著者らは、陽極テクスチャアルミマスターとスイス連邦エネルギー局と資金調達のためのスイス国立科学財団（NSF）のAFM、W.リーの支援についてはM.ルブーフに感謝します。本研究の一部はグラント契約なし283501下のEC FP7の資金によるプロジェクト &quot;ファストトラック&quot;の枠組みの中で行われた。

1。金型製作我々は、6。文献続く負の金型の製造のための私達の自作ナノインプリントセットアップを使用しますが、任意の代替ナノインプリントのセットアップが正常に動作します。あるいは官能ポリジメチルシロキサン（PDMS）モールドもうまくいくかもしれない。 <ol><li>転送されるナノスケールのパターンを有する適切なマスターを製造または購入しています。原則として、ナノインプリントに適した任意のマスターが仕事を行います。我々は、メソッドを説明するためにマスター構造として3.1で説明され堆積したガラス板上に配向ZnO層（Schott社、AF32エコ、41ミリメートル×41ミリメートル×0.5 mm）を使用しています。 </li><li> 2で説明したように、マスター·構造上の接着防止層を適用します。 </li><li>さらに2分間超音波イソプロパノール浴続いて2分間超音波アセトン浴中のポリエチレンナフタ（PEN）シート（グッドフェロー、82ミリメートル×41ミリメートル×0.125 mm）を清掃してください。イソプロパノールでもう一度すすぎ、窒素でブロードライ。 </li><li>預金PENシート上のCr接着層（5-10 nm）をスパッタ。 </li><li>均一なカバレッジを得るために5,000 rpmで、PENシート上にスピンコートUV硬化樹脂（マイクロレジスト、ORMOCER、1-2）を加えた。 </li><li> ℃で溶媒を蒸発させるために80℃のホットプレート上で5分間プリベークを行い、PENのシートに膜均一性と接着性を向上させる。 </li><li> UV硬化樹脂にマスターパターンをスタンプするためにあなたのナノインプリントセットアップを使用します。必須ではありませんが、我々は柔軟性のあるシリコン膜上に1バールの均質な圧力を加えることによって、バブルの介在を防ぐために真空下でスタンピング行う。我々のセットアップでは、シリコーン膜は2つのサブコンパートメントに真空チャンバーを分離します。下部コンパートメントは、真空下でのまま圧力は、通気上部コンパートメントによって生成されます。ベントは、スタンピングを開始底部に向かって柔軟な膜をプッシュします。 </li><li>樹脂の架橋反応を誘発する紫外線に樹脂を公開します。私達は適度な光を適用いくつかのLEDが提供する365nmの波長で1.4 mW / cm 2での強さ。 PENのシートを介して露光時間は、通常15〜20分です。 </li><li>慎重に手動でマスタ構造オフモールドを剥離することにより、demould。 </li><li>樹脂は、さらに処理する前に周囲の雰囲気とのオーブンで6〜8時間の間に自然剥離、我々は150で穏やかな熱ポストベークを行う℃につながる可能性があり、機能性材料の成膜時のわずかな収縮を経るかもしれませんが。 </li></ol> 2。接着防止層成功した離型については、接着防止層は、材料やパターンの粗さに適合させる必要があります。一般的に粗いパターンは低付着係数が必要になります。滑らかなパターン上の低付着係数は、金型から機能性材料の剥離につながる可能性があります。ラフパターンで高い付着係数はadherenとして金型の製作中のPEN樹脂シートからの剥離をもたらすかもしれませんマスターへの樹脂のceが強い。 <ol><li>コー​​ト抗接着剤の付着を促進するためのスパッタクロム層（5-10 nm）で金型（またはマスタ​​ー）。滑らかなパターンのために私達は、このステップをドロップします。いくつかのケースではクロム層はエッチマスタ構造に付着防止剤を防ぐことができます。 </li><li>スライドガラス上の付着防止剤の小滴（Sigma-Aldrich社、（1H、1H、2H、2H-Perfluoroctyl）trichlorsilane）を適用します。真空チャンバ内に金型と一緒にスライドガラスを入れて、ポンプダウン。付着防止剤は蒸発し、金型上の単分子層として堆積するであろう。 </li><li> 80℃で1〜2時間の間アニーリング℃を介して付着防止剤を固定する</li></ol> 3。材料堆積我々はnanomouldingの汎用性を示すために、ここで材料堆積に適した3蒸着技術を実証する。他の堆積技術を適用することも可能性があります。三番目の例は、FAを説明完全な薄膜シリコン太陽電池のbrication。 <ol><li>酸化亜鉛の化学気相成長（CVD）：180に加熱CVD反応炉の加熱板上に金型を入れ℃、 ZnOの堆積中にペン型から曲げないように金属フレームを使用しています。原子炉を閉じ、ポンプダウンと熱化を可能にします。前駆体ガス（H 2 Oおよび（C 2 H 5）2 Zn）を認める。ドーピングに加えて、我々は、用量、B 2 H 6を少量。 ZnO層の厚さは蒸着時間に比例します。我々は、ZnO層は、通常、1〜5μmの厚さを使用します。典型的な蒸着パラメータの詳細については文献で ​​見つけられるかもしれません。7 </li><li>物理蒸着（PVD）/銀のスパッタリング：PVDシステムに金を入れてください。システムを閉じ、ポンプダウン。アルゴンプロセスガスを認める。直流発電機の電源をオンにします。 Ag層の厚さが再び蒸着時間に比例します。我々は、Ag層、典型的には1ミクロンの厚さを使用します。典型的な堆積Parametersは5.5x10 -3 mbarのアルゴン圧力と約45nm /秒の蒸着速度をもたらす250 Wのセットアップ特定のDC電源です。 </li><li>プラズマ化学気相堆積（PE-CVD）：3.1のように預金のZnO）。 200に加熱し、PE-CVDリアクタ℃に金型を入れて原子炉を閉じ、ポンプダウンと熱化を可能にします。前駆体ガス（SiH 4とH 2）を認める。加えて、我々は線量それぞれドーピングp型およびn型を達成するためにB（CH 3）3、PH 3の少量。太陽電池の開放電圧を向上させるために、我々はまた、ドープされた層のためのCH 4とCO 2の少量を使用しています。 3.1で説明したようにピンアモルファスシリコン太陽電池スタックを堆積した後、我々は、ZnO backcontactを預ける。 </li><li>曲げは、堆積層の剥離が原因となり、金型の過度の屈曲を避けてください。 </li></ol> 4。層転写我々はGLASを使用最終基板としてのスライド（Schott社A​​F32エコ、41ミリメートル×41ミリメートル×0.5ミリメートル）。しかし、金属箔またはポリマーシートを含む他の基板は、代わりに使用することができる。 <ol><li>アセトン、イソプロパノールで清掃したガラススライドし、窒素でブロードライ。 </li><li> 5,000 rpmでスライドガラス上にスピンコートUV硬化樹脂（マイクロレジスト、ORMOCER、1-2）を加えた。 </li><li>最終的な基板上に堆積層を運ぶ金型を固定するために、ナノインプリントのセットアップを使用します。刻印につきましては、1バールの均質な圧力を加えることによって、真空下でアンカー実行します。 </li><li>架橋反応を誘発する紫外線に樹脂を公開します。我々は、いくつかのLEDが提供する365nmの波長で1.4 mW / cm 2で 、適度な強度を適用します。スライドガラスを介して露光時間は、PENに比べてガラスの高いUV透過率に起因する唯一の1から3分です。 </li><li>手動でスライドガラスオフモールドを剥離しDemould。 </li></ol> 5。サンプルキャラクタリゼーション<ol&gt; <li> nanomouldedサンプルを特徴づけるためにあなたの好みの形態学的、電気的または光学的な手法を使用しています。ここでは、走査型電子顕微鏡（SEM）や原子間力顕微鏡（AFM）を用いて私たちのnanomouldedサンプルを特徴付ける。 </li></ol>

<ol>
	<li>Geissler, M., Xia, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Patterning:+Principles+and+Some+New+Developments.">Patterning: Principles and Some New Developments.</a> Advanced Materials. 16 (15), 1249-1269 (2004).</li><li>Guo, L. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nanoimprint+Lithography:+Methods+and+Material+Requirements.">Nanoimprint Lithography: Methods and Material Requirements.</a> Advanced Materials. 19, 495-513 (2007).</li><li>Ahn, S. H., Guo, L. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Large-Area+Roll-to-Roll+and+Roll-to-Plate+Nanoimprint+Lithography:+A+Step+toward+High-Throughput.">Large-Area Roll-to-Roll and Roll-to-Plate Nanoimprint Lithography: A Step toward High-Throughput.</a> Application of Continuous Nanoimprinting. ACS Nano. 3 (8), 2304-2310 (2009).</li><li>Battaglia, C., Escarr&#233;, J., 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=Nanoimprint+Lithography+for+High-Efficiency+Thin-Film+Silicon+Solar+Cells.">Nanoimprint Lithography for High-Efficiency Thin-Film Silicon Solar Cells.</a> Nano Letters. 11, 661-665 (2011).</li><li>Battaglia, C., Escarr&#233;, J., 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=Nanomoulding+of+Transparent+Zinc+Oxide+Electrodes+for+Efficient+Light+Trapping+in+Solar+Cells.">Nanomoulding of Transparent Zinc Oxide Electrodes for Efficient Light Trapping in Solar Cells.</a> Nature Photonics. 5, 535-538 (2012).</li><li>Escarr&#233;, J., S&#246;derstr&#246;m, K., 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=High+Fidelity+Transfer+of+Nanometric+Random+Textures+by+UV+Embossing+for+Thin+Film+Solar+Cells+Applications.">High Fidelity Transfer of Nanometric Random Textures by UV Embossing for Thin Film Solar Cells Applications.</a> Solar Energy Materials &amp; Solar Cells. 95, 881-886 (2011).</li><li>Fa&#255;, S., Feitknecht, L., Schl&#252;chter, R., Kroll, U., Vallat-Sauvain, E., Shah, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Rough+ZnO+layers+by+LP-CVD+process+and+their+effect+in+improving+performances+of+amorphous+and+microcrystalline+silicon+solar+cells.">Rough ZnO layers by LP-CVD process and their effect in improving performances of amorphous and microcrystalline silicon solar cells.</a> Solar Energy Materials and Solar Cells. 90, 2960-2967 (2006).</li><li>Zhao, X. -. M., Xia, Y., Whitesides, G. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Fabrication+of+Three-Dimensional+Micro-Structures:+Microtransfer+Molding.">Fabrication of Three-Dimensional Micro-Structures: Microtransfer Molding.</a> Advanced Materials. 8, 837-840 (1996).</li><li>Hampton, M. J., Williams, S. S., 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=The+Patterning+of+Sub-500+nm+Inorganic+Oxide+Structures.">The Patterning of Sub-500 nm Inorganic Oxide Structures.</a> Advanced Materials. 20, 2667-2673 (2008).</li><li>Bass, J. D., Schaper, C. D., 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=Transfer+Molding+of+Nanoscale+Oxides+Using+Water-Soluble+Templates.">Transfer Molding of Nanoscale Oxides Using Water-Soluble Templates.</a> ACS Nano. 5 (5), 4065-4072 (2011).</li><li>Escarr&#233;, J., Nicolay, S., 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=Nanomoulded+front+ZnO+contacts+for+thin+film+silicon+solar+cell+applications.">Nanomoulded front ZnO contacts for thin film silicon solar cell applications.</a> , (2012).</li><li>Sontheimer, T., Rudigier-Voigt, E., Bockmeyer, M., Klimm, C., Schubert-Bischoff, P., Becker, C., Rech, B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Large-area+fabrication+of+equidistant+free-standing+Si+crystals+on+nanoimprinted+glass.">Large-area fabrication of equidistant free-standing Si crystals on nanoimprinted glass.</a> Phys. Status Solidi. RRL. 5, 376-379 (2011).</li></ol>

特別な利害関係は宣言されません。

Nanomouldingは、任意の機能材料にナノパターンの転送を行うことができます。 図1および図2に、個々の処理工程の比較がnanomouldingとナノインプリントの間の密接な関係を明らかにする。 nanomouldingとナノインプリントの主な違いは、 図2Eに追加の材料堆積ステップです。残りのプロセスの流れは同じです。 Nanomouldingしたがって、利用可能な任意のナノイン?...

ナノパターニングは、ナノテクノロジーと応用科学の多くの分野で多大な重要性を獲得しています。パターン生成は最初の一歩であり、そのような電子ビームリソグラフィまたはナノスフェアリソグラフィまたはブロック共重合体リソグラフィ1などの自己組織化法に基づいたボトムアップアプローチとしてトップダウンアプローチによって達成することができる。パターン生成と同様に重要なのは、パターン複製です。フォトリソグラフィ技術に加えて、ナノインプリント（ 図1）は、低コストの2月4日での高スループットの大面積ナノパターニングに適し特に有望な代替として浮上している。フォトリソグラフィがパターン化されたマスクが必要ですが、ナノインプリントはプレハブマスタ構造に依存しています。マスターからのパターン転写は、一般的に熱可塑性樹脂または紫外線または熱硬化性ポリマーに実行されます。しかしそれは、機能性材料の上に直接パターンを転写することが望ましい場合が多くあります。 &lt;Pクラス= &quot;jove_content&quot;&gt;ここでnanomoulding、我々は最近、文献で ​​導入された層の転送（ 図2）に基づいてレプリケーションを行う手法について述べる。5機能酸化亜鉛電極上にナノスケールのパターンを転写する。ナノインプリントの設定が利用可能であれば私たちのnanomoulding方法は簡単に実装できます。 Nanomouldingは、金型材料は、材料の蒸着プロセス（ES）と互換性があるように選択されていれば、他の多くの機能材料、材料スタックとさえ完全なデバイスに一般化することができる可能性を提供しています。ここでお見せする例として、透明導電性酸化亜鉛（ZnO）の電極nanomouldingは、太陽電池5の光閉じ込めを強化するために、アプリケーションを見つける化学蒸着（CVD）により堆積。

<table border="1"><tbody><tr><td> 試薬の名称 </td><td> 会社 </td><td> カタログ番号 </td><td> コメント（オプション） </td></tr><tr><td>ナノインプリント樹脂</td><td>マイクロレジスト</td><td> Ormostamp </td><td></td></tr><tr><td> （1H、1H、2H、2H-Perfluoroctyl）trichlorsilane、付着防止剤</td><td>シグマアルドリッチ</td><td> 448931-10G </td><td></td></tr><tr><td>スライドガラス</td><td>ショット</td><td> AF32エコ</td><td> 0.5ミリメートル</td></tr><tr><td>ポリエチレンナフタ（PEN）シート</td><td>グッドフェロー</td><td> ES361090 </td><td> 0.125ミリメートル</td></tr><tr><td> （C 2 H 5）2 Znの</td><td>アクゾノーベル</td><td></td><td></td></tr><tr><td> Agは4Nターゲットをスパッタ</td><td>ヘレウス</td><td> 81062165 </td><td></td></tr><tr><td> B 2 H 6は、SiH 4、H 2、B（CH 3）3、PH 3、CH 4、CO 2 </td><td>メッサー</td><td></td><td></td></tr><tr><td></td><td></td><td></td><td> 機器 </td></tr><tr><td>ナノインプリントシステム</td><td>自作</td><td></td><td></td></tr><tr><td> LP-CVD装置</td><td>自作</td><td></td><td></td></tr><tr><td> PVDシステム</td><td>ライボルト</td><td> Univex 450 B </td><td></td></tr><tr><td> PE-CVDリアクタ</td><td> Indeotec </td><td>かわた</td><td></td></tr><tr><td> SEMの</td><td> JEOL </td><td> JSM-7500、TFE </td><td></td></tr><tr><td> AFM </td><td>デジタルインスツルメンツ</td><td>ナノスコープ3100 </td><td></td></tr></tbody></table>

nanomoulding of functional materials, a versatile complementary pattern replication method to nanoimprinting

我々は、機能材料、材料スタックとフルデバイスの低コストのナノスケールのパターニングを可能nanomoulding手法を説明します。層転写と組み合わせるNanomoulding機能性材料へのマスタ構造から任意の表面パターンのレプリケーションが可能になります。 Nanomouldingはどのナノインプリントセットアップで実行することができ、材料や成膜プロセスの広い範囲に適用することができます。特に、我々は、太陽電池の光閉じ込めのアプリケーションにパターニングされた透明な酸化亜鉛電極の作製を実証する。

<html> 図3は nanomoulded構造のいくつかの実例をまとめたものです。ガラス上にCVD法によるZnOのマスタ構造は、（）で表示されます。対応nanomoulded ZnOのレプリカは、（d）に示されています。 AFM像から抽出された地元の高さの比較（g）と角度（j）のヒストグラムはnanomouldingプロセスの高忠実度を明らかにする。同様の結果が干渉リソグラフィ（B、E、H、K）と陽極テクスチャアルミニ?...

Watch this Scientific Journal Video about Nanomoulding of Functional Materials, a Versatile Complementary Pattern Replication Method to Nanoimprinting at JoVE.com

Nanomoulding of Functional Materials, a Versatile Complementary Pattern Replication Method to Nanoimprinting

我々は、機能材料、材料スタックとフルデバイスの低コストのナノスケールのパターニングを可能nanomoulding手法を説明します。 Nanomouldingはどのナノインプリントセットアップで実行することができ、材料や成膜プロセスの広い範囲に適用することができます。

機能材料のNanomoulding、ナノインプリントへ多目的相補パターンレプリケーション方法

We describe a nanomoulding technique which  allows low-cost nanoscale patterning of functional materials, materials stacks  and full devices. Nanomoulding ...

nanomoulding-functional-materials-versatile-complementary-pattern

Universidad San Sebastian

Research

JoVE Journal

Engineering

11.6K ビュー.  Ecole Polytechnique Fédérale de Lausanne (EPFL). 我々は、機能材料、材料スタックとフルデバイスの低コストのナノスケールのパターニングを可能nanomoulding手法を説明します。 Nanomouldingはどのナノインプリントセットアップで実行することができ、材料や成膜プロセスの広い範囲に適用することができます。

ビデオ: Nanomoulding of Functional Materials, a Versatile Complementary Pattern Replication Method to Nanoimprinting

Using Neutron Spin Echo Resolved Grazing Incidence Scattering to Investigate Organic Solar Cell Materials

The spin echo resolved grazing incidence scattering (SERGIS) technique has been used to probe the length-scales associated with irregularly shaped crystallites. Neutrons are passed through two well defined regions of magnetic field; one before and one after the sample. The two magnetic field regions have opposite polarity and are tuned such that neutrons travelling through both regions, without being perturbed, will undergo the same number of precessions in opposing directions. In this case the neutron precession in the second arm is said to &#34;echo&#34; the first, and the original polarization of the beam is preserved. If the neutron interacts with a sample and scatters elastically the path through the second arm is not the same as the first and the original polarization is not recovered. Depolarization of the neutron beam is a highly sensitive probe at very small angles (&#60;50&#160;&#956;rad) but still allows a high intensity, divergent beam to be used. The decrease in polarization of the beam reflected from the sample as compared to that from the reference sample can be directly related to structure within the sample.
In comparison to scattering observed in neutron reflection measurements the SERGIS signals are often weak and are unlikely to be observed if the in-plane structures within the sample under investigation are dilute, disordered, small in size and polydisperse or the neutron scattering contrast is low. Therefore, good results will most likely be obtained using the SERGIS technique if the sample being measured consist of thin films on a flat substrate and contain scattering features that contains a high density of moderately sized features (30 nm to 5 &#181;m) which scatter neutrons strongly or the features are arranged on a lattice. An advantage of the SERGIS technique is that it can probe structures in the plane of the sample.

Progress has been made in utilizing spin echo resolved grazing incidence scattering (SERGIS) as a neutron scattering technique to probe the length-scales in irregular samples. Crystallites of [6,6]-phenyl-C61-butyric acid methyl ester have been probed using the SERGIS technique and the results confirmed by optical and atomic force microscopy.

中性子スピンエコーを使用して放牧発生率散乱を解決し、有機太陽電池材料を調査する

The spin echo resolved grazing incidence scattering (SERGIS) technique has been used to probe the length-scales associated with irregularly shaped ...

工学

Casting Protocols for the Production of Open Cell Aluminum Foams by the Replication Technique and the Effect on Porosity

Metal foams are interesting materials from both a fundamental understanding and practical applications point of view. Uses have been proposed, and in many cases validated experimentally, for light weight or impact energy absorbing structures, as high surface area heat exchangers or electrodes, as implants to the body, and many more. Although great progress has been made in understanding their structure-properties relationships, the large number of different processing techniques, each producing material with different characteristics and structure, means that understanding of the individual effects of all aspects of structure is not complete. The replication process, where molten metal is infiltrated between grains of a removable preform material, allows a markedly high degree of control and has been used to good effect to elucidate some of these relationships. Nevertheless, the process has many steps that are dependent on individual &#8220;know-how&#8221;, and this paper aims to provide a detailed description of all stages of one embodiment of this processing method, using materials and equipment that would be relatively easy to set up in a research environment. The goal of this protocol and its variants is to produce metal foams in an effective and simple way, giving the possibility to tailor the outcome of the samples by modifying certain steps within the process. By following this, open cell aluminum foams with pore sizes of 1&#8211;2.36 mm diameter and 61% to 77% porosity can be obtained.

Replication is one of the processing techniques used for the production of porous metal sponges. In this paper one implementation of the method for the production of open celled porous aluminum is shown in detail.

気孔率に複製技術とエフェクトでオープンセルアルミフォームの製造のためのプロトコルのキャスト

Metal foams are interesting materials from both a fundamental understanding and practical applications point of view. Uses have been proposed, and in many ...

Preparation and Reactivity of Gasless Nanostructured Energetic Materials

High-Energy Ball Milling (HEBM) is a ball milling process where a powder mixture placed in the ball mill is subjected to high-energy collisions from the balls. Among other applications, it is a versatile technique that allows for effective preparation of gasless reactive nanostructured materials with high energy density per volume (Ni+Al, Ta+C, Ti+C). The structural transformations of reactive media, which take place during HEBM, define the reaction mechanism in the produced energetic&#160;composites. Varying the processing conditions permits fine tuning of the milling-induced microstructures of the fabricated composite particles. In turn, the reactivity, i.e., self-ignition temperature, ignition delay time, as well as reaction kinetics, of high energy density materials depends on its microstructure. Analysis of the milling-induced microstructures suggests that the formation of fresh oxygen-free intimate high surface area contacts between the reagents is responsible for the enhancement of their reactivity. This manifests itself in a reduction of ignition temperature and delay time, an increased rate of chemical reaction, and an overall decrease of the effective activation energy of the reaction. The protocol provides a detailed description for the preparation of reactive nanocomposites with tailored microstructure using short-term HEBM method. It also describes a high-speed thermal imaging technique to determine the ignition/combustion characteristics of the energetic materials. The protocol can be adapted to preparation and characterization of a variety of nanostructured energetic composites.

This protocol describes the preparation of gasless nanostructured energetic materials (Ni+Al, Ta+C, Ti+C) using the short-term high-energy ball milling (HEBM) technique. It also describes a high-speed thermal imaging method to study the reactivity of mechanically fabricated nanocomposites. These protocols can be extended to other reactive nanostructured energetic materials.

Gaslessナノエネルギー物質の調製と反応性

High-Energy Ball Milling (HEBM) is a ball milling process where a powder mixture placed in the ball mill is subjected to high-energy collisions from the ...

Energy Dispersive X-ray Tomography for 3D Elemental Mapping of Individual Nanoparticles

Energy dispersive X-ray spectroscopy within the scanning transmission electron microscope (STEM) provides accurate elemental analysis with high spatial resolution, and is even capable of providing atomically resolved elemental maps. In this technique, a highly focused electron beam is incident upon a thin sample and the energy of emitted X-rays is measured in order to determine the atomic species of material within the beam path. This elementally sensitive spectroscopy technique can be extended to three dimensional tomographic imaging by acquiring multiple spectrum images with the sample tilted along an axis perpendicular to the electron beam direction.
Elemental distributions within single nanoparticles are often important for determining their optical, catalytic and magnetic properties. Techniques such as X-ray tomography and slice and view energy dispersive X-ray mapping in the scanning electron microscope provide elementally sensitive three dimensional imaging but are typically limited to spatial resolutions of &gt; 20 nm. Atom probe tomography provides near atomic resolution but preparing nanoparticle samples for atom probe analysis is often challenging. Thus, elementally sensitive techniques applied within the scanning transmission electron microscope are uniquely placed to study elemental distributions within nanoparticles of dimensions 10-100 nm.
Here, energy dispersive X-ray (EDX) spectroscopy within the STEM is applied to investigate the distribution of elements in single AgAu nanoparticles. The surface segregation of both Ag and Au, at different nanoparticle compositions, has been observed.

The use of energy dispersive X-ray tomography in the scanning transmission electron microscope to characterize elemental distributions within single nanoparticles in three dimensions is described.

個々のナノ粒子の3次元元素マッピングのためのエネルギー分散型X線トモグラフィー

Energy dispersive X-ray spectroscopy within the scanning transmission electron microscope (STEM) provides accurate elemental analysis with high spatial ...

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 ...

Standardized Method for Measuring Collection Efficiency from Wipe-sampling of Trace Explosives

One of the limiting steps to detecting traces of explosives at screening venues is effective collection of the sample. Wipe-sampling is the most common procedure for collecting traces of explosives, and standardized measurements of collection efficiency are needed to evaluate and optimize sampling protocols. The approach described here is designed to provide this measurement infrastructure, and controls most of the factors known to be relevant to wipe-sampling. Three critical factors (the applied force, travel distance, and travel speed) are controlled using an automated device. Test surfaces are chosen based on similarity to the screening environment, and the wipes can be made from any material considered for use in wipe-sampling. Particle samples of the explosive 1,3,5-trinitroperhydro-1,3,5-triazine (RDX) are applied in a fixed location on the surface using a dry-transfer technique. The particle samples, recently developed to simulate residues made after handling explosives, are produced by inkjet printing of RDX solutions onto polytetrafluoroethylene (PTFE) substrates. Collection efficiency is measured by extracting collected explosive from the wipe, and then related to critical sampling factors and the selection of wipe material and test surface. These measurements are meant to guide the development of sampling protocols at screening venues, where speed and throughput are primary considerations.

Optimized sampling protocols and the development of new wipe materials can be facilitated by standardized measurements of collection efficiency from wipe-sampling. Our approach for sampling trace explosives uses an automated device to control speed, force, and distance during wipe-sampling followed by extraction of collected explosives.

トレース爆発物のワイプサンプリングから収集効率を測定するための標準化された方法

One of the limiting steps to detecting traces of explosives at screening venues is effective collection of the sample. Wipe-sampling is the most common ...

A Novel Method for In Situ Electromechanical Characterization of Nanoscale Specimens

Electrically assisted deformation (EAD) is increasingly being used to improve the formability of metals during processes such as sheet metal rolling and forging. Adoption of this technique is proceeding despite disagreement concerning the underlying mechanism responsible for EAD. The experimental procedure described herein enables a more explicit study compared to previous EAD research by removing thermal effects, which are responsible for disagreement in interpreting previous EAD results. Furthermore, as the procedure described here enables EAD observation in situ and in real time in a transmission electron microscope (TEM), it is superior to existing post-mortem methods that observe EAD effects post-test. Test samples consist of a single crystal copper (SCC) foil having a free-standing tensile test section of nanoscale thickness, fabricated using a combination of laser and ion beam milling. The SCC is mounted to an etched silicon base that provides mechanical support and electrical isolation while serving as a heat sink. Using this geometry, even at high current density (~3,500 A/mm2), the test section experiences a negligible temperature increase (&#60;0.02 &#176;C), thus eliminating Joule heating effects. Monitoring material deformation and identifying the corresponding changes to microstructures, e.g. dislocations, are accomplished by acquiring and analyzing a series of TEM images. Our sample preparation and in situ experiment procedures are robust and versatile as they can be readily utilized to test materials with different microstructures, e.g., single and polycrystalline copper.

A Novel Method for In Situ Electromechanical Characterization of Nanoscale Specimens

Isolating electrical and thermal effects on electrically assisted deformation (EAD) is very difficult using macroscopic samples. Metallic sample micro- and nanostructures together with a custom test procedure have been developed to evaluate the impact of applied current on the formation without joule heating and evolution of dislocations on these samples.

のための新しい方法<em&gt;現場で</em&gt;ナノスケール試料の電気機械的特性

Electrically assisted deformation (EAD) is increasingly being used to improve the formability of metals during processes such as sheet metal rolling and ...

A Fabrication and Measurement Method for a Flexible Ferroelectric Element Based on Van Der Waals Heteroepitaxy

Flexible non-volatile memories have received much attention as they are applicable for portable smart electronic device in the future, relying on high-density data storage and low-power consumption capabilities. However, the high-quality oxide based nonvolatile memory on flexible substrates is often constrained by the material characteristics and the inevitable high-temperature fabrication process. In this paper, a protocol is proposed to directly grow an epitaxial yet flexible lead zirconium titanate memory element on muscovite mica. The versatile deposition technique and measurement method enable the fabrication of flexible yet single-crystalline non-volatile memory elements necessary for the next generation of smart devices.

In this paper, we present a protocol to directly grow an epitaxial yet flexible lead zirconium titanate memory element on muscovite mica.

作製と Van Der waals 力ヘテロエピタキシーに基づくフレキシブル強誘電性要素の測定法

Flexible non-volatile memories have received much attention as they are applicable for portable smart electronic device in the future, relying on ...

Multiscale Structures Aggregated by Imprinted Nanofibers for Functional Surfaces

Multiscale surface structures have attracted increasing interest owing to several potential applications in surface devices. However, an existing challenge in the field is the fabrication of hybrid micro-nano structures using a facile, cost-effective, and high-throughput method. To overcome these challenges, this paper proposes a protocol to fabricate multiscale structures using only an imprint process with an anodic aluminum oxide (AAO) filter and an evaporative self-aggregation process of nanofibers. Unlike previous attempts that have aimed to straighten nanofibers, we demonstrate a unique fabrication method for multiscale aggregated nanofibers with high aspect ratios. Furthermore, the surface morphology and wettability of these structures on various liquids were investigated to facilitate their use in multifunctional surfaces.

Presented is an easy method to fabricate nano-micro multiscale structures, for functional surfaces, by aggregating nanofibers fabricated using an anodic aluminum oxide filter.

マルチ スケール構造機能表面の刻印ナノファイバーによる集計

Multiscale surface structures have attracted increasing interest owing to several potential applications in surface devices. However, an existing ...

Studying Large Amplitude Oscillatory Shear Response of Soft Materials

We investigate the sequence of physical processes exhibited during large amplitude oscillatory shearing (LAOS) of polyethylene oxide (PEO) in dimethyl sulfoxide (DMSO) and xanthan gum in water &#8212; two concentrated polymer solutions used as viscosifiers in foods, enhanced oil recovery, and soil remediation. Understanding the nonlinear rheological behavior of soft materials is important in the design and controlled manufacturing of many consumer products. It is shown how the response to LAOS of these polymer solutions can be interpreted in terms of a clear transition from linear viscoelasticity to viscoplastic deformation and back again during a period. The LAOS results are analyzed via the fully quantitative Sequence of Physical Processes (SPP) technique, using free MATLAB-based software. A detailed protocol of performing a LAOS measurement with a commercial rheometer, analyzing nonlinear stress responses with the freeware, and interpreting physical processes under LAOS is presented. It is further shown that, within the SPP framework, a LAOS response contains information regarding the linear viscoelasticity, the transient flow curves, and the critical strain responsible for the onset of nonlinearity.

We present a detailed protocol outlining how to perform nonlinear oscillatory shear rheology on soft materials, and how to run the SPP-LAOS analysis to understand the responses as a sequence of physical processes.

ソフトマテリアルの大振幅振動せん断応答を勉強

We investigate the sequence of physical processes exhibited during large amplitude oscillatory shearing (LAOS) of polyethylene oxide (PEO) in dimethyl ...