JP7015445B2 - 導電性カーボン混合物の製造方法及びこの混合物を用いた電極の製造方法 - Google Patents
導電性カーボン混合物の製造方法及びこの混合物を用いた電極の製造方法 Download PDFInfo
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- JP7015445B2 JP7015445B2 JP2017136475A JP2017136475A JP7015445B2 JP 7015445 B2 JP7015445 B2 JP 7015445B2 JP 2017136475 A JP2017136475 A JP 2017136475A JP 2017136475 A JP2017136475 A JP 2017136475A JP 7015445 B2 JP7015445 B2 JP 7015445B2
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Images
Classifications
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- H—ELECTRICITY
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Description
本発明の蓄電デバイスの電極の製造のための導電性カーボン混合物は、導電性を有する酸化処理カーボンと、該酸化処理カーボンとは別の導電性カーボンと、を含み、上記酸化処理カーボンが上記別の導電性カーボンの表面を被覆している。好ましくは上記酸化処理カーボンの少なくとも一部が糊状である。そして、この導電性カーボン混合物のラマンスペクトルにおけるR2D/Dが、上記別の導電性カーボンのラマンスペクトルにおけるR2D/Dの55%以下、好ましくは20~55%、特に好ましくは20~35%の範囲である。
(a)空隙を有するカーボン原料を酸で処理する工程、
(b)酸処理後の生成物と遷移金属化合物とを混合する工程、
(c)得られた混合物を粉砕し、メカノケミカル反応を生じさせる工程、
(d)メカノケミカル反応後の生成物を非酸化雰囲気中で加熱する工程、及び、
(e)加熱後の生成物から、上記遷移金属化合物及び/又はその反応生成物を除去する工程
を含む製造方法によって、好適に得ることができる。
本発明の導電性カーボン混合物は、二次電池、電気二重層キャパシタ、レドックスキャパシタ及びハイブリッドキャパシタなどの蓄電デバイスの電極の製造のために、蓄電デバイスの電解質中のイオンとの電子の授受を伴うファラデー反応或いは電子の授受を伴わない非ファラデー反応により容量を発現する電極活物質と混合された形態で使用される。
本発明の電極は、二次電池、電気二重層キャパシタ、レドックスキャパシタ及びハイブリッドキャパシタなどの蓄電デバイスの電極のために使用される。蓄電デバイスは、一対の電極(正極、負極)とこれらの間に配置された電解質とを必須要素として含むが、正極及び負極の少なくとも一方が本発明の電極である。
60%硝酸300mLにケッチェンブラック(商品名EC300J、ケッチェンブラックインターナショナル社製、BET比表面積800m2/g)10gを添加し、得られた液に超音波を10分間照射した後、ろ過してケッチェンブラックを回収した。回収したケッチェンブラックを3回水洗し、乾燥することにより、酸処理ケッチェンブラックを得た。この酸処理ケッチェンブラック0.5gと、Fe(CH3COO)21.98gと、Li(CH3COO)0.77gと、C6H8O7・H2O1.10gと、CH3COOH1.32gと、H3PO41.31gと、蒸留水120mLとを混合し、得られた混合液をスターラーで1時間攪拌した後、空気中100℃で蒸発乾固させて混合物を採集した。次いで、得られた混合物を振動ボールミル装置に導入し、20hzで10分間の粉砕を行なった。粉砕後の粉体を、窒素中700℃で3分間加熱し、ケッチェンブラックにLiFePO4が担持された複合体を得た。
実施例1における導電性カーボン混合物を得るための振動ボールミル装置による乾式混合条件を、10hzでの20分間の条件から20hzでの10分間の条件に変更した点を除いて、実施例1を繰り返した。
実施例1における導電性カーボン混合物を得るための振動ボールミル装置による乾式混合条件を、10hzでの20分間の条件から20hzでの20分間の条件に変更した点を除いて、実施例1を繰り返した。
実施例1における導電性カーボン混合物を得るための振動ボールミル装置による乾式混合条件を、10hzでの20分間の条件から20hzでの30分間の条件に変更した点を除いて、実施例1を繰り返した。
実施例1における導電性カーボン混合物を得るための振動ボールミル装置による乾式混合条件を、10hzでの20分間の条件から30hzでの20分間の条件に変更した点を除いて、実施例1を繰り返した。
実施例1における導電性カーボン混合物を得るための振動ボールミル装置による乾式混合条件を、10hzでの20分間の条件から30hzでの30分間の条件に変更した点を除いて、実施例1を繰り返した。
実施例1における導電性カーボン混合物を得るための振動ボールミル装置による乾式混合条件を、10hzでの20分間の条件から10hzでの10分間の条件に変更した点を除いて、実施例1を繰り返した。
Claims (5)
- 導電性を有し且つ少なくとも一部が糊状である酸化処理カーボンと、
該酸化処理カーボンとは別の導電性カーボンと、
を含み、前記酸化処理カーボンが前記別の導電性カーボン混合物の表面を被覆している、蓄電デバイスの電極の製造のための導電剤として使用されるべき導電性カーボン混合物であって
該導電性カーボン混合物のラマンスペクトルにおける2Dバンドのピーク強度のDバンドのピーク強度に対する比が、前記別の導電性カーボンのラマンスペクトルにおける2Dバンドのピーク強度のDバンドのピーク強度に対する比の20~55%の範囲である導電性カーボン混合物の製造方法であって、
導電性を有するカーボン原料に酸化処理を施し、但し前記酸化処理を、該酸化処理によって得られる導電性を有する酸化処理カーボンが圧力を受けると糊状に広がる性質を有するようになるまで行う、酸化段階、及び、
前記酸化段階において得られた酸化処理カーボンと、該酸化処理カーボンとは別の導電性カーボンと、を乾式混合して、混合の圧力によって前記酸化処理カーボンの少なくとも一部を糊状に広げて前記別の導電性カーボンの表面を被覆させる混合処理を行い、但し前記混合処理を、該混合処理によって得られる導電性カーボン混合物のラマンスペクトルにおける2Dバンドのピーク強度のDバンドのピーク強度に対する比が、前記別の導電性カーボンのラマンスペクトルにおける2Dバンドのピーク強度のDバンドのピーク強度に対する比の20~55%の範囲になるように行う、混合段階、
を含むことを特徴とする導電性カーボン混合物の製造方法。 - 前記酸化段階における酸化処理を、該酸化処理によって得られる導電性を有する酸化処理カーボンが該酸化処理カーボン全体の10質量%以上の親水性部分を有するようになるまで行う、請求項1に記載の導電性カーボン混合物の製造方法。
- 前記混合段階における混合処理を、該混合処理によって得られる導電性カーボン混合物のラマンスペクトルにおける2Dバンドのピーク強度のDバンドのピーク強度に対する比が、前記別の導電性カーボンのラマンスペクトルにおける2Dバンドのピーク強度のDバンドのピーク強度に対する比の20~35%の範囲になるように行う、請求項1又は2に記載の導電性カーボン混合物の製造方法。
- 蓄電デバイス用の電極であって、
電極活物質と、
導電性を有し且つ少なくとも一部が糊状である酸化処理カーボンと、該酸化処理カーボンとは別の導電性カーボンと、を含み、前記酸化処理カーボンが前記別の導電性カーボン混合物の表面を被覆している、蓄電デバイスの電極の製造のための導電剤として使用されるべき導電性カーボン混合物であって、該導電性カーボン混合物のラマンスペクトルにおける2Dバンドのピーク強度のDバンドのピーク強度に対する比が、前記別の導電性カーボンのラマンスペクトルにおける2Dバンドのピーク強度のDバンドのピーク強度に対する比の20~55%の範囲である導電性カーボン混合物と、
を含む活物質層を有し、前記少なくとも一部が糊状である酸化処理カーボンが前記別の導電性カーボンの表面ばかりでなく前記電極活物質の表面も被覆している電極の製造方法であって、
電極活物質と、請求項1~3のいずれか1項に記載の製造方法によって得られた導電性カーボン混合物と、を混合して、混合の圧力により前記酸化処理カーボンをさらに糊状に広げて前記別の導電性カーボンの表面ばかりでなく前記電極活物質の表面も被覆させた電極材料を得る、調製段階、及び、
前記調製段階において得られた電極材料を用いて集電体上に活物質層を形成し、該活物質層に圧力を印加して、該圧力により、前記酸化処理カーボンをさらに糊状に広げて前記電極活物質の表面をさらに被覆させると共に前記導電性カーボン混合物を緻密化させる、加圧段階
を含むことを特徴とする電極の製造方法。 - 前記調製段階において用いられる前記電極活物質と前記導電性カーボン混合物との割合が、質量比で、97:3~99.5:0.5の範囲である、請求項4に記載の電極の製造方法。
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CN201880045991.1A CN110891900B (zh) | 2017-07-12 | 2018-07-03 | 导电性碳混合物及其制造方法、使用该混合物的电极及其制造方法、具备该电极的蓄电器件 |
US16/630,290 US11600824B2 (en) | 2017-07-12 | 2018-07-03 | Conductive carbon mixture and method for manufacturing same, electrode using conductive carbon mixture and method for manufacturing same, and electricity storage device provided with electrode |
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