Name: in situ characterization of boehmite particles in water using liquid sem
Uploaded: 2017-09-27T13:00:00.000+00:00
Duration: 11 min 59 s
Description: Watch this Scientific Journal Video about In Situ Characterization of Boehmite Particles in Water Using Liquid SEM at JoVE.com

太平洋の北西国立研究所 (なり) 核プロセス科学イニシアティブ (NPSI) 感謝しております-支援のため監督研究と開発 (LDRD) 基金。・ チャタジー博士 Sayandev は、合成ベーマイト粒子を提供されています。インストゥルメンタル アクセスが w. r. ワイリー環境分子科学研究所 (EMSL) 一般ユーザーの提案書を提供されました。EMSL はオフィスの生物と環境研究 (BER) なりで主催国立科学ユーザー施設です。バテル契約 DE AC05 76RL01830 下 DOE のなりが運営しています。

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著者が明らかに何もありません。

SEM は、高分解能1ナノ (nm) レベルの有機・無機材料における表面キャラクタリゼーションの強力な手法です。たとえば、地質試料26と半導体27などしっかりと乾燥試料を解析する広く使用されます。しかし、電子顕微鏡1に必要な高真空環境の中で液体の不適合による湿式、液体のサンプルを特徴付けることの制限がありま...

走査型電子顕微鏡 (SEM) は、高解像度イメージング1を生産することによって様々 な標本の調査に広く適用されています。エネルギー分散型 x 線分光 (EDX)、SEM に関連付けられているは、元素組成1の決定を可能。 にします。伝統的に、イメージングのだけ乾燥した固体サンプルの SEM が適用されます。最後の 30 年で環境 SEM (フラッディングガス) は、蒸気環境2,3,4、5の部分的な水和物サンプルを分析するため開発されました。ただし、フラッディングガスは目的の高解像度6でウェット、完全流体のサンプルをイメージできません。ウェットの SEM 細胞も濡れている画像試料の SEM7,8; を使用して開発されました。それにもかかわらず、これらの細胞が電子イメージングを後方散乱し、それらデザイン9,10アプリケーションのアクセシビリティの高いに生体試料を中心に開発されました。
SEM を使用して、ネイティブの液体環境の様々 なサンプルを分析する際の課題に対処するため、我々 は真空対応マイクロ流体デバイス、分析で、液体真空インターフェイス (サルヴィ)、高空間分解能セカンダリを有効にするためのシステムを発明しました。SEM の高真空モードを用いた液体試料の電子 (SE) イメージングと元素分析この手法には、次のユニークな機能が含まれています: 1) 液体が直接では、直径 1-2 マイクロメートルの小さな開口部でプローブ2) 液体は表面張力によって穴内に保持されます。・ 3) サルヴィはポータブルで、1 つ以上分析プラットフォーム11,12,13,14,15,16,17 に適応することができます ,18。
サルヴィは 100 nm 厚のシリコン窒化 (罪) 膜で構成されています、200 μ m の広いマイクロ製ポリジメチルシロキサン (PDMS) ブロック。罪膜ウィンドウは、マイクロをシールに適用されます。作製の詳細と重要な設計上の考慮事項は、以前の論文と特許11,19,20詳細いた。現在、大手メーカーと顕微鏡用消耗品の供給のディストリビューターは、液体 SEM アプリケーション21,22の市販サルヴィ デバイスを販売するためのライセンスを購入しています。
分析機器の真空ベースのサルヴィのアプリケーションは、さまざまな水溶液とバイオ フィルム、哺乳類細胞、ナノ粒子、および電極材料12,を含む複雑な液体混合物を使用して実証されています。14,17,20,23,24します。 ただし、前述の仕事のほとんどは従って液体のアプリケーション キー分析ツールとして飛行時間二次イオン質量分析 (TOF-SIMS) を利用サルヴィの SEM が十分に検討されていません。今回、サルヴィは液体の SEM 画像と EDX 元素分析を用いた液体の大きい非球状粒子の研究に使用されています。サンプルは研究室で合成された AlOOH 粒子から成っています。サブマイクロ メーター サイズ ベーマイト粒子は、ハンフォード ・ サイトで高レベル放射性廃棄物に存在する知られています。溶解する遅く、廃棄物処理にレオロジーの問題を引き起こす可能性があります。したがって、液体25ベーマイト粒子を特徴付ける機能を持つことが重要です。この技術的なアプローチは、これらの粒子と関連のレオロジー特性の改善された理解の様々 な物理化学的条件のベーマイトを研究に使用できます。これらの粒子は、液体中に浮遊する粒子を研究するために高真空 SEM にサルヴィを適用する方法を示すステップバイ ステップを利用しました。サルヴィと SEM の統合および SEM データ集録のための重要な技術的なポイントは、用紙内で強調表示されます。
プロトコルは、将来的に液体の SEM の多様なアプリケーションでこの手法を活用に興味がある人のためサルヴィと液体の SEM イメージングを用いた液体試料解析のデモを提供します。

<table><tbody><tr><td>Carbon Coater</td><td>Cressington</td><td>208 Carbon</td><td>It is accompanied with thickness monitor MTM-10.</td></tr><tr><td>SEM</td><td>FEI</td><td>Quanta 3D FEG</td><td>It provides highly resolved scanning electron microscopy and elemental analysis.</td></tr><tr><td>System for Analysis at the Liquid Vacuum Interface (SALVI)</td><td>Pacific Northwest National Laboratory</td><td>N/A</td><td>SALVI is a unique, vacuum compatible microfluidic cell that enables the characterization of the liquid sample using vacuu- based scientific instrument.</td></tr><tr><td>PEEK Union</td><td>Valco</td><td>ZU1TPK</td><td>The polyether ether ketone union is used for connecting the inlet and outlet of SALVI</td></tr><tr><td>Syringe</td><td>BD</td><td>309659</td><td>1 mL</td></tr><tr><td>Pipette</td><td>Thermo Fisher Scientific</td><td>21-377-821</td><td>Range: 100 to 1,000 mL</td></tr><tr><td>Pipette Tip 1</td><td>Neptune</td><td>2112.96.BS</td><td>1,000 &amp;micro;L</td></tr><tr><td>Pipette Tip 2</td><td>Rainin</td><td>17001865</td><td>20 &amp;micro;L</td></tr><tr><td>Syringe Pump</td><td>Harvard Apparatus</td><td>70-2213</td><td>It is used to inject the liquid sample into the SALVI device.</td></tr><tr><td>pH meter</td><td>Fisher Scientific/accumet</td><td>13-636-AP72</td><td>It is used for measuring the pH of AlOOH in DI water.</td></tr><tr><td>Barnstead Ultrapure Water System, UV/UF</td><td>Thermo Scientific Barnstead</td><td>Nanopure diamond D11931</td><td>It is used for producing DI water.</td></tr><tr><td>Centrifuge tubes</td><td>Fisher scientific/Falcon</td><td>15-527-90</td><td>15 mL</td></tr><tr><td>Bransonic ultrasonic cleaner</td><td>Sigma-Aldrich</td><td>2510</td><td>It is used to ultrasonicate the AlOOH liquid sample.</td></tr><tr><td>Balance</td><td>Mettler Toledo</td><td>11106015</td><td>XS64</td></tr><tr><td>AlOOH</td><td>Pacific Northwest National Laboratory</td><td>N/A</td><td>It is synthesized by scientists at Pacific Northwest National Laboratory.</td></tr><tr><td>xT microscope Control</td><td>FEI</td><td>Quanta 3D FEG</td><td>Default microscope control software of SEM Quanta 3D FEG</td></tr><tr><td>EDAX Genesis software</td><td>EDAX</td><td>N/A</td><td>The software is used for collecting the EDX elemental information of the samples.</td></tr><tr><td>Teflon tubing</td><td>SUPELCO</td><td>58697-U</td><td>It is used for introducing the sample into the microchannel and holding adequate volume of liquid.</td></tr></tbody></table>

in situ characterization of boehmite particles in water using liquid sem

液体真空インターフェイス (サルヴィ) と走査型電子顕微鏡 (SEM) での解析システムを用いたin situイメージングおよび元素ベーマイト (AlOOH) 中の異物分析水を実現します。本稿では、法と真空を統合することの重要なステップ SEM と二次電子の高真空下での液体中の粒子の (SE) 画像を得るに互換性のある SAVLI。エネルギー分散型 x 線分光 (EDX) を使用 (DI) 純水のみと同様空のチャネルを含む液とコントロールのサンプル中の粒子の元素分析を取得します。液中粒子合成ベーマイト (AlOOH) は、液体の SEM 図にモデルとして使用されます。結果は良好な分解能を持つ SE モードで粒子がイメージ化されることを示す (すなわち、400 nm)。AlOOH EDX スペクトルは、アルミニウム (Al) ・ ディ ・水と比較すると、空のチャネル コントロールから重要な信号を示しています。液体 SEMその場では、多くのエキサイティングなアプリケーションと液体中の粒子を研究する強力な手法です。この手順は、液体の SEM 画像とサルヴィを用いた EDX 分析を実施するために、このアプローチを使用する場合、潜在的な落とし穴を減らすために技術的なノウハウを提供するために目指しています。

粒子のイメージを作成する方法を示す代表的な結果を示す EDX と相まって液体 SEM 画像その場を用いた解析と。結果には、SE の画像と EDX スペクトルがあります。100,000 X と図 1に 200,000 X 倍率で SE の画像を得た。図 1 aは、AlOOH の SE のイメージを示しています図 1 b ・ ディ ・水と?...

Watch this Scientific Journal Video about In Situ Characterization of Boehmite Particles in Water Using Liquid SEM at JoVE.com

In Situ Characterization of Boehmite Particles in Water Using Liquid SEM

その場で液体の SEM を用いた水中のベーマイト粒子のキャラクタリゼーション

その場で液体走査型電子顕微鏡によってリアルタイム イメージングおよび脱イオン水にベーマイト粒子の元素組成分析の手順を紹介します。

In situ imaging and elemental analysis of boehmite (AlOOH) particles in water is realized using the System for Analysis at the Liquid Vacuum Interface ...

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In Situ Characterization of Boehmite Particles in Water Using Liquid SEM

9.2K ビュー.  Pacific Northwest National Laboratory. その場で液体走査型電子顕微鏡によってリアルタイム イメージングおよび脱イオン水にベーマイト粒子の元素組成分析の手順を紹介します。

ビデオ: In Situ Characterization of Boehmite Particles in Water Using Liquid SEM

VacuSIP, an Improved InEx Method for In Situ Measurement of Particulate and Dissolved Compounds Processed by Active Suspension Feeders

Benthic suspension feeders play essential roles in the functioning of marine ecosystems. By filtering large volumes of water, removing plankton and detritus, and excreting particulate and dissolved compounds, they serve as important agents for benthic-pelagic coupling. Accurately measuring the compounds removed and excreted by suspension feeders (such as sponges, ascidians, polychaetes, bivalves) is crucial for the study of their physiology, metabolism, and feeding ecology, and is fundamental to determine the ecological relevance of the nutrient fluxes mediated by these organisms. However, the assessment of the rate by which suspension feeders process particulate and dissolved compounds in nature is restricted by the limitations of the currently available methodologies. Our goal was to develop a simple, reliable, and non-intrusive method that would allow clean and controlled water sampling from a specific point, such as the excurrent aperture of benthic suspension feeders, in situ. Our method allows simultaneous sampling of inhaled and exhaled water of the studied organism by using minute tubes installed on a custom-built manipulator device and carefully positioned inside the exhalant orifice of the sampled organism. Piercing a septum on the collecting vessel with a syringe needle attached to the distal end of each tube allows the external pressure to slowly force the sampled water into the vessel through the sampling tube. The slow and controlled sampling rate allows integrating the inherent patchiness in the water while ensuring contamination free sampling. We provide recommendations for the most suitable filtering devices, collection vessel, and storing procedures for the analyses of different particulate and dissolved compounds. The VacuSIP system offers a reliable method for the quantification of undisturbed suspension feeder metabolism in natural conditions that is cheap and easy to learn and apply to assess the physiology and functional role of filter feeders in different ecosystems.

VacuSIP, an Improved InEx Method for In Situ Measurement of Particulate and Dissolved Compounds Processed by Active Suspension Feeders

We introduce the VacuSIP, a simple, non-intrusive, and reliable method for clean and accurate point sampling of water. The system was developed and evaluated for the simultaneous collection of the water inhaled and exhaled by benthic suspension feeders in situ, to cleanly measure removal and excretion of particulate and dissolved compounds.

VacuSIP、のための改良INEX方法<em&gt;その場で</em&gt;微粒子と溶解した化合物の測定は、アクティブサスペンションフィーダによって処理します

Benthic suspension feeders play essential roles in the functioning of marine ecosystems. By filtering large volumes of water, removing plankton and ...

環境学

Phase Diagram Characterization Using Magnetic Beads as Liquid Carriers

Magnetic beads with ~1.9 &#181;m average diameter were used to transport microliter volumes of liquids between contiguous liquid segments with a tube for the purpose of investigating phase change of those liquid segments. The magnetic beads were externally controlled using a magnet, allowing for the beads to bridge the air valve between the adjacent liquid segments. A hydrophobic coating was applied to the inner surface of the tube to enhance the separation between two liquid segments. The applied magnetic field formed an aggregate cluster of magnetic beads, capturing a certain liquid amount within the cluster that is referred to as carry-over volume. A fluorescent dye was added to one liquid segment, followed by a series of liquid transfers, which then changed the fluorescence intensity in the neighboring liquid segment. Based on the numerical analysis of the measured fluorescence intensity change, the carry-over volume per mass of magnetic beads has been found to be ~2 to 3 &#181;l/mg. This small amount of liquid allowed for the use of comparatively small liquid segments of a couple hundred microliters, enhancing the feasibility of the device for a lab-in-tube approach. This technique of applying small compositional variation in a liquid volume was applied to analyzing the binary phase diagram between water and the surfactant C12E5 (pentaethylene glycol monododecyl ether), leading to quicker analysis with smaller sample volumes than conventional methods.

Here, we present a protocol to investigate multi-component phase diagrams using externally controlled magnetic beads as liquid carriers in a lab-in-tube approach. This approach can aid in applications that seek to gather further information on phase change in complex liquid systems.

相図の特徴付け液体担体として磁気ビーズを使用しました

Magnetic beads with ~1.9 &#181;m average diameter were used to transport microliter volumes of liquids between contiguous liquid segments with a tube for ...

工学

In Situ Characterization of Hydrated Proteins in Water by SALVI and ToF-SIMS

This work demonstrates in situ characterization of protein biomolecules in the aqueous solution using the System for Analysis at the Liquid Vacuum Interface (SALVI) and time-of-flight secondary ion mass spectrometry (ToF-SIMS). The fibronectin protein film was immobilized on the silicon nitride (SiN) membrane that forms the SALVI detection area. During ToF-SIMS analysis, three modes of analysis were conducted including high spatial resolution mass spectrometry, two-dimensional (2D) imaging, and depth profiling. Mass spectra were acquired in both positive and negative modes. Deionized water was also analyzed as a reference sample. Our results show that the fibronectin film in water has more distinct and stronger water cluster peaks compared to water alone. Characteristic peaks of amino acid fragments are also observable in the hydrated protein ToF-SIMS spectra. These results illustrate that protein molecule adsorption on a surface can be studied dynamically using SALVI and ToF-SIMS in the liquid environment for the first time.

In Situ Characterization of Hydrated Proteins in Water by SALVI and ToF-SIMS

This work presents a protocol for liquid handling and sample introduction to a microchannel for in situ time-of-flight secondary ion mass spectrometry analysis of protein biomolecules in an aqueous solution.

サルヴィとTOF-SIMSによる水中で水和タンパク質のその場キャラクタリゼーションで

This work demonstrates in situ characterization of protein biomolecules in the aqueous solution using the System for Analysis at the Liquid Vacuum ...

化学

Nanostructured Ag-zeolite Composites as Luminescence-based Humidity Sensors

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

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

発光ベースの湿度センサなどのナノ構造のAg-ゼオライト複合

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

Sub-nanometer Resolution Imaging with Amplitude-modulation Atomic Force Microscopy in Liquid

Atomic force microscopy (AFM) has become a well-established technique for nanoscale imaging of samples in air and in liquid. Recent studies have shown that when operated in amplitude-modulation (tapping) mode, atomic or molecular-level resolution images can be achieved over a wide range of soft and hard samples in liquid. In these situations, small oscillation amplitudes (SAM-AFM) enhance the resolution by exploiting the solvated liquid at the surface of the sample. Although the technique has been successfully applied across fields as diverse as materials science, biology and biophysics and surface chemistry, obtaining high-resolution images in liquid can still remain challenging for novice users. This is partly due to the large number of variables to control and optimize such as the choice of cantilever, the sample preparation, and the correct manipulation of the imaging parameters. Here, we present a protocol for achieving high-resolution images of hard and soft samples in fluid using SAM-AFM on a commercial instrument. Our goal is to provide a step-by-step practical guide to achieving high-resolution images, including the cleaning and preparation of the apparatus and the sample, the choice of cantilever and optimization of the imaging parameters. For each step, we explain the scientific rationale behind our choices to facilitate the adaptation of the methodology to every user's specific system.

We present a method for achieving sub-nanometer resolution images with amplitude-modulation (tapping mode) atomic force microscopy in liquid. The method is demonstrated on commercial atomic force microscopes. We explain the rationale behind our choices of parameters and suggest strategies for resolution optimization.

液体中の振幅変調原子間力顕微鏡でのサブナノメートル分解能イメージング

Atomic force microscopy (AFM) has become a well-established technique for nanoscale imaging of samples in air and in liquid. Recent studies have shown ...

A Facile Synthetic Method to Obtain Bismuth Oxyiodide Microspheres Highly Functional for the Photocatalytic Processes of Water Depuration

Bismuth oxyhalide (BiOI) is a promising material for sunlight-driven-environmental photocatalysis. Given that the physical structure of this kind of materials is highly related to its photocatalytic performance, it is necessary to standardize the synthetic methods in order to obtain the most functional architectures and, thus, the highest photocatalytic efficiency. Here, we report a reliable route to obtain BiOI microspheres via the solvothermal process, using Bi(NO3)3 and potassium iodide (KI) as precursors, and ethylene glycol as a template. The synthesis is standardized in a 150 mL autoclave, at 126 &#176;C for 18 h. This results in 2-3 &#181;m-sized mesoporous microspheres, with a relevant specific surface area (61.3 m2/g). Shortening the reaction times in the synthesis results in amorphous structures, while higher temperatures lead to a slight increase in the porosity of the microspheres, with no effect in the photocatalytic performance. The materials are photo-active under UV-A/visible light irradiation for the degradation of the antibiotic ciprofloxacin in water. This method has demonstrated to be effective in interlaboratory tests, obtaining similar BiOI microspheres in Mexican and Chilean research groups.

This article describes a synthetic method to obtain bismuth oxyiodide microspheres, which are highly functional to perform the photocatalytic removal of organic pollutants, such as ciprofloxacin, in water under UV-A/visible light irradiation.

水洗水の光触媒プロセスのビスマス Oxyiodide 微粒子高機能を取得する簡便な合成法

Bismuth oxyhalide (BiOI) is a promising material for sunlight-driven-environmental photocatalysis. Given that the physical structure of this kind of ...

In situ FTIR Spectroscopy as a Tool for Investigation of Gas/Solid Interaction: Water-Enhanced CO2 Adsorption in UiO-66 Metal-Organic Framework

In situ infrared spectroscopy is an inexpensive, highly sensitive, and selective valuable tool to investigate the interaction of polycrystalline solids with adsorbates. Vibrational spectra provide information on the chemical nature of adsorbed species and their structure. Thus, they are very useful for obtaining molecular level understanding of surface species. The IR spectrum of the sample itself gives some direct information about the material. General conclusions can be drawn concerning hydroxyl groups, some stable surface species and impurities. However, the spectrum of the sample is &#34;blind&#34; with respect to the presence of coordinatively unsaturated ions and gives rather poor information about the acidity of surface hydroxyls, species decisive for the adsorption and catalytic properties of the materials. Furthermore, no discrimination between bulk and surface species can be made. These problems are solved by the use of probe molecules, substances that interact specifically with the surface; the alteration of some spectral features of these molecules as a result of adsorption provides valuable information about the nature, properties, location, concentration, etc., of the surface sites.
The experimental protocol for in-situ IR studies of gas/sample interaction includes preparation of a sample pellet, activation of the material, initial spectral characterization through the analysis of the background spectra, characterization by probe molecules, and study of the interaction with a particular set of gas mixtures. In this paper we investigate a zirconium terephthalate metal organic framework, Zr6O4(OH)4(BDC)6 (BDC = benzene-1,4-dicarboxylate), namely UiO-66 (UiO refers to University of Oslo). The acid sites of the UiO-66 sample are determined by using CO and CD3CN as molecular probes. Furthermore, we have demonstrated that CO2 is adsorbed on basic sites exposed on dehydroxylated UiO-66. Introduction of water to the system produces hydroxyl groups acting as additional CO2 adsorption sites. As a result, CO2 adsorption capacity of the sample is strongly enhanced.

In situ FTIR Spectroscopy as a Tool for Investigation of Gas/Solid Interaction: Water-Enhanced CO2 Adsorption in UiO-66 Metal-Organic Framework

The use of FTIR spectroscopy for investigation of the surface properties of polycrystalline solids is described. Preparation of sample pellets, activation procedures, characterization with probe molecules and model studies of CO2 adsorption are discussed.

イン・シチュガス・固体相互作用の調査ツールとしてのFTIR分光法:UiO-66金属有機フレームワークにおける水強化CO2吸着

In situ infrared spectroscopy is an inexpensive, highly sensitive, and selective valuable tool to investigate the interaction of polycrystalline solids ...

Nanoscale Characterization of Liquid-Solid Interfaces by Coupling Cryo-Focused Ion Beam Milling with Scanning Electron Microscopy and Spectroscopy

Physical and chemical processes at solid-liquid interfaces play a crucial role in many natural and technological phenomena, including catalysis, solar energy and fuel generation, and electrochemical energy storage. Nanoscale characterization of such interfaces has recently been achieved using cryogenic electron microscopy, thereby providing a new path to advancing our fundamental understanding of interface processes.
This contribution provides a practical guide to mapping the structure and chemistry of solid-liquid interfaces in materials and devices using an integrated cryogenic electron microscopy approach. In this approach, we pair cryogenic sample preparation which allows stabilization of solid-liquid interfaces with cryogenic focused ion beam (cryo-FIB) milling to create cross-sections through these complex buried structures. Cryogenic scanning electron microscopy (cryo-SEM) techniques performed in a dual-beam FIB/SEM enable direct imaging as well as chemical mapping at the nanoscale. We discuss practical challenges, strategies to overcome them, as well as protocols for obtaining optimal results. While we focus in our discussion on interfaces in energy storage devices, the methods outlined are broadly applicable to a range of fields where solid-liquid interface play a key role.

Cryogenic Focused Ion Beam (FIB) and Scanning Electron Microscopy (SEM) techniques can provide key insights into the chemistry and morphology of intact solid-liquid interfaces. Methods for preparing high quality Energy Dispersive X-ray (EDX) spectroscopic maps of such interfaces are detailed, with a focus on energy storage devices.

クライオ集束イオンビームフライス加工と走査型電子顕微鏡・分光法の結合による液体-固体界面のナノスケール特性評価

Physical and chemical processes at solid-liquid interfaces play a crucial role in many natural and technological phenomena, including catalysis, solar ...

Performing In Situ Closed-Cell Gas Reactions in the Transmission Electron Microscope

Gas reactions studied by in situ electron microscopy can be used to capture the real-time morphological and microchemical transformations of materials at length scales down to the atomic level. In situ closed-cell gas reaction (CCGR) studies performed using (scanning) transmission electron microscopy (STEM) can separate and identify localized dynamic reactions, which are extremely challenging to capture using other characterization techniques. For these experiments, we used a CCGR holder that utilizes microelectromechanical systems (MEMS)-based heating microchips (hereafter referred to as &#34;E-chips&#34;). The experimental protocol described here details the method for performing in situ gas reactions in dry and wet gases in an aberration-corrected STEM. This method finds relevance in many different materials systems, such as catalysis and high-temperature oxidation of structural materials at atmospheric pressure and in the presence of various gases with or without water vapor. Here, several sample preparation methods are described for various material form factors. During the reaction, mass spectra obtained with a residual gas analyzer (RGA) system with and without water vapor further validates gas exposure conditions during reactions. Integrating an RGA with an in situ CCGR-STEM system can, therefore, provide critical insight to correlate gas composition with the dynamic surface evolution of materials during reactions. In situ/operando studies using this approach allow&#160;for detailed investigation of the fundamental reaction mechanisms and kinetics that occur at specific environmental conditions (time, temperature, gas, pressure), in real-time, and at high spatial resolution.

Performing In Situ Closed-Cell Gas Reactions in the Transmission Electron Microscope

Here, we present a protocol for performing in situ TEM closed-cell gas reaction experiments while detailing several commonly used sample preparation methods.

透過型電子顕微鏡 で の密閉セルガス反応の実施

Gas reactions studied by in situ electron microscopy can be used to capture the real-time morphological and microchemical transformations of materials at ...

Characterization of Calcification Events Using Live Optical and Electron Microscopy Techniques in a Marine Tubeworm

Characterizing the first event of biological production of calcium carbonate requires a combination of microscopy approaches. First, intracellular pH distribution and calcium ions can be observed using live microscopy over time. This allows identification of the life stage and the tissue with the feature of interest for further electron microscopy studies. Life stage and tissues of interest are typically higher in pH and Ca signals. 
Here, using H. elegans, we present a protocol to characterize the presence of calcium carbonate structures in a biological specimen on the scanning electron microscope (SEM), using energy-dispersive X-ray spectroscopy (EDS) to visualize elemental composition, using electron backscatter diffraction (EBSD) to determine the presence of crystalline structures, and using transmission electron microscopy (TEM) to analyze the composition and structure of the material. In this protocol, a focused ion beam (FIB) is used to isolate samples with dimension suitable for TEM analysis. As FIB is a site specific technique, we demonstrate how information from the previous techniques can be used to identify the region of interest, where Ca signals are highest.

We demonstrate the use of various microscopy methods that are useful in observing the calcification of a tubeworm, Hydroides elegans, as well as locating and characterizing the first calcified material. Live microscopy and electron microscopy are used together to provide functional and material information that are important in studying biomineralization.

マリンTubewormでライブ光学および電子顕微鏡技術を用いた石灰化イベントのキャラクタリゼーション

Characterizing the first event of biological production of calcium carbonate requires a combination of microscopy approaches. First, intracellular pH ...

その場で液体の SEM を用いた水中のベーマイト粒子のキャラクタリゼーション

要約

さらに動画を探す

この動画の章

VacuSIP、のための改良INEX方法

相図の特徴付け液体担体として磁気ビーズを使用しました

サルヴィとTOF-SIMSによる水中で水和タンパク質のその場キャラクタリゼーションで

発光ベースの湿度センサなどのナノ構造のAg-ゼオライト複合

液体中の振幅変調原子間力顕微鏡でのサブナノメートル分解能イメージング

水洗水の光触媒プロセスのビスマス Oxyiodide 微粒子高機能を取得する簡便な合成法

イン・シチュガス・固体相互作用の調査ツールとしてのFTIR分光法:UiO-66金属有機フレームワークにおける水強化_CO2吸着

クライオ集束イオンビームフライス加工と走査型電子顕微鏡・分光法の結合による液体-固体界面のナノスケール特性評価

透過型電子顕微鏡での密閉セルガス反応の実施

マリンTubewormでライブ光学および電子顕微鏡技術を用いた石灰化イベントのキャラクタリゼーション

その場で液体の SEM を用いた水中のベーマイト粒子のキャラクタリゼーション

要約

さらに動画を探す

この動画の章

VacuSIP、のための改良INEX方法

相図の特徴付け液体担体として磁気ビーズを使用しました

サルヴィとTOF-SIMSによる水中で水和タンパク質のその場キャラクタリゼーションで

発光ベースの湿度センサなどのナノ構造のAg-ゼオライト複合

液体中の振幅変調原子間力顕微鏡でのサブナノメートル分解能イメージング

水洗水の光触媒プロセスのビスマス Oxyiodide 微粒子高機能を取得する簡便な合成法

イン・シチュガス・固体相互作用の調査ツールとしてのFTIR分光法:UiO-66金属有機フレームワークにおける水強化CO2吸着

クライオ集束イオンビームフライス加工と走査型電子顕微鏡・分光法の結合による液体-固体界面のナノスケール特性評価

透過型電子顕微鏡 で の密閉セルガス反応の実施

マリンTubewormでライブ光学および電子顕微鏡技術を用いた石灰化イベントのキャラクタリゼーション

イン・シチュガス・固体相互作用の調査ツールとしてのFTIR分光法:UiO-66金属有機フレームワークにおける水強化_CO2吸着

透過型電子顕微鏡での密閉セルガス反応の実施