのリチウムイオン二次電池を製造した。
実施例1−P、比較例1−P〜比較例3−Pのリチウムイオン二次電池につき、0.3Cレートの一定電流で4.9Vまで充電を行い、その後、0.3Cレートの一定電流で3.5Vまで放電を行うとの充放電サイクルを20回繰り返した。以下の式に従い、容量維持率を算出した。結果を表2に示す。
容量維持率(%)=100×(20サイクル目の放電容量)/(1サイクル目の放電容量)
実施例1の溶液を用いて、実施例1−Nの負極及びリチウムイオン二次電池を以下のとおり製造した。
実施例1の溶液に替えて、実施例2の溶液を用いた以外は、実施例1−Nと同様の方法で、実施例2−Nの負極及びリチウムイオン二次電池を製造した。
3gの実施例1の溶液に対して、20mgの水酸化ナトリウム粉末を添加して、60℃で撹拌した。徐々に水酸化ナトリウムが溶液に溶解していく様子が観察された。水酸化ナトリウムが溶解した上記の溶液を実施例3の溶液とした。
実施例3の溶液を用いた以外は、実施例1−Nと同様の方法で、実施例3−Nの負極及びリチウムイオン二次電池を製造した。
ポリアクリル酸(重量平均分子量250000、和光純薬工業株式会社)0.5質量部を4.5質量部のエタノールに溶解したポリアクリル酸溶液を調製した。実施例1の溶液に替えて、当該ポリアクリル酸溶液を用いた以外は、実施例1−Nと同様の方法で、比較例1−Nの負極及びリチウムイオン二次電池を製造した。
0.985質量部の五酸化二リンを2質量部のエタノールに溶解した五酸化二リン溶液を調製した。実施例1の溶液に替えて、当該五酸化二リン溶液を用いた以外は、実施例1−Nと同様の方法で、比較例2−Nの負極及びリチウムイオン二次電池を製造した。
実施例1の溶液を用いずに、実施例1−Nの負極前駆体を比較例3−Nの負極として用いた以外は、実施例1−Nと同様の方法で、比較例3−Nのリチウムイオン二次電池を製造した。
実施例1−N〜実施例3−N、比較例1−N〜比較例3−Nのリチウムイオン二次電池につき、0.3Cレートの一定電流で0.01Vまで充電を行い、その後、0.3Cレートの一定電流で1.0Vまで放電を行うとの充放電サイクルを20回繰り返した。以下の式に従い、容量維持率を算出した。結果を表3に示す。
容量維持率(%)=100×(20サイクル目の放電容量)/(1サイクル目の放電容量)
負極活物質であるシリコン材料は充放電時に大きな膨張及び収縮が生じる。実施例2−Nの負極においては、Caが−CO−O−PO構造含有ポリマーを架橋して強靭かつ柔軟な保護層を形成したこと、及び、当該保護層がシリコン材料の膨張及び収縮に追従可能であったことが、上記の結果に反映されたと考えられる。
Claims (4)
- −CO−O−PO(OR) 2 構造含有ポリマーを含むイオン伝導性材料(ただし、Rはそれぞれ独立に水素、アルキル基又は第2族元素から選択される。)を具備する蓄電装置。
- −CO−O−PO(OR) 2 構造含有ポリマーを含むイオン伝導性材料(ただし、Rはそれぞれ独立に水素、アルキル基又は第2族元素から選択される。)で被覆されている電極を具備する蓄電装置。
- カルボン酸基含有ポリマー若しくはその塩と5価のリン化合物との反応工程を含む、−CO−O−PO(OR) 2 構造含有ポリマーを含むイオン伝導性材料(ただし、Rはそれぞれ独立に水素、アルキル基又は第2族元素から選択される。)の製造方法。
- −CO−O−PO(OR) 2 構造含有ポリマーを含むイオン伝導性材料(ただし、Rはそれぞれ独立に水素、アルキル基又は第2族元素から選択される。)で電極を被覆する工程を含む、蓄電装置の製造方法。
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