作者は感謝してLabex-Imustによって財政支援を認める。

1。生物試料の調製 この研究で説明されているすべての実験はCECCAPP（リヨン、フランス）（承認番号のLYONSUD_2012_004）の動物実験委員会によって承認された、そして実験が許可された個人（L. Sancey、DDPP承認番号の監督の下で実施した38 05 32）。 <ol><li> 、ガドリニウム（Gd）系ナノ粒子の100マイクロモルに、H 2 Oを1ミリリットルを追加し、15分待ってから、H 2 Oを100μLと80μlに、HEPES 5020μlのmMの、塩化ナトリウム1.325 M、 塩化カルシウム20ミリ追加のGd系ナノ粒子の一次溶液をすぐに注入を40mM（：ヴィルール、実験室での市）で200μlの溶液を得た。 </li><li>静脈麻酔し、腫瘍を有するげっ歯類（：リヨンシュッド（ウラン）、研究室から15キロ市）に200μLのGd系ナノ粒子液を注入する。 </li><li> 1月24日時間注射後、マウスを犠牲に液体窒素で冷却したイソペンタンへの生物学的サンプルを入れてDをサンプルで保存 - 80℃（市：リヨンシュッド（ウラン）、研究室から15キロ）。 </li><li>サンプルスライス（市：通常グルノーブル、研究室から100キロを、私はリヨンシュッドでのアクセスを持つようにしようとします）厚さ100μmのスライドで、特定のプラスチック皿（シャーレ）に生物学的なスライドを置く。 -80℃で保存 注意：プラスチック皿、基本的には非常に純粋なポリマーサンプルです。これらは、組織に含まれる要素との干渉を回避するために使用される。 </li></ol> キャリブレーションのための2。サンプル調製 <ol><li> （0 nMで、100nmであり、500nmであり、1μM、5μM、10μM、50、100μM、500μMの、1 mmであり、5 mM）を水の中にGdをベースナノ粒子の投与量の増加に伴って、バイアルを準備します。 </li><li>定期的にペトリ皿に3ミリメートルだけ離れた各溶液5μLドロップを置く。 </li><li> 20分間室温で乾燥した。 </li></ol>3。LIBS実験<ol><li> LIBSの設定​​を初期化する<ol><li>レーザー設定。楽器を切り替えた後、レーザパルスエネルギーの安定化のために10〜20分待ってから-20℃にICCDカメラの上下冷却アッテネータとパルスエネルギーを調整します。 注：マッピング組織に対する最適なレーザパラメータは、5ナノ秒のパルス持続時間、波長1064nm、及び約4ミリジュールのパルスエネルギーである。レーザー使用する典型的なのNdです：YAGレーザーナノ秒レーザー。 </li><li> LIBS設定。小さいクレーター径（約50μm以下）を得るために（試料表面に対する）レーザー焦点位置を設定します。 注意：これは100μmの試料表面下のレーザパルスカリゼーションに対応しています。 </li><li>分光器の設定。 1200本/ mm回折格子と高時間分解能ICCDカメラと組み合わせたツェルニーターナー分光計を使用してください。コンピュータですべてのこれらのデバイスを制御します。 40μmの入射スリット値を設定します。スペクトル範囲の再設定解析対象となる要素をゴルディング。スペクトルを高感度でのGdを検出するために、325から355 nmの範囲をカバーするだけでなく、ナトリウム、CuおよびCAを使用。 300ナノ秒の遅延、2秒のゲート、および200のゲインとICCDのパラメータを設定します。 </li></ol></li><li>マッピング測定<ol><li> LIBS電動試料ホルダーに生物学的サンプルを置きます。 </li><li>レーザーの焦点位置に応じて、試料の高さを調整します。 </li><li>サンプルスライスの高解像度の写真を撮る。 </li><li>約100μmの解像度を隔て、通常100×100の測定点でマップを実行するために、LIBS取得ソフトウェアのマッピングモジュールを設定します。 </li><li>取得を開始します。この時点からすべてを自動化する。配列ならびにスペクトル記録を移動して保存する。 40分間、10,000点（100μmの解決のために1cm 2の等価）のマッピングのために必要とされる。同じファイルに記録されたすべてのスペクトルを再編成する。 </li><li>場合には、Finished、サンプルスライスの2枚目の写真を撮る</li></ol></li><li>キャリブレーション測定</li></ol>同じ実験パラメータを用いて、（、調製の詳細はセクション2を参照）キャリブレーションサンプルを測定する。マップを実行するか、または較正液滴の各々に（ドロップの中央部の測定部位から得られた）25のスペクトルを記録する。 4 LIBSスペクトル解析：化学·イメージの構築 <ol><li>レコードのすべてのLIBS組織マッピングからのスペクトルとLIBSのソフトウェア解析でそれらをロードします。各スペクトルのベースラインを引き、偽色を使用して、相対強度スケールとの化学的画像を構築する。 注意：このアルゴリズムは、Gdの、銅、ナトリウム、またはCaなどの特定のライン強度を取得します。 </li><li>検量線の計算（強度と濃度との関係）を許可し、水溶液を構築するために校正されたサンプルから測定されたスペクトルに同じ操作を実行uantitativeマップや画像のGd（または関心のある他の要素）。 </li><li>このような補間やスムージングなどの化学画像に適切な治療法を適用します。画像フォーマット（ビットマップ）での強度や濃度マップを保存します。 </li></ol>

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著者らは、開示することは何もありません。

生物学的サンプルに適用され、この技術は、異なる器官内に注射のGd系ナノ粒子からのGdとSiのマッピングと定量化、 すなわち 、化学イメージングを可能にする。主な重要な設定から、レーザ特性（波長、パルスエネルギー、フォーカス、および安定性）の制御が正確かつ細かい組織切除（ すなわちマッピング分解能）のためだけでなく、感度のために重要である。高エネルギ?...

生物学的用途のためのナノ粒子の広い開発は、生物学的サンプルでの定量化や画像化のための分析技術の並列改善を促した。通常、臓器中のナノ粒子の検出およびマッピングは、蛍光または共焦点顕微鏡法によって作製される。残念ながら、これらの方法は、特にその疎水性のために、非常に小さいナノ粒子、ナノ粒子の生体内分布を変更することができ、近赤外色素によるナノ粒子のラベル付けを必要とする。ラベルされたナノ粒子の検出、および特に非常に小さいナノ粒子（サイズ&lt;10 nm）は、このように全身の規模ではなく、組織および細胞レベルでその生体内分布を妨害する可能性があります。任意のラベルなしでナノ粒子を検出することができ、新しいデバイスの開発は、彼らの行動や反応速度の研究のための新たな可能性を提供しています。さらに、脳内の鉄や銅などの微量元素の役割は、傷病アルツハイマー1、メンケス2,3、またはウィルソン4などのDの神経変性疾患は、組織におけるこれらの要素を研究し、ローカライズするために興味をお勧めします。 様々な技術が、異なる材料の元素マッピング又は微量分析を提供するために使用されてきた。 2006年に公開された彼らのレビュー論文では、R. Lobinski らは、生物学的環境、分析科学5のための最も挑戦的な環境の一つでの微量元素分析のために利用可能な標準的な技術の概要を説明しました。元素濃度が十分であれば、透過型電子顕微鏡におけるエネルギー分散型X線マイクロアナリシスから成り電子マイクロプローブが、多数の研究に適用することができる（&gt; 100〜1,000μgの/ g）であった。検出下限に到達するために、以下の技術が使用されている。 <ul><li>用いたイオンビームマイクロ粒子励起X線発光μ-PIXE（1月10日μgの/ g）を6 </li><li> SYNchrotron放射微量分析μ-SXRF（0.1〜1μgの/ g）を7 </li><li>二次イオン質量分析法（SIMS 0.1μgの/ g）を8 </li><li> （/ gの0.01μgのまで）レーザーアブレーション誘導結合質量分析、LA-ICP-MS 9,10 </li></ul> Lobinski らから抽出された表1に示すように、上記の技術は、マイクロメートル分解能を提供する。 シリアル2D調査の3次元再構成も深部組織11の再構築のために提案することができた。しかし、すべてのデバイスとシステムが両方の高い高価な機器への適度な有資格の専門家、および長期的な実験（μ-SXRF用×100〜100μmでとLA-ICP-MS用のX 10ミリメートル10ミリメートルのため、通常以上の4時間を必要とする）12。要するに、これらの要件は、微量元素分析が非常に制限し、従来の光学イメージングシステムとの互換性が確認蛍光顕微鏡や非線形顕微鏡。ここで言及することができますもう一つのポイントは、定量的な測定能力はまだかなり限られており、マトリックスマッチング実験室の規格の利用可能性に依存することである。さらに、業界プロセスにおける微量元素分析の利用の一般化、地質学、生物学、アプリケーションの他のドメインは、重要な概念や技術革新を生成します。 現在の原稿の目的は、従来の光学顕微鏡と完全な互換性を卓上計測機器との生物学的組織における定量元素マッピング（または微量元素分析）のためのソリューションを提案することである。我々のアプローチは、レーザー誘起ブレークダウン分光法（LIBS技術）に基づいています。 LIBSに、レーザーパルスは、材料の破壊や火花を作成するために、対象サンプルに焦点を当てています。血漿中に放出された原子放射線は、その後、分光計とエレメンによって解析されているTAL濃度は13,14予め行わ較正測定で取得できます。 LIBSの利点は、感度（μgの/ gで、ほぼすべての要素）、コンパクト、非常に基本的なサンプル調製、試料との接触がない場合、瞬時の応答と正確にローカライズされた（マイクロ）表面分析が含まれています。組織のレーザアブレーションは、微細に一緒μgの/ gの範囲15,16内の感度で高空間分解能でマッピングを行うように制御しなければならないので、組織化学的画像化の適用は困難なままである。 このようなソリューションでは、トレーサーまたは標識剤の付加は、生物学的組織におけるそれらのネイティブ環境で直接無機元素を検出することを可能にする、必要とされていません。我々の研究室で開発されたLIBS機器が可能に0.1 mMの16に相当35μgの/ g未満のGdの推定感度が100μmよりも劣っ現在の解像度を提供しています大規模なサンプルのマッピング（&gt; 1 cm 2）を 30分以内。また、自家製のソフトウェアは、データの取得や活用を促進します。この器具は、（Gdの）マップを検出し、およびガドリニウムの組織分布を定量化するために使用される系ナノ粒子17 -小動物から腎臓および腫瘍サンプル18 1〜24時間の粒子の静脈内注射（サイズ&lt;5 nm）の後に。例えば、鉄、カルシウム、ナトリウム、及びPのような本質的に、生体組織に含まれる無機元素は、、、も検出し、画像化されている。

<table border="0" cellpadding="0" cellspacing="0" width="747">
	<colgroup>
		<col />
		<col />
		<col />
		<col />
	</colgroup>
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Laser nanosecond Nd:YAG</td>
			<td style="width:129px;">Quantel</td>
			<td style="width:119px;">Brillant</td>
			<td style="width:283px;">5ns pulse witdh, wavelength 1064 nm</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Spectrometer</td>
			<td>Andor Technology</td>
			<td>Shamrock 303</td>
			<td>with 1200 l/mm blazed at 300 nm grating</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Detector ICCD</td>
			<td>Andor Technology</td>
			<td style="width:119px;">Istar</td>
			<td>2 ns temporal resolution</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">LIBS Unit</td>
			<td style="width:129px;">ILM</td>
			<td style="width:119px;"></td>
			<td>Homemade Instrumentation</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;"></td>
			<td style="width:129px;"></td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Gd-based nanoparticles</td>
			<td style="width:129px;">Nano-H</td>
			<td style="width:119px;"></td>
			<td>particles</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">HEPES</td>
			<td style="width:129px;">Sigma-Aldrich</td>
			<td style="width:119px;">H4034</td>
			<td>for particle&#39;s dilution</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">CaCl2</td>
			<td style="width:129px;">Sigma-Aldrich</td>
			<td style="width:119px;">21108</td>
			<td>for particle&#39;s dilution</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">NaCl</td>
			<td style="width:129px;">Sigma-Aldrich</td>
			<td style="width:119px;">S5886</td>
			<td>for particle&#39;s dilution</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">mice</td>
			<td style="width:129px;">Charles River</td>
			<td style="width:119px;">depending of animal breeding</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">isoflurane</td>
			<td style="width:129px;">Coveto / Virbac</td>
			<td style="width:119px;"></td>
			<td>for anaesthesia - Isofluranum</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">isopentane</td>
			<td style="width:129px;">Sigma-Aldrich</td>
			<td style="width:119px;">59060</td>
			<td>to froze the sample&#160; slowly</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">liquide nitrogen</td>
			<td style="width:129px;">Air Liquide</td>
			<td style="width:119px;"></td>
			<td>to cool down the isopentane</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">cryostat</td>
			<td style="width:129px;">Leica</td>
			<td style="width:119px;">CM-3050S</td>
			<td>to slide the samples</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">petri dishes</td>
			<td style="width:129px;">Dutscher</td>
			<td style="width:119px;">353004</td>
			<td>to stick the sample</td>
		</tr>
	</tbody>
</table>

laser-induced breakdown spectroscopy: a new approach for nanoparticle's mapping and quantification in organ tissue

レーザ誘起プラズマの発光分光法は、生体試料の元素分析に適用した。レーザ誘起ブレークダウン分光法（LIBS）げっ歯類組織の薄切片上で行わ：、腎臓および腫瘍例えば、（i）のNa、Ca、CuやMgの、P、及びFe等の無機元素の検出を可能にする、体内に自然に存在し（II）SiとGdが、ガドリニウム系ナノ粒子の注入後に検出。動物は、粒子の静脈内注射後1〜24時間後に安楽死させた。試料の二次元走査が、赤外レーザ光 ​​が横解像度が100未満μmは表面を探索させ、電動マイクロメートル3Dステージを用いて行わ。臓器内部のGd元素の定量化学画像は、サブmMの感度が得られた。 LIBSは、特定のlabeliなしに無機材料の分布を研究するためのシンプルかつ堅牢な方法を提供していますNG。 、元素、分子、または細胞：さらに、標準的な光学顕微鏡法を使用してセットアップの適合性は、応答の異なる種類の同じ生物学的組織の複数の画像を提供するためのその可能性を強調している。

図1に示すように、Ndをビームが：1064nmの基本波長でのYAGレーザは50ミリメートルの焦点距離の石英レンズにより組織切片上に垂直に集中していた。パルスエネルギーは4ミリジュール及び繰返し率10Hzであった。空気中でプラズマの発生を回避するために、レーザビームが試料の表面下100μmの周りに集中していた。空気プラズマは、この状態で観察されなかった。実験の間、サンプ...

Watch this Scientific Journal Video about Laser-induced Breakdown Spectroscopy: A New Approach for Nanoparticle's Mapping and Quantification in Organ Tissue at JoVE.com

Laser-induced Breakdown Spectroscopy: A New Approach for Nanoparticle&#039;s Mapping and Quantification in Organ Tissue

薄い臓器や腫瘍組織で実行レーザー誘起ブレークダウン分光法は、成功したGd系ナノ粒子から発行された自然の要素と人工的に注入されたガドリニウム（Gd）を検出しました。化学元素の画像が100μmであり、定量的なサブミリ感度の解像度に達した。標準的な光学顕微鏡法を使用してセットアップの相溶性が同じ生物学的組織の複数の画像を提供するためのその可能性を強調している。

レーザー誘起ブレークダウン分光法：臓器組織内のナノ粒子のマッピングと定量化のための新たなアプローチ

Emission spectroscopy of laser-induced plasma was applied to elemental analysis of biological samples. Laser-induced breakdown spectroscopy (LIBS) ...

laser-induced-breakdown-spectroscopy-new-approach-for-nanoparticle-s

Research

JoVE Journal

Engineering

Laser-induced Breakdown Spectroscopy: A New Approach for Nanoparticle's Mapping and Quantification in Organ Tissue

13.6K ビュー.  CNRS - Université Lyon 1. 薄い臓器や腫瘍組織で実行レーザー誘起ブレークダウン分光法は、成功したGd系ナノ粒子から発行された自然の要素と人工的に注入されたガドリニウム（Gd）を検出しました。化学元素の画像が100μmであり、定量的なサブミリ感度の解像度に達した。標準的な光学顕微鏡法を使用してセットアップの相溶性が同じ生物学的組織の複数の画像を提供するため?...

ビデオ: Laser-induced Breakdown Spectroscopy: A New Approach for Nanoparticle's Mapping and Quantification in Organ Tissue

Angle-resolved Photoemission Spectroscopy At Ultra-low Temperatures

The physical properties of a material are defined by its electronic structure. Electrons in solids are characterized by energy (&omega;) and momentum (k) and the probability to find them in a particular state with given &omega; and k is described by the spectral function A(k, &omega;). This function can be directly measured in an experiment based on the well-known photoelectric effect, for the explanation of which Albert Einstein received the Nobel Prize back in 1921. In the photoelectric effect the light shone on a surface ejects electrons from the material. According to Einstein, energy conservation allows one to determine the energy of an electron inside the sample, provided the energy of the light photon and kinetic energy of the outgoing photoelectron are known. Momentum conservation makes it also possible to estimate k relating it to the momentum of the photoelectron by measuring the angle at which the photoelectron left the surface. The modern version of this technique is called Angle-Resolved Photoemission Spectroscopy (ARPES) and exploits both conservation laws in order to determine the electronic structure, i.e. energy and momentum of electrons inside the solid. In order to resolve the details crucial for understanding the topical problems of condensed matter physics, three quantities need to be minimized: uncertainty* in photon energy, uncertainty in kinetic energy of photoelectrons and temperature of the sample.
In our approach we combine three recent achievements in the field of synchrotron radiation, surface science and cryogenics. We use synchrotron radiation with tunable photon energy contributing an uncertainty of the order of 1 meV, an electron energy analyzer which detects the kinetic energies with a precision of the order of 1 meV and a He3 cryostat which allows us to keep the temperature of the sample below 1 K. We discuss the exemplary results obtained on single crystals of Sr2RuO4 and some other materials. The electronic structure of this material can be determined with an unprecedented clarity.

The overall goal of this method is to determine the low-energy electronic structure of solids at ultra-low temperatures using Angle-Resolved Photoemission Spectroscopy with synchrotron radiation.

超低温での角度分解光電子分光

The physical properties of a material are defined by its  electronic structure. Electrons in solids are characterized by energy (&omega;)  and momentum ...

工学

Probing and Mapping Electrode Surfaces in Solid Oxide Fuel Cells

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

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

固体酸化物形燃料電池の電極表面をプロービングとマッピング

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

Scanning-probe Single-electron Capacitance Spectroscopy

The integration of low-temperature scanning-probe techniques and single-electron capacitance spectroscopy represents a powerful tool to study the electronic quantum structure of small systems - including individual atomic dopants in semiconductors. Here we present a capacitance-based method, known as Subsurface Charge Accumulation (SCA) imaging, which is capable of resolving single-electron charging while achieving sufficient spatial resolution to image individual atomic dopants. The use of a capacitance technique enables observation of subsurface features, such as dopants buried many nanometers beneath the surface of a semiconductor material1,2,3. In principle, this technique can be applied to any system to resolve electron motion below an insulating surface.
As in other electric-field-sensitive scanned-probe techniques4, the lateral spatial resolution of the measurement depends in part on the radius of curvature of the probe tip. Using tips with a small radius of curvature can enable spatial resolution of a few tens of nanometers. This fine spatial resolution allows investigations of small numbers (down to one) of subsurface dopants1,2. The charge resolution depends greatly on the sensitivity of the charge detection circuitry; using high electron mobility transistors (HEMT) in such circuits at cryogenic temperatures enables a sensitivity of approximately 0.01 electrons/Hz&frac12; at 0.3 K 5.

Scanning-probe single-electron capacitance spectroscopy facilitates the study of single-electron motion in localized subsurface regions. A sensitive charge-detection circuit is incorporated into a cryogenic scanning probe microscope to investigate small systems of dopant atoms beneath the surface of semiconductor samples.

走査プローブ単電子容量分光

The integration of low-temperature scanning-probe techniques and single-electron capacitance spectroscopy represents a powerful tool to study the ...

Measurement and Analysis of Atomic Hydrogen and Diatomic Molecular AlO, C2, CN, and TiO Spectra Following Laser-induced Optical Breakdown

In this work, we present time-resolved measurements of atomic and diatomic spectra following laser-induced optical breakdown. A typical LIBS arrangement is used. Here we operate a Nd:YAG laser at a frequency of 10 Hz at the fundamental wavelength of 1,064 nm. The 14 nsec pulses with anenergy of 190 mJ/pulse are focused to a 50 &#181;m spot size to generate a plasma from optical breakdown or laser ablation in air. The microplasma is imaged onto the entrance slit of a 0.6 m spectrometer, and spectra are recorded using an 1,800 grooves/mm grating an intensified linear diode array and optical multichannel analyzer (OMA) or an ICCD. Of interest are Stark-broadened atomic lines of the hydrogen Balmer series to infer electron density. We also elaborate on temperature measurements from diatomic emission spectra of aluminum monoxide (AlO), carbon (C2), cyanogen (CN), and titanium monoxide (TiO).
The experimental procedures include wavelength and sensitivity calibrations. Analysis of the recorded molecular spectra is accomplished by the fitting of data with tabulated line strengths. Furthermore, Monte-Carlo type simulations are performed to estimate the error margins. Time-resolved measurements are essential for the transient plasma commonly encountered in LIBS.

Measurement and Analysis of Atomic Hydrogen and Diatomic Molecular AlO, C2, CN, and TiO Spectra Following Laser-induced Optical Breakdown

Time-resolved atomic and diatomic molecular species are measured using LIBS. The spectra are collected at various time delays following the generation of optical breakdown plasma with Nd:YAG laser radiation&#160;and are analyzed to infer electron density and temperature.

測定と原子状水素と二原子分子のAlO、Cの分析<sub&gt; 2</sub&gt;、CN、およびTiOスペクトラ[次のレーザー誘起光学破壊

In this work, we present time-resolved measurements of atomic and diatomic spectra following laser-induced optical breakdown. A typical LIBS arrangement ...

Proton Transfer and Protein Conformation Dynamics in Photosensitive Proteins by Time-resolved Step-scan Fourier-transform Infrared Spectroscopy

Monitoring the dynamics of protonation and protein backbone conformation changes during the function of a protein is an essential step towards understanding its mechanism. Protonation and conformational changes affect the vibration pattern of amino acid side chains and of the peptide bond, respectively, both of which can be probed by infrared (IR) difference spectroscopy. For proteins whose function can be repetitively and reproducibly triggered by light, it is possible to obtain infrared difference spectra with (sub)microsecond resolution over a broad spectral range using the step-scan Fourier transform infrared technique. With ~102-103 repetitions of the photoreaction, the minimum number to complete a scan at reasonable spectral resolution and bandwidth, the noise level in the absorption difference spectra can be as low as ~10-4, sufficient to follow the kinetics of protonation changes from a single amino acid. Lower noise levels can be accomplished by more data averaging and/or mathematical processing. The amount of protein required for optimal results is between 5-100 &#181;g, depending on the sampling technique used. Regarding additional requirements, the protein needs to be first concentrated in a low ionic strength buffer and then dried to form a film. The protein film is hydrated prior to the experiment, either with little droplets of water or under controlled atmospheric humidity. The attained hydration level (g of water / g of protein) is gauged from an IR absorption spectrum. To showcase the technique, we studied the photocycle of the light-driven proton-pump bacteriorhodopsin in its native purple membrane environment, and of the light-gated ion channel channelrhodopsin-2 solubilized in detergent.

Key steps of protein function, in particular backbone conformational changes and proton transfer reactions, often take place in the microsecond to millisecond time scale. These dynamical processes can be studied by time-resolved step-scan Fourier-transform infrared spectroscopy, in particular for proteins whose function is triggered by light.

感光性タンパク質中のプロトン移動とプロテイン立体配座ダイナミクスの時間分解ステップスキャンフーリエ変換赤外分光法により

Monitoring the dynamics of protonation and protein backbone conformation changes during the function of a protein is an essential step towards ...

In Situ Time-dependent Dielectric Breakdown in the Transmission Electron Microscope: A Possibility to Understand the Failure Mechanism in Microelectronic Devices

The time-dependent dielectric breakdown (TDDB) in on-chip interconnect stacks is one of the most critical failure mechanisms for microelectronic devices. The aggressive scaling of feature sizes, both on devices and interconnects, leads to serious challenges to ensure the required product reliability. Standard reliability tests and post-mortem failure analysis provide only limited information about the physics of failure mechanisms and degradation kinetics. Therefore it is necessary to develop new experimental approaches and procedures to study the TDDB failure mechanisms and degradation kinetics in particular. In this paper, an in situ experimental methodology in the transmission electron microscope (TEM) is demonstrated to investigate the TDDB degradation and failure mechanisms in Cu/ULK interconnect stacks. High quality imaging and chemical analysis are used to study the kinetic process. The in situ electrical test is integrated into the TEM to provide an elevated electrical field to the dielectrics. Electron tomography is utilized to characterize the directed Cu diffusion in the insulating dielectrics. This experimental procedure opens a possibility to study the failure mechanism in interconnect stacks of microelectronic products, and it could also be extended to other structures in active devices.

In Situ Time-dependent Dielectric Breakdown in the Transmission Electron Microscope: A Possibility to Understand the Failure Mechanism in Microelectronic Devices

The time-dependent dielectric breakdown (TDDB) in on-chip interconnect stacks is one of the most critical failure mechanisms for microelectronic devices. This paper demonstrates the procedure of an in situ TDDB experiment in the transmission electron microscope, which opens a possibility to study the failure mechanism in microelectronic products.

その場での透過型電子顕微鏡での時間依存絶縁破壊：マイクロエレクトロニクスデバイスの故障メカニズムを理解することが可能

The time-dependent dielectric breakdown (TDDB) in on-chip interconnect stacks is one of the most critical failure mechanisms for microelectronic devices. ...

Laser-induced Forward Transfer for Flip-chip Packaging of Single Dies

Flip-chip (FC) packaging is a key technology for realizing high performance, ultra-miniaturized and high-density circuits in the micro-electronics industry. In this technique the chip and/or the substrate is bumped and the two are bonded via these conductive bumps. Many bumping techniques have been developed and intensively investigated since the introduction of the FC technology in 19601 such as stencil printing, stud bumping, evaporation and electroless/electroplating2. Despite the progress that these methods have made they all suffer from one or more than one drawbacks that need to be addressed such as cost, complex processing steps, high processing temperatures, manufacturing time and most importantly the lack of flexibility. In this paper, we demonstrate a simple and cost-effective laser-based bump forming technique known as Laser-induced Forward Transfer (LIFT)3. Using the LIFT technique a wide range of bump materials can be printed in a single-step with great flexibility, high speed and accuracy at RT. In addition, LIFT enables the bumping and bonding down to chip-scale, which is critical for fabricating ultra-miniature circuitry.

We demonstrate the use of the Laser-induced Forward Transfer (LIFT) technique for flip-chip assembly of optoelectronic components. This approach provides a simple, cost-effective, low-temperature, fast and flexible solution for fine-pitch bumping and bonding on chip-scale for achieving high-density circuits for optoelectronic applications.

シングルダイのフリップチップ実装用のレーザー誘起フォワード転送

Flip-chip (FC) packaging is a key technology for realizing high performance, ultra-miniaturized and high-density circuits in the micro-electronics ...

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 ...

Detection and Recovery of Palladium, Gold and Cobalt Metals from the Urban Mine Using Novel Sensors/Adsorbents Designated with Nanoscale Wagon-wheel-shaped Pores

Developing low-cost, efficient processes for recovering and recycling palladium, gold and cobalt metals from urban mine remains a significant challenge in industrialized countries. Here, the development of optical mesosensors/adsorbents (MSAs) for efficient recognition and selective recovery of Pd(II), Au(III), and Co(II) from urban mine was achieved. A simple, general method for preparing MSAs based on using high-order mesoporous monolithic scaffolds was described. Hierarchical cubic Ia3d wagon-wheel-shaped MSAs were fabricated by anchoring chelating agents (colorants) into three-dimensional pores and micrometric particle surfaces of the mesoporous monolithic scaffolds. Findings show, for the first time, evidence of controlled optical recognition of Pd(II), Au(III), and Co(II) ions and a highly selective system for recovery of Pd(II) ions (up to ~95%) in ores and industrial wastes. Furthermore, the controlled assessment processes described herein involve evaluation of intrinsic properties (e.g., visual signal change, long-term stability, adsorption efficiency, extraordinary sensitivity, selectivity, and reusability); thus, expensive, sophisticated instruments are not required. Results show evidence that MSAs will attract worldwide attention as a promising technological means of recovering and recycling palladium, gold and cobalt metals.

Because of the importance and extensive use of palladium, gold and cobalt metals in high-technology equipment, their recovery and recycling constitute an important industrial challenge. The metal recovery system described herein is a simple, low-cost means for the effective detection, removal, and recovery of these metals from the urban mine.

検出とパラジウムの回収は、都市鉱山からの金やコバルト金属は、ナノスケールワゴンホイール形の細孔を有する指定小説センサ/吸着剤を使用しました

Developing low-cost, efficient processes for recovering and recycling palladium, gold and cobalt metals from urban mine remains a significant challenge in ...

Blast Quantification Using Hopkinson Pressure Bars

Near-field blast load measurement presents an issue to many sensor types as they must endure very aggressive environments and be able to measure pressures up to many hundreds of megapascals. In this respect the simplicity of the Hopkinson pressure bar has a major advantage in that while the measurement end of the Hopkinson bar can endure and be exposed to harsh conditions, the strain gauge mounted to the bar can be affixed some distance away. This allows protective housings to be utilized which protect the strain gauge but do not interfere with the measurement acquisition. The use of an array of pressure bars allows the pressure-time histories at discrete known points to be measured. This article also describes the interpolation routine used to derive pressure-time histories at un-instrumented locations on the plane of interest. Currently the technique has been used to measure loading from high explosives in free air and buried shallowly in various soils.

This protocol details the use of Hopkinson pressure bars to measure reflected blast loading from near-field explosive events. It is capable of interpolating a pressure-time history at any point on a reflective boundary and as such can be used to fully characterize the spatial and temporal variations in loading produced.

ブラスト定量ホプキンソン圧力棒を使用して

Near-field blast load measurement presents an issue to many sensor types as they must endure very aggressive environments and be able to measure pressures ...