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1。グラフト共重合体の合成18-19 <ol><li> 26 POEM mlの（またはPOEA）モノマー（ 図3）を混合することによってフリーラジカル重合法を用いてグラフト共重合体の（POEM-G-PDMSとPOEA-G-PDMS 70:30重量比で）、PDMSマクロモノマー12mlのを合成、2,2 12mgの &#39; - アゾビス（2 - メチルプロピオニトリル）（AIBN）（モノマー：イニシエータ[825:1]）EA 160mlのである。 </li><li> 45分間の超高純度アルゴンでゴム隔膜とパージと、透明な溶液を含むフラスコを密封。 </li><li> 72溶液を加熱°Cで24時間一定に攪拌しながらオイルバス中で（AIBNが3.2×10 -5秒-1の分解速度を有する）。 </li><li>当初は明確な解決策は、典型的には、2時間以内に目に見えて乳白色になりました。非混和性溶剤、PEで最終的な解決を沈殿させる。残留水分を除去するために5日間未満5ミリトルの真空下、80℃でポリマーを乾燥させる。 </li><li>これは、ポリマーがn個された場合ことがわかったOTが正常に乾燥、過度の湿気は、ポリマーを薄膜にキャストされたときに形成をクラックするためにつながる。 </li><li>最後のグラフト共重合体は、（ 図4に示されている）、ポリスチレン較正標準をゲル浸透クロマトグラフィーを用いて50万グラム/モルの分子量を有していた。 </li><li>李にLiTFSIを持つ複雑なグラフトコポリマー：電解質を形成するTHFの共通溶媒中1:20 EO比（LiTFSIを170mgのとPOEM-G-PDMS（70:30）の1グラム）。 </li></ol> 2。複合カソードの作製<ol><li>混合ボールミルのLiFePO 4粉末（臨沂Gelon新電池材料）、カーボンブラック（スーパーP）、及び5時01分01秒の重量比でGCE溶液に混合物を溶解することによりカソードを合成する。 </li><li> 80にスラリーを加熱°C（オープンキャップ）攪拌しながら。次に磁気適切な混合を確実にするために攪拌してスラリーを超音波処理。 10ミリグラム/ cm 2の上への装填率でアルミニウム箔上にドクターブレードアルミニウム箔は、アルミニウムの優れた積層を確実にする。 </li><li>残留THFおよび水分を除去するために80℃でCO / Nの真空オーブンで複合カソードを乾燥させる。 </li></ol> 3。コイン電池の準備とテスト<ol><li>高精度電極カッターEL-CUT（EL-CELL）を用いた小型ディスク（面積= 1.4 cm 2）の中に複合アルゴン充填グローブボックスにカソードと、パンチを輸送。電解質層を形成するための電極ディスクに純粋GCE液（ポエム-γ-PDMS、LiTFSIを、両方のTHFに溶解）をドロップキャスト。 </li><li> -80の露点とグローブボックスの内側ホットプレート上で最終的なカソード - 電解質ディスクを熱し℃のTHFを蒸発させると、等しいサイズGCEコーティングされた金属リチウムディスク（Sigma-Aldrich社とともにCR2032コイン電池に組み立てるためには、マニュアル閉ツール（宝泉）を用いて厚さの0.75ミリメートル）。セルの回路図は、灰色の粒子がLiFePO 4を、黒粒子REPを表す図5に示されています炭素を再送、青 &quot;スパゲッティ&quot;はGCEを表し、アノードはリチウム金属である。 </li><li>同一のLiFePO 4粉末およびリチウム金属アノードからなるセルの第2のセットを組み立てるのではなく、PVDFバインダー樹脂（カイナー）、PVDFセパレータ（セルガード）、およびEC中の1M LiPF 6を液体電解質に使用：1:1 DMCを比（LP30、メルク）、性能を比較する。 </li><li>すべてのアセンブリは、-80℃までの露点とグローブボックスで行われていた32チャネルMACCOR 4000電池テスターを周囲温度でサイクル試験に用いた。 </li></ol> 4。ポリマーの伝導機構<ol><li> PEO分節運動は通常、CCとCO結合の周りのねじれに関連付けられています。セミランダムセグメント運動が形成し、分解溶媒和イオンの配位部位を電界の影響下に拡散するイオンと自由体積を提供することにより、イオン伝導を助ける。セグメント運動の発症はvicinitで発生ガラス転移温度のy、T gの温度がT gを超えてさらに増加するにつれて、より容易になる。より高い温度で、ローカルボイドがポリマーセグメントは、自由体積19内に移動することができ、ポリマーの膨張により製造される。 </li><li>セグメント運動がはるかに迅速なT gは上記のアモルファス相における結晶相に比べてですので、ポリマー中のイオン輸送は、アモルファス相で主に発生します。しかし、近年のLi +結晶の伝導（PEO）6：伝導度がアモルファスPEOよりも2桁以上低いがヒ酸6は 、実証された。 PEO /塩複合体の結晶又はアモルファス相は、組成、温度、および調製法20-22に依存します。 </li><li>イオンは、その溶剤シースそのまま輸送に動く液体とは異なりの巨視的粘度に関係している溶媒、ポリマー鎖が絡み合っており、ますます長距離移動できない固体高分子において、イオン輸送は、ポリマー鎖のセグメントの微視的な粘度に関連している。ポリマー鎖に沿ったイオンの輸送には、2つの活性化障壁を克服する必要があり、両方とも図6及び図7に示されている。一つは、調整のEO単位によるイオンの溶媒和である。このプロセスは形成し、化学結合の破壊を伴う、アレニウス依存性を有し、導電率は次式で与えられる。 σ（E / kTの） σは導電性である場合、債券に関連付けられた活性化エネルギーは定数であり、Eです。イオンが結合が強すぎる場合には、固体ポリマーで移動するために配位部位から解離する必要があるため、カチオンが不動になる。カチオンポリマー結合は塩の溶解のために十分に強いことが必要ですが、弱い十分トンoが陽イオンの移動を可能にします。 </li><li>イオンの輸送は、一配位部位から別のものになります。このプロセスは、ポリマーのセグメント運動に関連して、フォーゲル-タンマン-フルチャー（VTF）22-25依存性を有しており、T 0は 、一般的にT g未満50 Kなるように選択された基準温度である導電性である。この式は、T 0上記の熱運動がプロセスを輸送するために寄与し、より高速な動作が低いT gのポリマーが期待されていることを示唆している。 VTFプロセスはT gの関連性が、このように低温で律速。高温では、分節運動はアレニウスのプロセスが律速になることは十分容易になります。 </li></ol>

<ol>
	<li>Tarascon, J. M., Armand, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Issues+and+challenges+facing+rechargeable+lithium+batteries.">Issues and challenges facing rechargeable lithium batteries.</a> Nature. 414 (6861), 359-367 (2001).</li><li>Scrosati, B., Hassoun, J., Sun, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Lithium-ion+batteries.+A+look+into+the+future.">Lithium-ion batteries. A look into the future.</a> Energy Environ. Sci. 4 (9), 3287-3295 (2011).</li><li>Goodenough, J. B., Kim, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Challenges+for+rechargeable+batteries.">Challenges for rechargeable batteries.</a> J. Power Sources. 196 (16), 6688-6694 (2011).</li><li>Wang, Y., He, P., Zhou, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Olivine+LiFePO4:+development+and+future.">Olivine LiFePO4: development and future.</a> Energy Environ. Sci. 4 (3), 805-817 (2011).</li><li>Bruce, P. G., Scrosati, B., Tarason, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nanomaterials+for+rechargeable+lithium+batteries.">Nanomaterials for rechargeable lithium batteries.</a> Angew. Chem. 47 (16), 2930-2946 (2008).</li><li>Choi, N., Yao, Y., Cui, Y., Cho, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=One+dimensional+Si/Sn+-+based+nanowires+and+nanotubes+for+lithium-ion+energy+storage+materials.">One dimensional Si/Sn - based nanowires and nanotubes for lithium-ion energy storage materials.</a> J. Mater. Chem. 21 (27), 9825-9840 (2011).</li><li>Jeong, G., Kim, Y. U., Kim, H., Kim, Y. J., Sohn, H. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Prospective+materials+and+applications+for+Li+secondary+batteries.">Prospective materials and applications for Li secondary batteries.</a> Energy Environ. Sci. 4 (6), 1986-2002 (2011).</li><li>Walker, C. W., Salomon, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Improvement+of+ionic+conductivity+in+plasticized+PEO-Based+solid+polymer+electrolytes.">Improvement of ionic conductivity in plasticized PEO-Based solid polymer electrolytes.</a> J. Electrochem. Soc. 140 (12), 3409-3412 (1993).</li><li>Daniels, C., Besenhard, J. O. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Handbook of battery materials. , (2011).</li><li>Bard, A. J., Faulkner, L. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Electrochemical methods: fundamentals and applications. , 864 (2001).</li><li>Newman, J., Thomas-Alyea, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Electrochemical systems. , 672 (2004).</li><li>Zu, C., Li, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Thermodynamic+analysis+on+energy+densities+of+batteries.">Thermodynamic analysis on energy densities of batteries.</a> Energy Environ. Sci. 4 (8), 2614-2624 (2011).</li><li>Balbuena, P., Wang, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Lithium-ion Batteries: solid-electrolyte interphase. , (2004).</li><li>Appetecchi, G. B., Scaccia, S., Passerini, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Investigation+on+the+Stability+of+the+Lithium-Polymer+Electrolyte+Interface.">Investigation on the Stability of the Lithium-Polymer Electrolyte Interface.</a> J. Electrochem. Soc. 147 (12), 4448-4452 (2000).</li><li>Bruce, P. G., Krok, F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Characterisation+of+the+electrode/electrolyte+interfaces+in+cells+of+the+type+Li/PEO+LiCF3SO3/V6O13+by+ac+impedance+methods.">Characterisation of the electrode/electrolyte interfaces in cells of the type Li/PEO LiCF3SO3/V6O13 by ac impedance methods.</a> Solid State Ionics. 36 (3-4), 171-174 (1989).</li><li>Huggins, R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Energy Storage. , 400 (2010).</li><li>Lee, S., Sch&#246;mer, M., Peng, H., Page, K. A., Wilms, D., Frey, H., Soles, C. L., Yoon, D. Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Correlations+between+ion+conductivity+and+polymer+dynamics+in+hyperbranched+poly(ethylene+oxide)+llectrolytes+for+lithium-ion+batteries.">Correlations between ion conductivity and polymer dynamics in hyperbranched poly(ethylene oxide) llectrolytes for lithium-ion batteries.</a> Chem. Mater. 23 (11), 2685-2688 (2011).</li><li>Trapa, P. E., Reyes, A. B., Das Gupta, R. S., Mayes, A. M., Sadoway, D. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Polarization+in+cells+containing+single-ion+graft+copolymer+electrolytes.">Polarization in cells containing single-ion graft copolymer electrolytes.</a> J. Electrochem. Soc. 153 (6), 1098-1101 (2006).</li><li>Trapa, P. E., Won, Y. Y., Mui, S. C., Olivetti, E. A., Huang, B., Sadoway, D. R., Mayes, A. M., Dallek, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Rubbery+graft+copolymer+electrolytes+for+solid-state+thin-film+lithium+batteries.">Rubbery graft copolymer electrolytes for solid-state thin-film lithium batteries.</a> J. Electrochem. Soc. 152 (1), A1-A5 (2005).</li><li>Walker, C. W., Salomon, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Improvement+of+ionic+conductivity+in+plasticized+peo-based+solid+polymer+electrolytes.">Improvement of ionic conductivity in plasticized peo-based solid polymer electrolytes.</a> J. Electrochem. Soc. 140 (12), 3409-3412 (1993).</li><li>Bard, A. J., Faulkner, L. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Electrochemical methods: fundamentals and applications. , 864 (2001).</li><li>Michnick, R. B., Rhoads, K. G., Sadoway, D. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Relative+dielectric+constant+measurements+in+the+butyronitrile-chloroethane+system+at+subambient+temperatures.">Relative dielectric constant measurements in the butyronitrile-chloroethane system at subambient temperatures.</a> J. Electrochem. Soc. 144 (7), 2392-2398 (1997).</li><li>Orazem, M. E., Tribollet, B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Electrochemical impedance spectroscopy. , (2008).</li><li>Cogger, N. D., Evans, N. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=An+introduction+to+electrochemical+impedance+measurement.">An introduction to electrochemical impedance measurement.</a> Technical Note, Solartron Analytical Technical Report. No. 6, (1999).</li><li>Marzantowiz, M., Dygas, J. R., Krok, F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Impedance+of+interface+between+PEO:LiTFSI+polymer+electrolyte+and+blocking+electrodes.">Impedance of interface between PEO:LiTFSI polymer electrolyte and blocking electrodes.</a> Electrochim. Acta. 53 (25), 7417-7425 (2008).</li><li>Clarson, S. J., Semlyen, J. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Studies+of+cyclic+and+linear+poly(dimethyl-siloxanes):+21.+high+temperature+thermal+behavior.">Studies of cyclic and linear poly(dimethyl-siloxanes): 21. high temperature thermal behavior.</a> Polymer. 27 (1), 91-95 (1986).</li></ol>

利害の衝突は宣言されていない。

LiFePO 4を/ GCE /李曲線は充電と放電の両方でのLiFePO 4 / LP30/Li曲線よりも大きい過電圧を示しています。 GCEを電解質とバインダーの両方として使用されるので、イオン伝導は、カソード粒子のすべてに設けられており、ほぼ全実用比容量（mAhの150 / g）はアクセス可能であっれる。それは室温で低いのLiFePO 4粒子内にリチウム拡散によって制限されるので、170ミリアンペ?...

リチウム（Li）は非常に陽性金属（標準水素電極に対して-3.04 V）、軽量金属（6.94グラム/モル当量および0.53グラム/ cm 3での比重）である。これは、サイズと重量物質ポータブルエネルギー貯蔵装置用負極と理想中の活性物質のための選択肢として、それを魅力的になる。リチウム系電池（リチウムイオン、PLiON、およびLi金属）がより高いエネルギー密度を有することを図1に示してい鉛酸、ニッケル·カドミウム、ニッケル水素電池1以下である。 完全なリチウムイオン電池は、正極（正）、アノード（負）、電解液、およびセパレータ（ 図2）から構成される。陰極と陽極の両方が、リチウムイオンがインターカレートまたは（アノードが炭素である場合、Liはリチウム中立としてインターカレー）可逆的にインターカレートすることができるデインターカレーション化合物である。電解質は、イオン伝導と絶縁し、電気を提供しています電極間のNIC伝導。セパレータは、イオン透過性が、短絡からの2つの電極を保つために機械的に剛性である。セルが満充電状態にあるときLiの全ては、アノードにインターカレートしており、セルが完全に放電状態である場合、リチウムイオンの全てが陰極でインターカレートされている。電解質を通ってアノードからカソードへのイオンが流れている間、電源装置への外部回路を通ってカソードにアノードからの電子の流れを放電する、自発的な反応中。電荷中性を維持するために、カソードにおけるイオンと電子が再結合する。充電時に、流れが逆転する。 彼らはほとんど何十年も同じままである電解液、上のエネルギー電池の密度よりもむしろが決まるので、これまでほとんどのリチウムイオン電池の開発は陰極材料に焦点を当てている。それはimpedanのための全体的なパワー能力に影響を与えるので、電解液は、電池の重要な部分である電解質自体を通って、電極 - 電解質界面で両方CE。 リチウムイオン電池で用いられる電解質は、一般式LIXおよび非水性溶媒の塩から構成される。他の電気化学システムで使用される水性電解質に比べて、リチウムイオン電解質の不利な点は、導電性、コストが高く、引火性、及び環境問題である。利点は、-150℃から300℃、広い電圧ウィンドウ（最大5 V対のLi / Li +（リチウムイオン）まで）と、電極（水電解だろうとの互換性を高めるには、広い温度範囲（電解質が液体のままその上に）含まれて4-6、3）Li金属とフォームのLiOHと水素と激しく反応する2。 電池に使用される主な非水性電解質は有機カーボネート系液体、ポリマー、イオン性液体、及びセラミックスが含まれています。これらの電解質は、実用的なリチウムイオン（Li-ion）batteriに使用する特定のベンチマークを満たす必要がES。それらは少なくとも10ミリ秒/ cmの大型電気化学窓（高電圧用カソード&gt; 4.5 V）、低蒸気圧、良好な熱的および化学的安定性、低毒性、低コストの導電率を含む。例えば、電気自動車などの特定の厳しい用途では、これらのベンチマークのすべてが60℃まで-20°Cから典型的に、広い温度範囲で満たされなければならないこの作業の焦点は、有機および高分子電解質であるため、本稿の残りの部分では、これらの電解質に焦点を当てます。 カーボネート系電解質は、有機溶媒に溶解したリチウム塩から成る。しかし、すべての要件を満たすために溶媒のいずれかのために困難である。例えば、エチレンカーボネート（EC）とプロピレンカーボネート（PC）等の低蒸気圧を有する溶媒は、低い導電率をもたらす、より高い粘度を有する傾向がある。またECは、室温で固体であり、これは、それが別の溶媒と組み合わせることを必要とする。一般的には電解質いくつかの溶媒の組み合わせである。一般的な溶媒とその物理的性質のいくつかを表1に示す。 <table border="1"><tbody><tr><td> 名前 </td><td> 融解温度（°C） </td><td> 沸騰温度（℃） </td><td> 粘度（MPA *秒） </td></tr><tr><td>ジメチルカーボネート（DMC） </td><td> 4.6 </td><td> 90 </td><td> 0.5902（25℃） </td></tr><tr><td>ジエチルカーボネート（DEC） </td><td> -43 </td><td> 126.8 </td><td> 0.7529（25℃） </td></tr><tr><td>エチレンカーボネート（EC） </td><td> 36.5 </td><td> 238 </td><td> 1.9（40°C） </td></tr><tr><td>プロピレンカーボネート（PC） </td><td> -54.53 </td><td> 242 </td><td> 2.512（25℃） </td></tr></tbody></table> 表1。一般的な炭酸溶剤 7。 ORGAへ安全交互NIC電解質、ポリマー電解質をベースにしています。ポリマー電解質は、薄膜、不揮発性、不燃性、および柔軟性は、それらがロールバックされ、大規模な商業規模で印刷することが可能である。ライトらは 1973年に初めてのイオンの伝導ポリ（エチレンオキシド） -塩錯体（PEO）を実証した。これは、後で液体電解質中のLi金属上にデンドライトの成長に関連する安全上の問題がデンドライト8-17の増殖を抑制しPEO系固体高分子電解質を使用することによって解決することができることが発見された。 （1）無溶剤乾燥固体ポリマー、（2）ゲル電解質、そして我々の仕事で使用する無溶剤乾燥合成と（3）可塑化ポリマー：ポリマー電解質の3つの主要な種類があります。 本論文では、（a）は無溶剤ドライポリマー合成、（b）はポリマー伝導機構を議論し、そして（c）固体高分子および有機電解質の両方の温度サイクルを提供します。ます

<table border="1">
	<tbody>
		<tr>
			<td>Name of the reagent</td>
			<td>Company</td>
			<td>Catalogue number</td>
			<td>Comments (optional)</td>
		</tr>
		<tr>
			<td>POEM</td>
			<td>Sigma Aldrich</td>
			<td>26915-72-0</td>
			<td>&nbsp;</td>
		</tr>
		<tr>
			<td>POEA</td>
			<td>Sigma Aldrich</td>
			<td>32171-39-4</td>
			<td>&nbsp;</td>
		</tr>
		<tr>
			<td>LiTFSI</td>
			<td>Sigma Aldrich</td>
			<td>90076-65-6</td>
			<td>&nbsp;</td>
		</tr>
		<tr>
			<td>AIBN</td>
			<td>Sigma Aldrich</td>
			<td>78-67-1</td>
			<td>&nbsp;</td>
		</tr>
		<tr>
			<td>EA</td>
			<td>Sigma Aldrich</td>
			<td>141-78-6</td>
			<td>&nbsp;</td>
		</tr>
		<tr>
			<td>THF</td>
			<td>Sigma Aldrich</td>
			<td>109-99-9</td>
			<td>&nbsp;</td>
		</tr>
		<tr>
			<td>PDMS</td>
			<td>Gelest</td>
			<td>146632-07-7</td>
			<td>&nbsp;</td>
		</tr>
		<tr>
			<td>Argon Gas</td>
			<td>Air Gas</td>
			<td>&nbsp;</td>
			<td>Ultra high purity (Grade 5)</td>
		</tr>
		<tr>
			<td>PE</td>
			<td>Sigma Aldrich</td>
			<td>8032-32-4</td>
			<td>&nbsp;</td>
		</tr>
		<tr>
			<td>LiFePO4</td>
			<td>Gelon</td>
			<td>&nbsp;</td>
			<td>&nbsp;</td>
		</tr>
		<tr>
			<td>Carbon black</td>
			<td>SuperP</td>
			<td>&nbsp;</td>
			<td>Super P</td>
		</tr>
		<tr>
			<td>Lithium metal</td>
			<td>Alfa Aesar</td>
			<td>7439-93-2</td>
			<td>&nbsp;</td>
		</tr>
		<tr>
			<td>PVDF binder resin</td>
			<td>Kynar</td>
			<td>&nbsp;</td>
			<td>Kynar</td>
		</tr>
		<tr>
			<td>PVDF Separator</td>
			<td>Celgard</td>
			<td>&nbsp;</td>
			<td>&nbsp;</td>
		</tr>
		<tr>
			<td>LP30</td>
			<td>Merck</td>
			<td>&nbsp;</td>
			<td>LiPF6 in EC:DMC</td>
		</tr>
		<tr>
			<td>MACCOR battery tester</td>
			<td>MACCOR</td>
			<td>&nbsp;</td>
			<td>&nbsp;</td>
		</tr>
		<tr>
			<td>El-Cut</td>
			<td>EL-CELL</td>
			<td>&nbsp;</td>
			<td>&nbsp;</td>
		</tr>
	</tbody>
</table>

solid-state graft copolymer electrolytes for lithium battery applications

電池の安全性は、過去10年間にわたって非常に重要な研究分野となっています。市販のリチウムイオン電池は、低引火点（&lt;80°C）、可燃性、揮発性有機電解用いる。これらの有機系電解質系は、周囲温度で生存可能であるが、温度が80℃を超えないようにするために冷却システムを必要とするこれらの冷却システムは、バッテリーのコストが増加する傾向があり、バッテリーの故障や爆発につながる可能性が誤動作が、このように人間の生命を危険にさらすことができます。石油価格の上昇は、原油価格が上昇し続けるように動作するように、より経済的に実行可能であり、安全、電気のハイブリッド車のための巨大な需要につながる。リチウムイオン電池で使用されている既存の有機系電解質は、高温の自動車用途には適用されません。有機電解質へのより安全な代替手段は、固体高分子電解質である。この作品は、グラフト共重合体電解質（GCE）ポリ（O用合成を強調表示されますxyethylene）低いガラス転移温度（T g）のポリ（オキシエチレン）アクリレート（POEA）を有するブロックへメタクリレート（POEM）。伝導機構が議論されており、それは、ポリマーセグメント運動とイオン伝導度との関係が実際にボーゲル·タンマン-フルチャー（VTF）依存性を有する実証されている。市販のLP30有機（エチレンカーボネートにLiPF 6を （EC）：1:1の比率で、ジメチルカーボネート（DMC））を含む電池およびGCEは、周囲温度で循環させていた。なお、LP30電解質と比較して、周囲温度で、GCEを含む電池が大きい過電圧を示したことが見出された。しかし60°Cより高い温度で、GCEセルは、はるかに低い過電圧により速く高分子電解質伝導性を示し、ほぼ170のmAh / gで完全理論比容量がアクセスされました。

室温セルサイクル特性を図8に示されている。左のプロットは、10ミリアンペア/ gで15ミリアンペア/ gであり、GCE /バインダーで従来の液体電解質（LP30）のセルの充放電プロファイルを示す図9は、室温で固体高分子セルの放電電圧プロファイルを示す、 60°Cおよび120°C 0.05℃の低電流を使用して、特定の能力の関数としての放電電圧プロファイルは、放電電流がμAであ?...

Watch this Scientific Journal Video about Solid-state Graft Copolymer Electrolytes for Lithium Battery Applications at JoVE.com

Solid-state Graft Copolymer Electrolytes for Lithium Battery Applications

リチウムイオン電池は、周囲温度の用途に適している可燃性及び揮発性有機電解質を用いる。有機電解質へのより安全な代替手段は、固体ポリマー電池です。固体ポリマー電池は、このように深い石油掘削およびハイブリッド電気自動車などの高温用途にそれらが適用されること、高温（&gt; 120℃）で安全に動作します。本論文では、（b）はポリマー伝導機構、（）ポリマー合成を議論し、そして（c）固体高分子および有機電解質の両方の温度サイクルを提供します。ます

リチウム電池アプリケーションのためのソリッドステートグラフトコポリマー電解質

Battery safety has been a very important research area over the past decade. Commercially available lithium ion batteries employ low flash point (&lt;80 ...

solid-state-graft-copolymer-electrolytes-for-lithium-battery

Research

JoVE Journal

Engineering

21.5K ビュー.  Massachusetts Institute of Technology. リチウムイオン電池は、周囲温度の用途に適している可燃性及び揮発性有機電解質を用いる。有機電解質へのより安全な代替手段は、固体ポリマー電池です。固体ポリマー電池は、このように深い石油掘削およびハイブリッド電気自動車などの高温用途にそれらが適用されること、高温（> 120℃）で安全に動作します。本論文では、（b）はポリマー伝?...

ビデオ: Solid-state Graft Copolymer Electrolytes for Lithium Battery Applications

Construction and Testing of Coin Cells of Lithium Ion Batteries

Rechargeable lithium ion batteries have wide applications in electronics, where customers always demand more capacity and longer lifetime. Lithium ion batteries have also been considered to be used in electric and hybrid vehicles1 or even electrical grid stabilization systems2. All these applications simulate a dramatic increase in the research and development of battery materials3-7, including new materials3,8, doping9, nanostructuring10-13, coatings or surface modifications14-17 and novel binders18. Consequently, an increasing number of physicists, chemists and materials scientists have recently ventured into this area. Coin cells are widely used in research laboratories to test new battery materials; even for the research and development that target large-scale and high-power applications, small coin cells are often used to test the capacities and rate capabilities of new materials in the initial stage. 
 In 2010, we started a National Science Foundation (NSF) sponsored research project to investigate the surface adsorption and disordering in battery materials (grant no. DMR-1006515). In the initial stage of this project, we have struggled to learn the techniques of assembling and testing coin cells, which cannot be achieved without numerous help of other researchers in other universities (through frequent calls, email exchanges and two site visits). Thus, we feel that it is beneficial to document, by both text and video, a protocol of assembling and testing a coin cell, which will help other new researchers in this field. This effort represents the "Broader Impact" activities of our NSF project, and it will also help to educate and inspire students.
In this video article, we document a protocol to assemble a CR2032 coin cell with a LiCoO2 working electrode, a Li counter electrode, and (the mostly commonly used) polyvinylidene fluoride (PVDF) binder. To ensure new learners to readily repeat the protocol, we keep the protocol as specific and explicit as we can. However, it is important to note that in specific research and development work, many parameters adopted here can be varied. First, one can make coin cells of different sizes and test the working electrode against a counter electrode other than Li. Second, the amounts of C black and binder added into the working electrodes are often varied to suit the particular purpose of research; for example, large amounts of C black or even inert powder were added to the working electrode to test the "intrinsic" performance of cathode materials14. Third, better binders (other than PVDF) have also developed and used18. Finally, other types of electrolytes (instead of LiPF6) can also be used; in fact, certain high-voltage electrode materials will require the uses of special electrolytes7.

A protocol to construct and test coin cells of lithium ion batteries is described. The specific procedures of making a working electrode, preparing a counter electrode, assembling a cell inside a glovebox and testing the cell are presented.

リチウムイオン電池のコイン細胞の構築とテスト

Rechargeable lithium ion batteries have wide applications in electronics, where customers always demand more capacity and longer lifetime.  Lithium ion ...

工学

Probing and Mapping Electrode Surfaces in Solid Oxide Fuel Cells

Solid oxide fuel cells (SOFCs) are potentially the most efficient and cost-effective solution to utilization of a wide variety of fuels beyond hydrogen 1-7. The performance of SOFCs and the rates of many chemical and energy transformation processes in energy storage and conversion devices in general are limited primarily by charge and mass transfer along electrode surfaces and across interfaces. Unfortunately, the mechanistic understanding of these processes is still lacking, due largely to the difficulty of characterizing these processes under in situ conditions. This knowledge gap is a chief obstacle to SOFC commercialization. The development of tools for probing and mapping surface chemistries relevant to electrode reactions is vital to unraveling the mechanisms of surface processes and to achieving rational design of new electrode materials for more efficient energy storage and conversion2. Among the relatively few in situ surface analysis methods, Raman spectroscopy can be performed even with high temperatures and harsh atmospheres, making it ideal for characterizing chemical processes relevant to SOFC anode performance and degradation8-12. It can also be used alongside electrochemical measurements, potentially allowing direct correlation of electrochemistry to surface chemistry in an operating cell. Proper in situ Raman mapping measurements would be useful for pin-pointing important anode reaction mechanisms because of its sensitivity to the relevant species, including anode performance degradation through carbon deposition8, 10, 13, 14 ("coking") and sulfur poisoning11, 15 and the manner in which surface modifications stave off this degradation16. The current work demonstrates significant progress towards this capability. In addition, the family of scanning probe microscopy (SPM) techniques provides a special approach to interrogate the electrode surface with nanoscale resolution. Besides the surface topography that is routinely collected by AFM and STM, other properties such as local electronic states, ion diffusion coefficient and surface potential can also be investigated17-22. In this work, electrochemical measurements, Raman spectroscopy, and SPM were used in conjunction with a novel test electrode platform that consists of a Ni mesh electrode embedded in an yttria-stabilized zirconia (YSZ) electrolyte. Cell performance testing and impedance spectroscopy under fuel containing H2S was characterized, and Raman mapping was used to further elucidate the nature of sulfur poisoning. In situ Raman monitoring was used to investigate coking behavior. Finally, atomic force microscopy (AFM) and electrostatic force microscopy (EFM) were used to further visualize carbon deposition on the nanoscale. From this research, we desire to produce a more complete picture of the SOFC anode.

We present a unique platform for characterizing electrode surfaces in solid oxide fuel cells (SOFCs) that allows simultaneous performance of multiple characterization techniques (e.g. in situ Raman spectroscopy and scanning probe microscopy alongside electrochemical measurements). Complementary information from these analyses may help to advance toward a more profound understanding of electrode reaction and degradation mechanisms, providing insights into rational design of better materials for SOFCs.

固体酸化物形燃料電池の電極表面をプロービングとマッピング

Solid oxide fuel cells (SOFCs) are potentially the most efficient and cost-effective solution to utilization of a wide variety of fuels beyond hydrogen ...

Characterization of Electrode Materials for Lithium Ion and Sodium Ion Batteries Using Synchrotron Radiation Techniques

Intercalation compounds such as transition metal oxides or phosphates are the most commonly used electrode materials in Li-ion and Na-ion batteries. During insertion or removal of alkali metal ions, the redox states of transition metals in the compounds change and structural transformations such as phase transitions and/or lattice parameter increases or decreases occur. These behaviors in turn determine important characteristics of the batteries such as the potential profiles, rate capabilities, and cycle lives. The extremely bright and tunable x-rays produced by synchrotron radiation allow rapid acquisition of high-resolution data that provide information about these processes. Transformations in the bulk materials, such as phase transitions, can be directly observed using X-ray diffraction (XRD), while X-ray absorption spectroscopy (XAS) gives information about the local electronic and geometric structures (e.g.&#160;changes in redox states and bond lengths). In situ experiments carried out on operating cells are particularly useful because they allow direct correlation between the electrochemical and structural properties of the materials. These experiments are time-consuming and can be challenging to design due to the reactivity and air-sensitivity of the alkali metal anodes used in the half-cell configurations, and/or the possibility of signal interference from other cell components and hardware. For these reasons, it is appropriate to carry out ex situ experiments (e.g.&#160;on electrodes harvested from partially charged or cycled cells) in some cases. Here, we present detailed protocols for the preparation of both ex situ and in situ samples for experiments involving synchrotron radiation and demonstrate how these experiments are done.

We describe the use of synchrotron X-ray absorption spectroscopy (XAS) and X-ray diffraction (XRD) techniques to probe details of intercalation/deintercalation processes in electrode materials for Li-ion and Na-ion batteries. Both in situ and ex situ experiments are used to understand structural behavior relevant to the operation of devices

放射光技術を用いたリチウムイオンとナトリウムイオン電池用電極材料のキャラクタリゼーション

Intercalation compounds such as transition metal oxides or phosphates are the most commonly used electrode materials in Li-ion and Na-ion batteries. ...

Fine-tuning the Size and Minimizing the Noise of Solid-state Nanopores

Solid-state nanopores have emerged as a versatile tool for the characterization of single biomolecules such as nucleic acids and proteins1. However, the creation of a nanopore in a thin insulating membrane remains challenging. Fabrication methods involving specialized focused electron beam systems can produce well-defined nanopores, but yield of reliable and low-noise nanopores in commercially available membranes remains low2,3 and size control is nontrivial4,5. Here, the application of high electric fields to fine-tune the size of the nanopore while ensuring optimal low-noise performance is demonstrated. These short pulses of high electric field are used to produce a pristine electrical signal and allow for enlarging of nanopores with subnanometer precision upon prolonged exposure. This method is performed in situ in an aqueous environment using standard laboratory equipment, improving the yield and reproducibility of solid-state nanopore fabrication.

A methodology for preparing solid-state nanopores in solution for biomolecular translocation experiments is presented. By applying short pulses of high electric fields, the nanopore diameter can be controllably enlarged with subnanometer precision and its electrical noise characteristics significantly improved. This procedure is performed in situ using standard laboratory equipment under experimental conditions.

サイズを微調整すると固体ナノ細孔のノイズを最小限

Solid-state nanopores have emerged as a versatile tool for the characterization of single biomolecules such as nucleic acids and proteins1. However, the ...

In Situ Neutron Powder Diffraction Using Custom-made Lithium-ion Batteries

Li-ion batteries are widely used in portable electronic devices and are considered as promising candidates for higher-energy applications such as electric vehicles.1,2 However, many challenges, such as energy density and battery lifetimes, need to be overcome before this particular battery technology can be widely implemented in such applications.3 This research is challenging, and we outline a method to address these challenges using in situ NPD to probe the crystal structure of electrodes undergoing electrochemical cycling (charge/discharge) in a battery. NPD data help determine the underlying structural mechanism responsible for a range of electrode properties, and this information can direct the development of better electrodes and batteries.
We briefly review six types of battery designs custom-made for NPD experiments and detail the method to construct the &#8216;roll-over&#8217; cell that we have successfully used on the high-intensity NPD instrument, WOMBAT, at the Australian Nuclear Science and Technology Organisation (ANSTO). The design considerations and materials used for cell construction are discussed in conjunction with aspects of the actual in situ NPD experiment and initial directions are presented on how to analyze such complex in situ data.

In Situ Neutron Powder Diffraction Using Custom-made Lithium-ion Batteries

We describe the design and construction of an electrochemical cell for the examination of electrode materials using in situ neutron powder diffraction (NPD). We briefly comment on alternate in situ NPD cell designs and discuss methods for the analysis of the corresponding in situ NPD data produced using this cell.

その場中性子粉末回折ではカスタムメイドのリチウムイオン電池を使用して、

Li-ion batteries are widely used in portable electronic devices and are considered as promising candidates for higher-energy applications such as electric ...

Focused Ion Beam Fabrication of LiPON-based Solid-state Lithium-ion Nanobatteries for In Situ Testing

Solid-state electrolytes are a promising replacement for current organic liquid electrolytes, enabling higher energy densities and improved safety of lithium-ion (Li-ion) batteries. However, a number of setbacks prevent their integration into commercial devices. The main limiting factor is due to nanoscale phenomena occurring at the electrode/electrolyte interfaces, ultimately leading to degradation of battery operation. These key problems are highly challenging to observe and characterize as these batteries contain multiple buried interfaces. One approach for direct observation of interfacial phenomena in thin film batteries is through the fabrication of electrochemically active nanobatteries by a focused ion beam (FIB). As such, a reliable technique to fabricate nanobatteries was developed and demonstrated in recent work. Herein, a detailed protocol with a step-by-step process is presented to enable the reproduction of this nanobattery fabrication process. In particular, this technique was applied to a thin film battery consisting of LiCoO2/LiPON/a-Si, and has further been previously demonstrated by in situ cycling within a transmission electron microscope.

Focused Ion Beam Fabrication of LiPON-based Solid-state Lithium-ion Nanobatteries for In Situ Testing

A protocol for the fabrication of electrochemically active LiPON-based solid-state lithium-ion nanobatteries using a focused ion beam is presented.

その場でテスト用 LiPON ベース固体リチウム イオン Nanobatteries の集束イオンビーム ビーム加工

Solid-state electrolytes are a promising replacement for current organic liquid electrolytes, enabling higher energy densities and improved safety of ...

All-electronic Nanosecond-resolved Scanning Tunneling Microscopy: Facilitating the Investigation of Single Dopant Charge Dynamics

The miniaturization of semiconductor devices to scales where small numbers of dopants can control device properties requires the development of new techniques capable of characterizing their dynamics. Investigating single dopants requires sub-nanometer spatial resolution, which motivates the use of scanning tunneling microscopy (STM). However, conventional STM is limited to millisecond temporal resolution. Several methods have been developed to overcome this shortcoming, including all-electronic time-resolved STM, which is used in this study to examine dopant dynamics in silicon with nanosecond resolution. The methods presented here are widely accessible and allow for local measurement of a wide variety of dynamics at the atomic scale. A novel time-resolved scanning tunneling spectroscopy technique is presented and used to efficiently search for dynamics.

We demonstrate an all-electronic method to observe nanosecond-resolved charge dynamics of dopant atoms in silicon with a scanning tunneling microscope.

すべて電子ナノ秒分解走査型トンネル顕微鏡: 単一ドーパントの電荷ダイナミクスの調査を促進します。

The miniaturization of semiconductor devices to scales where small numbers of dopants can control device properties requires the development of new ...

Electric-field Control of Electronic States in WS2 Nanodevices by Electrolyte Gating

A method of carrier number control by electrolyte gating is demonstrated. We have obtained WS2 thin flakes with atomically flat surface via scotch tape method or individual WS2 nanotubes by dispersing the suspension of WS2 nanotubes. The selected samples have been fabricated into devices by the use of the electron beam lithography and electrolyte is put on the devices. We have characterized the electronic properties of the devices under applying the gate voltage. In the small gate voltage region, ions in the electrolyte are accumulated on the surface of the samples which leads to the large electric potential drop and resultant electrostatic carrier doping at the interface. Ambipolar transfer curve has been observed in this electrostatic doping region. When the gate voltage is further increased, we met another drastic increase of source-drain current which implies that ions are intercalated into layers of WS2 and electrochemical carrier doping is realized. In such electrochemical doping region, superconductivity has been observed. The focused technique provides a powerful strategy for achieving the electric-filed-induced quantum phase transition.

Electric-field Control of Electronic States in WS2 Nanodevices by Electrolyte Gating

Here, we present a protocol to control the carrier number in solids by using the electrolyte.

電解質ゲートによって WS2ナノデバイスにおける電子状態の電界制御

A method of carrier number control by electrolyte gating is demonstrated. We have obtained WS2 thin flakes with atomically flat surface via scotch tape ...

Experimental Methods for Spin- and Angle-Resolved Photoemission Spectroscopy Combined with Polarization-Variable Laser

The goal of this protocol is to present how to perform spin- and angle-resolved photoemission spectroscopy combined with polarization-variable 7-eV laser (laser-SARPES), and demonstrate a power of this technique for studying solid state physics. Laser-SARPES achieves two great capabilities. Firstly, by examining orbital selection rule of linearly polarized lasers, orbital selective excitation can be carried out in SAPRES experiment. Secondly, the technique can show full information of a variation of the spin quantum axis as a function of the light polarization. To demonstrate the power of the collaboration of these capabilities in laser-SARPES, we apply this technique for the investigations of spin-orbit coupled surface states of Bi2Se3. This technique affords to decompose spin and orbital components from the spin-orbit coupled wavefunctions. Moreover, as a representative advantage of using the direct spin detection collaborated with the polarization-variable laser, the technique unambiguously visualizes the light polarization dependence of the spin quantum axis in three-dimension. Laser-SARPES dramatically increases a capability of photoemission technique.

Here, we combine polarization-variable 7-eV laser with spin- and angle-resolved photoemission technique to visualize the spin-orbital coupling effect in solid states.

偏波可変レーザーと組み合わせてスピン角度分解光電子分光の実験法

The goal of this protocol is to present how to perform spin- and angle-resolved photoemission spectroscopy combined with polarization-variable 7-eV laser ...

Three-electrode Coin Cell Preparation and Electrodeposition Analytics for Lithium-ion Batteries

As lithium-ion batteries find use in high energy and power applications, such as in electric and hybrid-electric vehicles, monitoring the degradation and subsequent safety issues becomes increasingly important. In a Li-ion cell setup, the voltage measurement across the positive and negative terminals inherently includes the effect of the cathode and anode which are coupled and sum to the total cell performance. Accordingly, the ability to monitor the degradation aspects associated with a specific electrode is extremely difficult because the electrodes are fundamentally coupled. A three-electrode setup can overcome this problem. By introducing a third (reference) electrode, the influence of each electrode can be decoupled, and the electrochemical properties can be measured independently. The reference electrode (RE) must have a stable potential that can then be calibrated against a known reference, for example, lithium metal. The three-electrode cell can be used to run electrochemical tests such as cycling, cyclic voltammetry, and electrochemical impedance spectroscopy (EIS). Three-electrode cell EIS measurements can elucidate the contribution of individual electrode impedance to the full cell. In addition, monitoring the anode potential allows the detection of electrodeposition due to lithium plating, which can cause safety concerns. This is especially important for the fast charging of Li-ion batteries in electric vehicles. In order to monitor and characterize the safety and degradation aspects of an electrochemical cell, a three-electrode setup can prove invaluable. This paper aims to provide a guide to constructing a three-electrode coin cell setup using the 2032-coin cell architecture, which is easy to produce, reliable, and cost-effective.

Three-electrode cells are useful in studying the electrochemistry of lithium-ion batteries. Such an electrochemical setup allows the phenomena associated with the cathode and anode to be decoupled and examined independently. Here, we present a guide for construction and use of a three-electrode coin cell with emphasis on lithium plating analytics.

3 電極コイン セル準備およびリチウム イオン電池用電着分析

As lithium-ion batteries find use in high energy and power applications, such as in electric and hybrid-electric vehicles, monitoring the degradation and ...