C.R.C. would like to acknowledge the Ramsay Memorial Trust for funding.

CdSe / ZnSのコア/シェル量子ドットの作製<ol><li> トリオクチルホスフィンの調製（TOP）-Seソリューション <ol><li>窒素下またはグローブボックス中のシュレンクフラスコにTOPへのSeの適切な量を混合することにより、TOP中のセレンの0.5M溶液（反応ごとに必要な8ミリリットル、TOPの10ミリリットルに溶かし、通常、0.4グラム）を準備します。 </li><li> TOP-Seの複合体の灰色溶液が得られ、1時間のSeを溶解するために混合物を撹拌しました。 </li><li>溶液を凍結 - ポンプ - 解凍を5回脱気した後であることを確認します。得られたストック溶液は、3ヶ月間、窒素下で保存することができます。 </li></ol></li><li> CdSeコアの調製 <ol><li>酸化カドミウム（51ミリグラム、0.4ミリモル）、TOP酸化物（3.7グラム、9.6ミリモル）、ヘキサデシルアミン（1.93グラム、8ミリモル）及び1-ドデシル酸（0.22グラム、0.88ミリモル）を秤量し、3首に結合し、250 mlの丸底フラスコ。攪拌棒を追加します。 </li><li>隔壁を2首を閉じ、確保第三は、長い還流冷却器および窒素/真空シュレンクラインに取り付けられています。混合物に直接1セプタムを通して加熱マントルの温度プローブを挿入します。ポンプ/窒素で5回フラスコを補充します。 </li><li> 320℃までフラスコを加熱し、窒素雰囲気下で1時間溶融物を攪拌します。 </li><li> 270°Cまでのマントルピースの温度を下げた後、窒素で脱気に5回大きな注射器と広い口径の針（20ミリリットル、3ミリメートルの穴）を使用します。 </li><li>アップTOP-Seの溶液（ステップ1.1）の8ミリリットルを取り、セプタムを通して、3口フラスコに慎重が、急速に注入します。 </li><li> secで製造された粒子のサイズを制御するために、10分間、30〜270℃で反応を撹拌しました。赤色発光（〜600 nm）のために、7~9分が好適です。 </li><li> （反応容器の半分水没するのに十分な大きさ）を加え、反応混合物を次に沸騰したお湯を入れたボウルを準備します。反応時間が完了した後、急速にboili反応を冷却かき混ぜながら水をngの。 注意：冷却はフラスコに亀裂を引き起こす可能性があります。細心の注意を払って、厚い不浸透性の手袋を着用してください。 </li><li>冷却したら、すべての製品を溶解し、2つの50ml遠心管の間の混合物を分割するためにフラスコに10mlのクロロホルムを注入。 </li><li> 3600×gで10分で各チューブアップエタノール、遠心分離で50mlにトップアップは、粒子を沈殿させました。上清を捨て、n-ヘキサン10ミリリットルの合計でペレットを再分散させます。 </li></ol></li><li> CdSeコアのZnSの砲撃： <ol><li> 100mlにヘキサン中のコアを追加ジエチルジチオカルバミン酸亜鉛（0.8 gであり、1.4ミリモル）を含有する丸底フラスコに、オレイルアミン（3 mlの9.12ミリモル）、トリオクチルホスフィン（3 mlの6.73ミリモル）及び1-オクタデセン（10ml）溶液。攪拌棒を追加します。窒素に反応雰囲気を交換します。 </li><li> 70°Cまで、部分真空下で3.3℃/分でホットプレート攪拌機上の反応を熱し、そしてシュレンクラインを使用してヘキサンを除去。 </li&gt; <li>窒素に雰囲気を切り替えて、120℃にこのレートで加熱を続けます。 2時間120℃で撹拌します。 </li><li>反応を冷却することを可能にし、2×50mlの遠心分離管の間の混合物を分割します。チューブを10分間3600×gで粒子と遠心分離を沈殿させEtOHで50ミリリットルまで突破していることを確認します。 </li><li>上清を捨て、n-ヘキサン10ミリリットルの合計でペレットを再分散させます。 </li><li>遠心分離機この溶​​液（3600×gで、10分）を1回以上までの3ヶ月間、サンプル管にデカントされる前に、任意の不溶性不純物を除去し、窒素雰囲気下、冷蔵庫（4℃）に格納します。 </li></ol></li></ol> PDMSへのナノ粒子の2膨潤カプセル化<ol><li> 溶液の調製を膨潤： <ol><li> 4（合成される）のCdSe量子ドットの分散液mlのn-ヘキサン36ミリリットルを混合したCdSe量子ドットのストック溶液を調製し、磁気的に溶液を攪拌します。&lt;/李&gt; <li>別に指定腫れソリューションとして原液の9ミリリットルを含む2つのバイアルをそれぞれ設定します。 </li><li> QD濃度を変化させ、さらに膨潤溶液の調製のためのストック溶液の残りの部分を使用してください。 66％（v / v）の溶液を、50％溶液および33％の溶液を得たストック溶液を希釈することによって減少QD濃度の三膨潤溶液を調製します。 <ol><li> n-ヘキサン3mlでのCdSe QDストック溶液を6mlを混合することにより、66％（v / v）の溶液を調製します。完全な混合を確実にするために、磁気的に溶液を攪拌します。 </li><li> 4.5 mlのn-ヘキサンでのCdSe QDストック溶液4.5mlを混合することによって、50％（v / v）の溶液を調製します。完全な混合を確実にするために、磁気的に溶液を攪拌します。 </li><li> n-ヘキサン6ミリリットルでのCdSe QDストック溶液3mlを混合することにより、33％（v / v）の溶液を調製します。完全な混合を確実にするために、磁気的に溶液を攪拌します。 </li></ol></li><li>室温で、暗条件下でQDソリューションのすべてを格納します。&lt;/李&gt; </ol></li><li> ポリマーの調製およびQD取り込み-膨潤液にQDの濃度を変化させること： <ol><li>新鮮な手術用メスの刃を使用して、4つの医療グレードのシリコーンの正方形（11ミリメートル×11 mm）を切り出します。 </li><li>変化％のQD濃度の4膨潤溶液のそれぞれにおける医療グレードシリコーン正方形浸し：ストック溶液を、66％（v / v）で、50％（v / v）の33％（v / v）です。ポリマーサンプルは、暗条件下で、及び室温で24時間膨潤することを可能にします。 </li><li>残留溶剤が蒸発し、ポリマーが戻って自分の初期の寸法に縮小された時間の間に、48時間暗条件下でそれぞれの腫れソリューション、空気乾燥から膨潤したポリマーサンプルを削除します。 </li><li>任意の表面に結合した物質を除去するために脱イオン水で十分にQD-組み込まれたサンプルを洗ってください。 </li></ol></li><li> ポリマーの調製およびQD取り込み-膨潤液にポリマーの露出時間を変えます： </stronグラム&gt; <ol><li> 2.2.1で述べたように、4つの医療グレードのシリコーンの正方形（11ミリメートル×11 mm）を準備します。 </li><li>期間を変化させるための解決策を膨れ入荷医療グレードのシリコーンの正方形を浸し：1時間、3時間、6時間および24時間。 </li><li>膨潤液から取り出した後、空気はサンプルが戻ってその前の寸法を縮小するように、48時間暗条件下で膨潤したポリマー試料を乾燥させます。 </li><li>任意の表面に結合した物質や残留溶媒を除去するために、脱イオン水で十分にQD-組み込まれたサンプルを洗ってください。 </li></ol></li></ol>ナノ粒子の3可視化は、PDMSにカプセル化スウェル<ol><li> シリコーンサンプル調製： <ol><li>新鮮なメスの刃（5.5ミリメートル×11 mm）の2つのシリコーンの正方形を切り取ります。これはシリコーンサンプルの内部表面を露出させていることを確認してください。 </li></ol></li><li> 蛍光イメージング： <ol><li> microscoにシリコーンサンプルを置きますポリマーの新たにカット側はスライドガラスに完全に密着していることを保証するイメージングのためのPEのスライド、。顕微鏡スライドとの円滑な接触を確保するために軽くシリコーン部分を押し下げます。顕微鏡のステージ上にサンプルを置きます。 </li><li> 20 MHzまたは類似の速度で5ピコ秒のパルスからなる488nmの分光濾過レーザー線を使用して完全な寿命の蛍光測定値23 488 ​​を生成するために、レーザ出力の直接結合、音響光学可変フィルタシステムを使用してnmレーザーライン。 10X対物レンズの背面開口部にダイクロイックミラー（488 nm）ので反射してサンプルの上にされ、特注のレーザースキャニングユニットを（補足情報を参照してください）​​、使用したレーザー光の焦点を合わせます。 <ol><li>その後、同じダイクロイックミラーを透過していることを、同じ目的を持つ蛍光発光を収集します。単一光子計数モードで動作するアバランシェフォトダイオードに向けて、この光を向けます。プロセスlifeti<html>時間相関単一光子計数（TCSPC）ボードを使用して私の測定。23 </li></ol></li><li>開始時の機器の応答関数（IRF）と各実験セッションの終了を記録します。23 注：TCSPC実験で記録された信号は、検出器における光子の到着とその後のレーザーパルスの生成との間の時間遅延を示すべきです。この時間遅延は、しかしながら、測定装置のIRFと畳み込みされるべきです。したがって、IRFは、楽器の応答と比較して有意に短い寿命（〜100ピコ秒）を持つ100 nMのオーラミンO、に機器の応答として測定されます。 </li><li>蛍光強度の指数関数的減衰の非線形フィッティングにより寿命を抽出し、最尤推定量（MLE）アルゴリズム25-27を使用して、IRFからこれをデコンボリューション。 MLE（γjは ）のように計算されます eq1.jpg &quot;/&gt; N iは 、チャネルIでの光子カウント数であり、kは各蛍光減衰のためのチャネル（またはビン）の数であり、pはI（j）は 、光子のグループは、粒子が持っている私場合、チャネルに分類する確率であります生涯jは 、Nは与えられた減衰のためのカウントの総数です。 </li><li>サイズ512×512ピクセルと264の画像からなる連続スキャンを作成し、5分間、各サンプルの蛍光強度と寿命のデータを記録します。 150光子とプロセスのしきい​​値と計算されたMLEこの使用して、MATLABで、2次元の蛍光強度、寿命や強度加重寿命マップを提供するために、これらを組み合わせます。 </li></ol></li></ol>

<ol>
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Lett. 250 (3-4), 355-360 (1996).</li><li>K&#246;llner, M., Wolfrum, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=How+many+photons+are+necessary+for+fluorescence-lifetime+measurements.">How many photons are necessary for fluorescence-lifetime measurements.</a> Chem. Phys. Lett. 200 (1-2), 199-204 (1992).</li><li>Edel, J. B., Eid, J. S., Meller, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Accurate+Single+Molecule+FRET+Efficiency+Determination+for+Surface+Immobilized+DNA+Using+Maximum+Likelihood+Calculated+Lifetimes.">Accurate Single Molecule FRET Efficiency Determination for Surface Immobilized DNA Using Maximum Likelihood Calculated Lifetimes.</a> J. Phys. Chem., B. 111 (11), 2986-2990 (2007).</li><li>Bear, J. C., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Doping+Group+IIB+Metal+Ions+into+Quantum+Dot+Shells+via+the+One-Pot+Decomposition+of+Metal-Dithiocarbamates.">Doping Group IIB Metal Ions into Quantum Dot Shells via the One-Pot Decomposition of Metal-Dithiocarbamates.</a> Adv. Opt. Mater. 3 (5), 704-712 (2015).</li><li>Li, L., Hu, J., Yang, W., Alivisatos, A. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Band+Gap+Variation+of+Size-+and+Shape-Controlled+Colloidal+CdSe+Quantum+Rods.">Band Gap Variation of Size- and Shape-Controlled Colloidal CdSe Quantum Rods.</a> Nano Letters. 1 (7), 349-351 (2001).</li></ol>

The authors have nothing to disclose.

Cross-sectional fluorescence imaging allows for direct visualization of nanoparticles during swell encapsulation. The kinetics of encapsulation has been shown, with the drive toward a high nanoparticle surface concentration demonstrated. The extent of nanoparticle incorporation is shown to vary with swell encapsulation time (described in section 2.3), with the total amount of incorporated nanoparticles increasing as this time is extended, with the particle concentration localized at the surface if the polymer samples are...

ナノ材料の適用は、長い間、新規技術への関心の高まりの面積を務めています。1-3。これは、化粧品、衣類、包装、エレクトロニクスなどの日用品、中のナノ粒子の成長の使用を含んでいた。4-6ナノ粒子を用い向けて主要なドライブ機能材料に、7つ別の利点は、ホストマトリックスに重要な特性を導入する、容易に複合材料を形成する能力である。粒径の変動によって調整プロパティする能力に加えて、材料への高い反応性の相対由来など触媒機能、材料の強化および電気的特性のチューニング。8-12 ナノ粒子-高分子複合材料は、ホストマトリックスの製造中に所望のナノ粒子の直接積分である最も単純なそれらの技術の範囲を介して達成することができる。13,14これR全体にナノ粒子材料の均等間隔で均質な材料でesults。しかし、多くのアプリケーションでは、ナノ複合材料の外部インタフェースに存在する活性物質を必要とします。材料のバルクを通じて多くのナノ粒子の廃棄物が存在する結果として、直接の取り込みは、時には高価なナノ粒子材料の効率的な使用にはなりません。15,16を直接取り込みを達成するために、ナノ粒子はまた、ホストマトリックスの形成と互換性がなければなりません。これは、特に、一般的に高活性なナノ粒子によって影響を受ける可能性がある金属錯体触媒機構によって促進される熱硬化性ポリマーの場合のように多面的な反応を必要とする合成に、挑戦することができる。14 ポリマー合成中に直接ナノ粒子の取り込みに関連したかなりの欠点は、ナノ粒子incorporatiを制限することを目的とした技術の開発につながっています表面層に上。17-21スウェルカプセル化は、ポリマーのバルク中の限られた無駄で、高い表面のナノ粒子の濃度を達成するために、文献で ​​報告された最も成功した戦略の一つである。17-19技術は、ポリマーの溶剤駆動膨潤を利用します行列は、分子種とナノ粒子の侵入を可能にします。膨潤溶媒を除去すると、マトリックス内の種は表面に局在する種の最高濃度で、所定の位置に固定となります。現在までに、うねりカプセル化の報告用途のほとんどは、活性剤は、材料表面であることが鍵である抗菌ポリマーの製造、に向けられています。これらのレポートの多くが強化された抗菌活性を示しているが、正確な表面ナノ粒子組成物はほとんど詳細に精査されていません。クリックらは最近、重要なINSIを提供し、ナノ粒子の侵入の直接可視化するための方法を実証しましたうねりのカプセル化によって達成動態および表面のナノ粒子の濃度にGHT。22 この作品は、セレン化カドミウム量子ドット（QD）、ポリジメチルシロキサン（PDMS）と蛍光イメージングを使用して、それらの組み込みの直接可視化へのそれらのうねりのカプセル化の合成を詳述します。膨潤溶液中で膨潤カプセル化時間及びナノ粒子の濃度を変化させることの効果が検討されています。蛍光可視化技術は、PDMS中にナノ粒子侵入の直接的なイメージングを可能にし、QDの最高濃度は、材料の表面であることを示しています。

<table border="0" cellpadding="0" cellspacing="0" width="573">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Polydimethylsiloxane sheets</td>
			<td style="width:71px;">NuSil</td>
			<td style="width:119px;">-</td>
			<td style="width:167px;">Medical Grade</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Oleylamine</td>
			<td style="width:71px;">Sigma Aldrich</td>
			<td style="width:119px;">O7805</td>
			<td>Technical Grade</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Trioctylphosphine</td>
			<td style="width:71px;">Sigma Aldrich</td>
			<td style="width:119px;">117854</td>
			<td>Technical Grade</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Trioctylphosphine oxide</td>
			<td style="width:71px;">Sigma Aldrich</td>
			<td style="width:119px;">346187</td>
			<td>Technical Grade</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">1-Octadecene</td>
			<td style="width:71px;">Sigma Aldrich</td>
			<td style="width:119px;">O806</td>
			<td>Technical Grade</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Zinc diethyldithiocarbamate</td>
			<td style="width:71px;">Sigma Aldrich</td>
			<td style="width:119px;">329703</td>
			<td>-</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Oleic acid</td>
			<td style="width:71px;">Sigma Aldrich</td>
			<td style="width:119px;">364525</td>
			<td>Technical Grade</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Triethylamine</td>
			<td style="width:71px;">Sigma Aldrich</td>
			<td style="width:119px;">471283</td>
			<td>-</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Cadmium oxide</td>
			<td style="width:71px;">Alfa Aesar</td>
			<td style="width:119px;">33235</td>
			<td>-</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Hexadecylamine</td>
			<td style="width:71px;">Alfa Aesar</td>
			<td style="width:119px;">B22459</td>
			<td>Technical Grade</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">1-Dodecylphosphonic acid</td>
			<td style="width:71px;">Alfa Aesar</td>
			<td style="width:119px;">H26259</td>
			<td>-</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Selenium powder</td>
			<td style="width:71px;">Acros</td>
			<td style="width:119px;">19807</td>
			<td>-</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Chloroform</td>
			<td style="width:71px;">Sigma Aldrich</td>
			<td style="width:119px;">366919</td>
			<td>-</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">n-Hexane</td>
			<td style="width:71px;">Sigma Aldrich</td>
			<td style="width:119px;">208752</td>
			<td>-</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Microscope slides</td>
			<td style="width:71px;">VWR</td>
			<td style="width:119px;">631-0137</td>
			<td>Thickness No. 1</td>
		</tr>
	</tbody>
</table>

advanced compositional analysis of nanoparticle-polymer composites using direct fluorescence imaging

The fabrication of polymer-nanoparticle composites is extremely important in the development of many functional materials. Identifying the precise composition of these materials is essential, especially in the design of surface catalysts, where the surface concentration of the active component determines the activity of the material. Antimicrobial materials which utilize nanoparticles are a particular focus of this technology. Recently swell encapsulation has emerged as a technique for inserting antimicrobial nanoparticles into a host polymer matrix. Swell encapsulation provides the advantage of localizing the incorporation to the external surfaces of materials, which act as the active sites of these materials. However, quantification of this nanoparticle uptake is challenging. Previous studies explore the link between antimicrobial activity and surface concentration of the active component, but this is not directly visualized. Here we show a reliable method to monitor the incorporation of nanoparticles into a polymer host matrix via swell encapsulation. We show that the surface concentration of CdSe/ZnS nanoparticles can be accurately visualized through cross-sectional fluorescence imaging. Using this method, we can quantify the uptake of nanoparticles via swell encapsulation and measure the surface concentration of encapsulated particles, which is key in optimizing the activity of functional materials.

600nm程度のラムダ最大で、赤色蛍光を示した。22,28赤色発光量子ドットはサイズ寸法強い閉じ込め政権内にある量子ロッドによって励起子の閉じ込めによるものでした。 Li らは、量子ロッドのため、発光シフト幅またはロッドの長さのいずれかの増加に伴ってエネルギーを低下させることを示しました。彼らはさらに、放出は、主ロッドの幅は、それ?...

Watch this Scientific Journal Video about Advanced Compositional Analysis of Nanoparticle-polymer Composites Using Direct Fluorescence Imaging at JoVE.com

Advanced Compositional Analysis of Nanoparticle-polymer Composites Using Direct Fluorescence Imaging

Here we present a reliable method to monitor the incorporation of nanoparticles into a polymer host matrix via swell encapsulation. We show that the surface concentration of cadmium selenide quantum dots can be accurately visualized through cross-sectional fluorescence imaging.

直接蛍光イメージングを用いたナノ粒子 - ポリマー複合材料の高度な組成分析

The fabrication of polymer-nanoparticle composites is extremely important in the development of many functional materials. Identifying the precise ...

advanced-compositional-analysis-nanoparticle-polymer-composites-using

Research

JoVE Journal

Engineering

7.6K ビュー.  Imperial College London. Here we present a reliable method to monitor the incorporation of nanoparticles into a polymer host matrix via swell encapsulation. We show that the surface concentration of cadmium selenide quantum dots can be accurately visualized through cross-sectional fluorescence imaging.

ビデオ: Advanced Compositional Analysis of Nanoparticle-polymer Composites Using Direct Fluorescence Imaging

Preparation and Evaluation of Hybrid Composites of Chemical Fuel and Multi-walled Carbon Nanotubes in the Study of Thermopower Waves

When a chemical fuel at a certain position in a hybrid composite of the fuel and a micro/nanostructured material is ignited, chemical combustion occurs along the interface between the fuel and core materials. Simultaneously, dynamic changes in thermal and chemical potentials across the micro/nanostructured materials result in concomitant electrical energy generation induced by charge transfer in the form of a high-output voltage pulse. We demonstrate the entire procedure of a thermopower wave experiment, from synthesis to evaluation. Thermal chemical vapor deposition and the wet impregnation process are respectively employed for the synthesis of a multi-walled carbon nanotube array and a hybrid composite of picric acid/sodium azide/multi-walled carbon nanotubes. The prepared hybrid composites are used to fabricate a thermopower wave generator with connecting electrodes. The combustion of the hybrid composite is initiated by laser heating or Joule-heating, and the corresponding combustion propagation, direct electrical energy generation, and real-time temperature changes are measured using a high-speed microscopy system, an oscilloscope, and an optical pyrometer, respectively. Furthermore, the crucial strategies to be adopted in the synthesis of hybrid composite and initiation of their combustion that enhance the overall thermopower wave energy transfer are proposed.

A protocol for conducting thermopower wave experiments is presented. The synthesis of hybrid composites of a chemical fuel and micro/nanostructured material, manufacturing of a thermopower wave generator, and methods for measuring the corresponding physical phenomena are described.

熱電波の研究における化学燃料と多層カーボンナノチューブのハイブリッド複合材料の作製と評価

When a chemical fuel at a certain position in a hybrid composite of the fuel and a micro/nanostructured material is ignited, chemical combustion occurs ...

工学

Failure Analysis of Batteries Using Synchrotron-based Hard X-ray Microtomography

Imaging morphological changes that occur during the lifetime of rechargeable batteries is necessary to understand how these devices fail. Since the advent of lithium-ion batteries, researchers have known that the lithium metal anode has the highest theoretical energy density of any anode material. However, rechargeable batteries containing a lithium metal anode are not widely used in consumer products because the growth of lithium dendrites from the anode upon charging of the battery causes premature cell failure by short circuit. Lithium dendrites can also form in commercial lithium-ion batteries with graphite anodes if they are improperly charged. We demonstrate that lithium dendrite growth can be studied using synchrotron-based hard X-ray microtomography. This non-destructive imaging technique allows researchers to study the growth of lithium dendrites, in addition to other morphological changes inside batteries, and subsequently develop methods to extend battery life.

Synchrotron-based hard X-ray microtomography is used to image the electrochemical growth of dendrites from a lithium metal electrode through a solid polymer electrolyte membrane.

シンクロトロンベースのハードX線マイクロトモグラフィーを用いて電池の故障解析

Imaging morphological changes that occur during the lifetime of rechargeable batteries is necessary to understand how these devices fail. Since the advent ...

Advanced Experimental Methods for Low-temperature Magnetotransport Measurement of Novel Materials

Novel electronic materials are often produced for the first time by synthesis processes that yield bulk crystals (in contrast to single crystal thin film synthesis) for the purpose of exploratory materials research. Certain materials pose a challenge wherein the traditional bulk Hall bar device fabrication method is insufficient to produce a measureable device for sample transport measurement, principally because the single crystal size is too small to attach wire leads to the sample in a Hall bar configuration. This can be, for example, because the first batch of a new material synthesized yields very small single crystals or because flakes of samples of one to very few monolayers are desired. In order to enable rapid characterization of materials that may be carried out in parallel with improvements to their growth methodology, a method of device fabrication for very small samples has been devised to permit the characterization of novel materials as soon as a preliminary batch has been produced. A slight variation of this methodology is applicable to producing devices using exfoliated samples of two-dimensional materials such as graphene, hexagonal boron nitride (hBN), and transition metal dichalcogenides (TMDs), as well as multilayer heterostructures of such materials. Here we present detailed protocols for the experimental device fabrication of fragments and flakes of novel materials with micron-sized dimensions onto substrate and subsequent measurement in a commercial superconducting magnet, dry helium close-cycle cryostat magnetotransport system at temperatures down to 0.300 K and magnetic fields up to 12 T.

We describe the methodology of mechanical exfoliation and deposition of flakes of novel materials with micron-sized dimensions onto substrate, fabrication of experimental device structures for transport experimentation, and the magnetotransport measurement in a dry helium close-cycle cryostat at temperatures down to 0.300 K and magnetic fields up to 12 T.

新規材料の低温磁気伝導測定のための高度な実験方法

Novel electronic materials are often produced for the first time by synthesis processes that yield bulk crystals (in contrast to single crystal thin film ...

Ultrasonic Welding of Thermoplastic Composite Coupons for Mechanical Characterization of Welded Joints through Single Lap Shear Testing

This paper presents a novel straightforward method for ultrasonic welding of thermoplastic-composite coupons in optimum processing conditions. The ultrasonic welding process described in this paper is based on three main pillars. Firstly, flat energy directors are used for preferential heat generation at the joining interface during the welding process. A flat energy director is a neat thermoplastic resin film that is placed between the parts to be joined prior to the welding process and heats up preferentially owing to its lower compressive stiffness relative to the composite substrates. Consequently, flat energy directors provide a simple solution that does not require molding of resin protrusions on the surfaces of the composite substrates, as opposed to ultrasonic welding of unreinforced plastics. Secondly, the process data provided by the ultrasonic welder is used to rapidly define the optimum welding parameters for any thermoplastic composite material combination. Thirdly, displacement control is used in the welding process to ensure consistent quality of the welded joints. According to this method, thermoplastic-composite flat coupons are individually welded in a single lap configuration. Mechanical testing of the welded coupons allows determining the apparent lap shear strength of the joints, which is one of the properties most commonly used to quantify the strength of thermoplastic composite welded joints.

A straightforward procedure for ultrasonic welding of thermoplastic composite coupons for basic mechanical testing is described. Key characteristics of this ultrasonic welding process are the use of flat energy directors for simplified process preparation and the use of process data for the fast definition of optimum processing conditions.

シングルラップせん断試験を経て溶接継手の機械的特性評価のための熱可塑性コンポジットクーポンの超音波溶接

This paper presents a novel straightforward method for ultrasonic welding of thermoplastic-composite coupons in optimum processing conditions. The ...

Use of a Multi-compartment Dynamic Single Enzyme Phantom for Studies of Hyperpolarized Magnetic Resonance Agents

Imaging of hyperpolarized substrates by magnetic resonance shows great clinical promise for assessment of critical biochemical processes in real time. Due to fundamental constraints imposed by the hyperpolarized state, exotic imaging and reconstruction techniques are commonly used. A practical system for characterization of dynamic, multi-spectral imaging methods is critically needed. Such a system must reproducibly recapitulate the relevant chemical dynamics of normal and pathological tissues. The most widely utilized substrate to date is hyperpolarized [1-13C]-pyruvate for assessment of cancer metabolism. We describe an enzyme-based phantom system that mediates the conversion of pyruvate to lactate. The reaction is initiated by injection of the hyperpolarized agent into multiple chambers within the phantom, each of which contains varying concentrations of reagents that control the reaction rate. Multiple compartments are necessary to ensure that imaging sequences faithfully capture the spatial and metabolic heterogeneity of tissue. This system will aid the development and validation of advanced imaging strategies by providing chemical dynamics that are not available from conventional phantoms, as well as control and reproducibility that is not possible in vivo.

A multi-compartment dynamic phantom is used to simulate some biology of interest for metabolic studies using hyperpolarized magnet resonance agents.

過分極磁気共鳴剤の研究のための多区画動的単一酵素ファントムの使用

Imaging of hyperpolarized substrates by magnetic resonance shows great clinical promise for assessment of critical biochemical processes in real time. Due ...

Using Synchrotron Radiation Microtomography to Investigate Multi-scale Three-dimensional Microelectronic Packages

Synchrotron radiation micro-tomography (SR&#181;T) is a non-destructive three-dimensional (3D) imaging technique that offers high flux for fast data acquisition times with high spatial resolution. In the electronics industry there is serious interest in performing failure analysis on 3D microelectronic packages, many which contain multiple levels of high-density interconnections. Often in tomography there is a trade-off between image resolution and the volume of a sample that can be imaged. This inverse relationship limits the usefulness of conventional computed tomography (CT) systems since a microelectronic package is often large in cross sectional area 100-3,600 mm2, but has important features on the micron scale. The micro-tomography beamline at the Advanced Light Source (ALS), in Berkeley, CA USA, has a setup which is adaptable and can be tailored to a sample&#39;s properties, i.e., density, thickness, etc., with a maximum allowable cross-section of 36 x 36 mm. This setup also has the option of being either monochromatic in the energy range ~7-43 keV or operating with maximum flux in white light mode using a polychromatic beam. Presented here are details of the experimental steps taken to image an entire 16 x 16 mm system within a package, in order to obtain 3D images of the system with a spatial resolution of 8.7 &#181;m all within a scan time of less than 3 min. Also shown are results from packages scanned in different orientations and a sectioned package for higher resolution imaging. In contrast a conventional CT system would take hours to record data with potentially poorer resolution. Indeed, the ratio of field-of-view to throughput time is much higher when using the synchrotron radiation tomography setup. The description below of the experimental setup can be implemented and adapted for use with many other multi-materials.

For this study synchrotron radiation micro-tomography, a non-destructive three-dimensional imaging technique, is employed to investigate an entire microelectronic package with a cross-sectional area of 16 x 16 mm. Due to the synchrotron&#39;s high flux and brightness the sample was imaged in just 3 min&#160;with an 8.7 &#181;m spatial resolution.

マルチスケール三次元マイクロエレクト​​ロニクスパッケージを調査するために放射光マイクロトモグラフィーを用いて、

Synchrotron radiation micro-tomography (SR&#181;T) is a non-destructive three-dimensional (3D) imaging technique that offers high flux for fast data ...

Nanostructured Ag-zeolite Composites as Luminescence-based Humidity Sensors

Small silver clusters confined inside zeolite matrices have recently emerged as a novel type of highly luminescent materials. Their emission has high external quantum efficiencies (EQE) and spans the whole visible spectrum. It has been recently reported that the UV excited luminescence of partially Li-exchanged sodium Linde type A zeolites [LTA(Na)] containing luminescent silver clusters can be controlled by adjusting the water content of the zeolite. These samples showed a dynamic change in their emission color from blue to green and yellow upon an increase of the hydration level of the zeolite, showing the great potential that these materials can have as luminescence-based humidity sensors at the macro and micro scale. Here, we describe the detailed procedure to fabricate a humidity sensor prototype using silver-exchanged zeolite composites. The sensor is produced by suspending the luminescent Ag-zeolites in an aqueous solution of polyethylenimine (PEI) to subsequently deposit a film of the material onto a quartz plate. The coated plate is subjected to several hydration/dehydration cycles to show the functionality of the sensing film.

A protocol for the synthesis of moisture-responsive luminescent Ag-zeolite composites is described in this report.

発光ベースの湿度センサなどのナノ構造のAg-ゼオライト複合

Small silver clusters confined inside zeolite matrices have recently emerged as a novel type of highly luminescent materials. Their emission has high ...

Synchrotron X-ray Microdiffraction and Fluorescence Imaging of Mineral and Rock Samples

In this report, we describe a detailed procedure for acquiring and processing&#160;x-ray microfluorescence (&#956;XRF), and Laue and powder microdiffraction two-dimensional (2D) maps at beamline 12.3.2 of the Advanced Light Source (ALS), Lawrence Berkeley National Laboratory. Measurements can be performed on any sample that is less than 10 cm x 10 cm x 5 cm, with a flat exposed surface. The experimental geometry is calibrated using standard materials (elemental standards for XRF, and crystalline samples such as Si, quartz, or Al2O3 for diffraction). Samples are aligned to the focal point of the x-ray microbeam, and raster scans are performed, where each pixel of a map corresponds to one measurement, e.g., one XRF spectrum or one diffraction pattern. The data are then processed using the in-house developed software XMAS, which outputs text files, where each row corresponds to a pixel position. Representative data from moissanite and an olive snail shell are presented to demonstrate data quality, collection, and analysis strategies.

We describe a beamline setup meant to carry out rapid two-dimensional x-ray fluorescence and x-ray microdiffraction mapping of single crystal or powder samples using either Laue (polychromatic radiation) or powder (monochromatic radiation) diffraction. The resulting maps give information about strain, orientation, phase distribution, and plastic deformation.

・鉱物及び岩石試料の蛍光を放射光 x 線回折

In this report, we describe a detailed procedure for acquiring and processing&#160;x-ray microfluorescence (&#956;XRF), and Laue and powder ...

Expression of Cementitious Pore Solution and the Analysis of Its Chemical Composition and Resistivity Using X-ray Fluorescence

The goal of this method is to determine the chemical composition and electrical resistivity of cementitious pore solution expressed from a fresh paste sample. The pore solution is expressed from a fresh paste sample using a pressurized nitrogen gas system. The pore solution is then immediately transferred to a syringe to minimize evaporation and carbonation. After that, assembled testing containers are used for the X-ray fluorescence (XRF) measurement. These containers consist of two concentric plastic cylinders and a polypropylene film which seals one of the two open sides. The pore solution is added into the container immediately prior to the XRF measurement. The XRF is calibrated to detect the main ionic species in the pore solution, in particular, sodium (Na+), potassium (K+), calcium (Ca2+), and sulfide (S2-), to calculate sulfate (SO42-) using stoichiometry. The hydroxides (OH-) can be calculated from a charge balance. To calculate the electrical resistivity of the solution, the concentrations of the main ionic species and a model by Snyder et al. are used. The electrical resistivity of the pore solution can be used, along with the electrical resistivity of concrete, to determine the formation factor of concrete. XRF is a potential alternative to current methods to determine the composition of pore solution, which can provide benefits in terms of reduction in time and costs.

This protocol describes the procedure to express fresh pore solution from cementitious systems and the measurement of its ionic composition using X-ray fluorescence. The ionic composition can be used to calculate pore solution electrical resistivity, which can be used, together with concrete electrical resistivity, to determine the formation factor.

セメント細孔溶液の化学組成の蛍光 x 線を用いた比抵抗解析式

The goal of this method is to determine the chemical composition and electrical resistivity of cementitious pore solution expressed from a fresh paste ...

Excitation-Scanning Hyperspectral Imaging Microscopy to Efficiently Discriminate Fluorescence Signals

Several techniques rely on detection of fluorescence signals to identify or study phenomena or to elucidate functions. Separation of these fluorescence signals were proven cumbersome until the advent of hyperspectral imaging, in which fluorescence sources can be separated from each other as well as from background signals and autofluorescence (given knowledge of their spectral signatures). However, traditional, emission-scanning hyperspectral imaging suffers from slow acquisition times and low signal-to-noise ratios due to the necessary filtering of both excitation and emission light. It has been previously shown that excitation-scanning hyperspectral imaging reduces the necessary acquisition time while simultaneously increasing the signal-to-noise ratio of acquired data. Using commercially available equipment, this protocol describes how to assemble, calibrate, and use an excitation-scanning hyperspectral imaging microscopy system for separation of signals from several fluorescence sources in a single sample. While highly applicable to microscopic imaging of cells and tissues, this technique may also be useful for any type of experiment utilizing fluorescence in which it is possible to vary excitation wavelengths, including but not limited to: chemical imaging, environmental applications, eye care, food science, forensic science, medical science, and mineralogy.

Spectral imaging has become a reliable solution for identification and separation of multiple fluorescence signals in a single sample and can readily distinguish signals of interest from background or autofluorescence. Excitation-scanning hyperspectral imaging improves on this technique by decreasing the necessary image acquisition time while simultaneously increasing the signal-to-noise ratio.

蛍光信号を効率的に判別する励起走査察ハイパースペクトルイメージング顕微鏡

Several techniques rely on detection of fluorescence signals to identify or study phenomena or to elucidate functions. Separation of these fluorescence ...

直接蛍光イメージングを用いたナノ粒子 - ポリマー複合材料の高度な組成分析

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この動画の章

熱電波の研究における化学燃料と多層カーボンナノチューブのハイブリッド複合材料の作製と評価

シンクロトロンベースのハードX線マイクロトモグラフィーを用いて電池の故障解析

新規材料の低温磁気伝導測定のための高度な実験方法

シングルラップせん断試験を経て溶接継手の機械的特性評価のための熱可塑性コンポジットクーポンの超音波溶接

過分極磁気共鳴剤の研究のための多区画動的単一酵素ファントムの使用

マルチスケール三次元マイクロエレクトロニクスパッケージを調査するために放射光マイクロトモグラフィーを用いて、

発光ベースの湿度センサなどのナノ構造のAg-ゼオライト複合

・鉱物及び岩石試料の蛍光を放射光 x 線回折

セメント細孔溶液の化学組成の蛍光 x 線を用いた比抵抗解析式

蛍光信号を効率的に判別する励起走査察ハイパースペクトルイメージング顕微鏡

直接蛍光イメージングを用いたナノ粒子 - ポリマー複合材料の高度な組成分析

要約

さらに動画を探す

この動画の章

熱電波の研究における化学燃料と多層カーボンナノチューブのハイブリッド複合材料の作製と評価

シンクロトロンベースのハードX線マイクロトモグラフィーを用いて電池の故障解析

新規材料の低温磁気伝導測定のための高度な実験方法

シングルラップせん断試験を経て溶接継手の機械的特性評価のための熱可塑性コンポジットクーポンの超音波溶接

過分極磁気共鳴剤の研究のための多区画動的単一酵素ファントムの使用

マルチスケール三次元マイクロエレクト​​ロニクスパッケージを調査するために放射光マイクロトモグラフィーを用いて、

発光ベースの湿度センサなどのナノ構造のAg-ゼオライト複合

・鉱物及び岩石試料の蛍光を放射光 x 線回折

セメント細孔溶液の化学組成の蛍光 x 線を用いた比抵抗解析式

蛍光信号を効率的に判別する励起走査察ハイパースペクトルイメージング顕微鏡

マルチスケール三次元マイクロエレクトロニクスパッケージを調査するために放射光マイクロトモグラフィーを用いて、