JP2019511982A - 柔軟性炭素ポケット複合構造体、その製造方法、それを含む電極及び前記電極を含むエネルギー貯蔵デバイス - Google Patents
柔軟性炭素ポケット複合構造体、その製造方法、それを含む電極及び前記電極を含むエネルギー貯蔵デバイス Download PDFInfo
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- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 1
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- 239000007784 solid electrolyte Substances 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical class O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
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- 229910052715 tantalum Inorganic materials 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
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- 238000005406 washing Methods 0.000 description 1
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Abstract
Description
明示されていない場合、全ての試薬は、商業的出処(Junsei、Henkel、Grapheneスーパーマーケット、US Research Nanomaterials、Inc.,Angstron Materials及びドクサン)で得られ、精製せずに使用された。特に、シリコンナノ粒子 (粒子サイズ:30nm〜50nm、98+%)は、Nanostructured&Amorphous Materials,Inc.で購入した。水酸化カリウム(KOH)はJunseiから購入した。シアノアクリレート(Cyanoacrylate)グルーは、Henkelで購入した。グラフェン粉末は、Graphene Supermarket、US Research Nanomaterials、Inc.及びAngstron Materialsで購入した。アセトンと蒸留水は、ドクサンで購入した。全ての化学物質は、大気中で使用された。
グラフェン粉末とシリコンナノ粒子は、超音波処理を使用してアセトン中で重量比(1:9、2:8、3:7及び4:6)で混合した。その後、前記混合溶液にシアノアクリレートグルーモノマーを添加し、数時間直ちに手で揺すった。この時、使用されるグラフェン及びアセトンの量によってシアノアクリレートグルーモノマーの量が調節された。前記グルーモノマーは、前記アセトンと同じ重量を使用し、それは、グラフェン重量の数十倍にあたる。シアノアクリレートグルーモノマーは、数秒内に重合反応を開始し、前記反応は1分以内に終了した。
1.FE−TEM(電界放出−透過顕微鏡)
TEM観察(FEI社製、Titan cubed G2)の場合、Si_GPPがアセトン溶媒を用いて分散し、Cuメッシュグリッド上に位置した。前記TEMに付着したエネルギー分散分光器(EDS:Energy Dispersive Spectrometry)を使用して局所の元素情報及び元素マッピングを得た。
SEM観察(FEI社のMagellan 400、Hitachi社の SU8230)の場合、Si_GPP及びSi_ECA_Gがアセトン溶媒内に分散してシリコンウェハの小さい切れ上に滴加した。また、SEMに付着した後方散乱電子(BSE)検出器が区別されるシリコン粒子のイメージを得るために使用された。Si_GPP断面観察のための試料を製造するために、5mgのSi_GPPがNafion 117溶液内に分散した後、シリコンウェハ上にも滴加した。イオンビーム断面ポリッシャ(IB09010CP、JEOL)がイオンビームを使用して断面サンプルを作るのに使用された。
Si_GPP及びSi_ECA_GのXPSスペクトルは、多重−アノード、パルス係数及び半球型分析機を具備した350W AlアノードX線光源が装着されたThermo VG ScientificのSigma Probeを使用して得られた。前記スペクトルは、1486.6eVの入射光子エネルギーを使って収集され、検出器の仕事関数に対して校正された。
粉末X線データは、1200W(40KV、30mA)電力でJohansson型Ge(111)単色光フィルターCu Kα1放射線を使用して、反射Bragg−Brentano幾何(geometry)で高速1D検出器 (D/teX Ultra)が具備されたSmartLab θ−2θ回折機を利用して収集された。Si_GPP、シリコンナノ粒子及び純粋グラフェンの粉末をホルダーステージに装着し、連続モードで2゜/分のスキャン速度でスキャンした。
Si_GPPサンプルで純粋シリコンの重量の割合は、TGA(TG209 F1 Libra、NETZSCH)を使用して決められた。熱処理によってSi_GPPがSi_ECA_Gとして生成される時、熱分解(pyrolysis)を測定した。
Si_GPPとSi_ECA_Gで炭素マトリックスの欠陥または変形は、ArイオンCWレーザー(514.5nm)を具備した高分解分散ラマン顕微鏡(ARAMIS、HORIBA)を使用して得たラマンスペクトルによって観察された。
MALDI−TOFデータは、Bruker autoflex III(Bruker Daltonics)を使って収集した。前記分析によって重合されたECAの分子量が測定された。前記測定のために、CHCl3にSi_GPPを溶解させ、HCCA(α−Cyano−4−hydroxycinnamic acid)マトリックスを使用した。
ハーフセルの電気化学的特性:
アノード用作動電極は、N−メチル−2−ピロリドン(NMP)でSi_GPP(80重量%)、カーボンブラック(Super−P、10重量%)及びポリ(ビニリデンフルオライド)結合剤(PAA、10重量%)を混合させてスラリーを形成することで製造された。前記スラリーは、ドクターブレード (doctor blade)を使って純粋な銅ホイールにペーストされ、真空オーブンで70℃で一晩中乾燥させた。前記製造された試料の電気化学的性能は、カウンター/レファレンス電極として純粋なリチウム金属(Honjo Chemical Co.)を使ってアルゴン充填グローブボックス内で組み立てられたCR2032タイプのバッテリを使って調査された。エチレンカーボネート(EC)とジエチルカーボネート(DEC)/ ビニレンカーボネート(EC/DEC/VC=1:1:0.02、v/v/v)の助溶媒に溶解された1Mリチウムヘキサフルオロホスフェート(LiPF6)が電解質として使用された。Celgard 2400ポリプロピレンが分離膜として使用された。
Si_GPP電極は、カウンター金属/レファレンス電極としてLi金属及び分離膜を利用してハーフ−セルで組み立てられた。前記セルは、可変抵抗器を具備したリチウム化用回路に設置された後、30分間リチウム化された。本発明者は、100オームの抵抗を使ってリチウム化速度を制御し、事前リチウム化の間にSEI形成を制御した。事前リチウム化後、前記セルを解体した後、ハーフセル及びフルセル配列で製造した。
フルセル配列において、Si_GPP/カソード及び黒鉛/カソードデバイスの電気化学的性能を評価するために、Si_GPPをアノードとして使用し、代表的なカソード物質(LCO、LMO及びLFP)を使用するSi_GPP ベースフルセル及びアノードとして黒鉛を使用し、前記代表的なカソード物質をカソードとして使用する黒鉛ベースフルセルを小銭タイプのセルを使って製造した。前記製作の前に、前記Si_GPP電極は、作動中にLiイオン損失を防止するために、最大初期クーロン効率を得るように事前リチウム化された。
Claims (44)
- 互いに対向する炭素質第1シート及び炭素質第2シートによって形成された一つ以上の炭素質第1ポケットのそれぞれによって包接された粒子を含む複合体を含む、柔軟性炭素ポケット複合構造体。
- 前記互いに対向する炭素質第1シート及び炭素質第2シートは、一つ以上の領域で互いに接触しており、前記炭素質第1シート及び前記炭素質第2シートが互いに接触していない一つ以上の領域は、それぞれ前記炭素質第1ポケットを形成する、請求項1に記載の柔軟性炭素ポケット複合構造体。
- 前記一つ以上の炭素質第1ポケットは、互いに離隔して形成される、請求項1に記載の柔軟性炭素ポケット複合構造体。
- 前記炭素質第1ポケットは、閉鎖型(closed type)ポケットを含む、請求項1に記載の柔軟性炭素ポケット複合構造体。
- 前記炭素質第1シート及び前記炭素質第2シートのそれぞれは、皺(wrinkle)を有する、請求項1に記載の柔軟性炭素ポケット複合構造体。
- 前記炭素質第1シート及び前記炭素質第2シートは、それぞれ独立して、グラフェン、グラファイト、炭素ナノチューブ、カーボンファイバー、カーボンブラック、活性炭、グラフェンオキサイド(GO)、または還元されたグラフェンオキサイド(rGO)を含有するシートを含む、請求項1に記載の柔軟性炭素ポケット複合構造体。
- 前記複合体のそれぞれに含まれた前記炭素質第1ポケットの相互接触によって、二つ以上の前記複合体が互いに接触している、請求項1に記載の柔軟性炭素ポケット複合構造体。
- 前記複合体の一つ以上を包接する炭素質第2ポケットをさらに含む、請求項1に記載の柔軟性炭素ポケット複合構造体。
- 前記柔軟性炭素ポケット複合構造体のそれぞれに含まれた前記炭素質第2ポケットの相互接触によって、二つ以上の前記柔軟性炭素ポケット複合構造体が互いに接触している、請求項8に記載の柔軟性炭素ポケット複合構造体。
- 多孔性を有する、請求項8に記載の柔軟性炭素ポケット複合構造体。
- 前記炭素質第2ポケットは、複数個の炭素質シートを含む、請求項8に記載の柔軟性炭素ポケット複合構造体。
- 前記炭素質第2ポケットは、グラフェン、グラファイト、炭素ナノチューブ、カーボンファイバー、カーボンブラック、活性炭、グラフェンオキサイド(GO)、または還元されたグラフェンオキサイド(rGO)を含有する炭素質シートを含む、請求項11に記載の柔軟性炭素ポケット複合構造体。
- 前記粒子は、半導体性、伝導性または絶縁性を有する、請求項1に記載の柔軟性炭素ポケット複合構造体。
- 前記粒子は、電極材料物質を含む、請求項1に記載の柔軟性炭素ポケット複合構造体。
- 前記粒子は、Si、Ge、Sn、Cd、Sb、Pb、Bi、Zn、Al、Co、Ni、Ti、Te、Mn、Fe、W、Ag、Au、Pt、V、Cu、Ga、P、及びSからなる群より選択されるいずれか一つ以上の元素を含む、請求項1に記載の柔軟性炭素ポケット複合構造体。
- 前記粒子は、ナノメートルサイズを有する、請求項1に記載の柔軟性炭素ポケット複合構造体。
- 炭素質シートと前記粒子との重量比は、1:0.001またはそれ以上である、請求項1に記載の柔軟性炭素ポケット複合構造体。
- 前記柔軟性炭素ポケット複合構造体は、溶媒で分散性を有する、請求項1に記載の柔軟性炭素ポケット複合構造体。
- 請求項1から18のいずれか一項に記載の柔軟性炭素ポケット複合構造体を含む、電極。
- エネルギー貯蔵デバイスのアノードまたはカソードとして使用される、請求項19に記載の電極。
- 請求項19に記載の電極を含む、エネルギー貯蔵デバイス。
- 前記電極は、アノードまたはカソードとして使用される、請求項21に記載のエネルギー貯蔵デバイス。
- 前記電極がアノードとして使用される場合、前記粒子は、Si、Ge、Sn、Cd、Sb、Pb、Bi、Zn、Al、Co、Ni、Ti、Te、Mn、Fe、W、Ag、Au、Pt、V、Cu、Ga、及びPからなる群より選択されるいずれか一つ以上の元素を含む、請求項22に記載のエネルギー貯蔵デバイス。
- 前記電極がカソードとして使用される場合、前記粒子は、Sを含む、請求項22に記載のエネルギー貯蔵デバイス。
- 前記エネルギー貯蔵デバイスは、バッテリもしくはキャパシタ、またはバッテリ−キャパシタハイブリッドである、請求項21に記載のエネルギー貯蔵デバイス。
- 前記エネルギー貯蔵デバイスは、リチウムイオンバッテリ、ナトリウムイオンバッテリ、リチウムエアバッテリ、ナトリウムエアバッテリ、リチウムメタルバッテリ、ナトリウムメタルバッテリ、リチウムイオンハイブリッドキャパシタ、またはナトリウムイオンハイブリッドキャパシタである、請求項21に記載のエネルギー貯蔵デバイス。
- (a)粒子、高分子及び炭素質シートを含む層状複合体を形成するものであって、前記層状複合体は、炭素質第1シート及び炭素質第2シートとして表示される、互いに対向する二つの炭素質シートの間に一つ以上の前記粒子が配置され、前記粒子は、前記炭素質第1シート及び前記炭素質第2シートのそれぞれと前記高分子によって連結され、
(b)前記層状複合体から前記高分子を除去することで、前記互いに対向する前記炭素質第1シート及び前記炭素質第2シートによって形成された一つ以上の炭素質第1ポケットのそれぞれによって包接された粒子を含む複合体を含む柔軟性炭素ポケット複合構造体を得ること、
を含む、柔軟性炭素ポケット複合構造体の製造方法。 - 前記(a)において、前記高分子は、溶媒中に前記炭素質シート(carbonaceous sheets)と前記粒子を含む溶液に高分子形成用モノマーを添加して重合させることによって、前記粒子と前記炭素質第1シート及び前記炭素質第2シートのそれぞれを前記高分子によって連結することを含む工程によって形成される、請求項27に記載の柔軟性炭素ポケット複合構造体の製造方法。
- 前記(b)において、前記層状複合体から前記高分子を除去する前に前記層状複合体を粉砕して前記層状複合体の粒子体を形成した後、前記粒子体から前記高分子を除去することで、前記複合体の一つ以上を包接する炭素質第2ポケットを形成することをさらに含む、請求項27に記載の柔軟性炭素ポケット複合構造体の製造方法。
- 前記(a)において、前記高分子形成用モノマーは、アニオン重合性モノマーを含む、請求項28に記載の柔軟性炭素ポケット複合構造体の製造方法。
- 前記高分子形成用モノマーは、C1−10アルキルシアノアクリレートを含む、請求項30に記載の柔軟性炭素ポケット複合構造体の製造方法。
- 前記(a)において、前記溶媒は、前記高分子形成用モノマーの重合時に発生する反応熱によって蒸発して除去されるか、または前記重合後に除去されて前記柔軟性炭素ポケット複合構造体内に孔(pore)を形成する、請求項28に記載の柔軟性炭素ポケット複合構造体の製造方法。
- 前記溶媒は、100℃以下の沸点を有する、請求項32に記載の柔軟性炭素ポケット複合構造体の製造方法。
- 前記層状複合体の粉砕は、ボールミル、グラインディング、ミキサー機またはふるい(sieve)を利用して行われる、請求項29に記載の柔軟性炭素ポケット複合構造体の製造方法。
- 前記(b)において、前記粉砕によって得られた前記層状複合体の粒子体は、マイクロメートル以上のサイズを有する、請求項29に記載の柔軟性炭素ポケット複合構造体の製造方法。
- 前記層状複合体の前記粉砕によって得られた前記粒子体から前記高分子を除去する前に、前記粒子体の外部表面に存在する包接されていない前記粒子を除去することをさらに含む、請求項29に記載の柔軟性炭素ポケット複合構造体の製造方法。
- 前記互いに対向する炭素質第1シート及び炭素質第2シートは、一つ以上の領域で互いに接触しており、前記炭素質第1シート及び前記炭素質第2シートが互いに接触されていない一つ以上の領域は、それぞれ前記炭素質第1ポケットを形成する、請求項27に記載の柔軟性炭素ポケット複合構造体の製造方法。
- 前記炭素質第1シート及び前記炭素質第2シートは、皺(wrinkle)を有する、請求項27に記載の柔軟性炭素ポケット複合構造体の製造方法。
- 前記炭素質シートは、グラフェン、グラファイト、炭素ナノチューブ、カーボンファイバー、カーボンブラック、活性炭、グラフェンオキサイド(GO)、または還元されたグラフェンオキサイド(rGO)を含有するシートを含む、請求項27に記載の柔軟性炭素ポケット複合構造体の製造方法。
- 前記粒子は、半導体性、伝導性または絶縁性を有する、請求項27に記載の柔軟性炭素ポケット複合構造体の製造方法。
- 前記粒子は、電極材料物質を含む、請求項27に記載の柔軟性炭素ポケット複合構造体の製造方法。
- 前記粒子は、Si、Ge、Sn、Cd、Sb、Pb、Bi、Zn、Al、Co、Ni、Ti、Te、Mn、Fe、W、Ag、Au、Pt、V、Cu、Ga、P、及びSからなる群より選択されるいずれか一つ以上の元素を含む、請求項27に記載の柔軟性炭素ポケット複合構造体の製造方法。
- 前記粒子は、ナノメートルサイズを有する、請求項27に記載の柔軟性炭素ポケット複合構造体の製造方法。
- 前記炭素質シートと前記粒子との重量比は、1:0.001またはそれ以上である、請求項27に記載の柔軟性炭素ポケット複合構造体の製造方法。
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