JP2015529933A - 不連続カーボンナノチューブを使用した、エネルギー蓄積および回収装置のためのバインダ、電解質およびセパレータフィルム - Google Patents
不連続カーボンナノチューブを使用した、エネルギー蓄積および回収装置のためのバインダ、電解質およびセパレータフィルム Download PDFInfo
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- 229910052725 zinc Inorganic materials 0.000 description 1
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Abstract
Description
本特許出願は、2012年6月21日に出願された米国特許出願第61/662393号および2012年6月22日に出願された米国特許出願第61/663513号の優先権を主張するものであり、2011年6月20に出願された米国特許出願第13/164456号、2010年12月14日に出願された米国特許出願第12/968151号、2009年12月18日に出願された米国特許出願第13/140029号、2011年6月23日に出願された米国特許出願第61/500561号、2011年6月23日に出願された米国特許出願第61/500560号、および2012年4月25日に出願された米国特許出願第61/638454号に関連する。これらの特許文献の開示内容は、参照により本明細書に組み込まれている。
該当なし。
電解質という用語は、電流を担持することが可能な溶液と定義される。イオン性塩が、イオン輸送を可能にする媒体に溶解される。イオン輸送は、電解質を通じたイオンの移動と定義される。イオンは、好ましくは単一種類のイオンであるが、複数種類のイオンの混合物であり得る。媒体は、固体、液体、または半固体、例えばゲル状であり得る。例えば、鉛酸蓄電池において、電解質媒体は、液体またはゲル状であることが好ましい。リチウム系電池では、電解質媒体は、ゲル状であることが好ましく、ショートまたは浸透による電池の故障に際して高濃度の可燃性有機液体が漏出することを防止するために、使用温度で固体であることがより好ましい。電解質は、貯蔵安定性の低下またはショートを防止するために十分に非導電性でなければならない。
22mm径のパンチを使用して各乾燥サンプルフィルムを得る。また、フィルムを室温で1〜20日間浸漬することによって、純電解質(炭酸エチレンと炭酸プロピレンとの50/50組成物)および電解質ならびに50重量%の過塩素酸リチウムで飽和されたフィルムを得る。フィルムの膨潤を重量増加によって評価し、摂氏25度、および1Khzで約70psi(0.483MPa)の圧力下にてLCRメーター(Agilent 4263B)を使用してフィルムのインピーダンスを試験する。インピーダンスの単位は、通常、オーム−メートルで与えられる。
電解質フィルムを2つの電極間に配置し、摂氏25度、および正弦波試験レベルが20mvの2ボルト直流バイアスにてLCRメーター(Agilent 4263B)を使用して、100Hz、120Hz、1KHz、10KHzおよび100KHzの周波数で抵抗およびリアクタンスを測定する。ナイキストプロットは、電荷移動抵抗が得られるインピーダンスの実数および虚数成分で構成されている。
(実施例1〜3)
一般手順。最初に、酸化部分が約2重量%であり、平均アスペクト比が約60のカーボンナノチューブを激しく撹拌しながらNMPに添加することによってn−メチル−2−ピロリドン(NMP)中不連続カーボンナノチューブの分散体を作製する。添加に続いて、音波処理を約15分間にわたって施して、カーボンナノチューブを剥離させる。ある量のPVDFを30分の時間にわたって系に徐々に添加して、PVDFに対して所望の重量分率のカーボンナノチューブを得る。均質な分散体が得られるまで激しい撹拌および音波処理を継続する。NMPを真空中で一定重量まで除去することによってPVDFの均一な黒色フィルムを得る。
不連続カーボンナノチューブ用の分散助剤としてのポリエーテル(BASF社、Pluronic F−127)を逆浸透圧法によって清浄化した水に、ポリエーテル対乾燥酸化カーボンナノチューブの重量比が1.5対1になるように溶解させ、次いで酸化カーボンナノチューブを1.5重量/体積のカーボンナノチューブの濃度で水に添加し、30分間にわたって音波処理をして酸化カーボンナノチューブを分散させる。SBRラテックス(Dow Chemical社、グレードCP615NA、固形分50%)を、所望のカーボンナノチューブ対SBRの重量比で剥離カーボンナノチューブに直接添加し、均質になるまで激しく撹拌する。混合物を空気中で乾燥させた後、フィルムの重量が一定になるまで真空中で乾燥させて黒色フィルムを得る。
最初に、濃硫酸/硝酸の混合物中1w/v%のカーボンナノチューブ繊維束(CNano社、グレード9000)を約30℃で2時間以上にわたって音波処理することによって酸化カーボンナノチューブ繊維を作製する。濾過および水洗後、最終洗浄物のpHは約4である。酸化カーボンナノチューブ繊維を約80℃にて4時間にわたって真空中で乾燥させる。得られた酸化チューブは、200から600℃の窒素中で熱重量分析により測定したところ、概して約1.5〜6重量%の酸素化種を含有し、二次電子顕微鏡法で測定したところ、チューブの少なくとも一部が開放端を有する。酸化カーボンナノチューブを空気中で800℃まで燃焼させた後の残留灰分は、約0.5から2w/w%である。分子量が約1900ダルトンのモノヒドロキシポリ(エチレングリコール)(PEG−MH)(Sigma Aldridge社)を触媒としての少量の硫酸とともに乾燥酸化ナノチューブに過剰に添加し、混合物を約1時間にわたって音波処理しながら100℃まで加熱する。冷却し、水を添加した後、官能化カーボンナノチューブを濾過し、その後洗浄して過剰のPEG−MHおよび硫酸を除去する。官能化カーボンナノチューブを40℃にて真空中で終夜乾燥させる。PEG−MHと反応した0.5w/w%のカーボンナノチューブをPEG−MHに添加し、60℃まで加熱し、30分間にわたって音波処理する。倍率150倍までの光学顕微鏡法によって液体の状態で調べたところ識別可能なカーボンナノチューブの凝集体を示さない、すなわちチューブが不連続かつ分散している均一な黒色液体を得る。PEG−MHを不連続カーボンナノチューブとともに冷却すると、PEG−MHは、結晶化していることが確認され、カーボンナノチューブは、結晶ラメラ間、すなわち固体ポリマーの非晶質領域に存在していることが確認される。これは、イオンが非晶質領域で優先的に移動することが認識されるため非常に有利であると考えられる。
(実施例7〜15)
酸化率が約2%であり、平均アスペクト比が60であり、カーボンナノチューブの一部が開放端を有する不連続カーボンナノチューブを80℃で約4時間にわたって真空中で乾燥させる。最初に、溶媒としてのアセトニトリル(Sigma Aldridge社、99.8%無水物)、不連続カーボンナノチューブの1w/v%溶液、一方の分子量が300000ダルトンであり、他方の分子量が4000ダルトンであるそれぞれ重量比が1:0.23であるある比率の2種類のPEOから構成される2.5w/v%のポリエチレンオキシド(PEO)(Alfa Aesar社)、およびトリフルオロメタンスルホン酸リチウムの5w/v%溶液(Aldrich社)を使用して成分の溶液を作製することによって、表3に詳記される組成を構成する。最初に、音波処理槽を使用して、乾燥した不連続カーボンナノチューブをアセトニトリル中で30分間にわたって音波処理する。溶液を表3に示されるそれぞれの組成(PEOの百分率)に構成し、次いで音波処理槽(Ultrasonics社)にて30℃付近で30分間にわたって音波処理する。次いで、混合物をガラス皿に移し、アセトニトリルを4時間にわたって蒸発させてフィルムを得る。フィルムを真空中で50℃にて2時間にわたって乾燥させた後、120℃で3分間にわたって、ポリエチレンテレフタレートシート間の20トンの圧板圧で圧縮成形し、室温まで冷却し、試験までデシケータに保管する。
対照6および実施例16に対応する鉛酸蓄電池用陽極ペーストを作製するための組成物を表4に示す。増量剤(Hammond社)は、それぞれ重量比が1:1:0.5のスルホン酸リグニン、硫酸バリウムおよびカーボンブラックの組成物である。増量剤を酸化鉛の乾燥粉末に添加し、次いで水を添加して混合した後、温度を55℃未満に維持しながら酸(硫酸、比重1.4)を徐々に添加して混合する。実施例16では、平均長さが700ナノメートルで酸化レベルが約2%の不連続カーボンナノチューブ、およびポリビニルアルコール(PVA)(Sigma Aldridge、平均分子量30000から70000ダルトン、加水分解率87から90%)を水と混合し、音波処理して、2.25重量%の不連続カーボンナノチューブと3.375重量%のPVAとの分散体を得る。不連続カーボンナノチューブ溶液を水とともに酸化鉛に添加した後、硫酸を徐々に添加する。陽極材料を鉛格子に貼り付け、酸化鉛陰極とともに電池に組み立てた後、他の場所、すなわちLead-Acid Batteries: Science and Technology: Science and Technology、Elsevier 2011. 著者: D. Pavlovに記録されているように標準電池を形成する。陽極ペーストにおける乾燥酸化鉛に対する不連続カーボンナノチューブの重量%は0.16である。
Claims (20)
- エネルギー蓄積または回収装置のバインダ材料、電解質材料またはセパレータフィルム材料として使用される組成物であって、複数の不連続カーボンナノチューブ繊維を含み、前記繊維が約10から約500のアスペクト比を有し、前記不連続カーボンナノチューブ繊維の少なくとも一部が開放端を有する組成物。
- 前記開放端を有する不連続カーボンナノチューブの部分がイオン伝導性である、請求項1に記載の組成物。
- 少なくとも1種のポリマーをさらに含む、請求項1に記載の組成物。
- 前記カーボンナノチューブがさらに官能化されている、請求項1に記載の組成物。
- 少なくとも1種の分散助剤をさらに含む、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)、部分または完全水素化ポリ(スチレンブタジエン)含有コポリマー、カルボキシル化ポリ(スチレンブタジエン)などの官能化ポリ(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)、フッ化ポリマー、ポリビニルピロリドン、伝導性ポリマー、天然源由来のポリマー、ポリエーテル、ポリエステル、ポリウレタンおよびポリアミド、ホモポリマー、グラフト、ブロックまたはランダムコポリマーまたはターポリマー、ならびにそれらの混合物からなる群から選択される、請求項3に記載の組成物。
- 元素周期表の第2族から第14族の元素を含むさらなる無機構造体をさらに含む、請求項2に記載の組成物。
- カーボンブラック、黒鉛、グラフェン、酸化グラフェン、フラーレン、およびそれらの混合物からなる群から選択される非繊維炭素構造体をさらに含む、請求項2に記載のバインダ組成物。
- グラフェンおよび/または酸化グラフェン板の間に散在した不連続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9に記載の組成物。
- バインダ材料が、約10億オーム−m以下のインピーダンスを有する、請求項1に記載の組成物。
- 前記電解質材料またはセパレータフィルムが、約1000万オーム−m以下の電荷移動抵抗を有する、請求項1に記載の組成物。
- 前記カーボンナノチューブが配向されている、請求項1に記載の組成物。
- 前記配向が、シート加工法、ミクロ層加工法、垂直フィルム配向ミクロ層加工法、フィルム加工法、成形加工法、押出加工法または繊維紡糸加工法で実施される、請求項13に記載の組成物。
- 前記配向が、幅出し、一軸配向、二軸配向および熱成形のような後加工法を含む、請求項14に記載の組成物。
- 開放端チューブの一部が電解質を含む、請求項1に記載の組成物。
- 前記電解質がポリマーまたは液体を含む、請求項16に記載の組成物。
- 40から90個数%の不連続カーボンナノチューブが30〜70のアスペクト比を有する、請求項1に記載の組成物。
- 1から30個数%のカーボンナノチューブが80〜140の平均アスペクト比を有する、請求項18に記載の組成物。
- 約400nmから約1400nmの平均長さを有する不連続カーボンナノチューブと、ポリビニルアルコールとを含む鉛酸蓄電池用電極ペースト。
- バインダ材料、電解質材料またはセパレータフィルム材料として使用される組成物の製造方法であって、
a)カーボンナノチューブを液体、溶媒またはポリマー溶融物に添加する工程と、
b)ある時間にわたって音波処理器または高剪断ミキサーなどで激しく混合する工程と、
c)均質な分散体が得られるまで混合を継続する工程と
を含む方法。
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JP2018508961A (ja) * | 2015-03-05 | 2018-03-29 | アルケマ フランス | 鉛電池電極配合物用の炭素系ナノフィラーの液状組成物の使用 |
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WO2013192513A3 (en) | 2014-03-06 |
EP2865031A2 (en) | 2015-04-29 |
KR20150036108A (ko) | 2015-04-07 |
CN104603980B (zh) | 2017-07-21 |
AU2013278063A1 (en) | 2015-01-22 |
CA2876494A1 (en) | 2013-12-27 |
EP2865031B1 (en) | 2016-08-31 |
CA2876494C (en) | 2021-09-21 |
WO2013192513A2 (en) | 2013-12-27 |
RU2625910C2 (ru) | 2017-07-19 |
US20180261884A1 (en) | 2018-09-13 |
AU2013278063B2 (en) | 2016-07-07 |
JP6294873B2 (ja) | 2018-03-14 |
MX2014015896A (es) | 2015-08-14 |
US20130344396A1 (en) | 2013-12-26 |
IN2015DN00108A (ja) | 2015-05-29 |
RU2014150431A (ru) | 2016-08-20 |
RU2625910C9 (ru) | 2018-01-09 |
CN104603980A (zh) | 2015-05-06 |
SG11201408474SA (en) | 2015-01-29 |
BR112014032138A2 (pt) | 2021-08-03 |
US10608282B2 (en) | 2020-03-31 |
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