JP7176735B2 - セル式グラフェン膜 - Google Patents
セル式グラフェン膜 Download PDFInfo
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- JP7176735B2 JP7176735B2 JP2018532233A JP2018532233A JP7176735B2 JP 7176735 B2 JP7176735 B2 JP 7176735B2 JP 2018532233 A JP2018532233 A JP 2018532233A JP 2018532233 A JP2018532233 A JP 2018532233A JP 7176735 B2 JP7176735 B2 JP 7176735B2
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- graphene oxide
- oxide film
- seconds
- acid
- reduced graphene
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- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
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- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
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- 230000004660 morphological change Effects 0.000 description 1
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- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
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- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
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- 238000010257 thawing Methods 0.000 description 1
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
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- 229920000785 ultra high molecular weight polyethylene Polymers 0.000 description 1
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- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
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Images
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Description
本出願は、2015年12月22日に出願された米国仮特許出願シリアルナンバー第62/271,115号の利益を主張し、2016年12月1日に出願された米国仮特許出願シリアルナンバー第62/428,608号の利益を主張するものである。それらの開示全体は、参照により本明細書に組み込まれる。
本開示のエネルギー貯蔵デバイス(例えば、スーパーキャパシタ)は、市場で入手可能なスーパーキャパシタ(例えば、1~10kW/kgの出力密度を有するスーパーキャパシタ)よりも少なくとも約1.5、2、5、10、20、50、100、200または300倍大きい出力密度を有することができる。本開示のエネルギー貯蔵デバイス(例えば、スーパーキャパシタ)は、市場で入手可能なスーパーキャパシタ(例えば、サイクル安定性または500サイクルのサイクル寿命のスーパーキャパシタ)より少なくとも約1.5、2または2.5倍大きいサイクル安定性またはサイクル寿命を有することができる。例えば、本開示のエネルギー貯蔵デバイス(例えば、スーパーキャパシタ)は、競合する技術の500のみのサイクルに比べて、電子デバイス(複数可)を2倍の長さ動作させることができ、5000サイクル超使用することができる。
本開示のエネルギー貯蔵デバイスは、少なくとも1本の電極(例えば、正極及び負極)を含むことができる。本開示のグラフェン材料は、正極(放電中のカソード)、負極(放電中のアノード)または両方に設けることができる。特定の実施形態では、エネルギー貯蔵デバイスはスーパーキャパシタであってもよい。
図1は、酸化グラフェン(GO)の分散101、GOの部分的前還元102、還元したGOの濾過103、及び凍結鋳造の工程を含む多孔質グラフェン膜105の形成を概略的に示す。水相の図は、異なる処置の間の水溶液の状態及び例示的な多孔質グラフェン膜の典型的な断面SEM画像を示す。
図7A~図7Dは、それぞれ5分、10分、20分及び30分前に前還元した例示的な還元型GOの3D多孔質グラフェン膜701、702、703、704のSEM画像を示す。
2電極システムにおけるスーパーキャパシタ(Ccell)の容量は、以下を使用して、異なる電流密度でのそのガルバノスタット充放電曲線から計算される:
電界放出型走査電子顕微鏡(FE-SEM、JEOL6701F)及び透過型電子顕微鏡(TEM、FEI TF20)を用いて、例示的に調製した膜の形態及び微細構造を特徴付けた。Cu-Kα線(/c=1.54184A)を有するPanalytical X’Pert Pro X線粉末回折計を用いて、X線回折パターンを収集した。例示的なラマン分光測定は、633nmの励起波長でレーザーマイクロラマンシステム(Renishaw)を用いて行った。原子間力顕微鏡画像を走査型プローブ顕微鏡(Bruker Dimension 5000)を用いて記録した。引張試験機(Q800 DMA(Dynamic Mechanical Analyzer))を用いて各膜の引張強さを検証した。X線光電子分光データは、単色のAlKa X線源(hv 1486.6eV)を用いて分光計(Kratos AXIS Ultra DLD)で収集した。
他に定義されない限り、本明細書で使用するすべての技術用語は、本発明が属する技術分野の当業者が一般的に理解するのと同じ意味を有する。本明細書及び添付の特許請求の範囲で使用している場合、単数形「a」、「an」及び「the」には、文脈上他に明確に指示されていない限り、複数の言及が含まれる。「または」へのいかなる言及も、他に記載がない限り、「及び/または」を含むことを意図している。
10年前にグラフェンが発見されて以来ずっと、研究者らは、より速いコンピュータチップ及びフレキシブルなタッチスクリーンから並外れて効果的な太陽電池及び脱塩膜まで、数十個の潜在的な用途を提案してきた。重要な関心を呼んできた1つの高揚を覚える用途は、グラフェンが電荷を蓄える能力である。サッカー場全体を覆うのに十分な大きさのグラフェンの1枚のシートは、約6グラムの重さにすぎない。このわずかな量のグラフェンに関連したこの巨大な表面積により、AAサイズのバッテリの内部で圧迫され、膨大な量の電荷を蓄える新しいエネルギー貯蔵デバイスの実現が可能になる。しかし、現在の3次元(3D)グラフェン膜は、導電性が乏しく、機械的強度が弱く、破滅的な多孔率という問題を抱えている。
Claims (26)
- 1000nm未満のサイズを有する細孔を形成する2次元グラフェンシートの3次元ネットワークを含む還元型酸化グラフェン膜であって、少なくとも約0.1g/cm3の密度を有し、26ms未満の時定数を有する、エネルギー貯蔵デバイスの電極に用いるための還元型酸化グラフェン膜。
- 前記還元型酸化グラフェン膜が、少なくとも約0.1mg/cm2の面積質量負荷を有する、請求項1に記載の還元型酸化グラフェン膜。
- 前記還元型酸化グラフェン膜が、少なくとも約9MPaの引張強さを有する、請求項1に記載の還元型酸化グラフェン膜。
- 前記還元型酸化グラフェン膜が、少なくとも約1,000S/mの導電率を有する、請求項1に記載の還元型酸化グラフェン膜。
- 前記還元型酸化グラフェン膜が、少なくとも約4Wh/kgの質量エネルギー密度を有する、請求項1に記載の還元型酸化グラフェン膜。
- 前記還元型酸化グラフェン膜が、少なくとも約25kW/kgの質量出力密度を有する、請求項1に記載の還元型酸化グラフェン膜。
- 前記還元型酸化グラフェン膜が、1A/gの電流密度において少なくとも約90F/gの質量容量を有する、請求項1に記載の還元型酸化グラフェン膜。
- 前記還元型酸化グラフェン膜が、約1000サイクルの充電後に少なくとも約50%の容量保持を有する、請求項1に記載の還元型酸化グラフェン膜。
- 前記還元型酸化グラフェン膜が、少なくとも約25mF/cm2の面積容量を有する、請求項1に記載の還元型酸化グラフェン膜。
- (a)2本の電極であり、そのうちの少なくとも1本の電極が、1000nm未満のサイズを有する細孔を形成する2次元グラフェンシートの3次元ネットワークを含む還元型酸化グラフェン膜を含み、前記還元型酸化グラフェン膜が、少なくとも約0.1g/cm3の密度を有し、26ms未満の時定数を有する、上記2本の電極、
(b)電解質、及び
(c)前記2本の電極の間に配置されたセパレータ
を含む、スーパーキャパシタデバイス。 - 還元型酸化グラフェン膜を含む前記少なくとも1本の電極が、約6μm~約60μmの厚さを有する、請求項10に記載のスーパーキャパシタ。
- 前記電解質が、過塩素酸、ヨウ化水素酸、臭化水素酸、塩酸、硫酸、p-トルエンスルホン酸、メタンスルホン酸、またはそれらの任意の組み合わせを含む強酸を含む、請求項10に記載のスーパーキャパシタ。
- 前記セパレータが、ネオプレン、ナイロン、ポリ塩化ビニル、ポリスチレン、ポリエチレン、ポリプロピレン、ポリアクリロニトリル、ポリビニルブチラール、シリコーン、またはそれらの任意の組み合わせを含むポリマーを含む、請求項10に記載のスーパーキャパシタ。
- 少なくとも約0.1Wh/Lの容積エネルギー密度を有することを条件とする、請求項10に記載のスーパーキャパシタ。
- 少なくとも約3kW/Lの容積出力密度を有することを条件とする、請求項10に記載のスーパーキャパシタ。
- (a)酸化グラフェン懸濁液を形成するために酸化グラフェンを第1の溶媒中に懸濁させること、ここで、前記第1の溶媒は、テトラヒドロフラン、酢酸エチル、ジメチルホルムアミド、アセトニトリル、アセトン、ジメチルスルホキシド、ニトロメタン、プロピレンカーボネート、エタノール、ギ酸、n-ブタノール、メタノール、酢酸、水、脱イオン水、またはそれらの任意の組み合わせを含む、
(b)酸化グラフェン分散液を形成するために前記酸化グラフェン懸濁液を、弱酸を含む第2の溶媒に分散させること、
(c)前記酸化グラフェン分散液を還元すること、
(d)薄膜上に還元型酸化グラフェン膜を形成するために前記薄膜を介して前記還元された酸化グラフェン分散液を濾過すること、及び
(e)前記薄膜上の前記還元型酸化グラフェン膜を凍結鋳造すること
を含む、請求項1に記載のエネルギー貯蔵デバイスの電極に用いるための還元型酸化グラフェン膜の製造方法。 - 前記第1の溶媒中の前記酸化グラフェンの濃度が、約1mg/mL~約6mg/mLである、請求項16に記載の方法。
- 前記弱酸が、ギ酸、クエン酸、酢酸、アスコルビン酸、リンゴ酸、酒石酸、プロピオン酸、酪酸、吉草酸、カプロン酸、シュウ酸、安息香酸、炭酸、またはそれらの任意の組み合わせを含む、請求項16に記載の方法。
- 前記酸化グラフェン分散液が、約0.5mL~約10mLの体積の前記酸化グラフェン
懸濁液と、約3mg~約70mgの質量の前記第2溶媒とを含む、請求項16に記載の方法。 - (c)が、約25℃~約100℃の温度で前記酸化グラフェン分散液を加熱することを含む、請求項16に記載の方法。
- (c)が、約1分~約100分の期間にわたって前記酸化グラフェン分散液を加熱することを含む、請求項16に記載の方法。
- 前記薄膜が、約0.1μm~約0.5μmの孔径を有する、請求項16に記載の方法。
- (e)が、
(f)前記薄膜上の前記還元型酸化グラフェン膜を凍結すること、
(g)前記薄膜上の前記凍結した還元型酸化グラフェン膜を融解すること、
(h)前記薄膜上の前記融解した還元型酸化グラフェン膜を加熱すること、及び、
(i)第3の溶媒中に前記薄膜上の前記加熱した還元型酸化グラフェン膜を浸漬すること
を含み、
前記第3の溶媒が、テトラヒドロフラン、酢酸エチル、ジメチルホルムアミド、アセトニトリル、アセトン、ジメチルスルホキシド、ニトロメタン、プロピレンカーボネート、エタノール、ギ酸、n-ブタノール、メタノール、酢酸、水、脱イオン水、またはそれらの任意の組み合わせを含む、請求項16に記載の方法。 - 前記還元型酸化グラフェン膜が、少なくとも約15分の期間にわたって前記薄膜上で凍結される、請求項23に記載の方法。
- 前記薄膜上の前記還元型酸化グラフェン膜を前記加熱することが、約50℃~約200℃の温度で生じる、請求項23に記載の方法。
- 前記還元型酸化グラフェン膜の厚さが約6μm~約60μmであることを条件とする、請求項16に記載の方法。
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