JP7345453B2 - 垂直に配向したカーボンナノチューブの製造方法、及びそのようなナノチューブを電極として使用する電気化学キャパシタ - Google Patents
垂直に配向したカーボンナノチューブの製造方法、及びそのようなナノチューブを電極として使用する電気化学キャパシタ Download PDFInfo
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Description
本発明によると、基板上のVACNTの成長は、反応器に連続的に注入される触媒源及び炭素源の存在下で行われる。非常に有利な実施形態によると、触媒源は炭素溶媒に触媒前駆体を溶解した後、液体状態で反応器に導入され、炭素源は気体状態である。これは、上記の欧州特許第1515911号明細書に記載されているように、注入ポンプを使用してパルプ注入によって行われ得る。
本発明の本質的な様態によると、VACNTマットは追加の無秩序な炭素を含む。この追加の無秩序な炭素の存在はラマン分光法によって実証され得るが、この手法ではその位置を特定することは不可能である。追加の無秩序な炭素は、走査型電子顕微鏡(SEM)で直接見られ得るが、この手法では無秩序の程度を特徴付けることは不可能である。無秩序な構造を把握し、特徴付けることを可能とする唯一の手法は、高分解能透過型電子顕微鏡(HR-TEM)であるが、その視野は非常に限られている。
スーパーキャパシタを製造するために、電子を伝導しない材料(セパレータ及び液体電解質)によって電気的に分離された少なくとも2つの電極を組み立てる必要がある。このステップは組み立てと呼ばれる。種々の組み立て技術があり、その選択はスーパーキャパシタの所望の特性に依存する。当社の製品に使用されるものは、本明細書の残りの部分で定義される。
VACNTマットは、触媒前駆体(トルエン中に溶解したフェロセン)の連続的なパルス注入によって3つの異なる反応器で製造され、炭素源はアセチレンである。この手法の原理は、国際公開第2004/000727号(Commissariat a l‘Energie Atomique et aux Energies Alternatives)に記載されている。第1反応器(「炉1」を参照)は、加熱された筐体内に330mm2の円形断面を有する石英チューブを含む管状炉で、その中に基板が配置された。第2反応器(「炉2」を参照)は、加熱された筐体内に1917mm2の円形断面を有する石英チューブを含む管状炉で、その中に基板が配置された。これら2つの炉はバッチ炉であった。第3反応器(「パイロット」を参照)は、金属ベルトが925mm2の長方形断面を移動し得る連続的な反応器であった。この反応器は静的モード中に本明細書で使用された(すなわち、1000mm×300mmの反応領域で移動しない)。
Mref=1.11(mg/cm2):追加の無秩序な炭素を含まない参照VACNTマットの単位面積あたりの質量
CNTの外径=9nm
href=59μm:測定した参照VACNTマットの高さ
Mmes:測定したVACNTマットの単位面積あたりの質量(mg/cm2)
hmes:測定したVACNTマットの高さ
Mest:追加の無秩序な炭素を含まない場合のVACNTマットの単位面積あたりの推定の質量(mg/cm2)、
無秩序な炭素(%):VACNTマット内の追加の無秩序な炭素の推定の割合
Mest=(Mref×hmes)/href
無秩序な炭素(%)=(Mmes-Mest)/Mmes×100
対称スーパーキャパシタは、記載の電極材料(本発明に係るVACNT、又は比較試験用の活性炭(ACと略す))から構成される電極から製造された。反対の指示がない限り、スーパーキャパシタは、アセトニトリル中1mol/リットルでセルロースベースとテトラエチルアンモニウムテトラフルオロホウ酸タイプの電解質を含むセパレータを使用して、2つの単相電極(直径10mmのディスクの形状)の対称組立体によって製造された。これらの電極の組立体は、Swagelok(登録商標)タイプの合成でカプセル化された。
図13は、アセトニトリル中1MのET4NBF4電解質と、厚さ46μm及び36μmのVACNTマットから形成された2つの電極とを使用したスーパーキャパシタの2.5Vラゴーンプロットを示す。電流の強さは、1~400mA/cm2の間で変化する。この図は、各材料が貯蔵し得るエネルギー(E)(E=1/2CV2)を、材料の電力(P)の関数(P=E/t)として示す。低電力の場合、追加の無秩序な炭素を56%含むシステム(サンプルNGI-1113、四角点)は、追加の無秩序な炭素を含まない場合(サンプルNI-766、三角点)よりも4倍多くのエネルギーを貯蔵する。高電力の場合、追加の無秩序な炭素を含まないシステムよりも常に多くのエネルギーを貯蔵する。
図16はラゴーンプロットであり、VACNTマットの様々な厚さ(高さ)において、56%~64%の範囲で、追加の無秩序な炭素を含むVACNTに基づいて本発明に係るスーパーキャパシタの性能を比較する。マットの高さを42μmから119μmに増加させると、貯蔵エネルギーに関する性能の向上が見られ、この効果は電力に依存しない。119μm~152μmの高さを通過することにより(NGI-1050を参照)、低速でも単位面積あたりのエネルギー量の減少が観察される。
本実施例では、本発明に係る対称プリズム型スーパーキャパシタ(R17017041-C1-C3-Powerを参照)は、市販のスーパーキャパシタ(Maxwell 10F BCAP0010を参照)と比較される。本発明に係るスーパーキャパシタは、セルロースベースのセパレータによって分離された、VACNTマットに基づく2つの片面電極(C1、C3)(寸法4cm×6cmの長方形)、及びアセトニトリ中1mol/リットルのテトラエチルアンモニウムテトラフルオロホウ酸タイプの電解質を含んでいた。組み立ては、フレキシブルパウチ(パウチセル)内で行われた。VACNTマットに基づく電極は、追加の無秩序な炭素を有した。それらは、連続的な反応器(パイロットS01)からきた。市販のスーパーキャパシタ(Maxwell 10F BCAP0010を参照)は円筒コイル型で、電極は活性炭で作製された。
Claims (19)
- 基板上に垂直に配向したカーボンナノチューブ(VACNT)を含む複合材料を調製する方法であって、該複合材料は、該カーボンナノチューブの外面上に堆積した追加の無秩序な炭素を含み、
前記方法は、触媒存在下で加熱された筐体を含む反応器内での炭素源ガスの化学蒸着と、基板上のVACNTの成長とを含み、
前記炭素源及び前記触媒前駆体を含む気相は、500℃~700℃の温度、かつ0.5bar~1.5barの圧力で前記加熱された筐体に連続的に注入され、
前記触媒前駆体は遷移金属を含み、
前記VACNT及び前記追加の無秩序な炭素の成長は、同一の気相成長ステップで行われる、方法。 - 前記追加の無秩序な炭素は、グラファイト領域を含む、請求項1に記載の方法。
- 前記遷移金属は、鉄、ニッケル、及びコバルトからなる群から選択される、請求項1又は2に記載の方法。
- 前記筐体に注入される前記気相は、炭素源としてのアセチレン、キャリアガスを備えた前記触媒前駆体、及び不活性ガスを含む、請求項1~3のいずれか1項に記載の方法。
- 前記筐体に注入される前記気相は、炭素源としてのアセチレン、水素、触媒前駆体としてのフェロセン、フェロセンでのキャリアガスとしてのトルエン、及び不活性ガスとしてのアルゴンからなる、請求項1~4のいずれか1項に記載の方法。
- 前記気相の通過速度は、1mm/s~15mm/sである、請求項1~5のいずれか1項に記載の方法。
- 前記気相の通過速度は、3mm/s~10mm/sである、請求項1~5のいずれか1項に記載の方法。
- 前記気相中の炭素の総含有量に基づいた鉄の含有量は、0.4%~1.2%である(質量%として)、請求項1~7のいずれか1項に記載の方法。
- 前記気相中の炭素の総含有量に基づいた鉄の含有量は、0.55%~0.9%である(質量%として)、請求項1~7のいずれか1項に記載の方法。
- アセチレンの総体積は、0.7~6ml/mm2であり、
アセチレン流の通過速度は、1mm/s~15mm/sであり、
Fe/C比に基づいて質量で表された鉄の含有量は、0.4%~1.5%である、請求項1~9のいずれか1項に記載の方法。 - 電子デバイス又は電気デバイス用の電極の製造方法であって、
前記製造方法は、基板上に垂直に配向したカーボンナノチューブ(VACNT)を含む複合材料を調製することを含み、
前記複合材料は、該カーボンナノチューブの外面上に堆積した追加の無秩序な炭素を含み、
前記複合材料を調製する方法は、請求項1~10のいずれか1項に記載の方法である、製造方法。 - 0.01~1kW/m2の電力で、少なくとも0.8Wh/m2のエネルギーを貯蔵可能であるスーパーキャパシタデバイスの製造方法であって、
請求項11に記載の電極の製造方法を含む、製造方法。 - 前記スーパーキャパシタは、0.01~1kW/m2の電力で、少なくとも2Wh/m2のエネルギーを貯蔵可能であることを特徴とする、請求項12に記載の製造方法。
- 請求項12又は13に記載のスーパーキャパシタデバイスを製造する方法であって、
(i)請求項11に記載の方法によって電極を製造すること、及びセパレータ、集電体、電解質、及び筐体を準備することと、
(ii)前記電極上の前記集電体を溶接することと、
(iii)前記電極及び前記セパレータを組み立てることと、
(iv)前記電極の前記集電体を前記筐体の末端に溶接すること、
(v)前記筐体内に電極/セパレータ組立体を取り付けること(ステップ(iv)及び(v)は逆でもよい)、
(vi)前記筐体内に前記電解質を追加及び拡散することと、
(vii)前記筐体を密封すること
とのステップを含む、方法。 - 前記電解質は、アニオンに付随するカチオンを含むイオン液体、又は溶媒中に溶解した塩を含む電解質溶液であり、該溶媒はプロトン性溶媒、又は非プロトン性溶媒、又は少なくとも1つの非プロトン性溶媒及び少なくとも1つのプロトン性溶媒の混合物である、請求項14に記載の方法。
- 前記非プロトン性溶媒は、ジクロメタンのハロゲン化アルカン、ジメチルホルムアミド(DMF)、アセトン又は2-ブタノンのケトン、アセトニトリル、テトラヒドロフラン(THF)、N-メチルピロリド(NMP)、ジメチルスルホキシド(DMSO)、及びそれらの混合物、炭酸プロピレン、炭酸エチレン、炭酸ジメチル、及びそれらの混合物、又はラクトンからなる群から選択される、請求項15に記載の方法。
- 前記イオン液体は、
1-エチル-3-メチルイミダゾリウム、1-メチル-3-プロピルイミダゾリウム、1-メチル-3-イソプロピルイミダゾリウム、1-ブチル-3-メチルイミダゾリウム、1-エチル-2,3-ジメチルイミダゾリウム、1-エチル-3,4-ジメチルイミダゾリウム、N-プロピルピリジニウム、N-ブチルピリジニウム、N-tert-ブチルピリジニウム、N-tert-ブタノール-ペンチルピリジニウム、N-メチル-N-プロピルピロリジニウム、N-ブチル-N-メチル-ピロリジニウム、N-メチル-N-ペンチルピロリジニウム、N-プロポキシエチル-N-メチルピロリジニウム、N-メチル-N-プロピルピペリジニウム、N-メチル-N-イソプロピルピペリジニウム、N-ブチル-N-メチルピペリジニウム、N-N-イソブチルメチルピペリジニウム、N-sec-ブチル-N-メチルピペリジニウム、N-メトキシ-N-エチルメチルピペリジニウム、及びN-エトキシエチル-N-メチルピペリジニウムの4級アンモニウムイオンを含むイオン液体と、
テトラフルオロホウ酸アニオン(BF4 -)、ヘキサフルオロリン酸アニオン(PF6 -)、ビス(トリフルオロメタンスルホニル)アミドアニオン(TFSI-)、又はビス(フルオロスルホニル)アミドアニオン(FSI-)のアニオンに付随する、ブチル-N-N-トリメチルアンモニウム、N-エチル-N,N-ジメチル-N-プロピルアンモニウム、及びN,N,N-トリメチルアンモニウムを含むイオン液体とからなる群から選択される、請求項15又は請求項16に記載の方法。 - 前記電解質は、
ピリジン、ピリダジン、ピリミジン、ピラジン、イミダゾール、ピラゾール、チアゾール、オキサゾール、トリアゾール、アンモニウム、ピロリジン、ピロリン、ピロール、及びピペリジンの誘導体からなる群から選択される少なくとも1つのカチオンと、
F-、Cl-、Br-、I-、NO3 -、N(CN)2 -、BF4 -、ClO4 -、PF6 -、RSO3 -、RCOO-、ここでRはアルキル基又はフェニル基、(CF3)2PF4 -、(CF3)3PF3 -、(CF3)4PF2 -、(CF3)5PF-、(CF3)6P-、(CF2SO3 -)2、(CF2CF2SO3 -)2、(CF3SO2 -)2N-、CF3CF2(CF3)2CO-、(CF3SO2)2CH-、(SF5)3C-、(CF3SO2)3C-、[O(CF3)2C2(CF3)2O]2PO-、CF3(CF2)7SO3 -、1-エチル-3-メチルイミダゾール、ビス(トリフルオロメチルスルホニル)イミド([EMIM][Tf2N])からなる群から選択される少なくとも1つのアニオンとを含むイオン液体を含む、請求項15~17のいずれか1項に記載の方法。 - 前記電解質溶液は、溶媒に加えて溶媒中に溶解した塩の状態で電解質を含み、
前記塩のアニオンは、
F-、Br-、Cl-、I-、HCO3 -、H2PO4 -、Cr2O4 3-、BF4 -、PF6 -、又はN(CN)2 -の無機イオンと、
RSO3 -、RCOO-(Rは置換される可能性のあるアルキル基又はフェニル基)、(CF3)2PF4 -、(CF3)3PF3 -、(CF3)4PF2 -、(CF3)5PF-、(CF3)6P-、(CF2SO3 -)2、(CF2CF2SO3 -)2、(CF3SO2 -)2N-、CF3CF2(CF3)2CO-、(CF3SO2)2CH-、(SF5)3C-、(CF3SO2SO2)3C-、[O(CF3)2C2(CF3)2O]2PO-、CF3(CF2)7SO3 -、ビス(トリフルオロ-メタンスルホニル)アミドアニオン、ビス(フルオロスルホニル)アミドアニオンからなる群から選択される有機イオンと、
ポリマーアニオンと、
生物アニオンとから選択され、
及び/又は前記塩のカチオンは、
Li+、Na+、Mg2+、Cu2+、Zn2+及びAl3+からなる群から選択される金属カチオン、又は有機カチオンであることが知られている、請求項16~18のいずれか1項に記載の方法。
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