JEOL Resourceshttps://www.jeolusa.com/RESOURCES/Electron-Optics/Documents-Downloads(S)TEM Tomographyhttps://www.jeolusa.com/RESOURCES/Electron-Optics/Documents-Downloads/stem-tomographyTransmission Electron Microscope (TEM)Wed, 05 Oct 2022 13:21:34 GMTTomography is a technique that employs a series of images successively recorded from an object at different tilt angles with respect to the electron beam in order to obtain that object’s three-dimensional structure using a back projection technique. The images can be recorded in a Transmission Electron Microscope (TEM) or a Scanning Transmission Electron Microscope (STEM). JEOL have adopted SerialEM (Boulder laboratory for 3D electron microscopy of cells BL3DEMC) to either modality making tomography an accessible, efficient and easy technique for all aspects of scientific, industrial and medical research.<p>The modality of imaging depends primarily on the object being studied. For example, structures that show strong diffraction effects, very common in Materials, tend to be studied most effectively in STEM mode using images acquired on a High Angle Annular Detector (HAADF). Conversely, specimens in Life Sciences, characterized by an abundance of low Z elements and thus fairly devoid of diffraction effects, tend to be studied mostly using TEM bright field. SerialEM tomography can be applied to all TEMs in the JEOL line-­up thus providing a solution for every aspect of microscopy that targets 3D structures.</p> <p>Tomography is applicable to a wide variety of samples, such as ranging from beam-­resistant FIB lift-­out to frozen-­hydrated specimens. A low-­dose option in SerialEM tomography allows specimens to be imaged whilst in their native state, i.e., after vitrification. Entire tomographic series can be obtained without visibly damaging the sample (Fig. 2). JEOL USA’s choice for tomography includes processing using IMOD (also available from the BL3DEMC).</p> <p style="text-align: center;"><img alt="Fig.2: 3D rendering in chimera of frozen-­hydrated vesicles coated with viral proteins after tomography in a JEM-­3200FSC at 300 kV and 20 eV zero-­loss imaging. Processing included NAD filtering (Sample courtesy of B. Russin, Northwestern U.)" class="img-responsive" src="https://jeolusa.s3.amazonaws.com/resources_eo/(S)TEM%20Tomography%20002.jpg?AWSAccessKeyId=AKIAQJOI4KIAZPDULHNL&Expires=2145934800&Signature=5mkSX4VJO8vicdk%2FaYnN12SbjYo%3D" /><br /> <strong>Fig.2:</strong> 3D rendering in chimera of frozen-­hydrated vesicles coated with viral proteins after tomography in a JEM-­3200FSC at 300 kV and 20 eV zero-­loss imaging. Processing included NAD filtering (Sample courtesy of B. Russin, Northwestern U.)</p> <p>The low-­dose option also allows the use of extremely high magnification for imaging, as is the case for instance in STEM mode (Fig.3). The ability to perform critical steps in tomography, such as tracking, focusing and recording the final image, at different magnifications, ensures the operator that the object of interest remains on the camera/detector under all conditions as the sample is being tilted.</p> <p style="text-align: center;"><img alt="Fig. 3: 3D rendering in chimera of catalytic sample acquired in HAADF STEM mode in a JEM-­ARM200CF (Sample courtesy of R. Klie, UIC)." class="img-responsive" src="https://jeolusa.s3.amazonaws.com/resources_eo/(S)TEM%20Tomography%20003.jpg?AWSAccessKeyId=AKIAQJOI4KIAZPDULHNL&Expires=2145934800&Signature=IQSP06Q2Xvl3xLvZS7Y6g%2FoZ5JE%3D" /><br /> <strong>Fig. 3:</strong> 3D rendering in chimera of catalytic sample acquired in HAADF STEM mode in a JEM-­ARM200CF (Sample courtesy of R. Klie, UIC).</p> <p>Tomography is now also being applied in the field of diagnostic imaging, for instance in primary ciliary dyskineasia (see Brink and Carson, MSA Proc. (2010) 16: 970). Shown is a cilia cross section that has been obtained after applying 3D imaging by tomography. The reconstruction is rotated so as to yield views that are identical to perfect axial cross sections through the cilia (Fig. 4). Note the microtubule doublets in this view indicating the proper orientation of the cilia. A reliable workflow can thus be established that gives quick answers as this reconstruction can be obtained in roughly 30 minutes.</p> <p>Finally, SerialEM has the ability to capture large-scale montages as exemplified in the work from the Marc lab at University of Utah (Fig.4).</p> <p style="text-align: center;"><img alt="Fig. 4: 3D rendered cilia from sick patient after SerialEM tomography in a JEM-­1400 showing the disconnected dynein arms (Sample courtesy of Dr. Carson, UNC)." class="img-responsive" src="https://jeolusa.s3.amazonaws.com/resources_eo/(S)TEM%20Tomography%20004.jpg?AWSAccessKeyId=AKIAQJOI4KIAZPDULHNL&Expires=2145934800&Signature=iRamGgqTlykw%2FwjD6PNitkfMqkY%3D" /><br /> <strong>Fig. 4:</strong> 3D rendered cilia from sick patient after SerialEM tomography in a JEM-­1400 showing the disconnected dynein arms (Sample courtesy of Dr. Carson, UNC).</p> <p>Montages such as these are at the fingertips of researchers through a robust and easy to set up GUI in SerialEM. The montaging feature makes use of either stage-based or deflector-based navigation.</p> <p style="text-align: center;"><img alt="Fig. 5: Montage of mouse retina obtained in a JEM-­1400 using SerialEM stage-­based montaging. The area measures approx. 0.5 x 0.5 mm and was imaged at a magnification of 5000x. The montage contains circa 1000 images acquired from the 4k x 4k CCD camera." class="img-responsive" src="https://jeolusa.s3.amazonaws.com/resources_eo/(S)TEM%20Tomography%20005.jpg?AWSAccessKeyId=AKIAQJOI4KIAZPDULHNL&Expires=2145934800&Signature=dwxyQA8bgJCG7wbG%2BJmNMWS%2Fnyg%3D" /><br /> <strong>Fig. 5:</strong> Montage of mouse retina obtained in a JEM-­1400 using SerialEM stage-­based montaging. The area measures approx. 0.5 x 0.5 mm and was imaged at a magnification of 5000x. The montage contains circa 1000 images acquired from the 4k x 4k CCD camera.</p> 1.8 Å resolution structure of β-galactosidase with a 200 kV CRYO ARM electron microscopehttps://www.jeolusa.com/RESOURCES/Electron-Optics/Documents-Downloads/18-resolution-structure-of-galactosidase-with-a-200-kv-cryo-arm-electron-microscopeCRYO ARM™ 200Thu, 10 Dec 2020 11:35:20 GMTAs seen in IUCrJ Volume 7, July 2020, pages 639-643.<p>See <a href="https://journals.iucr.org/m/issues/2020/04/00/eh5008/index.html" target="_blank">IUCrJ Volume 7, July 2020, pages 639-643</a>.</p> A Guide to Scanning Microscope Observationhttps://www.jeolusa.com/RESOURCES/Electron-Optics/Documents-Downloads/a-guide-to-scanning-microscope-observationScanning Electron Microscope (SEM)Thu, 02 Apr 2020 12:53:57 GMTWe included in this book as many application examples as possible so that they can be used as criteria for judging what causes unsatisfactory image factors (hereinafter referred to as image disturbances). Although this edition does not describe all about image disturbances, it carries application photos to allow you to consider their causes. It is also important to correctly select the optimum observation conditions for various specimens. For instance, this book carries matters which are considered to be useful for using the instrument, such as the accelerating voltage, probe current and working distance (hereinafter abbreviated to WD).<p>We included in this book as many application examples as possible so that they can be used as criteria for judging what causes unsatisfactory image factors (hereinafter referred to as image disturbances). Although this edition does not describe all about image disturbances, it carries application photos to allow you to consider their causes. It is also important to correctly select the optimum observation conditions for various specimens. For instance, this book carries matters which are considered to be useful for using the instrument, such as the accelerating voltage, probe current and working distance (hereinafter abbreviated to WD).</p> <p>We shall be pleased if this publication is of help to people who are now using or going to use SEMS.</p> A New Take on the Phase Platehttps://www.jeolusa.com/RESOURCES/Electron-Optics/Documents-Downloads/a-new-take-on-the-phase-plate200kVThu, 10 Dec 2020 11:40:13 GMTTEM phase plate development was extensively pursued by Prof Nagayama’s lab in Japan for over ten years. Prof Chiu of Baylor College of Medicine has successfully applied the phase plate system on his Omega filtered TEM (JEM-2200FS) to the molecular structure characterization for proteins.<p>TEM phase plate development was extensively pursued by Prof Nagayama’s lab in Japan for over ten years. Prof Chiu of Baylor College of Medicine has successfully applied the phase plate system on his Omega filtered TEM (JEM-2200FS) to the molecular structure characterization for proteins.</p> <p>A reprint from <i>Lab Product News.</i></p> A Note on Magnificationhttps://www.jeolusa.com/RESOURCES/Electron-Optics/Documents-Downloads/a-note-on-magnificationIT200Mon, 02 Nov 2020 12:04:09 GMTSEM manufacturers can choose different output sizes for their images, making magnification a very deceptive number when comparing SEM micrographs from different SEM manufacturers. Because of this fact, the best way to compare images is to compare the length of the micron bar or field of view.<h4>JEOL Technical Note</h4> <p>Magnification is defined as the ratio of the size of the rastered area on the sample to the size of the rastered area of the output, as is shown in Figure 1. Traditionally, the output size was defined as a Polaroid 4x5 film size by all vendors and results were easy to compare. However, since images are now collected digitally and can be output at various sizes, this “output size” is ill-defined. SEM manufacturers can choose different output sizes for their images, making magnification a very deceptive number when comparing SEM micrographs from different SEM manufacturers. Because of this fact, the best way to compare images is to compare the length of the micron bar or field of view.</p> <p class="caption" style="text-align: center;"><img alt="" src="https://jeolusa.s3.amazonaws.com/resources_eo/A%20Note%20on%20Magnification%20fig1.png?AWSAccessKeyId=AKIAQJOI4KIAZPDULHNL&Expires=2145934800&Signature=qwBAKbK5vdFXBnMuqKvDTHaPuWU%3D" /><br /> <strong>Figure 1</strong>: A small raster on the specimen leads to a large magnification for the same output size.</p> <p>The SEM images of hematite from two different SEM manufacturers below illustrate this point. The left image is from a JEOL SEM and has a magnification labeled as 75,000 X with a 100 nm micron bar. The right image is from another SEM manufacturer and has a magnification labeled as 150,000 X with the exact same length 100 nm scale bar (highlighted in red). This shows that the enlargement of the sample is identical in the two images, even though the magnification value stated by the other SEM manufacturer is twice that of the JEOL image.</p> <p class="caption" style="text-align: center;"><img alt="" class="img-responsive" src="https://jeolusa.s3.amazonaws.com/resources_eo/A%20Note%20on%20Magnification%20fig2.png?AWSAccessKeyId=AKIAQJOI4KIAZPDULHNL&Expires=2145934800&Signature=ee9XnW4z%2FNODAGjnIrjYn%2B%2Bz9%2Fg%3D" /><br /> <strong>Figure 2</strong>: SEM images of hematite with the same enlargement of the sample despite having different magnification values stated. Left image: From a JEOL SEM Right image: From a different SEM manufacturer</p> A sneak peek inside tomorrow’s lithium-ion batterieshttps://www.jeolusa.com/RESOURCES/Electron-Optics/Documents-Downloads/a-sneak-peek-inside-tomorrows-lithium-ion-batteriesScanning Electron Microscope (SEM)Sat, 21 May 2022 17:50:43 GMTTo build better lithium-ion batteries, scientists are using advanced imaging and analysis tools to fine-tune battery materials.<h2>To build better lithium-ion batteries, scientists are using advanced imaging and analysis tools to fine-tune battery materials.</h2> <p style="text-align: center;"><img alt="" class="img-responsive" src="https://jeolusa.s3.amazonaws.com/resources_eo/A%20sneak%20peek%20inside%20tomorrow%E2%80%99s%20lithium-ion%20batteries.jpg?AWSAccessKeyId=AKIAQJOI4KIAZPDULHNL&Expires=2145934800&Signature=gBDPJvBHWwTMLJi4GzvWB%2F2vqmk%3D" /><br /> New sample analysis and visualization tools are yielding clear images of what happens when lithium-ion batteries charge and discharge, such as this 250X scanning electron micrograph of a sample created using a cryo-cooled cross-section polisher.</p> <p>Demand for rechargeable batteries is soaring, driven by electric vehicles, renewable energy storage, and portable electronics. Lithium-ion batteries attract the most attention because of their combination of longevity, rechargeability and low cost. Yet today’s lithium-ion systems are far from perfect — just ask anyone whose mobile phone died by mid-afternoon, or whose electric car took hours to recharge.</p> <p>Tomorrow’s batteries will have to do better, and that presents a challenge. “People want to have batteries with longer cycle life. We want higher energy density. We want higher capacity,” says Grace Gorman, senior director for characterization and failure analysis at Enovix, a company in Fremont, California, that’s developing new batteries for a variety of uses.</p> <p>Researchers have many potential ways to improve lithium-ion battery performance, ranging from new materials for electrodes to replacing liquid with solid electrolytes. But developing high-performing batteries means understanding lithium’s behavior inside them, and lithium has been loath to give up its secrets. Thanks to new imaging and analysis techniques, however, researchers are learning more about how the lightest of metals behaves in complex battery systems.</p> <h3>Replacement anodes</h3> <p>Whether it’s an iPhone, a laptop, or a car drawing power, what happens in a lithium-ion battery that’s discharging is similar to what happens in the familiar AA battery that has been powering devices for years. Positively charged ions move from the anode to the cathode through an electrolyte — a substance that allows the flow of charge. In lithium-ion batteries, positively charged lithium ions move from anode to cathode through a solution of lithium salts in a mixture of organic solvents. At the same time, electrons from the anode pass to the cathode through the laptop or whatever is drawing power, completing the circuit. When the battery is charging, the process reverses.</p> <p>In most of today’s lithium-ion batteries, the anode is made of graphite, a heat-resistant, crystalline form of carbon that can store lithium ions. The cathode consists of a lithium-containing compound, such as lithium cobalt oxide. Since lithium is the lightest metal and the third-lightest element, after hydrogen and helium, a lithium-ion battery can store 50% more energy per unit weight than older rechargeable battery chemistries that use heavier metals, such as nickel-cadmium or nickel-metal hydride batteries.</p> <p>The Enovix team is one of many that seek to increase energy density further by replacing the graphite anode with silicon, which can hold approximately 10 times as many lithium ions as graphite. This would offer a boost of between 15 and 30%, depending on the anode’s design.</p> <p>Such gains, however, come at a price: anodes expand as they absorb lithium ions, and as they move through charge-discharge cycles, this swelling generates mechanical forces that crack and degrade the anodes over time. But while graphite expands by about 10%, silicon anodes can quadruple in size, making them more vulnerable to degradation.</p> <h3>Visualizing lithium</h3> <p>Battery performance also depends on how lithium ions move through the electrolyte, and where precisely lithium ions sit within the cathode and anode. For that reason, battery makers seek detailed information about lithium’s behavior so they can fine-tune the device’s microstructure.</p> <p>Enovix’s researchers do this by imaging samples of a battery system at different points during the charge-discharge cycle. But here lithium’s small size becomes a disadvantage. Techniques for localizing atoms often rely on measuring how x-rays scatter as they interact with the electrons of a material. With just three electrons, lithium does not scatter X-rays as strongly as heavier atoms, and those scattered X-rays have very low energy, causing the signal they produce to be drowned out by stronger signals from other materials in the battery.</p> <p>“It's always a challenge to figure out where the lithium is,” Gorman says. “Lithium is very hard to detect, and a lot of techniques struggle with either the spatial resolution or the quantity.”</p> <p>What’s more, the same X-rays that visualize lithium ions can also knock lithium and other atoms out of place, damaging the battery material. To avoid this, Enovix researchers combine two techniques that together cause less damage and help find the hidden lithium.</p> <p>The first method, called soft X-ray emission spectroscopy (SXES), uses X-rays that have longer wavelengths than conventional, or hard, X-rays and are less energetic. These soft X-rays do not illuminate a material’s atoms as intensely as hard X-rays, reducing the background noise in SXES. This makes it easier for researchers to observe the weak lithium signal, says Patrick Phillips, assistant product manager for transmission electron microscopy at JEOL USA, a manufacturer of electron microscopes and other analytical instruments, including the soft X-ray spectrometer that Gorman used.</p> <p>The second method, called optimum bright-field imaging, was developed at the University of Tokyo and commercialized by JEOL. It uses a modified X-ray detector that separately visualizes images obtained using different X-ray frequencies and recombines them into a high-resolution image. This lowers the overall X-ray dose, protecting the material, while improving the signal-to-noise ratio.</p> <p>“The [optimum bright-field] imaging technique allows the researchers to look at a sample and to pick out exactly where the lithium atoms are,” says Tom Isabell, a materials scientist and vice president at JEOL.</p> <h3>Air-free analysis</h3> <p>Lithium-ion batteries are typically closed systems that react when exposed to air. To spot atoms of lithium and other elements in experimental batteries, Yan Yao, a materials scientist at the University of Houston, studies samples from batteries in an air-free environment.</p> <p>Yao is experimenting with different battery chemistries, such as replacing the transition metals used in cathodes with organic materials, which are cheaper and more readily available. To test each battery, he charges and discharges it, while watching how its materials change. He prepares samples with a JEOL ion-beam cross-section polisher that slices through various layers of the battery, leaving an even surface without imperfections. Then he uses a special sample holder he designed to move the sample from, say, a scanning electron microscope to a transmission electron microscope, without exposing it to air.</p> <p>Yao is also working on devices made with solid, rather than liquid, electrolytes. He has observed how defects along the interface between the electrode and the solid electrolyte develop cracks as the electrode expands and contracts. This causes lithium atoms to form finger-like crystalline growths called dendrites that eventually grow large enough to short-circuit the device. Visualizing dendrite growth is critical to understanding the failure mechanisms that researchers must address. “It’s very hard to predict where the cell will fail,” Yao says. “But now, with this tool, we actually are able to pinpoint the source of the failure.”</p> <p>And when it comes to understanding battery materials, imaging tools that predict failure may be the key to success. “These detectors are becoming faster,” JEOL’s Phillips says. “The cameras are getting better. Almost every aspect of the research is improving constantly.”</p> <p>To learn more about imaging methods that are fueling advanced battery research, click <a href="https://go.jeolusa.com/l/234012/2022-01-12/mztwsy">here</a>.</p> Ad-hoc Auto Tuninghttps://www.jeolusa.com/RESOURCES/Electron-Optics/Documents-Downloads/ad-hoc-auto-tuningNEOARMThu, 10 Dec 2020 11:09:18 GMTAuto Tuning for HR-STEM for crystalline sample.<p>Auto Tuning for HR-STEM for crystalline sample.</p> Advantages of Benchtop Scanning Electron Microscopy vs. Optical Microscopy for Pharmaceutical Applicationshttps://www.jeolusa.com/RESOURCES/Electron-Optics/Documents-Downloads/advantages-benchtop-scanning-electron-microscopy-vs-optical-microscopy-pharmaceutical-applicationsNeoScope™ Benchtop SEMSat, 20 Jan 2024 20:32:17 GMTWith the JEOL NeoScope Benchtop SEM, pharmaceutical companies gain a robust and versatile tool for analyzing substance morphology, topography and composition right from within their own laboratory environment. The small footprint and intuitive operation make it easy for any lab personnel to conduct the high resolution imaging and analysis that only an SEM can deliver.<p style="text-align: center;"><img alt="Optical microscope image (left) vs. Scanning Electron Microscope (SEM) image (right) of pharmaceutical tablet." src="https://jeolusa.s3.amazonaws.com/resources_eo/NeoScope%20for%20pharmaceuticals%2001.jpg?AWSAccessKeyId=AKIAQJOI4KIAZPDULHNL&Expires=2145934800&Signature=3WkDMib5MNxdPqWaX7HBAWoAOQM%3D" /><br /> <em>Optical microscope image (left) vs. Scanning Electron Microscope (SEM) image (right) of pharmaceutical tablet.</em></p> <p>Throughout the discovery and manufacturing phases of bringing pharmaceuticals to market, scanning electron microscopy (SEM) plays a pivotal role in design and quality control. For visual inspection, the benchtop SEM far surpasses the capabilities of traditional optical or light microscopy with its large depth of field and functionality.</p> <h2>Quality Imaging and Resolution</h2> <p>With SEM it is possible to observe the compositional contrast that cannot be seen on an optical image.  Examination of a pharmaceutical tablet or powder sample in the benchtop SEM reveals greater detail and compositional contrast than can be achieved with optical microscopes, even at the same magnification. With magnification up to 100,000X and versatile, automated settings, the SEM makes it possible to easily inspect the microstructure of tablets and powders, textures and coatings, foreign particles, and their chemical composition. Using the benchtop SEM, it is possible to identify the source of contamination from manufacturing processes.</p> <p style="text-align: center;"><img alt="SEM Image and EDS Analysis of Foreign Particle Contaminants (Metal and Glass)" src="https://jeolusa.s3.amazonaws.com/resources_eo/NeoScope%20for%20pharmaceuticals%2002.jpg?AWSAccessKeyId=AKIAQJOI4KIAZPDULHNL&Expires=2145934800&Signature=VLhUOFnWILszIhCI5WxCxXOJpV8%3D" /><br /> <em>SEM Image and EDS Analysis of Foreign Particle Contaminants (Metal and Glass)</em></p> <p>The JEOL benchtop SEM offers 100,000X magnification and selectable settings for imaging: backscattered electrons to reveal morphology and topography and give insight as to composition, or secondary electrons to reveal surface topography.</p> <p>Adding to these characterization capabilities, the JEOL NeoScope SEM has a 3D imaging feature for surface reconstruction using the multi-segmented BSE detector and automated montaging for high resolution view of a larger area.</p> <p style="text-align: center;"><img alt="Live 3D Surface Reconstruction – Pharmaceutical Tablet" src="https://jeolusa.s3.amazonaws.com/resources_eo/NeoScope%20for%20pharmaceuticals%2003.jpg?AWSAccessKeyId=AKIAQJOI4KIAZPDULHNL&Expires=2145934800&Signature=r9kLWcCKeTqw3vVQ%2BHO545XSSkc%3D" /><br /> Live 3D Surface Reconstruction – Pharmaceutical Tablet</p> <table class="table"> <tbody> <tr> <td><img alt="Specimen: Pharmaceutical Tablet" src="https://jeolusa.s3.amazonaws.com/resources_eo/NeoScope%20for%20pharmaceuticals%2004.jpg?AWSAccessKeyId=AKIAQJOI4KIAZPDULHNL&Expires=2145934800&Signature=EgrfB0bPAs1zukI0r%2FmAXd9PeeY%3D" style="width: 500px; height: 419px;" /></td> <td>Specimen: Pharmaceutical Tablet<br /> Montage – Composite Image<br /> Signal BED-C<br /> Landing Voltage 10.0 kV<br /> FOV 5.803 x 4.352 mm<br /> Number of Fields 4 x 4<br /> Field Magnification x75</td> </tr> </tbody> </table> <p>When configured with analytical capabilities, the SEM conducts real-time chemical analysis using Energy Dispersive Spectroscopy (EDS). The operator can view EDS spectra in real time, set the analysis points, areas of interest, and map position.</p> <table class="table"> <tbody> <tr> <td><img alt="EDS composite map of elements in Lantoprazole, a heartburn medication." src="https://jeolusa.s3.amazonaws.com/resources_eo/NeoScope%20for%20pharmaceuticals%2005.jpg?AWSAccessKeyId=AKIAQJOI4KIAZPDULHNL&Expires=2145934800&Signature=LVaUoh5xHrmgHGy8wXoZZ0Hysu4%3D" style="height: 276px; width: 500px;" /></td> <td>EDS composite map of elements in Lantoprazole, a heartburn medication.</td> </tr> </tbody> </table> <p>In most pharmaceutical products, drug molecules are present in a particulate, crystalline form. The Benchtop SEM can analyze the size, shape, purity, and other characteristics of a drug crystal to help predict its behavior in large-scale production. The characterization of these crystals can be used to guide the optimization of process parameters, minimizing manufacturing costs.</p> <p style="text-align: center;"><img alt="Insulin particles Au coated and imaged with the JEOL NeoScope Benchtop SEM." src="https://jeolusa.s3.amazonaws.com/resources_eo/NeoScope%20for%20pharmaceuticals%2006.jpg?AWSAccessKeyId=AKIAQJOI4KIAZPDULHNL&Expires=2145934800&Signature=13jJtD6rq060j4yYJOo7PZS5jp8%3D" /><br /> <em>Insulin particles Au coated and imaged with the JEOL NeoScope Benchtop SEM.</em></p> <p>JEOL’s <a href="/PRODUCTS/Scanning-Electron-Microscopes-SEM/Benchtop/NeoScope-Benchtop-SEM">NeoScope Benchtop SEM</a> features simple navigation software, auto functions, selectable High and Low Vacuum modes, and integrated management of data collected through imaging and elemental analysis.</p> <p style="text-align: center;"><img alt="JEOL 4th generation NeoScope Benchtop SEM." src="https://jeolusa.s3.amazonaws.com/resources_eo/NeoScope%20for%20pharmaceuticals%2007.jpg?AWSAccessKeyId=AKIAQJOI4KIAZPDULHNL&Expires=2145934800&Signature=LEgrMtTyOZzLctPIevsVLYDGEP8%3D" /><br /> <em>JEOL 4th generation NeoScope Benchtop SEM.</em></p> <p>With the JEOL NeoScope Benchtop SEM, pharmaceutical companies gain a robust and versatile tool for analyzing substance morphology, topography and composition right from within their own laboratory environment. The small footprint and intuitive operation make it easy for any lab personnel to conduct the high resolution imaging and analysis that only an SEM can deliver.</p> Air Isolated Transfer Systemhttps://www.jeolusa.com/RESOURCES/Electron-Optics/Documents-Downloads/air-isolated-transfer-systemIT200Mon, 02 Nov 2020 12:16:34 GMTThere are a number of applications where scientists and engineers are faced with air or moisture sensitive samples that require imaging and analysis using a scanning electron microscope (SEM). Applications include: components in rechargeable batteries, fuel cells, and catalysts among others. Any exposure to oxygen or moisture in the air can completely alter or destroy the structure of these highly reactive materials. JEOL has built a special air-lock system that can handle the transfer of air-sensitive specimens to be imaged in the SEM without atmospheric exposure.<h4>Latest Innovation in our FE SEMs</h4> <h3>SMART – POWERFUL – FLEXIBLE</h3> <p>There are a number of applications where scientists and engineers are faced with air or moisture sensitive samples that require imaging and analysis using a scanning electron microscope (SEM). Applications include: components in rechargeable batteries, fuel cells, and catalysts among others. Any exposure to oxygen or moisture in the air can completely alter or destroy the structure of these highly reactive materials. JEOL has built a special air-lock system that can handle the transfer of air-sensitive specimens to be imaged in the SEM without atmospheric exposure.</p> <p class="caption" style="text-align: center;"><img alt="" class="img-responsive" src="https://jeolusa.s3.amazonaws.com/resources_eo/Air%20Isolated%20Transfer%20System%201.jpg?AWSAccessKeyId=AKIAQJOI4KIAZPDULHNL&Expires=2145934800&Signature=xkpdwzMtMpoQzXu0bEdfuNq5TUI%3D" /><br /> The sample can be prepared, mounted on the holder, and covered with a cap while inside a glove box. The cap seals and isolates the sample from the environment.</p> <p class="caption" style="text-align: center;"><img alt="" class="img-responsive" src="https://jeolusa.s3.amazonaws.com/resources_eo/Air%20Isolated%20Transfer%20System%202.jpg?AWSAccessKeyId=AKIAQJOI4KIAZPDULHNL&Expires=2145934800&Signature=pNIu1zuAhMeq0w%2FJQiRX3%2Bm9R%2Fg%3D" /><br /> The sample holder (w/cap) is then removed from the glovebox and transferred into the load lock of the SEM. After the airlock is evacuated, the user can open the cap and put the sample into the FE-SEM without air exposure.</p> Air-Isolated Sampling of Solid-State Battery for TEMhttps://www.jeolusa.com/RESOURCES/Electron-Optics/Documents-Downloads/air-isolated-sampling-of-solid-state-battery-for-temTransmission Electron Microscope (TEM)Thu, 23 Sep 2021 11:53:17 GMTA solid-state battery is made of cathode, anode and electrolyte. This type of battery doesn’t use liquid state electrolyte, so it tends to avoid the issues associated with leakage of electrolyte and ignition/explosion. Recently, silicon has been used as an anode material to improve the battery charge capacity (can store ten times more charge as compared to graphite anodes), but some challenges remain in terms of volume expansion during cycling, low electrical conductivity, and instability of the SEI (solid electrolyte interphase) layer caused by repeated volume changes of the Si material.<p>A solid-state battery is made of cathode, anode and electrolyte (Fig. 1). This type of battery doesn’t use liquid state electrolyte, so it tends to avoid the issues associated with leakage of electrolyte and ignition/explosion. Recently, silicon has been used as an anode material to improve the battery charge capacity (can store ten times more charge as compared to graphite anodes), but some challenges remain in terms of volume expansion during cycling, low electrical conductivity, and instability of the SEI (solid electrolyte interphase) layer caused by repeated volume changes of the Si material.</p> <p>For the purpose of observing structure and shape of anode silicon grains (charged 90 %), a TEM sample was prepared under air isolated condition.</p> <p style="text-align: center;"><img alt="" class="img-responsive" src="https://jeolusa.s3.amazonaws.com/resources_eo/Air-Isolated%20Sampling%20of%20Solid-State%20Battery%20f1.jpg?AWSAccessKeyId=AKIAQJOI4KIAZPDULHNL&Expires=2145934800&Signature=IgiweGxq3nmzL8xZbprIaEtDD7Q%3D" /><br /> Fig. 1. The schematic of a structure of solid-state battery and charge/discharge</p> <h3>TEM Sampling Process under Air-Isolated Condition</h3> <p>A lithium battery sample was made under air-isolated conditions from start of preparation to observation to avoid reaction with air and potential oxidation (Fig. 2). For the sample transfer between instruments, a transfer vessel and slide cover holder were used. For the TEM sample preparation by FIB, an in-chamber manipulator (OmniProbe350, Oxford Instruments) was used. A cross section was first prepared by Ar-ion beam Cross-section Polisher (CP) to expose a large area showing the inner grain part of the battery, and subsequently decide the FIB processing area. JEOL air-isolated preparation methodology allows movement between all steps - CP process, SEM observation/analysis and TEM sampling - by using just one sample holder.</p> <p style="text-align: center;"><img alt="" class="img-responsive" src="https://jeolusa.s3.amazonaws.com/resources_eo/Air-Isolated%20Sampling%20of%20Solid-State%20Battery%20f2.jpg?AWSAccessKeyId=AKIAQJOI4KIAZPDULHNL&Expires=2145934800&Signature=463RIpHM64TJhkRUaai5MRiXzMQ%3D" /><br /> Fig. 2. Process of FIB TEM sample preparation under air-isolated condition</p> <h3>TEM sample preparation from CP-processed surface</h3> <p>A TEM sample of silicon anode material of charged all solid-state battery was made under air-isolated process which is shown in Fig. 2. Fig. 3 shows backscatter electron compositional (BEC) image and EDS map. This surface was prepared by CP. FIB process used this CP surface for choosing the correct position on the anode grain to subsequently prepare a thin TEM lamella (Fig. 4).</p> <p style="text-align: center;"><img alt="" class="img-responsive" src="https://jeolusa.s3.amazonaws.com/resources_eo/Air-Isolated%20Sampling%20of%20Solid-State%20Battery%20f3.jpg?AWSAccessKeyId=AKIAQJOI4KIAZPDULHNL&Expires=2145934800&Signature=SChYDHAxOpSj3OX1xiFhS%2FOsDbk%3D" /><br /> Fig. 3 SEM BEC image (left) and EDS map (right) of CP processed surface. The silicon grain position was found from SEM BEC image and EDS map. TEM lamella position is identified by the red line.</p> <p style="text-align: center;"><img alt="" class="img-responsive" src="https://jeolusa.s3.amazonaws.com/resources_eo/Air-Isolated%20Sampling%20of%20Solid-State%20Battery%20f4.jpg?AWSAccessKeyId=AKIAQJOI4KIAZPDULHNL&Expires=2145934800&Signature=D%2B%2FRGH4NFe1fBUF5aXwaW0Al%2FHo%3D" /><br /> Fig. 4 Images during FIB process of making TEM sample. Sample block (left) and TEM lamella (right). The sample block was made at the silicon grain position (left), and it was fixed to the FIB grid by using OmniProbe350, Oxford Instruments. After that, it was made into a lamella sample for TEM observation (right).</p> <h3>TEM observation and confirmation of air-isolated condition</h3> <p>Fig. 5 shows BF-STEM image of TEM sample. The red line encompasses the targeted silicon grain. After TEM observation, the sample was exposed to air, causing a change due to oxidation (Fig. 6). This result indicates that the entire sampling processes was indeed performed under air isolated condition.</p> <p style="text-align: center;"><img alt="" class="img-responsive" src="https://jeolusa.s3.amazonaws.com/resources_eo/Air-Isolated%20Sampling%20of%20Solid-State%20Battery%20f5.jpg?AWSAccessKeyId=AKIAQJOI4KIAZPDULHNL&Expires=2145934800&Signature=ZKA9Fu9WsyMwI59pz4Gl0%2BpdvWQ%3D" /><br /> Fig. 5 BF-STEM image. There were three layers in silicon grain inner part from the center to outside.<br /> It is speculated that the center part was a silicon single crystal, and the lithium density increases from the center to the outside.</p> <p style="text-align: center;"><img alt="" class="img-responsive" src="https://jeolusa.s3.amazonaws.com/resources_eo/Air-Isolated%20Sampling%20of%20Solid-State%20Battery%20f6.jpg?AWSAccessKeyId=AKIAQJOI4KIAZPDULHNL&Expires=2145934800&Signature=IjxZvQdv2nAZIaYlln8qk%2BqBZZQ%3D" /><br /> Fig. 6 BE-STEM image after exposed to air.<br /> After observation, the sample was exposed to air. Then retaken TEM image shows that it has reacted with air.</p> <p style="text-align: right;"><em>Sample provider: Prof. Atsunori Matsuda Toyohashi Univ. of Technology</em></p>