Wir sind dankbar, Pacific Northwest National Laboratory (PNNL) nuklearen Prozess Science Initiative (NPSI)-Labor leitete Forschung und Entwicklung (LDRD) Fonds für die Unterstützung. Dr. Sayandev Chatterjee vorgesehen die synthetisierte Böhmit Partikel. Instrumental wurde durch W. R. Wiley Umwelt Molecular Sciences Laboratory (EMSL) allgemeine Benutzer Vorschlag zur Verfügung. EMSL ist eine nationale wissenschaftliche Benutzer Einrichtung Büro der biologischen und ökologischen Forschung (BER) auf PNNL gesponsert. Battelle für DOE unter Vertrag DE AC05 76RL01830 PNNL gesteuert.

<ol>
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A., 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=.">.</a> Scanning Electron Microscopy (SEM) and Environmental SEM: Suitable Tools for Study of Adhesion Stage and Biofilm Formation. , (2012).</li><li>Thiberge, S. 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B., Buchanan, M., Wilmarth, B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Basic Research Needs for Environmental Management. , (2016).</li><li>Mills, O. P., Rose, W. I. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Shape+and+surface+area+measurements+using+scanning+electron+microscope+stereo-pair+images+of+volcanic+ash+particles.">Shape and surface area measurements using scanning electron microscope stereo-pair images of volcanic ash particles.</a> Geosphere. 6, 805-811 (2010).</li><li>Li, S., Jiang, F., Yin, Q., Jin, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Scanning+electron+acoustic+microscopy+of+semiconductor+materials.">Scanning electron acoustic microscopy of semiconductor materials.</a> Solid State Commun. 99 (11), 853-857 (1996).</li><li>Dohnalkova, A. C., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Imaging+Hydrated+Microbial+Extracellular+Polymers:+Comparative+Analysis+by+Electron+Microscopy.">Imaging Hydrated Microbial Extracellular Polymers: Comparative Analysis by Electron Microscopy.</a> Appl Environ Microbiol. 77 (4), 1254-1262 (2011).</li><li>Yu, X. -. Y., Liu, B., Yang, L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Imaging+liquids+using+microfluidic+cells.">Imaging liquids using microfluidic cells.</a> Microfluid Nanofluid. 15 (6), 725-744 (2013).</li><li>Barshack, I., 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=A+Novel+Method+for+"Wet"+SEM.">A Novel Method for "Wet" SEM.</a> Ultrastruct Pathol. 28 (1), 29-31 (2004).</li><li>Cameron, R. E., Donald, A. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Minizing+sample+evaporation+in+the+Environmental+Scanning+Microscope.">Minizing sample evaporation in the Environmental Scanning Microscope.</a> J Microsc. (Oxford, U. K.). 173 (3), 227-237 (1994).</li><li>Danilatos, G. 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Die Autoren haben nichts preisgeben.

SEM ist eine leistungsfähige Technik in Oberflächencharakterisierung von organischen und anorganischen Materialien auf ein Niveau von nanoskaligen (nm) mit hoher Auflösung1. Beispielsweise ist es für die Analyse von festen und trockenen Proben wie geologischen Materialien26 und Halbleiter27verbreitet. Es hat jedoch Einschränkungen bei der Charakterisierung von Feuchte und flüssige Proben durch die Unvereinbarkeit der Flüssigkeit innerhalb der ...

Rasterelektronenmikroskop (REM) hat weit angewendet worden, um eine Vielzahl von Proben zu untersuchen, indem Sie produzieren hochauflösende Bildgebung1. Die Energie energiedispersiver Röntgenspektroskopie (EDX) verbunden mit dem REM ermöglicht die Bestimmung der Elementarzusammensetzung1. Traditionell wird SEM für imaging nur trockene und feste Proben angewendet. In den letzten 30 Jahren entwickelte sich die Umwelt SEM (ESEM) für die Analyse von hydratisierten Teilstichproben in einem Dampf-Umgebung2,3,4,5. ESEM ist jedoch nicht in der Lage, die nassen, voll flüssigen Proben mit hoher Auflösung6Bild. Nassen SEM Zellen entstanden auch an Bild nasse Exemplare mit SEM7,8; Dennoch, diese Zellen wurden hauptsächlich für biologische Proben entwickelt zurückgestreuten Elektronen Bildgebung und sind leichter zugänglich für Anwendungen mit diesen Designs9,10.
Zur Bewältigung die Herausforderungen bei der Analyse von verschiedenen Proben in ihrer natürlichen flüssigen Umgebung mit SEM, erfanden wir eine Vakuum kompatibel mikrofluidischen Gerät, System zur Analyse an den flüssigen Vakuum Schnittstelle (SALVI), ermöglichen hohen räumlichen Auflösung sekundäre Elektronen (SE) Bildgebung und elementare Analyse von flüssigen Proben mit hohen Vakuumbetrieb in SEM Diese neuartige Technik umfasst die folgenden einzigartigen Eigenschaften: 1) Flüssigkeit wird direkt in eine kleine Öffnung von 1-2 µm im Durchmesser; sondiert (2) Flüssigkeit wird in der Bohrung durch Oberflächenspannung gehalten; und 3) SALVI ist portabel und kann auf mehr als eine analytische Plattform11,12,13,14,15,16,17 angepasst werden ,18.
SALVI besteht aus einer 100 nm dicken Silizium-Nitrid (SiN) Membran und einem 200 µm breite Microchannel aus Polydimethylsiloxan (PDMS) Block. Die Sünde Membran Fenster wird angewendet, um die Microchannel zu versiegeln. Die Verarbeitungsdetails und wichtigsten Entwurfsüberlegungen waren in früheren Arbeiten und Patente11,19,20detailliert. Derzeit hat ein führender Hersteller und Vertreiber von Verbrauchsmaterial Lieferung für die Mikroskopie die Lizenz um SALVI Geräte kommerziell für flüssige SEM Anwendungen21,22zu verkaufen gekauft.
Die Einsatzmöglichkeiten von SALVI in Vakuum-analytische Instrumente wurden nachgewiesen unter Verwendung einer Vielzahl von wässrigen Lösungen und komplexe Flüssigkeitsgemischen einschließlich Biofilme, Säugerzellen, Nanopartikeln und Elektrode Materialien12, 14 , 17 , 20 , 23 , 24. jedoch die meisten der oben genannten Arbeiten Time-of-Flight secondary Ion mass Spectrometry (ToF-SIMS) als wichtigen Analyse-Tool, damit die Anwendung der Flüssigkeit genutzt SEM mit SALVI nicht vollständig erforscht. In diesem Werk wurde SALVI zur größere nicht-sphärische kolloidale Teilchen in Flüssigkeit mit flüssigen SEM Bildgebung und EDX Elementaranalyse zu studieren. Das Beispiel besteht aus AlOOH Teilchen in unserem Labor synthetisiert. Submikrometer-mittlere Böhmit Partikel sind dafür bekannt, in hochradioaktiver Abfälle an der Hanford Site vorhanden sind. Sie sind langsam aufzulösen und in Abfallbehandlung rheologische Probleme verursachen können. Daher ist es wichtig, die Möglichkeit, Böhmit Teilchen in Flüssigkeit25charakterisieren. Dieser technische Ansatz kann verwendet werden, um Böhmit in verschiedenen physikalisch-chemischen Bedingungen für besseres Verständnis dieser Partikel und verwandte rheologischen Eigenschaften zu studieren. Diese Partikel wurden genutzt, um Schritt für Schritt zeigen, wie man Hochvakuum SEM SALVI zuweisen, um Schwebeteilchen in Flüssigkeit zu studieren. Technische Eckpunkte für SALVI und SEM Integration und SEM Datenerfassung werden in das Papier hervorgehoben.
Das Protokoll sieht Demonstration der flüssigen Probenanalyse mit SALVI und flüssigen SEM Bildgebung für diejenigen, die bei der Nutzung dieser neuartigen Technik in vielfältigen Einsatzmöglichkeiten von flüssigen SEM in der Zukunft interessiert.

<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

In Situ imaging und elementare Analyse von Böhmit (AlOOH) Partikeln im Wasser erfolgt mit dem System für die Analyse an der flüssigen Vakuum-Schnittstelle (SALVI) und Scanning Electron Microscopy (SEM). Dieses Paper beschreibt die Methode und wichtige Schritte bei der Integration des Vakuums kompatibel SAVLI SEM und Sekundär-Elektronen (SE) Bilder von Partikeln in Flüssigkeiten im Hochvakuum. Energie energiedispersiver Röntgenspektroskopie (EDX) dient zur Elementaranalyse von Partikeln in Flüssigkeiten und Kontrolle Proben einschließlich deionisiertes (DI) nur Wasser und einen leeren Kanal sowie zu erhalten. Synthetisierte Böhmit (AlOOH) Partikeln, die in der Flüssigkeit ausgesetzt sind als Modell in der flüssigen SEM Abbildung verwendet. Die Ergebnisse zeigen, dass die Partikel im SE-Modus mit guter Auflösung abgebildet werden können (d.h., 400 nm). Das AlOOH EDX-Spektrum zeigt signifikantes Signal aus Aluminium (Al) im Vergleich mit dem DI-Wasser und den leeren Kanal-Steuerung. In Situ flüssige SEM ist eine leistungsstarke Technik, Teilchen in Flüssigkeit mit viele interessante Anwendungen zu studieren. Dieses Verfahren zielt darauf ab, technisches Know-how, um flüssige SEM Bildgebung und EDX-Analyse mit SALVI zu betreiben und um potenzielle Fallstricke zu reduzieren, bei Verwendung dieser Methode bieten.

Die repräsentative Ergebnisse um zu zeigen, wie die Partikel abgebildet werden und mittels in Situ flüssige SEM Bildgebung gepaart mit EDX analysiert. Die Ergebnisse umfassen SE Bilder und EDX-Spektren. Die SE Bilder wurden auf X 100.000 und 200.000 X Vergrößerung Ebene in Abbildung 1erhalten. Abbildung 1a zeigt das SE Bild der AlOOH, Abb. 1 b DI-Wasser und Abbildung...

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

In Situ Charakterisierung von Böhmit Teilchen im Wasser mit flüssigem SEM

Wir präsentieren ein Verfahren zur Echtzeit-Bildverarbeitung und Analyse der Elementzusammensetzung Böhmit Partikel in entionisiertem Wasser durch in Situ Flüssigkeit Scanning Electron Microscopy.

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

in-situ-characterization-boehmite-particles-water-using-liquid

Universidad San Sebastian

Research

JoVE Journal

Chemistry

In Situ Characterization of Boehmite Particles in Water Using Liquid SEM

9.2K Aufrufe.  Pacific Northwest National Laboratory. Wir präsentieren ein Verfahren zur Echtzeit-Bildverarbeitung und Analyse der Elementzusammensetzung Böhmit Partikel in entionisiertem Wasser durch in Situ Flüssigkeit Scanning Electron Microscopy.

Serie: 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 eine verbesserte Inex Methode für<em&gt; In Situ</em&gt; Messung von partikulären und gelösten Verbindungen, die durch Active Suspension Feeders Verarbeitet

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

Forschung

Umwelt

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.

Phasendiagramm Charakterisierung mit Magnetic Beads als flüssige Träger

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 ...

Ingenieurwesen

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.

In-situ-Charakterisierung von Hydrated Proteine ​​in Wasser durch SALVI und TOF-SIMS

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

Chemie

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.

Nanostrukturierte Ag-Zeolith-Komposite als Lumineszenz-basierte Feuchtigkeitssensoren

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.

Sub-Nanometer Auflösung Belichtung mit Amplituden-Modulation der Rasterkraftmikroskopie 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 ...

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.

Ein Facile synthetische Methode, Wismut Oxyiodide Mikrosphären hochfunktionelle der photokatalytischen Prozesse der Wasser Depuration zu erhalten

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.

In situ FTIR Spektroskopie als Werkzeug zur Untersuchung von Gas/Feststoff-Wechselwirkungen: Wasserverstärkte 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 ...

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.

Nanoskalige Charakterisierung von Flüssig-Fest-Grenzflächen durch Kopplung von kryofokussiertem Ionenstrahlfräsen mit Rasterelektronenmikroskopie und Spektroskopie

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.

Durchführung von geschlossenzelligen In-situ-Gasreaktionen im Transmissionselektronenmikroskop

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.

Charakterisierung von Verkalkungen Events Verwendung von Live-optische und Elektronenmikroskopie-Techniken in einem Marine-Tubeworm

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

In Situ Charakterisierung von Böhmit Teilchen im Wasser mit flüssigem SEM

Zusammenfassung

Weitere Videos entdecken

Kapitel in diesem Video

VACUSIP eine verbesserte Inex Methode für

Phasendiagramm Charakterisierung mit Magnetic Beads als flüssige Träger

In-situ-Charakterisierung von Hydrated Proteine in Wasser durch SALVI und TOF-SIMS

Nanostrukturierte Ag-Zeolith-Komposite als Lumineszenz-basierte Feuchtigkeitssensoren

Sub-Nanometer Auflösung Belichtung mit Amplituden-Modulation der Rasterkraftmikroskopie in Liquid

Ein Facile synthetische Methode, Wismut Oxyiodide Mikrosphären hochfunktionelle der photokatalytischen Prozesse der Wasser Depuration zu erhalten

In situ FTIR Spektroskopie als Werkzeug zur Untersuchung von Gas/Feststoff-Wechselwirkungen: Wasserverstärkte CO2-Adsorption in UiO-66 Metal-Organic Framework

Nanoskalige Charakterisierung von Flüssig-Fest-Grenzflächen durch Kopplung von kryofokussiertem Ionenstrahlfräsen mit Rasterelektronenmikroskopie und Spektroskopie

Durchführung von geschlossenzelligen In-situ-Gasreaktionen im Transmissionselektronenmikroskop

Charakterisierung von Verkalkungen Events Verwendung von Live-optische und Elektronenmikroskopie-Techniken in einem Marine-Tubeworm

In Situ Charakterisierung von Böhmit Teilchen im Wasser mit flüssigem SEM

Zusammenfassung

Weitere Videos entdecken

Kapitel in diesem Video

VACUSIP eine verbesserte Inex Methode für

Phasendiagramm Charakterisierung mit Magnetic Beads als flüssige Träger

In-situ-Charakterisierung von Hydrated Proteine ​​in Wasser durch SALVI und TOF-SIMS

Nanostrukturierte Ag-Zeolith-Komposite als Lumineszenz-basierte Feuchtigkeitssensoren

Sub-Nanometer Auflösung Belichtung mit Amplituden-Modulation der Rasterkraftmikroskopie in Liquid

Ein Facile synthetische Methode, Wismut Oxyiodide Mikrosphären hochfunktionelle der photokatalytischen Prozesse der Wasser Depuration zu erhalten

In situ FTIR Spektroskopie als Werkzeug zur Untersuchung von Gas/Feststoff-Wechselwirkungen: Wasserverstärkte CO2-Adsorption in UiO-66 Metal-Organic Framework

Nanoskalige Charakterisierung von Flüssig-Fest-Grenzflächen durch Kopplung von kryofokussiertem Ionenstrahlfräsen mit Rasterelektronenmikroskopie und Spektroskopie

Durchführung von geschlossenzelligen In-situ-Gasreaktionen im Transmissionselektronenmikroskop

Charakterisierung von Verkalkungen Events Verwendung von Live-optische und Elektronenmikroskopie-Techniken in einem Marine-Tubeworm

In-situ-Charakterisierung von Hydrated Proteine in Wasser durch SALVI und TOF-SIMS