JP2018168058A - 炭素の凝集アセンブリおよびその用途 - Google Patents
炭素の凝集アセンブリおよびその用途 Download PDFInfo
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- JP2018168058A JP2018168058A JP2018082191A JP2018082191A JP2018168058A JP 2018168058 A JP2018168058 A JP 2018168058A JP 2018082191 A JP2018082191 A JP 2018082191A JP 2018082191 A JP2018082191 A JP 2018082191A JP 2018168058 A JP2018168058 A JP 2018168058A
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Abstract
【解決手段】凝集炭素アセンブリは、粉末、粒子、フレークまたは疎凝集体の形態の炭素出発材料を得るステップと、機械的混合および/または超音波処理により炭素を選択された有機溶媒に分散させるステップと、典型的には蒸発により有機溶媒を実質的に除去して、それによって炭素の凝集アセンブリを形成するステップとにより調製される。
【選択図】図9
Description
本発明の方法により調製された凝集炭素アセンブリは、調製中および最終生成物中の界面活性剤の実質的な非存在を特徴とする。
Rs=4.53(V/I)
ρ=Rs(t)
を使用して計算することができる。
本発明の別の態様は、基板と基板の少なくとも1つの表面上にコーティングされた凝集炭素アセンブリとを含む物品であって、凝集炭素アセンブリは上記方法により調製された物品に関する。
安定なSWCNTのo−ジクロロベンゼン(ODCB)中分散液を以下のように調製した。
(1)SWCNT(Thomas Swan「Elicarb SW」)600mgをODCB500gと混ぜ合わせて第1の混合物を得た。
(2)第1の混合物を密閉容器中で30分間、高せん断ミキサー(10000rpm)および任意の超音波槽中での同時超音波処理を使用して混合および分散して第2の混合物を得た。
(3)次いで、ミキサー速度を5000rpmに低下させ、溶液が容器の壁に飛び散らないようにした。ODCB100gを、洗浄瓶を用いて容器の壁に噴霧することにより添加して、SWCNTが容器の壁に固着したままにならないようにした。得られた混合物を、10分間、5000rpmおよび任意選択により超音波槽中での同時超音波処理の存在下で混合して第3の混合物を得た。
(4)高せん断ミキサープローブを除去した後に、密閉容器中の第3の混合物を45℃で2時間、超音波槽中で超音波処理して第4の混合物を得た。
(5)第4の混合物をコーティングまたはキャスティングのために使用される準備ができたSWCNT−ODCB分散液とした。
超音波洗浄した直径9cmのペトリ皿をキャスティング用の型として使用した。Yanらの米国特許第6,395,331B1号明細書に記載されているように、ペトリ皿を疎水性コーティング溶液でコーティングした。疎水性コーティングにより、80°以上の水接触角を有する表面が得られた。型上の疎水性コーティングは、ディップコーティング、フローコーティング、スピンコーティング、またはスプレーコーティング、次いで200℃で1時間の硬化(および乾燥)により調製した。
実施例1により調製されたSWCNT−ODCB分散液約165mgを、アルミニウム箔で裏打ちしたペトリ皿に注ぎ込んだ。ODCB溶媒を実施例2に記載するように蒸発により除去した。約20μm厚さのコーティングフィルムとしての接着性凝集SWCNTアセンブリがアルミニウム箔表面上に形成した。SWCNT−アルミニウム物品を300℃で4時間加熱下後、層間剥離も接着性の喪失も観察されなかった。
実施例1により調製されたSWCNT−ODCB分散液1mlを、500rpmで30秒間シリコンウエハー基板上にスピンコーティングする。ODCB溶媒を空気中で少なくとも1分間蒸発させることにより除去する。コーティングフィルムとしての凝集SWCNTアセンブリが基板上に形成し、これは約0.5μmの厚さを有する。
実施例1により調製されたSWCNT−ODCB分散液を少なくとも6インチ幅、1インチ深さおよび5インチ高さで長方形タンクに入れる。十分な量の分散液をタンクに入れてこれを上面の1インチ以内まで満たす。銅、アルミニウム、またはほかの金属基板、またはシリコンウエハーの4×6インチシートを、SWCNT−ODCB分散液のタンク中に降ろす。次いで、基板を0.2cm/秒の速度でタンクから垂直に引き出す。ODCB溶媒を空気中で少なくとも1分間蒸発させることにより除去する。コーティングフィルムとしての凝集SWCNTアセンブリが基板上に形成し、これは約5μmの厚さを有する。
実施例1により調製されたSWCNT−ODCB分散液を、アルミニウム箔基板上に噴霧する。ODCB溶媒を、0.25トルおよび50℃の真空オーブンで少なくとも10分間蒸発させることにより除去する。コーティングフィルムとしての凝集CNTアセンブリが基板上に形成し、これは約50μmの厚さを有する。
(I)電気シート抵抗および抵抗率
キャパシタ、燃料電池または電池のような装置用の集電装置として有用となるためには、材料は十分に低い抵抗率(10−2Ω・cm以下程度)および十分な機械的堅牢性(高い引張り強さおよび耐破損性)を有する必要がある。
Rs=4.53(V/I)
ρ=Rs(t)
を使用して計算した。
実施例2により調製されたSWCNTアセンブリおよび対応する炭素出発材料を、標準的方法を使用してラマンスペクトルにより特性評価した。SWCNTウエハーは、炭素出発材料の比(未処理のCNT粉末、ラマンG/D比4.6)に比べて改善したウエハーの上面の4.9と底面の7.1のラマンG/D比を示した(図3)。このことは、カーボンナノチューブと無定形炭素などの他の形態の炭素の比が多少高かったこと、および/またはカーボンナノチューブの欠陥濃度がアセンブリの底に向かって多少低かったことを示唆している。
実施例2および3により調製されたSWCNTアセンブリをSEM(JSM−7500F、JEOL Ltd.、東京)により画像処理および特性評価した。像は、得られたSWCNTアセンブリが溶媒蒸発工程中に織り合わせナノチューブ構造を形成し、ナノチューブの長さと直径のアスペクト比を保護していることを示した。
凝集炭素アセンブリを、実施例2に記載されている手順にしたがって調製した。SWCNTアセンブリは直径約9cmおよび厚さ約20〜35μm(側面計、モデルDektak 150、Veeco Instruments Inc.、Plainview、NYを用いて測定した)であった。直径約0.625インチのディスクを、標準的実験室ブレードを使用してアセンブリから切り抜いた。
1.1.0、1.5および2.0Vで30分後の漏洩電流
2.2.0Vバイアス電圧でEIS(電気化学インピーダンス分光法)測定
3.Arbinテスターを使用した一定電流および一定電力充電/放電測定。
凝集炭素アセンブリを、実施例2に記載されている手順にしたがって調製する。SWCNTアセンブリは、直径約9cmおよび厚さ約40〜60μmである。
凝集炭素アセンブリを、実施例2に記載されている手順にしたがって調製する。SWCNTアセンブリは、直径約9cmおよび厚さ約40〜60μmである(側面計により測定)。
SWCNTの液体溶媒中分散液を、トルエンをODCBの代わりに分散溶媒として使用し、SWCNT250mgをトルエン217.5g(約250ml)に分散させたことを除いて実施例1(ステップ1〜4)に記載されているのと同様の方法で調製した。結果として生じる混合物はコーティングまたはキャスティングに使用する準備ができた安定なSWCNT−トルエン分散液であった。
SWCNTのトルエン中分散液を実施例11に記載されるように調製した。約25μmの厚さを有するアルミニウム箔をアセトンですすぎ、乾燥窒素ガス流で乾燥させて任意の表面汚染物質を除去した。9cmペトリ皿の底面および側面を覆うのに十分大きい箔の小片を、より光る側を上にしてこの皿の内側に置いた。箔を皿の底面および側面に押し付けることにより、箔を手で成形して、皿の内側に箔の裏打ちを作成した。第2の皿も同様に箔で裏打ちした。SWCNT−トルエン分散液各々約43.5g(50ml)を、2つのアルミニウム箔裏打ちペトリ皿にゆっくり注ぎ込んだ(図7)。
2つの凝集SWCNTアセンブリ(ウエハー)に電気化学インピーダンス分光法(EIS)測定を行った。一方は、実施例12に記載されているように調製した、アルミニウム(Al)基板上の接着性SWCNTウエハーとした。他方は、分散溶媒として臭素を使用して、国際公開第2010/102250号に記載されているように調製し、その後、標準的工業法を使用してAl集電装置に結合させた自立SWCNTウエハーとした。両SWCNTウエハーは16.5±1.5μmの同様の厚さを有していた。
Claims (29)
- (a)粉末、粒子、フレークまたは疎凝集体の形態の炭素出発材料を得るステップと、
(b)トルエン、o−ジクロロベンゼン(ODCB)、イソプロピルアルコール(IPA)、N,N−ジメチルホルムアミド(DMF)、ベンゼン、クロロベンゼン、m−ジクロロベンゼン、1,2,4−トリクロロベンゼン、ブロモベンゼン、m−ジブロモベンゼン、o−ジブロモベンゼン、トルエン、o−キシレン、m−キシレン、p−キシレン、1,2−ジクロロエタン、1,2−ジブロモエタン、クロロホルム、ホルムアミド、N−メチルホルムアミド、N−ビニルホルムアミド、N−(フェネチル)ホルムアミド、N,N−ジエチルホルムアミド、N,N−ビス(1−メチルエチル)ホルムアミド、ジメチルスルホキシド、またはこれらの任意の組み合わせを含む有機溶媒に、前記炭素出発材料を所定の比で分散させて分散液を調製するステップと、
(c)制御された方法で前記有機溶媒を実質的に除去して、それによって凝集炭素アセンブリを形成するステップと、を含む、凝集炭素アセンブリを調製する方法。 - 前記炭素出発材料がカーボンナノチューブ、グラフェン、黒鉛、膨張黒鉛、剥離黒鉛、無定形炭素、およびこれらの任意の組み合わせからなる群から選択される炭素材料である、請求項1に記載の方法。
- 前記カーボンナノチューブが単層カーボンナノチューブ、二層カーボンナノチューブ、多層カーボンナノチューブ、またはこれらの任意の組み合わせである、請求項2に記載の方法。
- 前記形成された凝集炭素アセンブリのラマンG/D比が前記炭素出発材料のラマンG/D比とほぼ同じであるか、またはこれより大きい、請求項2に記載の方法。
- 前記有機溶媒がトルエンである、請求項1に記載の方法。
- 前記有機溶媒がo−ジクロロベンゼンである、請求項1に記載の方法。
- ステップ(b)で、前記炭素出発材料を、機械的攪拌の存在下で前記有機溶媒に分散させる、請求項1に記載の方法。
- 前記機械的攪拌が超音波処理、機械的攪拌またはこれらの組み合わせを含む、請求項7に記載の方法。
- 前記炭素出発材料が単層カーボンナノチューブであり、前記有機溶媒がo−ジクロロベンゼンまたはトルエンであり、前記炭素出発材料と前記有機溶媒との比が前記有機溶媒1g当たり炭素約0.1〜約20mgである、請求項1に記載の方法。
- 前記有機溶媒が結合材料を実質的に含まない、請求項1に記載の方法。
- 前記除去した有機溶媒を回収するステップをさらに含む、請求項1に記載の方法。
- ステップ(b)の後であって、かつステップ(c)の前に前記分散液を疎水性表面に塗布するステップをさらに含む、請求項1に記載の方法。
- 前記疎水性表面がジメチルオルガノシラン、フッ化ジメチルオルガノシラン、フッ化ポリマーまたはテフロン(登録商標)を含む、請求項12に記載の方法。
- 前記分散液がキャスティングにより前記疎水性表面に塗布される、請求項12に記載の方法。
- ステップ(b)の後であって、かつステップ(c)の前に前記分散液を親水性表面に塗布するステップをさらに含む、請求項1に記載の方法。
- 前記親水性表面が金属、ガラス、ケイ素、プラスチック、セラミック、およびこれらの任意の組み合わせからなる群から選択される、請求項15に記載の方法。
- 前記親水性表面がアルミニウム、ニッケル、銅、金、銀、白金、およびこれらの任意の組み合わせからなる群から選択される金属基板である、請求項15に記載の方法。
- 前記分散液を、スピンコーティング、ディップコーティング、フローコーティング、スプレーコーティング、キャスティング、またはこれらの任意の組み合わせにより前記親水性表面に塗布する、請求項15に記載の方法。
- 請求項17に記載の方法により調製された金属基板上の凝集炭素アセンブリ。
- 前記炭素出発材料がカーボンナノチューブであり、前記有機溶媒がo−ジクロロベンゼン、トルエン、またはこれらの組み合わせである、請求項19に記載の金属基板上の凝集炭素アセンブリ。
- 前記凝集アセンブリに、フーリエ変換赤外分光法(FT−IR)、エネルギー分散型X線分光法(EDS)または熱質量分析法(TGA)により検出可能な前記有機溶媒が残留していない、請求項19に記載の金属基板上の凝集炭素アセンブリ。
- 前記凝集アセンブリが約0.1Ω・cm未満の電気抵抗率を有する、請求項19に記載の金属基板上の凝集炭素アセンブリ。
- 前記凝集アセンブリが約2000Ω/スクエア未満の電気シート抵抗を有する、請求項19に記載の金属基板上の凝集炭素アセンブリ。
- 絶縁材料により分離された2つのキャパシタ電極を含むキャパシタであって、前記2つのキャパシタ電極の少なくとも1つは請求項17に記載の方法により調製された金属基板上の凝集炭素アセンブリを含む、キャパシタ。
- 電解液により分離された2つの電極を含む燃料電池であって、前記2つの電極の少なくとも1つは請求項17に記載の方法により調製された金属基板上の凝集炭素アセンブリを含む、燃料電池。
- 電解液により分離された2つの電極を含む電池であって、前記2つの電極の少なくとも1つは請求項17に記載の方法により調製された金属基板上の凝集炭素アセンブリを含む、電池。
- 絶縁材料の一方側の集電装置および電極と、前記絶縁材料の他方側の別の集電装置および別の電極とを含む、エネルギー貯蔵装置であって、前記2つの集電装置の少なくとも1つは請求項17に記載の方法により調製された金属基板上の凝集炭素アセンブリを含む、エネルギー貯蔵装置。
- 電解液の一方側の集電装置および電極と、前記電解液の他方側の別の集電装置および別の電極とを含む、エネルギー貯蔵装置であって、前記2つの集電装置の少なくとも1つは請求項17に記載の方法により調製された金属基板上の凝集炭素アセンブリを含む、エネルギー貯蔵装置。
- 請求項15に記載の方法により調製された親水性表面上の凝集炭素アセンブリ。
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EP3582239B1 (en) | 2023-05-10 |
US20140106257A1 (en) | 2014-04-17 |
US10312503B2 (en) | 2019-06-04 |
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EP3582239A1 (en) | 2019-12-18 |
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JP6387300B2 (ja) | 2018-09-05 |
US20170194629A1 (en) | 2017-07-06 |
EP2720975A4 (en) | 2015-05-27 |
WO2012177555A3 (en) | 2013-05-10 |
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US9617158B2 (en) | 2017-04-11 |
WO2012177555A2 (en) | 2012-12-27 |
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