JP2021527295A - 高表面積ナノチューブを使用する向上したリチウムイオン電池 - Google Patents
高表面積ナノチューブを使用する向上したリチウムイオン電池 Download PDFInfo
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- JP2021527295A JP2021527295A JP2020564914A JP2020564914A JP2021527295A JP 2021527295 A JP2021527295 A JP 2021527295A JP 2020564914 A JP2020564914 A JP 2020564914A JP 2020564914 A JP2020564914 A JP 2020564914A JP 2021527295 A JP2021527295 A JP 2021527295A
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- carbon nanotubes
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- nanotubes
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Abstract
【解決手段】
該カーボンナノチューブは、チューブ内表面の酸化をほとんど若しくはまったく有さず、又はチューブの内表面と外表面の間に異なる量及び/若しくはタイプの酸化を有し得る。さらに、そのような高表面積カーボンナノチューブは、より大きな長さ及び直径を有して、有用な機械的、電気的及び熱的特性を形成し得る。
【選択図】図1
Description
それに限定されないが、リチウムイオン電池技術を含むエネルギー貯蔵装置の向上した性能のために、高表面積カーボンナノチューブを含む組成物の実施形態を開示する。ある開示の実施形態では、アノードを含むシリコンにおける単層パウチセルは、OCSiAlによって生成されるようなカーボンナノチューブが開示される処理に従って処置されて高表面積単層ナノチューブを形成する場合に、大幅なサイクル寿命の向上を示す。ここで説明する用途における使用に適し得るナノチューブの他の製造業者は、例えば、Southwest Nanotechnologies、Zeonano or Zeon、CNano Technology、Nanocyl、ACS Materials、American Elements、Chasm Technologies、Haoxin Technology、Hanwha Nanotech Group、Hyperion Catalysis、KH Chemical、Klean Commodities、LG Chem、Nano−C,NTP Shenzhen Nanotech Port、Nikkiso、Raymor、Saratoga Energy、SK Global、Solid Carbon Products、Sigma Aldrich、Sun Nanotech、Thomas Swan、 TimesNano、Tokyo Chemical Industry、XF Nano、及びOCSiAlを含む。
>64%の硝酸35グラムを95℃に加熱する。受け取ったままの単層カーボンナノチューブ(Tuball(商標))15グラムを、その酸に添加する。受け取ったままのチューブは、堅くバンドル化された木の幹の形態を有する。酸及びカーボンナノチューブの混合物は、溶液を約95度に5時間維持しつつ混合され、「oSWCNT82−2」と付される。反応期間の終了時に、oSWCNT82−2を、ろ過して酸を除去し、逆浸透(RO)水でpH3〜4まで洗浄する。結果として得られるCNTは、約3.6%まで酸化され、約4.4%の金属残渣を含んでいた。
MAO処理によって酸化された試料:例えば、35gのHNO3(65%)/15gのTuball(商標)、95℃の酸化。
23.33gのHNO3(65%)+10.01gのCNT。T=95℃、CNTの添加時の初期の大きなプルームのNOX。
23.3gのHNO3、10gのTuball(商標)のCNT。5時間の酸化=2.5%のOx、9.95%の残渣、20.2%の固形分。31gを固形分@20.2%で回収。
試料体積〜1200mL。ロータ/ステータ(R/S)作業に対して1.5Lのステンレス鋼容器を使用。
酸化OCSiAl〜0.15%
酸化OCSiAl源:82−最終物(pH3.61、27.1%の固形分)
1200g×0.15%=1.8gの乾燥当量=6.64gのウェットケーク。6.65gのウェットケークを使用。
以下に示すようにロータ・ステータR/Sを通じて粘度を確認する。
600mLの固形分@0.4%=2.4gのOCSiAl。
OCSiAl源:Tuball(商標)の単層カーボンナノチューブ。バッチ番号01RW01.N1.257、製造日:2016年12月20日。
80/20の割合のMA14/酸化OCSiAlを調製した。これは、これらの構成要素の双方のウェットケークを採取し、それをロータ/ステータ、続いてせん断処置に通すことによって初期段階のものを生成し得るか確認するのに実施した。したがって、酸化OCSiAlは、リチウムイオン電池の性能にさらなる向上を与えるために、o−CNTをMolecular Rebar(登録商標)に変換しているのと同時に分解されている。
600mLの試料サイズ、1.5%MR。Molecular Rebar(登録商標)源のMA−14(固形分12.95%)。
酸化OCSiAl(「82−最終物」、固形分27.1%)
600×0.015=9g/0.1295=69.498gのMA14。
0.8gのMA−14/0.02gの酸化OCSiAl=9gのMA−14/0.225gの酸化OCSiAl。
0.225gの酸化OCSiAl=0.225/0.271=0.83gの82−最終物。
酸化及び未酸化OCSiAlセルが、Liイオン電池単層パウチセルに形成される−以下はセルの詳細:
NCM523 カソード//アノード
アノードの詳細:
20%のSiOx+71%のグラファイト+1%のCMC+1.5%のSBR+1%のC65+図2に示す%のXP。
装填:〜10mg/cm2
カソードの装填:4.2mAh/cm2
セパレータ:ガラス繊維−WhatmannGF/F
筐体:40mAhの単層パウチ
高純度のOCSiAlのSWCNTは、TGA分析によって測定されて、0.6%の酸化レベル及び17.7%の残渣(金属性不純物)を有する受け取ったままの低純度のOCSiAlのSWCNTと比べて、1.3%の酸化レベル及び0.6%の残渣を有した。高純度のOCSiAlのSWCNTの2.8gの試料は、脱イオン水で合計650gに希釈され(固形分0.43%)、ロータ/ステータを使用して10分処理された。そして、この材料は、装置を通じて単一パスに対して2000psiでせん断力を受けた。加圧を8000psiに増加させ、さらに8回せん断装置に通した。せん断処理したものに対するロータ/ステータ処理後の光学画像を、せん断前の高純度のOCSiAlのSWCNTを示す図8、及び広域せん断後の高純度のOCSiAlのSWCNTを示す図9に示す。図8及び9は双方とも倍率112.5倍である。
合計15グラムの高純度等級のOCSiAlのSWCNTを、35グラムの65%の硝酸水溶液に添加し、脱イオン水によって冷却された凝縮器に接続された丸底フラスコにおいて90℃で5時間加熱した。30分、及び1時間毎に、試料をフラスコから採取し、脱イオン水でpH3.9に洗浄し乾燥させた。そして、試料は、酸化レベル及び残渣(金属性不純物)についてTGAによって分析された。結果を以下の表に与える。
酸化後の高純度OCSiAl TuballのSWCNTについてのTGA結果の表
酸化処置前及び後の種々のSWCNTの酸化レベル及び残渣レベル
合計2グラムの高純度OCSiAl TuballのSWCNTを、脱イオン水で固形分0.4%に希釈した。混合物を、5分間10000rpmでロータ/ステータ処理した。試料を0.2%に希釈し、8500〜9000psiでせん断装置を2回通してせん断された。そのポイントで、脱イオン水中固形分3.79%の105グラムのWalocel CRT 30 PAカルボキシメチルセルロースナトリウム(CMC)を添加した。そして混合物は、その混合物を40℃未満の温度に維持しつつ、さらに8回せん断装置に通された。最終分散液と比べてロータ/ステータを通したSWCNTの光学顕微鏡写真を図10〜11に示す。図10はせん断前の高純度OCSiAl TuballのSWCNTを示し、図11はせん断装置及びCMC添加後の高純度OCSiAl TuballのSWCNTを示す。双方とも倍率11.25倍である。分散後の光学画像における任意の明白な粒子の欠如は、フィブリルのサイズが1ミリメートル未満であることを意味する(スケールバーは1ミリメートルである)。
脱イオン水中0.77%の酸化ZeonanoのSWCNTの水性混合物を、25分間10000rpmでロータ/ステータを使用して処理した。酸化は前述した。混合物を、処理中は27〜31℃に維持した。材料を固形分0.17%に希釈した。混合物を、5回せん断装置に通した。最初のパスでは6000psiでせん断され、後続のパスでは8000〜9000psiでせん断された。pHは、4回目のパス後にpH7に調整された。5回目のパス後に、CMCの1に対してSWCNTの1の質量比でWalocel CRT 30 PAカルボキシメチルセルロースナトリウム(CMC)を添加した。そして混合物は、その混合物の温度を40℃未満に維持しつつ、8000〜9000psiでさらに11回せん断装置に通された。14回目のパスでは、CMCの2.25に対してSWCNTの1の比で追加の界面活性剤を添加した。16回目のパスでは、CMCの2.75に対してSWCNTの1の比で追加の界面活性剤を添加した。図12はせん断前の酸化ZeonanoのSWCNTを示し、図13はせん断装置及びCMC添加後のそれを示す(倍率11.25倍)。
合計2グラムの受け取ったままの未酸化ZeonanoのSWCNTを、698グラムの脱イオン水と混合し、20分間10000rpmでロータ/ステータを使用して処理した。そして、脱イオン水を追加で195添加した。混合物を、8000〜9000psiで6回せん断装置に通した。そして、合計105.8グラムの固形分3.78%のWalocel CRT 30 PAカルボキシメチルセルロースナトリウム溶液を混合物に添加した。そして混合物は、その混合物の温度を40℃未満に維持しつつ、さらに14回せん断装置に通された。図14はせん断装置を5回通過した後の未酸化ZeonanoのSWCNTを示し(倍率35倍)、図15は20回のせん断装置の通過及びCMC添加後のそれを示す(倍率140倍)。
濃度0.3%の高純度OCSiAlをシレンに添加し、超音波浴において150分間超音波処理して、シレンにおけるSWCNTの分散液を生成した。図16は、30分の超音波処理後の高純度OCSiAlのSWCNTを示す(倍率169倍)。図17は、150分の超音波処理後の高純度OCSiAlのSWCNTを示す(倍率169倍)。
1.エネルギー貯蔵又は収集装置のバインダー材料、電解質材料又はセパレータフイルム材料として使用するための組成物であって、複数の高表面積カーボンナノチューブを備え、前記高表面積カーボンナノチューブの少なくとも一部が開口終端する、組成物。
Claims (11)
- エネルギー貯蔵又は収集装置のバインダー材料、電解質材料又はセパレータフイルム材料として使用するための組成物であって、
複数の高表面積カーボンナノチューブと、
少なくとも1つの分散助剤と
を含み、
前記高表面積カーボンナノチューブの少なくとも一部が開口終端しており、
前記複数の高表面積ナノチューブは酸化された単層ナノチューブであり、
前記複数の高表面積ナノチューブのBET表面が、ASTM D6556−16により550m2/g〜1500m2/gであり、
前記カーボンナノチューブはさらに機能化されており、
前記エネルギー貯蔵又は収集装置はリチウムイオン電池である、前記組成物。 - 少なくとも1つのポリマーをさらに含む請求項1に記載の組成物。
- 前記ポリマーが、ビニルポリマー、ポリ(スチレン−ブタジエン)、コポリマーを含む部分的又は完全に水素化されたポリ(スチレン−ブタジエン)、カルボキシル化されたポリ(スチレン−ブタジエン)などの機能化されたポリ(スチレン−ブタジエン)コポリマー、ポリ(スチレン−イソプレン)、ポリ(メタクリル酸)、ポリ(メタクリル酸メチル)、ポリ(アクリル酸)、ポリ(ビニルアルコール)、ポリ(酢酸ビニル)、フッ素化ポリマー、ポリビニルピロリドン、導電性ポリマー、天然源に由来するポリマー、ポリエーテル、ポリエステル、ポリウレタン及びポリアミドと、ホモポリマー、グラフト、ブロック又はランダムのコポリマー又はターポリマー、並びにそれらのコポリマー及び混合物とからなる群から選択される、請求項2に記載の組成物。
- カーボンブラック、グラファイト、グラフェン、酸化グラフェン、フラーレン及びそれらの混合物からなる群から選択されるカーボン構造体をさらに含む請求項1に記載の組成物。
- 離散カーボンナノチューブの少なくとも一部をさらに含む請求項1に記載の組成物。
- セルロースベースのポリマー又はその塩をさらに備える請求項1に記載の組成物。
- ポリスチレンスルホン酸塩又はその塩をさらに含む請求項1に記載の組成物。
- 親水性ポリマーをさらに含む請求項1に記載の組成物。
- 前記複数の酸化された高表面積カーボンナノチューブが、0.01〜2重量パーセントの酸化レベルを有する、請求項1に記載の組成物。
- 前記複数の酸化された高表面積カーボンナノチューブが、2〜5重量パーセントの酸化レベルを有する、請求項1に記載の組成物。
- 前記複数の高表面積カーボンナノチューブが、約25重量パーセント未満の不純物残渣を有する、請求項1に記載の組成物。
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