フランス高等教育・研究省に感謝しております規則 Industrielles ド形成パー ラ抜き (CIFRE) と金融支援 IFP エネルギーヌーヴェル。

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R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Computer+visualization+of+three-dimensional+image+data+using+IMOD.">Computer visualization of three-dimensional image data using IMOD.</a> J Struct Biol. 116 (1), 71-76 (1996).</li><li>Align RGB planes. ImageJ Available from: <a target="_blank" href="https://ImageJ.net/Align_RGB_planes">https://ImageJ.net/Align_RGB_planes</a> (2018)</li><li>MessaoudiI, C., Boudier, T., Sorzano, C., Marco, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=TomoJ:+tomography+software+for+three-dimensional+reconstruction+in+transmission+electron+microscopy.">TomoJ: tomography software for three-dimensional reconstruction in transmission electron microscopy.</a> BMC Bioinf. 8 (1), 288 (2007).</li><li>Saxton, W. 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著者が明らかに何もありません。

本稿の目的は、透過トモグラフィによる化学の 3 D のマップを取得する方法について説明することです。このプロトコルは完全にオリジナルと著者らによって開発されました。
EFTEM トモグラフィ前述のようにいくつかの欠点があります: フィルターされた画像を取得するために必要な長い露出時間による電子ビーム耐性は、(i) のみサンプルが分析できます。(ii) EFTEM トモ?...

機能性材料の特性は 3 D パラメーターに依存しています。完全に彼らの特性を理解し、その機能を強化、形態および 3 D で化学の分布を分析することが重要です。電子断層撮影法1 (ET) は、ナノメートル スケールの2,3でこの情報を提供する最高のテクニックのひとつです。それは広い角度範囲にサンプルを回転と角度ステップごとに 1 つの画像を記録から成っています。得られた傾きのシリーズを使用して、ラドン変換4,5に基づく数学的なアルゴリズムを使用して、サンプルのボリュームを再構築します。3 D のサンプルをモデルしのような粒子局在6とサイズ分布73D パラメーターを定量化、毛穴の位置とサイズ分布8等は、ボリュームの灰色レベルを選択すること
一般的には、ET は、できればどちらの方向に 70 ° 以上の最大の可能な角度にサンプルを傾けることによって電子顕微鏡で実行されます。各傾斜角に成型、画像の傾きシリーズ サンプルの投影が記録されます。その傾きの系列を整列し、セグメント化と定量化がサンプルのボリュームを再構築するために使用します。+90 °、-90 ° からサンプルを回転ことはできません、ために、盲検角度による直交軸9に沿って異方性解像度があります再構成ボリューム。
ET は、イメージングの異なるモードで実行できます。触媒サポート複雑な形状または明視野 TEM モード (BF TEM) は非晶質材料、生体試料、高分子を研究に使用されます。画像解析は、コンポーネント10 (高密度になります詳細ライターよりも暗い、すなわち密度の低いコンポーネント) の密度を特徴付ける灰色レベルの分化に基づいています。高角環状暗視野 TEM モード (関数幹) をスキャンする際に、結晶性試料を分析する使用されます。信号は、原子番号の機能として化学情報を提供しますサンプルの重いコンポーネントが明るく表示される、ライター 1 つ9。収集材料11、およびエネルギーによって放出される x 線エネルギー分散型 x 線分光 (EDX) のような他のモード イメージング モード (EFTEM)12,13をフィルタ リング、3 D の化学的分布を評価することができるもサンプル。
EFTEM イメージング、電子顕微鏡を用いた電子エネルギー分析器 2D 化学マップを記録できます。分光計は、彼らのエネルギーの機能として電子を分散させることによって磁気プリズムとして機能します。イメージは、特定の原子との相互作用から失われたエネルギーによって電子によって作成されます。同じ 2 D 化学マップが異なる傾きの角度、化学予測のシリーズを取得すると、傾斜で計算される場合 3 D 化学ボリュームを再構築するを使用できます。
すべての材料は、透過トモグラフィによる分析できます。テクニックは、弱いまたは不規則材料サンプルの予約されています。それにもかかわらず、他のイメージング技術を使用してときに区別し非常ににくい軽元素の分析に使用できます。さらに、信頼性の高い 2 D 化学マップを得るためには、材料の厚さは、材料14を介して電子の平均自由行程以下に必要です。この条件下で最大の単一電子単一原子との相互作用を持っていることの確率です。2 つのメソッドは、2 D 化学マップの計算に使用されます。1 番目は、最もよく使われるイオン化エッジ13後分析、および 3 分の 1 の下の要素のイオン化エッジの前に 2 つのフィルターが適用されたエネルギー ウィンドウを記録する場所「3 windows 法」をです。最初の 2 つの画像を用いて推定して、3 番目のウィンドウの位置から力法を使用して、それから差し引かれる背景を推定します。得られた画像は、3 D サンプル ボリュームの分析元素分布の投影です。2 番目のメソッドは、「ジャンプ比;」と呼ばれる前に、と後の 2 つだけエネルギー フィルター画像を使用してイオン化エッジ。この方法は質的、最終的なイメージはこれらの 2 つの画像間の比率を実行するだけで計算され、背景エネルギーの変化については考慮しません。
EFTEM ET と組み合わせることで、フィルター選択されたエネルギーの解析的トモグラフィーを得ることができます。EFTEM トモグラフィーとアトム プローブ断層レントゲン写真撮影 (APT) は、相補的な技術です。APT、に比べて EFTEM 断層レントゲン写真撮影は複雑な前処理を必要としない非破壊特性解析です。ユニークなナノ粒子の様々 な特徴を実行する使用できます。EFTEM トモグラフィーは、APT は、それらを測定する非常に少なくともレーザー支援で必要としながら絶縁材料を分析できます。EFTEM 断層が低解像度で適切に動作しながら、原子スケールの APT が実行されます。透過トモグラフィ実験中にビームの劣化に抵抗するサンプルに対してのみ適切であります。すべての傾斜角度でのすべてのフィルターが適用された画像を記録するには、サンプルは 2 時間限りの電子ビームを公開できます。さらに、2 D マップで最大の化学信号を記録する高いビーム強度で長い博覧会の期間は、必要かもしれません。このような条件でビームの敏感なサンプル抜本的な形態学的・化学的変化に苦しみます。したがって、電子ビームにサンプル感度の正確な測定は、実験前に確立されなければなりません。さらに、透過トモグラフィは空間的な位置およびサンプル.に存在する元素の性質を決定する必要に応じてできるだけ多くの断層を記録の結果それにもかかわらず、EFTEM トモグラフィーは、触媒アプリケーションをモデル化するための新たな洞察を与えるための触媒担体などのサンプルの 3 D 化学配分に関する重要な情報を提供できます。
今日それはエネルギー間隔を選択することができます専用のソフトウェアを使用することが可能、記録エネルギー ウィンドウ画像をフィルター処理し化学物質が異なる角度でマップを計算します。サンプルでは、追跡、焦点を当て、および透過モードでフィルター処理された画像の記録を傾斜できます。2D 化学マップを計算できると、フルティルト シリーズ配置できますが、反復的なアルゴリズムを使用して計算化学のボリュームとシリーズがセグメント化と定量化された15,16をすることができます最後に。

<table>
	<tbody>
		<tr>
			<td>JEOL 2100f</td>
			<td>JEOL</td>
			<td></td>
			<td>Electron microscope</td>
		</tr>
		<tr>
			<td>Tridiem Gatan Imaging Filter (GIF)</td>
			<td>Gatan</td>
			<td></td>
			<td>Post colum energy filter</td>
		</tr>
		<tr>
			<td>Digital micrograph</td>
			<td>Gatan</td>
			<td></td>
			<td>Software</td>
		</tr>
		<tr>
			<td>Gatan EFTEM tomography plugin</td>
			<td>Gatan</td>
			<td></td>
			<td>Dedicated software to record filtered tilt series for EFTEM tomograohy</td>
		</tr>
		<tr>
			<td>Tomoj</td>
			<td>Imagej plugin http://www.cmib.fr/en/download/softwares/</td>
			<td></td>
			<td>Free software developed by Currie Institute in Paris, France for electron tomography</td>
		</tr>
		<tr>
			<td>EFTEM-Tomoj</td>
			<td>Imagej plugin http://www.cmib.fr/en/download/softwares/</td>
			<td></td>
			<td>Free software developed by Currie Institute in Paris, France , for EFTEM imaging</td>
		</tr>
		<tr>
			<td>Imod</td>
			<td>http://bio3d.colorado.edu/imod/</td>
			<td></td>
			<td>Free software developed by University of Colorado, USA for electron tomography</td>
		</tr>
		<tr>
			<td>Imagej</td>
			<td>https://imagej.nih.gov/ij/</td>
			<td></td>
			<td>Free software developed by National Institute of Mental Health, Bethesda, Maryland, USA for images treatment</td>
		</tr>
		<tr>
			<td>Merge channels</td>
			<td>https://imagej.net/Color_Image_Processing</td>
			<td></td>
			<td>Fonction in Imagej allowing to give different colors to volumes while they are overlapped</td>
		</tr>
		<tr>
			<td>3D Slicer</td>
			<td>https://www.slicer.org/</td>
			<td></td>
			<td>Free software developed by a large consortium lead by Ron Kikinis , Harvard Medical School, Boston, MA, SUA</td>
		</tr>
		<tr>
			<td>Chimera</td>
			<td>https://www.cgl.ucsf.edu/chimera/</td>
			<td></td>
			<td>Free software developed by the Resource for Biocomputing, Visualization, and Informatics at the University of California, San Francisco,for data segmentation, cuatification and visualisation of 3D models</td>
		</tr>
		<tr>
			<td>silica alumina support of catalyst</td>
			<td>IFPEN</td>
			<td></td>
			<td>sample prepared for eleboration of this protocol</td>
		</tr>
		<tr>
			<td>titania alumina support of catalyst</td>
			<td>IFPEN</td>
			<td></td>
			<td>sample prepared for eleboration of this protocol</td>
		</tr>
		<tr>
			<td>alcohol</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>water</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Au nanoparticles of 5 nm</td>
			<td>BBI Solutions</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Holey carbn film 200 mesh microscopy grid</td>
			<td>Agar</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>EDX sepctrometer</td>
			<td>Oxford Instruments</td>
			<td></td>
			<td></td>
		</tr>
	</tbody>
</table>

obtaining 3d chemical maps by energy filtered transmission electron microscopy tomography

エネルギー フィルター透過電子顕微鏡トモグラフィー (EFTEM 断層レントゲン写真撮影) は、ナノメートル スケールでの材料の三次元 (3 D) 化学マップを提供できます。EFTEM 断層撮影は、他のイメージング技術を使用して区別するために非常に困難な化学元素を区切ることができます。ここで記述されている実験のプロトコルは、化学的分布と材料の形態を理解する化学 3 D のマップを作成する方法を示しています。データ分割の準備手順、サンプルが掲載されています。このプロトコルは、ナノメートルのサンプルの化学要素の 3次元分布解析を許可します。ただし、現在、3 D 化学マップのみ生成されることをサンプル フィルターされた画像の記録は、強烈なビームに長い露出時間を必要とするので、機密性の高い、ビームではないです。プロトコルは、2 つの異なる異種触媒担体の成分の化学分布の定量化に適用されました。最初の研究では、アルミニウム、チタン酸化チタン アルミナ サポートでの化学の分布を調べた。スイング pH メソッドを使用して調製します。第二に、ソル粉と機械的混合法を使用して作製したシリカ-アルミナ サポート中のアルミニウムおよび si の化学の分布を調べた。

参照13に、このプロトコルのアプリケーションの例を示します。EFTEM トモグラフィ チタニア アルミナ触媒担体の分析に用いる。水素化脱硫 (HDS) のようなアプリケーションで、MoS2ナノ粒子の活動的な段階の触媒の活性を強化するには、チタニアがトレード・マークの支持面で活動的な段階との接触が重要です。それは、チタニアがアルミナ?...

Watch this Scientific Journal Video about Obtaining 3D Chemical Maps by Energy Filtered Transmission Electron Microscopy Tomography at JoVE.com

Obtaining 3D Chemical Maps by Energy Filtered Transmission Electron Microscopy Tomography

エネルギー化学 3 D マップの取得フィルター透過電子顕微鏡トモグラフィー

本稿では、エネルギー フィルタ リング画像と電子線トモグラフィーを組み合わせた 3 D 化学マップを達成するためにプロトコルについて説明します。他のイメージング手法を区別することは困難である要素によって形成される 2 つの触媒担体の化学の分布を調べた。各アプリケーション重複元素それぞれ間隔がイオン化エッジのマッピングで構成されます。

Energy filtered transmission electron microscopy tomography (EFTEM tomography) can provide three-dimensional (3D) chemical maps of materials at a ...

obtaining-3d-chemical-maps-energy-filtered-transmission-electron

Research

JoVE Journal

Chemistry

6.4K ビュー.  Université Claude Bernard Lyon 1. 本稿では、エネルギー フィルタ リング画像と電子線トモグラフィーを組み合わせた 3 D 化学マップを達成するためにプロトコルについて説明します。他のイメージング手法を区別することは困難である要素によって形成される 2 つの触媒担体の化学の分布を調べた。各アプリケーション重複元素それぞれ間隔がイオン化エッジのマッピングで構成されま?...

ビデオ: Obtaining 3D Chemical Maps by Energy Filtered Transmission Electron Microscopy Tomography

Quantitative Detection of Trace Explosive Vapors by Programmed Temperature Desorption Gas Chromatography-Electron Capture Detector

The direct liquid deposition of solution standards onto sorbent-filled thermal desorption tubes is used for the quantitative analysis of trace explosive vapor samples. The direct liquid deposition method yields a higher fidelity between the analysis of vapor samples and the analysis of solution standards than using separate injection methods for vapors and solutions, i.e., samples collected on vapor collection tubes and standards prepared in solution vials. Additionally, the method can account for instrumentation losses, which makes it ideal for minimizing variability and quantitative trace chemical detection. Gas chromatography with an electron capture detector is an instrumentation configuration sensitive to nitro-energetics, such as TNT and RDX, due to their relatively high electron affinity. However, vapor quantitation of these compounds is difficult without viable vapor standards. Thus, we eliminate the requirement for vapor standards by combining the sensitivity of the instrumentation with a direct liquid deposition protocol to analyze trace explosive vapor samples.

Trace explosive vapors of TNT and RDX collected on sorbent-filled thermal desorption tubes were analyzed using a programmed temperature desorption system coupled to GC with an electron capture detector. The instrumental analysis is combined with direct liquid deposition method to reduce sample variability and account for instrumentation drift and losses.

プログラムされた温度脱着ガスクロマトグラフィー - 電子捕獲型検出器による微量爆発性気体の定量的検出

The direct liquid deposition of solution standards onto sorbent-filled thermal desorption tubes is used for the quantitative analysis of trace explosive ...

化学

1,3,5-Triphenylbenzene and Corannulene as Electron Receptors for Lithium Solvated Electron Solutions

The authors report on conductivity studies carried out on lithium solvated electron solutions (LiSES) prepared using two types of polyaromatic hydrocarbons (PAH), namely 1,3,5-triphenylbenzene and corannulene, as electron receptors. The solid PAHs were first dissolved in tetrahydrofuran (THF) to form a solution. Metallic lithium was then dissolved into these PAH/THF solutions to yield either blue or greenish blue solutions, colors which are indicative of the presence of solvated electrons. Conductivity measurements at ambient temperature carried out on 1,3,5-triphenylbenzene-based LiSES, denoted by LixTPB(THF)24.7 (x = 1, 2, 3, 4), showed an increase of conductivity with increase of Li:PAH ratio from x = 1 to 2. However, the conductivity gradually decreased upon further increasing the ratio. Indeed the conductivity of LixTPB(THF)24.7 for x = 4 is even lower than for x = 1. Such behavior is similar to that of the previously reported LiSES prepared from biphenyl and naphthalene. Conductivity versus temperature measurements on corannulene-based LiSES, denoted by LixCor(THF)247 (x = 1, 2, 3, 4, 5), showed linear relationships with negative slopes, indicating a metallic behavior similar to biphenyl and naphthalene-based LiSES.

The authors report on conductivity studies carried out on lithium solvated electron solutions (LiSES) prepared using 1,3,5-triphenylbenzene (TPB) and corannulene as electron receptors.

リチウム溶媒和電子ソリューションのための電子受容体として1,3,5-トリフェニルベンゼンとコランニュレン

The authors report on conductivity studies carried out on lithium solvated electron solutions (LiSES) prepared using two types of polyaromatic ...

A Simple, Low-cost, and Robust System to Measure the Volume of Hydrogen Evolved by Chemical Reactions with Aqueous Solutions

There is a growing research interest in the development of portable systems which can deliver hydrogen on-demand to proton exchange membrane (PEM) hydrogen fuel cells. Researchers seeking to develop such systems require a method of measuring the generated hydrogen. Herein, we describe a simple, low-cost, and robust method to measure the hydrogen generated from the reaction of solids with aqueous solutions. The reactions are conducted in a conventional one-necked round-bottomed flask placed in a temperature controlled water bath. The hydrogen generated from the reaction in the flask is channeled through tubing into a water-filled inverted measuring cylinder. The water displaced from the measuring cylinder by the incoming gas is diverted into a beaker on a balance. The balance is connected to a computer, and the change in the mass reading of the balance over time is recorded using data collection and spreadsheet software programs. The data can then be approximately corrected for water vapor using the method described herein, and parameters such as the total hydrogen yield, the hydrogen generation rate, and the induction period can also be deduced. The size of the measuring cylinder and the resolution of the balance can be changed to adapt the setup to different hydrogen volumes and flow rates.

The study of methods to generate on-demand hydrogen for fuel cells continues to grow in importance. However, systems to measure hydrogen evolution from the reaction of chemicals with water can be complicated and expensive. This article details a simple, low-cost, and robust method to measure the evolution of hydrogen gas.

シンプル、低コスト、及び水溶液で化学反応により発生した水素の体積を測定するための堅牢なシステム

There is a growing research interest in the development of portable systems which can deliver hydrogen on-demand to proton exchange membrane (PEM) ...

Determination of Carbonyl Functional Groups in Bio-oils by Potentiometric Titration: The Faix Method

Carbonyl compounds present in bio-oils are known to be responsible for bio-oil property changes upon storage and during upgrading. Specifically, carbonyls cause an increase in viscosity (often referred to as &#39;aging&#39;) during storage of bio-oils. As such, carbonyl content has previously been used as a method of tracking bio-oil aging and condensation reactions with less variability than viscosity measurements. Additionally, carbonyls are also responsible for coke formation in bio-oil upgrading processes. Given the importance of carbonyls in bio-oils, accurate analytical methods for their quantification are very important for the bio-oil community. Potentiometric titration methods based on carbonyl oximation have long been used for the determination of carbonyl content in pyrolysis bio-oils. Here, we present a modification of the traditional carbonyl oximation procedures that results in less reaction time, smaller sample size, higher precision, and more accurate carbonyl determinations. While traditional carbonyl oximation methods occur at room temperature, the Faix method presented here occurs at an elevated temperature of 80 &#176;C.

Here we present a potentiometric titration technique for accurately quantifying carbonyl compounds in pyrolysis bio-oils.

Faix方法：電位差滴定法によりバイオ油中のカルボニル官能基の決意

Carbonyl compounds present in bio-oils are known to be responsible for bio-oil property changes upon storage and during upgrading. Specifically, carbonyls ...

Facile Preparation of (2Z,4E)-Dienamides by the Olefination of Electron-deficient Alkenes with Allyl Acetate

Direct cross-coupling between two alkenes via vinylic C-H bond activation represents an efficient strategy for the synthesis of butadienes with high atomic and step economy. However, this functionality-directed cross-coupling reaction has not been developed, as there are still limited directing groups in practical use. In particular, a stoichiometric amount of oxidant is usually required, producing a large amount of waste. Due to our interest in novel 1,3-butadiene synthesis, we describe the ruthenium-catalyzed olefination of electron-deficient alkenes using allyl acetate and without external oxidant. The reaction of 2-phenyl acrylamide and allyl acetate was chosen as a model reaction, and the desired diene product was obtained in 80% isolated yield with good stereoselectivity (Z,E/Z,Z = 88:12) under optimal conditions: [Ru(p-cymene) Cl2]2 (3 mol %) and AgSbF6 (20 mol %) in DCE at 110 &#186;C for 16 h. With the optimized catalytic conditions in hand, representative &#945;- and/or &#946;-substituted acrylamides were investigated, and all reacted smoothly, regardless of aliphatic or aromatic groups. Also, differently N-substituted acrylamides have proven to be good substrates. Moreover, we examined the reactivity of different allyl derivatives, suggesting that the chelation of acetate oxygen to the metal is crucial for the catalytic process. Deuterium-labeled experiments were also conducted to investigate the reaction mechanism. Only Z-selective H/D exchanges on acrylamide were observed, indicating a reversible cyclometalation event. In addition, a kinetic isotope effect (KIE) of 3.2 was observed in the intermolecular isotopic study, suggesting that the olefinic C-H metalation step is probably involved in the rate-determining step.

Facile Preparation of 2Z,4E-Dienamides by the Olefination of Electron-deficient Alkenes with Allyl Acetate

The ruthenium-catalyzed olefination of electron-deficient alkenes with allyl acetate is described here. By using aminocarbonyl as a directing group, this external oxidant-free protocol has high efficiency and good stereo- and regioselectivity, opening a novel synthetic route to (Z,E)-butadiene skeletons.

（2<em&gt; Z</em&gt;、4<em&gt; E</em&gt;） - 電子不足アルケンと酢酸アリルとの合成によるジエナミド

Direct cross-coupling between two alkenes via vinylic C-H bond activation represents an efficient strategy for the synthesis of butadienes with high ...

Quantifying X-Ray Fluorescence Data Using MAPS

The quantification of X-ray fluorescence (XRF) microscopy maps by fitting the raw spectra to a known standard is crucial for evaluating chemical composition and elemental distribution within a material. Synchrotron-based XRF has become an integral characterization technique for a variety of research topics, particularly due to its non-destructive nature and its high sensitivity. Today, synchrotrons can acquire fluorescence data at spatial resolutions well below a micron, allowing for the evaluation of compositional variations at the nanoscale. Through proper quantification, it is then possible to obtain an in-depth, high-resolution understanding of elemental segregation, stoichiometric relationships, and clustering behavior.
This article explains how to use the MAPS fitting software developed by Argonne National Laboratory for the quantification of full 2-D XRF maps. We use as an example results from a Cu(In,Ga)Se2 solar cell, taken at the Advanced Photon Source beamline 2-ID-D at Argonne National Laboratory. We show the standard procedure for fitting raw data, demonstrate how to evaluate the quality of a fit and present the typical outputs generated by the program. In addition, we discuss in this manuscript certain software limitations and offer suggestions for how to further correct the data to be numerically accurate and representative of spatially resolved, elemental concentrations.

Here, we demonstrate the use of the X-ray fluorescence fitting software, MAPS, created by Argonne National Laboratory for the quantification of fluorescence microscopy data. The quantified data that results is useful for understanding the elemental distribution and stoichiometric ratios within a sample of interest.

X 線蛍光データ マップを使用しての定量化

The quantification of X-ray fluorescence (XRF) microscopy maps by fitting the raw spectra to a known standard is crucial for evaluating chemical ...

Liquid-cell Transmission Electron Microscopy for Tracking Self-assembly of Nanoparticles

Drying a nanoparticle dispersion is a versatile way to create self-assembled structures of nanoparticles, but the mechanism of this process is not fully understood. We have traced the trajectories of individual nanoparticles using liquid-cell transmission electron microscopy (TEM) to investigate the mechanism of the assembly process. Herein, we present the protocols used for liquid-cell TEM studies of the self-assembly mechanism. First, we introduce the detailed synthetic protocols used to produce uniformly sized platinum and lead selenide nanoparticles. Next, we present the microfabrication processes used to produce liquid cells with silicon nitride or silicon windows and then describe the loading and imaging procedures of the liquid-cell TEM technique. Several notes are included to provide helpful tips for the entire process, including how to manage the fragile cell windows. The individual motions of nanoparticles tracked by liquid-cell TEM revealed that changes in the solvent boundaries caused by evaporation affected the self-assembly process of nanoparticles. The solvent boundaries drove nanoparticles to primarily form amorphous aggregates, followed by flattening of the aggregates to produce a 2-dimensional (2D) self-assembled structure. These behaviors are also observed for different nanoparticle types and different liquid-cell compositions.

Here we introduce experimental protocols for the real-time observation of a self-assembly process using liquid-cell transmission electron microscopy.

ナノ粒子の自己集合の追跡のため液晶セルの透過電子顕微鏡観察

Drying a nanoparticle dispersion is a versatile way to create self-assembled structures of nanoparticles, but the mechanism of this process is not fully ...

Analysis of Minerals Produced by hFOB 1.19 and Saos-2 Cells Using Transmission Electron Microscopy with Energy Dispersive X-ray Microanalysis

This video presents the use of transmission electron microscopy with energy dispersive X-ray microanalysis (TEM-EDX) to compare the state of minerals in vesicles released by two human bone cell lines: hFOB 1.19 and Saos-2. These cell lines, after treatment with ascorbic acid (AA) and &#946;-glycerophosphate (&#946;-GP), undergo complete osteogenic transdifferentiation from proliferation to mineralization and produce matrix vesicles (MVs) that trigger apatite nucleation in the extracellular matrix (ECM).
Based on Alizarin Red-S (AR-S) staining and analysis of the composition of minerals in cell lysates using ultraviolet (UV) light or in vesicles using TEM imaging followed by EDX quantitation and ion mapping, we can infer that osteosarcoma Saos-2 and osteoblastic hFOB 1.19 cells reveal distinct mineralization profiles. Saos-2 cells mineralize more efficiently than hFOB 1.19 cells and produce larger mineral deposits that are not visible under UV light but are similar to hydroxyapatite (HA) in that they have more Ca and F substitutions.
The results obtained using these techniques allow us to conclude that the process of mineralization differs depending on the cell type. We propose that, at the cellular level, the origin and properties of vesicles predetermine the type of minerals.

We present a protocol to compare the state of minerals in vesicles released by two human bone cell lines: hFOB 1.19 and Saos-2. Their mineralization profiles were analyzed by Alizarin Red-S (AR-S) staining, ultraviolet (UV) light visualization, transmission electron microscopy (TEM) imaging and energy dispersive X-ray microanalysis (EDX).

HFOB 1.19 によって生成される鉱物と Sao 2 セルを使用して透過型電子顕微鏡エネルギー分散型 x 線微小分析での分析

This video presents the use of transmission electron microscopy with energy dispersive X-ray microanalysis (TEM-EDX) to compare the state of minerals in ...

Using Graphene Liquid Cell Transmission Electron Microscopy to Study in Situ Nanocrystal Etching

Graphene liquid cell electron microscopy provides the ability to observe nanoscale chemical transformations and dynamics as the reactions are occurring in liquid environments. This manuscript describes the process for making graphene liquid cells through the example of graphene liquid cell transmission electron microscopy (TEM) experiments of gold nanocrystal etching. The protocol for making graphene liquid cells involves coating gold, holey-carbon TEM grids with chemical vapor deposition graphene and then using those graphene-coated grids to encapsulate liquid between two graphene surfaces. These pockets of liquid, with the nanomaterial of interest, are imaged in the electron microscope to see the dynamics of the nanoscale process, in this case the oxidative etching of gold nanorods. By controlling the electron beam dose rate, which modulates the etching species in the liquid cell, the underlying mechanisms of how atoms are removed from nanocrystals to form different facets and shapes can be better understood. Graphene liquid cell TEM has the advantages of high spatial resolution, compatibility with traditional TEM holders, and low start-up costs for research groups. Current limitations include delicate sample preparation, lack of flow capability, and reliance on electron beam-generated radiolysis products to induce reactions. With further development and control, graphene liquid cell may become a ubiquitous technique in nanomaterials and biology, and is already being used to study mechanisms governing growth, etching, and self-assembly processes of nanomaterials in liquid on the single particle level.

Using Graphene Liquid Cell Transmission Electron Microscopy to Study in Situ Nanocrystal Etching

Graphene liquid cell electron microscopy can be used to observe nanocrystal dynamics in a liquid environment with greater spatial resolution than other liquid cell electron microscopy techniques. Etching premade nanocrystals and following their shape using graphene liquid cell Transmission Electron Microscopy can yield important mechanistic information about nanoparticle transformations.

グラフェン液セル透過型電子顕微鏡を使用してナノ結晶エッチングその場を研究するには

Graphene liquid cell electron microscopy provides the ability to observe nanoscale chemical transformations and dynamics as the reactions are occurring in ...

Preparation of Graphene-Supported Microwell Liquid Cells for In Situ Transmission Electron Microscopy

The fabrication and preparation of graphene-supported microwell liquid cells (GSMLCs) for in situ electron microscopy is presented in a stepwise protocol. The versatility of the GSMLCs is demonstrated in the context of a study about etching and growth dynamics of gold nanostructures from a HAuCl4 precursor solution. GSMLCs combine the advantages of conventional silicon- and graphene-based liquid cells by offering reproducible well depths together with facile cell manufacturing and handling of the specimen under investigation. The GSMLCs are fabricated on a single silicon substrate which drastically reduces the complexity of the manufacturing process compared to two-wafer-based liquid cell designs. Here, no bonding or alignment process steps are required. Furthermore, the enclosed liquid volume can be tailored to the respective experimental requirements by simply adjusting the thickness of a silicon nitride layer. This enables a significant reduction of window bulging in the electron microscope vacuum. Finally, a state-of-the-art quantitative evaluation of single particle tracking and dendrite formation in liquid cell experiments using only open source software is presented.

Preparation of Graphene-Supported Microwell Liquid Cells for In Situ Transmission Electron Microscopy

A protocol for preparation of graphene-supported microwell liquid cells for in situ electron microscopy of gold nanocrystals from HAuCl4 precursor solution is presented. Furthermore, an analysis routine is presented to quantify observed etching and growth dynamics.

その中透過電子顕微鏡におけるグラフェン支持マイクロウェル液体細胞の調製

The fabrication and preparation of graphene-supported microwell liquid cells (GSMLCs) for in situ electron microscopy is presented in a stepwise protocol. ...