本研究は、JSPS / MEXT Japan、朝日グラス財団、筑波大学の戦略的イニシアチブ「問題と人生の光のアンサンブル」からのKAKENHI（25708020、15K13812、15H00860、15H00986、16H02081）

高分子微小球の作製プロトコール<ol><li> 蒸気拡散法 <ol><li> P1（ポリ[（9,9-ジオクチルフルオレン-2,7-ジイル） - アルト - （5-オクチルチエノ[3,4- c ]ピロール-4,6-ジオン-1,2,3,4-テトラメチル-1,3,5-トリアジン）のような共役ポリマー2mgを、 P2）（ポリ（N-（2-ヘプチルウンデシル）カルバゾール-2,7-ジイル） -alt- （4,8-ビス[（ドデシル）カルボニル]ベンゾ[1,2- b ：4,5- b &#39;]ジチオフェン-2,6-ジイル）]） 28を 、5mLのバイアル中の2mLのクロロホルム（良溶媒）に溶解した。 </li><li>メタノール（貧溶媒）5 mLを50 mLのバイアルに入れます。 </li><li>ポリマーのクロロホルム溶液を含む5mLバイアルを、メタノールを含む50mLバイアルに入れる。 </li><li> 50 mLのバイアルにキャップをし、ポリマーマイクロスフェアーの沈殿を可能にするために25℃で3日間保持する。 </li></ol></li><li> ミニエマルジョン法 <ol><li> 5mgの共役ポリマー、例えばpol（PFO）およびポリ[2-メトキシ-5-（3 &#39;、7&#39;-ジメチルオクチルオキシ）-1,4-フェニレンビニレン]（MDMOPPV）からなる群から選択される少なくとも1種の化合物を含む。 1mLのクロロホルムに溶解した。 </li><li> 2mLの脱イオン水に30mg（〜50mM）のドデシル硫酸ナトリウム（SDS）を溶解する。 </li><li> SDSを含む水2 mLにポリマーのクロロホルム溶液100μLを加えます。 </li><li>超高速ホモジナイザーを用いてクロロホルム/水混合物を30,000rpmで2分間激しく撹拌して溶液を乳化させる。 </li><li>クロロホルムを蒸発させるためにバイアルをキャッピングすることなく1日間保管してください。 </li><li>分散液を1.5mLのマイクロ遠心チューブに2,200 x gで5分間遠心します。 SDSを含む上清水溶液を除去する。 </li><li> 2mLの脱イオン水を加え、激しく振盪する。 </li><li>残りのSDSを洗い流すために、ステップ1.2.6と1.2.7を3回繰り返す。 </li></ol></li><li> 界面降水法 </li><li> 200μgのポリスチレン（PS）および10μlgの蛍光色素（ボロンジピリン、BODIPY）を0.2mLのテトラヒドロフラン（THF）に溶解した。 </li><li>穏やかに1mLの水層にTHF溶液を注ぎます。 </li><li>バイアルをキャッピングすることなく、ポリマーマイクロスフェアの沈殿を可能にするために、2層に分離したTHF /水を6時間保持する。 </li></ol> 2.マイクロフォトルミネッセンス（μ-PL）測定<ol><li> サンプルの準備 <ol><li>セクション1で調製したミクロスフェアの懸濁液を非溶媒（ すなわち、メタノールまたは脱イオン水）で希釈する。 </li><li>スピンコーター（典型的には2000rpmで50秒間）を用いてマイクロスフェアの希釈懸濁液1滴（20〜30μL）を石英基板上にスピンキャストする。 </li><li>溶媒が完全に蒸発するまで（〜5分）、得られたキャストフィルムを空気乾燥する。 </li></ol></li><li> 実験的セットアップ <ol><li>石英基板（15×15×0.5mm 3 ）を光マイクロマシンの試料ステージオスコープ。 </li><li>他の球から分離され、μ-PL測定に適した、明確に定義されたミクロスフェアを見つけます。 </li><li>レーザー（ すなわち、波長、連続波またはパルス、照射時間、積分など ）を選択します。 </li><li>レンズの倍率を選択します。 </li></ol></li><li> 測定値 <ol><li>集光されたレーザービームを使用して微小球に照射します。 405 nm（cw）、450 nm（cw）、355 nm（パルスレーザー、周波数、1 kHz、パルス持続時間、7 ns）の励起波長（ λex ）を有するcwまたはパルスレーザー、および470 nm（パルスレーザー;周波数、2.5MHz;パルス持続時間、70ps）。 </li><li> 300または1,200の溝mm -1の格子を有する分光計を使用して、励起されたスポットにPLスペクトルを記録する。 </li><li>蛍光画像を撮る。 </li><li>サンプルステージを動かして励起スポットを変更します。 </li><li>コリメータを傾けて検出スポットを変更する（必要であれば）。 </li></ol></li></ol> 3.マイクロマニピュレーション技術<ol><li> マイクロスフェアの操作 <ol><li>ミクロスフェアが光学顕微鏡のサンプルステージ上に固定されている石英基板をセットする。 </li><li> μ-PL測定に適した明確に定義されたミクロスフェアを見つける。 </li><li>マイクロマニピュレーション装置にプラスチックマイクロニードルをセットする。 </li><li>コンピュータ制御のジョイスティックを使用してマイクロニードルを移動させ、マイクロスフィアをピックアップします。 </li><li>マイクロスフェアを移動して別のマイクロスフェアに接続します。 </li><li>接続された微小球からμ-PLを測定する。 </li></ol></li></ol>

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著者らは、競合する金銭的利益を宣言していない。

The selection of a good solvent and non-solvent is very important for the self-assembly of well-defined microspheres. If the solubility of a polymer is too high, precipitation will not occur. Also, in general, &#960;-conjugated polymers are hydrophobic, so polar non-solvents, such as MeOH, acetonitrile, and acetone, are often used in the vapor diffusion method to minimize the surface energy required to form a spherical shape. The interface precipitation method is often adopted for the preparation of dye-doped polymer microspheres. Non-conjugated polymers, such as polystyrene, poly(methylmethacrylate), and poly(dimethylsiloxane), are often used as the sphere medium. These polymers are less hydrophobic than typical &#960;-conjugated polymers, so heavy agglomeration does not occur after precipitation in water. If microspheres are not obtained using these methods, other methods, such as post-polymerization dispersion and emulsion polymerization, can be adopted33.
The crystallinity of polymers is the important factor. Generally, &#960;-conjugated polymers have a flat, &#960;-electronic plane. Thus, &#960;-stacking results in the crystallization of the polymers, which prevents the isotropic growth of spheres. Hence, polymers with highly twisted &#960;-electronic planes are favorable for the formation of well-defined microspheres, which prevents interchain &#960;-stacking and amorphous aggregation. To prepare microspheres from polymers with high crystallinity, the mini-emulsion method is appropriate. However, for this method, the surface morphology of the resultant spheres is not very smooth because of the coverage of the surfactant. 
The preferred method of observing WGM PL is to use a focused laser beam to irradiate the rim of a microsphere. The contact point with the substrate causes a defect in the microsphere where the confined light leaks. Therefore, when a focused laser is used to irradiate a microsphere, all the confined light passes through the contact point with the substrate. On the other hand, when the rim of the microsphere is excited, most routes of the confined light do not pass through the contact point with the substrate, leading to better confinement. Thus, well-defined, high-Q WGM PL lines appear.
To conduct WGM lasing from conjugated polymer microspheres, several conditions are required: [1] For the population inversion, high-density optical pumping is needed by using, for example, a femto-second laser pulse. [2] Polymers must hardly be photodamaged upon strong photoexcitation. [3] Highly dispersed microspheres with smooth surfaces are preferred. If these conditions are satisfied, WGM lasing properties can be observed from conjugated polymer microsphere resonators. Fluorescent dye-doped polymer microspheres are also applicable to chemical and biological sensing tools and can be used for laser and optical circuit applications34,35.

ポリマーナノ/マイクロサイズの粒子は、触媒担体、カラムクロマトグラフィー充填剤、薬物送達剤、細胞追跡用蛍光プローブ、光学媒体などを含む様々な用途に広く使用されている1,2,3,4,5 、 6,7,8,9 。特に、π共役ポリマーは、ポリマー球体10,11,12,13,14を使用する光学的、電子的、および光電子的な用途に有益な、固有のルミネセンスおよび電荷伝導特性、特に軟組織アニオン材料15,16,17。例えば、数百ナノメートルの直径を有する球体の三次元的な統合は、コロイド結晶を形成し、特定の波長でフォトニックバンドギャップを示す。格子間周期構造に光が閉じ込められると、停止帯の中央に発振作用が現れる。一方、球のサイズが数マイクロメートルスケールに増加すると、光は、ポリマー/空気境界面20での全反射を介して単一の微小球内部に閉じ込められる。最大円周における光波の伝搬は干渉を生じ、鋭くかつ周期的な放射ラインを有する共鳴モードの出現を導く。これらの光学モードは、いわゆる「ウィスパリングギャラリーモード」（WGM）である。 「ウィスパリングギャラリー」という用語は、ロンドンのセントポール大聖堂で、壁の周りに音波が伝播し、ギャラリーの向こう側の人が囁きを聞くことができます。光の波長は音波よりもはるかに小さいサブマイクロメータスケールであるため、WGMのような大きなドームは必要ではありません：マイクロスフェア、マイクロディスクなどの微小なマイクロメータスケールの明確な血管、および微結晶は、WGM条件を満たす。 方程式1は、WGM共振条件21の単純な形式である。 nπd = lλ （1） ここで、 nは共振器の屈折率であり、 dは直径であり、 lは整数であり、 λは光の波長である。 （1）の左部分は、1つの円伝播による光路長である。光路が他の波長では、光波は、丸めの際に減少する。 この論文では、蒸気拡散22,23,24,25,26,27,28,29,30、ミニエマルジョン31 、および界面析出32のような 、溶液中の共役ポリマーからWGM共鳴器用のマイクロスフェアを調製するためのいくつかの実験方法を紹介する。各メソッドには固有の特性があります。例えば、蒸気拡散法は、非常に高い球形度および滑らかな表面を有する明確なミクロスフェアを提供するが、低結晶性ポリマーのみがこれらのミクロスフェアを形成することができる。一方、ミニエマルションの場合高結晶性ポリマーを含む各種の共役高分子が球体を形成することができるが、表面拡散は蒸気拡散法よりも劣る。界面析出法は、色素がドープされた非共役ポリマーからマイクロスフェアを作製するために好ましい。すべての場合において、溶媒および非溶媒の選択は、球状形態の形成において重要な役割を果たす。 本稿の後半では、μ-PLとマイクロマニピュレーション技術を紹介します。 μ-PL法では、マイクロスフェアを基板上に分散させ、単一の隔離されたマイクロスフィア24を照射するために、顕微鏡レンズを通して集束されたレーザビームを使用する。生成された球体からのPLは、顕微鏡レンズを介して分光計によって検出される。サンプルステージを動かすと、励起スポットの位置が変わる可能性があります。検出点は、エキシーのコリメータ光学系を傾けることによっても可変である検出光路28,32の光軸に対して垂直なレーザ光を照射する。球間光の伝搬と波長変換を調べるために、マイクロマニピュレーション技術を使用することができます32 。異なる光学特性を有する複数の微小球を接続するために、微小針を使用して1つの球を拾い上げ、別の球に置くことが可能である。マイクロマニピュレーション技術およびμ-PL法に関連して、単純な自己組織化法によって調製された共役ポリマー球体を用いて、様々な光学的測定を行うことができる。このビデオペーパーは、光学用途にソフトポリマー材料を使用したい読者には有用です。

<table border="1" fo:keep-together.within-page="1" fo:keep-with-next.within-page="always">
	<tbody>
		<tr>
			<td>polystyrene</td>
			<td>Aldrich</td>
			<td>132427-25G</td>
			<td></td>
		</tr>
		<tr>
			<td>sodium dodecylsulfate</td>
			<td>Kanto Kagaku</td>
			<td>372035-31</td>
			<td></td>
		</tr>
		<tr>
			<td>tetrahydrofuran</td>
			<td>Wako</td>
			<td>206-08744</td>
			<td></td>
		</tr>
		<tr>
			<td>chloroform</td>
			<td>Wako</td>
			<td>038-18495</td>
			<td></td>
		</tr>
		<tr>
			<td>methanol</td>
			<td>Wako</td>
			<td>139-13995</td>
			<td></td>
		</tr>
		<tr>
			<td>Poly(9,9-di-n-octylfluorenyl-2,7-diyl)</td>
			<td>Aldrich</td>
			<td>571652-500MG</td>
			<td></td>
		</tr>
		<tr>
			<td>Poly[2-methoxy-5-(3&#8242;,7&#8242;-dimethyloctyloxy)-1,4-phenylenevinylene] (MDMOPPV)</td>
			<td>Aldrich</td>
			<td>546461-1G</td>
			<td></td>
		</tr>
		<tr>
			<td>poly[(9,9-dioctylfluorene-2,7-diyl)-alt-(5-octylthieno[3,4-c]pyrrole-4,6-dione-1,3-diyl)] (P1)</td>
			<td>synthesized</td>
			<td>-</td>
			<td>reference 28</td>
		</tr>
		<tr>
			<td>poly[(N-(2-heptylundecyl)carbazole-2,7-diyl)-alt-(4,8-bis[(dodecyl)carbonyl]benzo[1,2-b:4,5-b&#8242;]dithiophene-2,6-diyl)] (P2)</td>
			<td>synthesized</td>
			<td>-</td>
			<td>reference 28</td>
		</tr>
		<tr>
			<td>fluorescent dye (boron dipyrrin; BODIPY)</td>
			<td>synthesized</td>
			<td>-</td>
			<td>reference 32</td>
		</tr>
		<tr>
			<td>Optical Microscope</td>
			<td>Nicon</td>
			<td>Eclipse LV-N</td>
			<td></td>
		</tr>
		<tr>
			<td>laser_405 nm</td>
			<td>Hutech</td>
			<td>DH405-10-5</td>
			<td></td>
		</tr>
		<tr>
			<td>laser_355 nm</td>
			<td>CNI</td>
			<td>MPL-F-355-10&#65357;W</td>
			<td></td>
		</tr>
		<tr>
			<td>Spectrometer</td>
			<td>Lambda Vision</td>
			<td>LV-MC3/T</td>
			<td></td>
		</tr>
		<tr>
			<td>Homogenizer</td>
			<td>Microtech Nichion</td>
			<td>Physcotron NS-360D</td>
			<td></td>
		</tr>
		<tr>
			<td>micromanipulation</td>
			<td>Microsupport</td>
			<td>Quick Pro QP-3RH</td>
			<td></td>
		</tr>
	</tbody>
</table>

fabrication of polymer microspheres for optical resonator and laser applications

この論文は、π共役または非共役ポリマーを含む蛍光マイクロスフェアを調製する3つの方法、すなわち蒸気拡散、界面析出およびミニエマルジョンを記載する。すべての方法において、明確に定義されたマイクロメーターサイズの球体は、溶液中の自己集合プロセスから得られる。蒸気拡散法は、球形度および表面平滑性が最も高い球体をもたらすことができるが、これらの球体を形成することができるポリマーの種類は限られている。一方、ミニエマルジョン法では、コプレーナ型π共役骨格を有する高結晶性ポリマーからも、様々な種類のポリマーから微小球を作製することができる。単一の単離マイクロスフェアからの光ルミネッセンス（PL）特性は珍しい.PLは球の内部に閉じ込められ、ポリマー/空気界面での全内部反射を介して球の周囲を伝播し、自己干渉して鋭く周期的な共鳴を示すPLライン。これらの共鳴gモードは、いわゆる「ウィスパリングギャラリーモード」（WGMs）と呼ばれている。この作品は、マイクロフォトルミネッセンス（μ-PL）技術を用いて単一の孤立した球からWGM PLを測定する方法を示しています。この技術では、集束されたレーザービームが単一の微小球に照射され、その発光が分光計によって検出される。マイクロマニピュレーション技術を使用して、微小球を1つずつ接続し、一方の球の周辺での励起および他方の微小球からのPLの検出の際に、結合した微小球からの球間PLの増殖および色変換を実証する。これらの技術、μ-PLおよびマイクロマニピュレーションは、ポリマー材料を用いたマイクロオプティクス応用の実験に有用である。

図1は、蒸気拡散法（a）、ミニエマルジョン法（b）および界面析出法（c）の概略図を示す。蒸気拡散法（ 図1a ）では、ポリマーのCHCl 3溶液（0.5mg mL -1、2mL）を含む5mLのバイアルを、5mLの非溶媒、例えばMeOHを含む50mLバイアルに入れた。外部バイアルに蓋をし、次いで25℃で3日間放置した。非溶媒の蒸気はゆっくりと溶液中に拡散し、その結果、過飽和状態のポリマーが沈殿した。ミニエマルション法（ 図1b ）では、ポリマーのCHCl 3溶液（5mg mL -1、200μL）をn-ドデシル硫酸ナトリウム水溶液（SDS、1mM、2mL）に添加した。水/ CHCl 3二相分離溶液は、乳化ホモジナイザー（30,000rpm、5分）を用いて激しく攪拌することにより泡立てた。得られたエマルジョンを25℃、1気圧で24時間放置してCHCl 3を自然蒸発させた。遠心分離（3回）により上澄み水を交換することにより過剰のSDSを除去し、共役ポリマーの沈殿物を得た。界面析出法（ 図1c ）のために、ポリスチレン（PS、[PS] = 1.0mgmL -1 ）と蛍光色素（[dye] = 0.002-1.0mg mL -1 = 6.4-3,200 μM）を水/ EtOH混合物（6 / 1v / v、1mL）の非溶媒層に注意深く添加した。 THFの空気への同時蒸発に伴う溶媒のゆっくりした拡散は、6時間の熟成後に沈殿を生じた。 各方法で調製した得られた微小球の走査電子顕微鏡（SEM）顕微鏡写真を図1に示す1。蒸気拡散および界面析出法のために、球形度が高く滑らかな表面を有する明確なミクロスフェアが得られた。他方、ミニエマルション法では、明確なミクロスフェアが得られたが、他の方法で製造されたミクロスフェアと比較して、表面形態はあまり滑らかではなかった。これは、界面活性剤がマイクロスフェアの全表面を覆うためであった。しかしながら、ミニエマルション法のメリットは、マイクロスフェアが様々な種類の共役ポリマーから製造できることである。これは、蒸気拡散法を用いると、結晶化度の高いポリマーが球形をほとんど形成しないため、非常に有利である。界面析出法では、水が底層の非溶媒としてしばしば使用される。しかしながら、π共役ポリマーは、通常、非常に疎水性であり、その結果、得られるマイクロスフェアの重い凝集が起こる。これは、μ-PLのための基材上の各単一微小球を単離するためには不利である保証。 図2は、μ-PL実験セットアップの概略図を示しています。 50Xまたは100X対物レンズを備えた光学顕微鏡を用いて、適切な粒子を同定し、それらの直径（ d ）を決定した。測定には、モノクロメーター（格子：300または1,200溝mm -1 ）およびCCDカメラと組み合わせた顕微鏡でμ-PLシステムを使用した。単一ミクロスフェアの周囲は、405nm（cw）、532nm（cw）、355nm（パルスレーザー;周波数、波長）の励起波長（ λex ）を有するcwまたはパルスレーザーによって周囲条件下で25℃で光励起された。 1ns、パルス持続時間、7ns）、または470nm（パルスレーザ;周波数、2.5MHz;パルス持続時間、70ps）である。 異なる励起および検出位置を有するμ-PL測定のために、球体を405nmレーザで励起し、50X対物レンズにより共焦点設定で光を集め、300溝mm -1格子を有する分光計で検出した。スポットサイズ、レーザー出力、積分時間はそれぞれ0.5μm、0.5μW、1秒であった。検出スポットを励起から分離するために、励起レーザビームのコリメータ光学系を検出経路の光軸に対して傾斜させた。 図3は、π共役ポリマーの単一マイクロスフェアのWGM PLを示す： P1 16k 、 P2およびそれらのブレンド。すべての単一マイクロスフェアから、明確なWGM PLスペクトルが観察された。ピーク波長をピークの半値幅で割ったQファクターは、 P1 16kのマイクロスフェアでは2,200に達し、 P2のマイクロスフェアはわずか300であり、可能であった表面の形態が粗いためにy。ポリマー混合ミクロスフェアでは、効率的な腔内エネルギー移動が起こり、その結果、WGM PLが黄色から赤色の領域に有意にシフトした。滑らかな表面のため、高いQ値（1,500）が維持された。 さらに、マイクロスペーシングエネルギー伝達カスケードは、マイクロ操作技術とμ-PL技術の組み合わせによって研究された。したがって、緑、黄、オレンジ、および赤のPL色を有する多形ホウ素 - ジピリン（BODIPY）色素がドープされたPSミクロスフェアは、線状およびT字形の形状を有するテトラスフィアを1つずつ形成するように連結された（ 図4 ）。エネルギー移動効率の詳細な分析は、緑色から黄色へ、および黄色から橙色への光エネルギー移動が効率的に起こったが、オレンジ色から赤色へのエネルギー移動はほとんど起こらなかったことを示した<html>エネルギー供与体のPLバンドとエネルギー受容体の吸収帯との間の小さな重なりの原因となる。言うまでもなく、赤から橙、黄、緑などのアップコンバートされたエネルギー移動は起こりにくい。 <img alt="図1" class="xfigimg" src="/files/ftp_upload/55934/55934fig1.jpg" /> 図1：ポリマーミクロスフェアの調製方法。蒸気拡散法（ a ）、ミニエマルジョン法（ b ）および界面析出法（ c ）の模式図および得られたポリマー微小球の各製造法からのSEM顕微鏡写真。 <a href="https://ecsource-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/55934/55934fig1large.jpg" target="_blank">この図の拡大版を見るには、ここをクリックしてください。</a> 55934fig2.jpg &quot;/&gt; 図2：μ-PL測定の実験装置の概略図。 <a href="https://ecsource-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/55934/55934fig2large.jpg" target="_blank">この図の拡大版を見るには、ここをクリックしてください。</a> <img alt="図3" class="xfigimg" src="/files/ftp_upload/55934/55934fig3.jpg" /> 図3：単一の微小球からのPLスペクトル。 （ a ） P1 16kおよびP2の分子構造およびP1 16k 、 P2およびそれらのブレンド（ P1 16k / P2 = 8 / 2w / w）からの自己組織化マイクロスフェアの模式図ならびにそれらのSEM顕微鏡写真。 （ b - d ） P1 16k （ b ）から形成された単一微小球からのPLスペクトル、<html> P1 16k / P2ブレンド（ c ）、およびP2 （ d ）。 <a href="https://ecsource-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/55934/55934fig3large.jpg" target="_blank">この図の拡大版を見るには、ここをクリックしてください。</a> <img alt="図4" class="xfigimg" src="/files/ftp_upload/55934/55934fig4.jpg" /> 図4：マイクロスフェアを配置するためのマイクロマニピュレーション技術。 （ a ）薄いマイクロニードルで操作された多形BODIPYドープPSミクロスフェアの光学顕微鏡写真。 （ bおよびc ）線状（ b ）およびT字型（ c ）構成の接続されたマイクロスフェアの光学的（上）および蛍光（下）の顕微鏡写真。 （ d ）空洞介在、長距離粒子間エネルギー移動の模式図。jpg &quot;target =&quot; _ blank &quot;&gt;この図の拡大版を見るには、ここをクリックしてください。

Watch this Scientific Journal Video about Fabrication of Polymer Microspheres for Optical Resonator and Laser Applications at JoVE.com

Fabrication of Polymer Microspheres for Optical Resonator and Laser Applications

ポリマーからのミクロスフェアの合成、ミクロスフェアの操作、およびマイクロフォトルミネッセンス測定のためのプロトコールが提示されている。

光共振器およびレーザ応用のためのポリマーマイクロスフェアの作製

This paper describes three methods of preparing fluorescent microspheres comprising &#960;-conjugated or non-conjugated polymers: vapor diffusion, ...

fabrication-polymer-microspheres-for-optical-resonator-laser

Nanyang Technological University

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JoVE Journal

Engineering

13.9K ビュー.  University of Tsukuba. ポリマーからのミクロスフェアの合成、ミクロスフェアの操作、およびマイクロフォトルミネッセンス測定のためのプロトコールが提示されている。 

ビデオ: Fabrication of Polymer Microspheres for Optical Resonator and Laser 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

Fabrication of Nano-engineered Transparent Conducting Oxides by Pulsed Laser Deposition

Nanosecond Pulsed Laser Deposition (PLD) in the presence of a background gas allows the deposition of metal oxides with tunable morphology, structure, density and stoichiometry by a proper control of the plasma plume expansion dynamics. Such versatility can be exploited to produce nanostructured films from compact and dense to nanoporous characterized by a hierarchical assembly of nano-sized clusters. In particular we describe the detailed methodology to fabricate two types of Al-doped ZnO (AZO) films as transparent electrodes in photovoltaic devices: 1) at low O2 pressure, compact films with electrical conductivity and optical transparency close to the state of the art transparent conducting oxides (TCO) can be deposited at room temperature, to be compatible with thermally sensitive materials such as polymers used in organic photovoltaics (OPVs); 2) highly light scattering hierarchical structures resembling a forest of nano-trees are produced at higher pressures. Such structures show high Haze factor (&gt;80%) and may be exploited to enhance the light trapping capability. The method here described for AZO films can be applied to other metal oxides relevant for technological applications such as TiO2, Al2O3, WO3 and Ag4O4.

We describe the experimental method to deposit nanostructured oxide thin films by nanosecond Pulsed Laser Deposition (PLD) in the presence of a background gas. By using this method Al-doped ZnO (AZO) films, from compact to hierarchically structured as nano-tree forests, can be deposited.

パルスレーザー蒸着法によるナノエンジニアリング透明導電性酸化物の作製

Nanosecond Pulsed  Laser Deposition (PLD) in the presence of a background gas allows the deposition  of metal oxides with tunable morphology, structure, ...

Fabrication and Characterization of Disordered Polymer Optical Fibers for Transverse Anderson Localization of Light

We develop and characterize a disordered polymer optical fiber that uses transverse Anderson localization as a novel waveguiding mechanism. The developed polymer optical fiber is composed of 80,000 strands of poly (methyl methacrylate) (PMMA) and polystyrene (PS) that are randomly mixed and drawn into a square cross section optical fiber with a side width of 250 &mu;m. Initially, each strand is 200 &mu;m in diameter and 8-inches long. During the mixing process of the original fiber strands, the fibers cross over each other; however, a large draw ratio guarantees that the refractive index profile is invariant along the length of the fiber for several tens of centimeters. The large refractive index difference of 0.1 between the disordered sites results in a small localized beam radius that is comparable to the beam radius of conventional optical fibers. The input light is launched from a standard single mode optical fiber using the butt-coupling method and the near-field output beam from the disordered fiber is imaged using a 40X objective and a CCD camera. The output beam diameter agrees well with the expected results from the numerical simulations. The disordered optical fiber presented in this work is the first device-level implementation of 2D Anderson localization, and can potentially be used for image transport and short-haul optical communication systems.

We develop and characterize a disordered polymer optical fiber that uses transverse Anderson localization as a novel waveguiding mechanism. This microstructured fiber can transport a small localized beam with a radius that is comparable to the beam radius of conventional optical fibers.

ライトの横アンダーソン局在のために無秩序ポリマー光ファイバの作製と評価

We develop and characterize a disordered polymer optical fiber that uses transverse Anderson localization as a novel waveguiding mechanism. The developed ...

Patterning via Optical Saturable Transitions - Fabrication and Characterization

This protocol describes the fabrication and characterization of nanostructures using a novel nanolithographic technique called Patterning via Optical Saturable Transitions (POST). In this technique the chemical properties of organic photochromic molecules that undergo single-photon reactions are exploited, enabling rapid top-down nanopatterning over large areas at low light intensities, thereby, allowing for the circumvention of the far-field diffraction barrier.4 Simple, cost-effective, high throughput and resolution alternatives to nanopatterning are being explored, such as, two-photon polymerization5,6, beam pen lithography (BPL)7, scanning electron beam lithography (SEBL), and focused ion beam (FIB) patterning. However, multi-photon approaches require high light intensities, which limit their potential for high throughput and offer low image contrast. Although, electron and ion beam lithographic processes offer increased resolution, the serial nature of the process is limited to slow writing speeds, which also prevents patterning of features over large areas. Beam-pen lithography is an approach towards parallel near-field optical lithography. However, the gap between the source of the beam and the surface of the photoresist needs to be controlled extremely precisely for good pattern uniformity and this is very challenging to accomplish for large arrays of beams. Patterning via Optical Saturable Transitions (POST) is an alternative optical nanopatterning technique for patterning sub-wavelength features1-3. Since this technique uses single photons instead of electrons, it is extremely fast and does not require high light intensities1-3, opening the door to massive parallelization.

We report that the diffraction limit of conventional optical lithography can be overcome by exploiting the transitions of organic photochromic derivatives induced by their photoisomerization at low light intensities.1-3 This paper outlines our fabrication technique and two locking mechanisms, namely: dissolution of one photoisomer and electrochemical oxidation.

光可飽和遷移を経由してパターニング - 作製と特性評価

This protocol describes the fabrication and characterization of nanostructures using a novel nanolithographic technique called Patterning via Optical ...

Fabrication and Operation of a Nano-Optical Conveyor Belt

The technique of using focused laser beams to trap and exert forces on small particles has enabled many pivotal discoveries in the nanoscale biological and physical sciences over the past few decades. The progress made in this field invites further study of even smaller systems and at a larger scale, with tools that could be distributed more easily and made more widely available. Unfortunately, the fundamental laws of diffraction limit the minimum size of the focal spot of a laser beam, which makes particles smaller than a half-wavelength in diameter hard to trap and generally prevents an operator from discriminating between particles which are closer together than one half-wavelength. This precludes the optical manipulation of many closely-spaced nanoparticles and&#160;limits the&#160;resolution of optical-mechanical systems. Furthermore, manipulation using focused beams requires beam-forming or steering optics, which can be very bulky and expensive. To address these limitations in the system scalability of conventional optical trapping our lab has devised an alternative technique which utilizes near-field optics to move particles across a chip. Instead of focusing laser beams in the far-field, the optical near field of plasmonic resonators produces the necessary local optical intensity enhancement to overcome the restrictions of diffraction and manipulate particles at higher resolution. Closely-spaced resonators produce strong optical traps which can be addressed to mediate the hand-off of particles from one to the next in a conveyor-belt-like fashion. Here, we describe how to design and produce a conveyor belt using a gold surface patterned with plasmonic C-shaped resonators and how to operate it with polarized laser light to achieve super-resolution nanoparticle manipulation and transport. The nano-optical conveyor belt chip can be produced using lithography techniques and easily packaged and distributed.

The scalability and resolution of conventional optical manipulation techniques are limited by diffraction. We circumvent the diffraction limit and describe a method of optically transporting nanoparticles across a chip using a gold surface patterned with a path of closely spaced C-shaped plasmonic resonators.

ナノ光学コンベヤーベルトの作製と運用

The technique of using focused laser beams to trap and exert forces on small particles has enabled many pivotal discoveries in the nanoscale biological ...

Compact Lens-less Digital Holographic Microscope for MEMS Inspection and Characterization

A micro-electro-mechanical-system (MEMS) is a widely used component in many industries, including energy, biotechnology, medical, communications, and automotive. However, effective inspection and characterization metrology systems are needed to ensure the functional reliability of MEMS. This study presents a system based on digital holography as a tool for MEMS metrology. Digital holography has gained increasing attention in the past 20 years. With the fast development and decreasing cost of sensor arrays, resolution of such systems has increased broadening potential applications. Thus, it has attracted attention from both research and industry sides as a potential reliable tool for industrial metrology. Indeed, by recording the interference pattern between an object beam (which contains sample height information) and a reference beam on a CCD camera, one can retrieve the quantitative phase information of an object. However, most of digital holographic systems are bulky and thus not easy to implement on industry production lines. The novelty of the system presented is that it is lens-less and thus very compact. In this study, it is shown that the Compact Digital Holographic Microscope (CDHM) can be used to evaluate several characteristics typically consider as criteria in MEMS inspections. The surface profiles of MEMS in both static and dynamic conditions are presented. Comparison with AFM is investigated to validate the accuracy of the CDHM.

We present a compact reflection digital holographic system (CDHM) for inspection and characterization of MEMS devices. A lens-less design using a diverging input wave providing natural geometrical magnification is demonstrated. Both static and dynamic studies are presented.

MEMS検査および特性評価のためのコンパクトなレンズレスデジタルホログラフィック顕微鏡

A micro-electro-mechanical-system (MEMS) is a widely used component in many industries, including energy, biotechnology, medical, communications, and ...

Printing Fabrication of Bulk Heterojunction Solar Cells and In Situ Morphology Characterization

Polymer-based materials hold promise as low-cost, flexible efficient photovoltaic devices. Most laboratory efforts to achieve high performance devices have used devices prepared by spin coating, a process that is not amenable to large-scale fabrication. This mismatch in device fabrication makes it difficult to translate quantitative results obtained in the laboratory to the commercial level, making optimization difficult. Using a mini-slot die coater, this mismatch can be resolved by translating the commercial process to the laboratory and characterizing the structure formation in the active layer of the device in real time and in situ as films are coated onto a substrate. The evolution of the morphology was characterized under different conditions, allowing us to propose a mechanism by which the structures form and grow. This mini-slot die coater offers a simple, convenient, material efficient route by which the morphology in the active layer can be optimized under industrially relevant conditions. The goal of this protocol is to show experimental details of how a solar cell device is fabricated using a mini-slot die coater and technical details of running in situ structure characterization using the mini-slot die coater.

Printing Fabrication of Bulk Heterojunction Solar Cells and In Situ Morphology Characterization

Here, we present a protocol to fabricate organic thin film solar cells using a mini-slot die coater and related in-line structure characterizations using synchrotron scattering techniques.

バルクヘテロ接合太陽電池の印刷作製と<em&gt;その場で</em&gt;形態キャラクタリゼーション

Polymer-based materials hold promise as low-cost, flexible efficient photovoltaic devices. Most laboratory efforts to achieve high performance devices ...

Fabrication of 1-D Photonic Crystal Cavity on a Nanofiber Using Femtosecond Laser-induced Ablation

We present a protocol for fabricating 1-D Photonic Crystal (PhC) cavities on subwavelength-diameter tapered optical fibers, optical nanofibers, using femtosecond laser-induced ablation. We show that thousands of periodic nano-craters are fabricated on an optical nanofiber by irradiating with just a single femtosecond laser pulse. For a typical sample, periodic nano-craters with a period of 350 nm and with diameter gradually varying from 50 - 250 nm over a length of 1 mm are fabricated on a nanofiber with diameter around 450 - 550 nm. A key aspect of such a nanofabrication is that the nanofiber itself acts as a cylindrical lens and focuses the femtosecond laser beam on its shadow surface. Moreover, the single-shot fabrication makes it immune to mechanical instabilities and other fabrication imperfections. Such periodic nano-craters on nanofiber, act as a 1-D PhC and enable strong and broadband reflection while maintaining the high transmission out of the stopband. We also present a method to control the profile of the nano-crater array to fabricate apodized and defect-induced PhC cavities on the nanofiber. The strong confinement of the field, both transverse and longitudinal, in the nanofiber-based PhC cavities and the efficient integration to the fiber networks, may open new possibilities for nanophotonic applications and quantum information science.

We present a protocol for fabricating 1-D photonic crystal cavities on subwavelength diameter silica fibers (optical nanofibers) using femtosecond laser-induced ablation.

フェムト秒レーザー誘起アブレーションを用いたナノファイバー上の1次元フォトニック結晶共振器の作製

We present a protocol for fabricating 1-D Photonic Crystal (PhC) cavities on subwavelength-diameter tapered optical fibers, optical nanofibers, using ...

Fabrication of Superhydrophobic Metal Surfaces for Anti-Icing Applications

Several ways to produce superhydrophobic metal surfaces are presented in this work. Aluminum was chosen as the metal substrate due to its wide use in industry. The wettability of the produced surface was analyzed by bouncing drop experiments and the topography was analyzed by confocal microscopy. In addition, we show various methodologies to measure its durability and anti-icing properties. Superhydrophobic surfaces hold a special texture that must be preserved to keep their water-repellency. To fabricate durable surfaces, we followed two strategies to incorporate a resistant texture. The first strategy is a direct incorporation of roughness to the metal substrate by acid etching. After this surface texturization, the surface energy was decreased by silanization or fluoropolymer deposition. The second strategy is the growth of a ceria layer (after surface texturization) that should enhance the surface hardness and corrosion resistance. The surface energy was decreased with a stearic acid film.
The durability of the superhydrophobic surfaces was examined by a particle impact test, mechanical wear by lateral abrasion, and UV-ozone resistance. The anti-icing properties were explored by studying the ability to repeal subcooled water, freezing delay, and ice adhesion.

We illustrate several methodologies to produce superhydrophobic metal surfaces and to explore their durability and anti-icing properties.

防氷用超撥水の金属表面の作製

Several ways to produce superhydrophobic metal surfaces are presented in this work. Aluminum was chosen as the metal substrate due to its wide use in ...

Fused Filament Fabrication (FFF) of Metal-Ceramic Components

Technical ceramics are widely used for industrial and research applications, as well as for consumer goods. Today, the demand for complex geometries with diverse customization options and favorable production methods is increasing continuously. With fused filament fabrication (FFF), it is possible to produce large and complex components quickly with high material efficiency. In FFF, a continuous thermoplastic filament is melted in a heated nozzle and deposited below. The computer-controlled print head is moved in order to build up the desired shape layer by layer. Investigations regarding printing of metals or ceramics are increasing more and more in research and industry. This study focuses on additive manufacturing (AM) with a multi-material approach to combine a metal (stainless steel) with a technical ceramic (zirconia: ZrO2). Combining these materials offers a broad variety of applications due to their different electrical and mechanical properties. The paper shows the main issues in preparation of the material and feedstock, device development, and printing of these composites.

Fused Filament Fabrication FFF of Metal-Ceramic Components

This study shows multi-material additive manufacturing (AM) using fused filament fabrication (FFF) of stainless steel and zirconia.

金属-セラミック部品の溶融フィラメント製作 (FFF)

Technical ceramics are widely used for industrial and research applications, as well as for consumer goods. Today, the demand for complex geometries with ...