Cryo Note, une synthèse des différentes techniques de préparation cryo
« Visualize the truth » is a hope of researchers who use various measuring equipments. Researchers who use electron microscopes as well have a desire to observe the real structure. One recommended solution is to cool the specimen, that is « Cryo’ techniques. This Cryo Note introduces some of the diversified cryo-techniques.
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Easy cryo-SEM
The technique can be thought of as ‘easy cryo-SEM’ and is a simple and cost effective means of looking at fully hydrated materials or other electron beam and vacuum sensitive samples.
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Difference of observation result by cooling method – whipcream (frozen)
In this application note, we will introduce the observation results of whip cream which is easily impacted by the heat, by using three kinds of methods of different cooling temperatures : 1. cooling stage, 2. LV cooling holder, and 3. LV cryo SEM method.
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Yokogushi : TEM & NMR combine technique for full crystaline structure
Crystalline structure including hydrogen atoms are now available from nano- to micro-crystals of 100 nm to 1 μm using electron and NMR nano-crystallography approach. The overall crystalline structures can be determined by electron diffraction (ED) which is one of the observation mode of transmission electron microscope (TEM).
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JEOL Gatan 3View® Serial Block Face Imaging System
3View Serial Block Face Imaging of Synapse using JEOL Scanning Electron Microscope. Courtesy of Professor Deniz Kirik and Lina Gefors, Bioimaging Center, Medical Faculty, Lund University, Sweden.
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SEM-Correlative Microscopy_Photomontage_SEM Supporter
EM Supporter software automates SEM image collection, creation of a photo montage and image analysis*. Initial navigation and set up can be accomplished from any image (optical microscope, digital camera, SEM image) enabling correlative microscopy. Recipes can be created for moving to specific locations on a multiple sample set for collection of individual images or creating a grid for photo montage collection.
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SEM-STEM detector
STEM-in-SEM (Scanning Transmission Electron Microscopy in an SEM) has become a popular technique for biologists, polymer scientists and materials scientists for its ease of use, cost effectiveness and high resolution. It is especially suited to investigating the internal structure of thin film (100-200nm) samples as well as size and shape of submicron to nanometer particles.
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SEM – Aqua Cover tecnique for direct observation of water containing sample
Direct observation of water containing specimens as they are with ordinary SEMs is one of the long desired goals of SEM. We have succeeded to observe a water droplet with a newly developed technique, Aqua Cover technique, with a commercial SEM, JSM-IT300LV. Aqua Cover, as you will see, can easily be extended to observe any water containing specimen.
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Food analysis solutions application note
Four demands have developed in the food product field for highly accurate, objective evaluation technologies to analyze aspects such as nutritional components, flavors and tastes, texture, and antioxidation functions.
JEOL offers numerous analytical tools to support both “food safety & security” as well as various evaluations of primary, secondary and tertiary functions of foodstuffs which are useful for a wide range of users associated with this field.
This Foodnote introduces the features of each of the instruments and actual analysis examples, and is designed for researchers and engineers who are considering purchases of instruments. This brochure also presents comprehensive evaluations and analysis solutions that can be achieved with combinations of multiple instruments.
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BioNote
Instrumental analysis has contributed to the progress of biological science, through the observation of morphology, the chemical analysis of compounds, the elucidation of amino acid sequences of proteins, etc. Furthermore, this progress has been accelerated by the development of analytical methods, which are used in diverse fields like medical science, agriculture, food and biotechnology, as well as the basic research work like physiology, biochemistry and genetics.
This Bionote presents an overview of the basics, namely principles and features of various instruments, as well as application examples using numerous optional attachments. We hope that the Bionote will assist researchers and engineers who intend to perform analyses in finding and exploring new approaches.
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Electrostatic dose modulation improves lifespan of beam-sensitive specimens for advanced electron crystallography techniques
Introduction and Background – Objectives – Techniques
Electrostatic dose modulation
Experimental: crystalline glycine
Experimental: π-peptides
Conclusions
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NEW : Application of Nanoprobing and Electrical Failure Analysis
Product used： Scanning Electron Microscope (SEM)
The nanoprobing system, equipped with microscopic probes that directly contact the circuitry of semiconductor devices within the specimen chamber of a scanning electron microscope (SEM), is utilized for evaluating semiconductor devices, identifying failure locations, and determining the causes of these failures. By probing the electrodes of a transistor in a semiconductor device, the IV characteristics of the transistor can be evaluated. Additionally, an EBIC (Electron Beam Induced Current) image can be acquired to visualize the positions of depletion regions at the pn junctions of a semiconductor device. Furthermore, an EBAC (Electron Beam Absorption Current) image, which shows the current flowing through the wiring, can be obtained while probing the wiring in the semiconductor device, enabling the visualization of shorts and opens in the wiring. In these analyses, it is crucial to set the appropriate accelerating voltage.
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LIBnote : Lithium ion battery basic structure and fabrication process
The applications for lithium ion batteries (LIB) cover a wide range, from power sources for personal computers and mobile devices to automobiles, and there is always a demand for even better performance and safety. In order to ensure the performance and quality of LIB, analysis and evaluation using high-performance assessment systems is necessary. JEOL offers a full line-up of equipment to support the development of new LIB technologies and to improve product quality, including instruments for morphology observation and surface analysis, chemical analysis systems to perform structural analysis on a molecular level, as well as fabrication systems to create high-performance coatings and powders. This LIB note offers solutions for researchers and engineers who are looking for the best equipment for their application.
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Improvement of SEM-SXES analysis for beam sensitive materials by using cooling stage
Soft X-Ray Emission Spectrometer (SXES), which can be installed on SEM and EPMA (Electron probe microanalyzer), is a useful method for chemical state analysis by detecting the energy state of valence electrons. In particular, since SXES can detect low-energy characteristic X-rays such as lithium (Li) K-line and analyze the chemical state, it is expected to be a chemical state analysis method of Lithium Ion secondary Battery (LIB) materials in a charged state. Field Emission- SEM equipped with SXES enables us to obtain chemical state information in the vicinity of the bulk top surface by low-kV analysis. However, it is known that the irradiation of an electron beam causes a change in the chemical state of the beam- sensitive materials such as lithium compounds during the observation.
This study shows the improvement of chemical state analysis for beam-sensitive materials using the SEM-SXES system with a cooling stage.
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Soft X-ray Emission Spectroscopy for EPMA/SEM application
Study case : chemical state mapping of degraded B4C control rod
This study shows that SXES have an excellent energy and spatial resolution for boron, despite the fact it is an element with a very low atomic number : two different chemical states are clearly identified (pure B4C and three different oxides) at a very high resolution spatial distribution.
> télécharger le poster sur l’étude du bore avec le détecteur SXES
BatteryNote
Battery cells are essential in modern life as they are extensively used in mobile phones, personal computers, and even as the power source of some automobiles in recent years. In addition, the research and development of rechargeable batteries has become increasingly important in the endeavor to realize a low-carbon society.
The demand for fuel cells as hydrogen-based generators is also expected to grow, as fuel cells have already been widely applied to household equipment and automobiles.
JEOL believes that analyses and evaluations by using various high-performance evaluation instruments are required to improve both the performance and quality of these battery cells.
JEOL offers a wide variety of analytical instruments available for morphological observations, surface analyses, structure analyses, and chemical analyses at micro- to nano-scales for the purposes of research, development, and quality improvement.
This Battery Note has been created to provide solutions and reference information for research and development activities focused on lithium ion batteries (LIBs).
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Poster SXES sur la détection du lithium
Three samples of a lithium-ion battery anode with different charging conditions are analyzed with SXES: 0 % (A), 30 % (B) and 100 % (C).
→ 3 maps constructed in 3 energy ranges corresponding to satellite of Li-K, Li-K and C-K.
Imaging and Analyzing Graphene Layers
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Magnetic Material Analysis Using the Super Hybrid Lens (SHL)
The SHL is a newly designed objective lens for high-resolution observation at low accelerating voltages. Unlike the semi-in lens SEM, with a large electromagnetic field below the lens, which was widely used for high-resolution, low kV observation, the SHL achieves high resolution by superimposing a magnetic field onto the electrostatic field to suppress magnetic field leakage.
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Applications of Transmission Kikuchi Diffraction in FE-SEM
Natasha Erdman and Masateru Shibata
Recent developments in SEM column design have led to the ability to produce nanometer spot sizes even at high probe currents [1], thus pushing the analytical techniques available in the SEM to conduct microanalysis with ultra-high spatial resolution.
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TEM-HAADF – Quantification du contraste HAADF
A procedure that produces sub-nanometrically resolved chemical mappings of MOCVD-grown
InGaAs/InAlAs/InP quantum cascade lasers is presented. The chemical mappings reveal that, although the structure is lattice-matched to InP, the InAlAs barriers do not attain the nominal aluminum content—48%—and are, in fact, InGaAlAs quaternaries. This information is used to adjust the aluminum precursor flow and fine-tune the composition of the barriers, resulting in a significant improvement of the fabricated lasers.
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YOKOGUSHI – Study of a gold star mothers stamp
Experimental : A Gold Star Mothers Stamp from 1948 has a lead chromate pigment that we analyzed via: the JSM-IT300LV with an EDS spectrometer, the JMS-T100LP “AccuTOF DART” and the JMS-S3000 “SpiralTOF”.
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SEM – Extreme Low Voltage Imaging with JEOL FE-SEMs
The current lineup of JEOL FE-SEMs offers a cutting edge Through-The-Lens (TTL) electron column design that minimizes effects of chromatic and spherical aberrations on the ultimate probe size (improved resolution). This novel electron column design also features a TTL detector with an energy filter combined with a precise control of the landing energy of the primary electron beam (beam deceleration via Gentle Beam function), which has created new opportunities for specimen observation.
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SEM – Energy Filter-UED
JEOL’s in column Upper Electron Detector (Through The Lens Detector) provides not only ultra-high resolution imaging but also includes a user selectable energy filter allowing the user to study a sample under different contrast mechanisms.
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TEM – TEM sample holder for Lithium or air sensitive sample study
The lithium analysis by TEM requires to keep the sample under neutral atmosphere preventing its oxidation. For this purpose, JEOL has developed a special TEM sample holder.
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SEM – 3D Image software
JEOL’s Three Dimensional Image Software is a program that uses stereo pair SEM images to construct a three dimensional (3D) image of the sample surface. From this 3D image, height and contour maps can be created to provide cross sectional shape and height data.
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MS SpiralTOF – TOF Synthetic Polymer Structure Analysis PPG
In this work, we analyzed Polypropylene Glycol (PPG) by using the JMS-S3000 SpiralTOF with the TOF-TOF option. The resulting high-energy CID data was then processed using the Polymerix™ (Sierra Analytics, Inc., http://massspec.com/) analysis software.
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SEM – What is the magnification ?
Magnification can be a very deceptive number on SEM micrographs. As we all know, 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.
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JSX-JXA – Analyse by X ray fluorescence and microprobe of cracks in brass piping parts
In order to understand the cause and minimize the recurrence of a product malfunction, it is necessary to pursue defects at an early stage. An X-ray fluorescence spectrometer (ED-XRF) can provide fast, non-destructive elemental analysis for any sample state such as solid, liquid, or powder. It can be utilized as a quick screening instrument to track down the source of problems.
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Co-localized microscopy techniques for pyrite mineral spatial characterization
All SEM-BSE experiments were conducted using the SEM instrument, model JSM-IT800 from JEOL. All SEM-EDS experiments were conducted by using the SEM instrument from JEOL, equipped with EDS add-on detector. Soft X-Ray Emission Spectroscopy (SXES) is a complementary SEM technique developed by JEOL using high spectral resolution grating and a CCD detector for X-Rays, allowing to differentiate various phases of elements, such like iron alpha and beta phases (in this study) at the nanoscale. All SEM-SXES experiments were conducted by using the SEM IT800 instrument from JEOL, equipped with SXES add-on detector. All SEM-CL experiments were conducted by using the SEM instrument from JEOL, equipped with the HORIBA F-CLUE add-on detector.
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High-resolution spatial distribution of chemical composition on a pyrite surrounded by oxide / hydroxide phases
In this study, a geological thin section of a meta-arkose in a serpentinite was
chosen. Within the meta-arkose rock is a pyrite surrounded by different mineral phases that appear to have variable chemical composition. This area was therefore selected for the identification and distribution of the different elemental assemblages.
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Natasha Erdman and Nicholas Drenzek, 2013, Integrated preparation and imaging techniques for the microstructural and geochemical characterization of shale by scanning electron microscopy, in W. Camp, E. Diaz, and B. Wawak, eds., Electron microscopy of shale hydrocarbon reservoirs: AAPG Memoir 102, p. 7–14.
To better understand the influence of microscale geochemical and microstructural relationships on the bulk petrophysical properties of unconventional shale systems, core samples from four producing North American formations were cross-sectioned with an argon ion polisher and imaged with a field emission scanning electron microscope (FE-SEM) using a variety of complementary detectors. We demonstrate distinct advantages of the ion-polishing technique for the preservation of the internal shale structure. Moreover, we show how such preparation affords a wider choice of imaging options for both chemical and structural characterization, such as backscatter electron observation at varying beam potentials coupled with x-ray and cathodoluminescence spectroscopic techniques.
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Meteorite application with SEM
Meteorite with EPMA
Microbeam and x-ray analysis of minerals, water analysis, stable isotope analysis, and age-dating in labs at UNM.
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JXA-Monazite
JEOL’s MonaziteAge program follows the dating procedure outlined originally by Suzuki and Adachi (1991, 1994), and Suzuki and others (1994). It can be used with both Th-rich phases and more U- rich phases, such as zircon or xenotime. It allows the user to calculate the age of a monazite grain from a single analytical point or from a set of analyses. When multiple analyses are used to determine a single age, the method will correct for non-radiogenic lead or for lead leaching that may have taken place. When creating age maps, the method uses the same procedure as that for a single analysis, but applies it to each pixel.
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JXA-Trace element mapping
Backscatterred electron images of monazite, WDS trace element mapping.
> télécharger les images et la cartographie
SEM-MLA
AZtecMineral is a powerful, automated, Mineral Liberation Analysis solution. It enables ore characterisation, provides vital data on metal recovery and enables process yield characterisation using multipurpose SEMs. It is also a valuable tool for the characterisation of rocks in research environments, enabling the automation of otherwise laborious optical analyses.
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Polymers note. Characterization of Polymers by JEOL Solutions
Polymers are used in a wide range of fields such as food wrapping materials, medicine packing, and industrial materials and products. Properties and functionalities of polymer materials are dependent on various factors, including molecular weight, molecular weight distribution, molecular chemical structures (primary structures), morphology of molecular chains (secondary structures) depending on the spinning angles of chemical bonds, and crystalline or non-crystalline structures of inner-molecules and inter-molecules, as well as spherulite structure aggregates, phase separation structures and orientations (higher-order structures). It is of prime importance to analyze and evaluate the structures and properties of polymers as well as the correlation between these two factors, and to feed these analysis and evaluation results to the development and manufacturing sites for the enhancement of the performance and quality control of polymer materials and polymer products. On the other hand, industry in Japan is supported by functional molecules, which are becoming more advanced and more complicated. This makes it more difficult to characterize such polymers, thereby increasing the importance of multiple analyses that combine a variety of analytical methods. This Polymer note introduces a broad range of instruments used for polymer analysis and their applications.
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Yokogushi : TEM & NMR combine technique for full crystaline structure
Crystalline structure including hydrogen atoms are now available from nano- to micro-crystals of 100 nm to 1 μm using electron and NMR nano-crystallography approach. The overall crystalline structures can be determined by electron diffraction (ED) which is one of the observation mode of transmission electron microscope (TEM).
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Direct analysis of a methanol flame by using a compact high-resolution multi-turn mass spectrometer
The InfiTOF can be used for “In-situ” high-resolution monitoring of real-time gas phase reactions like combustion. In this work, we show the real-time monitoring of combustion products in a diffuse methanol flame by using this compact high resolution TOF-MS system.
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Analysis of a gas mixture containing ammonia and methane by using a compact high-resolution multi-turn mass spectrometer
Analysis of a chemical ionization reagent gas consisting of a 5% mixture of ammonia in methane is demonstrated by using the JEOL InfiTOFTM compact high-resolution mass spectrometer.
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Real time monitoring for gas phase h/d exchange reaction in H2O and D2O by using a compact high-resolution multi-turn mass spectrometer
The InfiTOF is suitable for real time gas reaction monitoring. In this report, we showed real time monitoring for H/D exchange reaction of light water (H2O) and heavy water (D2O) which is one of the simplest chemical reaction.
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YOKOGUSHI-Study of a gold star mothers stamp
In this applications note, we performed an analysis of a Gold Star Mothers Postage Stamp by using three JEOL instruments. We used the JSM-IT300LV, the JMS-T100LP « AccuTOF-DART » and the JMS-S3000 « SpiralTOF ».
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MS SpiralTOF MALDI for small molecule analysis : A complex drug mixture
This is shown here for the high-resolution analysis of a mixture of 32 small-molecule drugs analyzed by MALDI with the JEOL SpiralTOF mass spectrometer.
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MS SpiralTOF-TOF Synthetic Polymer Structure Anlaysis PPG
In this work, we analyzed Polypropylene Glycol (PPG) by using the JMS-S3000 SpiralTOF with the TOF-TOF option.
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NMR Single-Tuned 4 mm Cryocoil MAS Probe
A tunable single-tuned 4 mm Cryocoil MAS probe was developed, and demonstrated for 6Li and 29Si under 14.1 T WB magnet.
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What conductive coating is the best for you ?
SEM-TTL System-New approach for reduction of the effects of lens aberrations
Imaging of nanostructured materials requires a new design of SEM that provides ultimate resolution for both imaging and microanalysis, combined with the ability to image any type of material. An innovative new SEM column design from JEOL Ltd. utilizes a hybrid lens (combination electrostatic and electromagnetic lenses) in conjunction with a Through-The-Lens (TTL) detection system to provide the user with ultimate imaging and analytical performance.
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SEM- Extreme Low Voltage Imaging with JEOL FE-SEMs
Low voltage imaging has become a key technique for charge control and reduction, especially in the cases where no surface modification (for example conductive coating) can be employed to alleviate specimen charging during SEM observation.
The current lineup of JEOL FE-SEMs offers a cutting edge Through-The-Lens (TTL) electron column design that minimizes effects of chromatic and spherical aberrations on the ultimate probe size (improved resolution).
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SEM- CD Energy Filter-UED
JEOL’s in column Upper Electron Detector (Through The Lens Detector) provides not only ultra-high resolution imaging but also includes a user selectable energy filter allowing the user to study a sample under different contrast mechanisms.
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COATER-SMART COATER
JEOL’s Smart Coater is a fully automated sputter coater that applies a fine grained gold or platinum coating on samples for imaging in a scanning electron microscope.
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NEW : LIBnote : Lithium ion battery basic structure and fabrication process
The applications for lithium ion batteries (LIB) cover a wide range, from power sources for personal computers and mobile devices to automobiles, and there is always a demand for even better performance and safety. In order to ensure the performance and quality of LIB, analysis and evaluation using high-performance assessment systems is necessary. JEOL offers a full line-up of equipment to support the development of new LIB technologies and to improve product quality, including instruments for morphology observation and surface analysis, chemical analysis systems to perform structural analysis on a molecular level, as well as fabrication systems to create high-performance coatings and powders. This LIB note offers solutions for researchers and engineers who are looking for the best equipment for their application.
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Battery Analysis SEM : In situ charging / discharging Analysis system for LIBs
Chemical state analysis of Li and Si for Si negative electrode of solid-state lithium ion battery by using combination of windowless EDS and SXES on a SEM
Silicon (Si) negative electrode material has problems such as volume expansion and decrease of charging efficiency during charging-discharging, but it has a large theoretical capacitance of 4200 mAh/g, and is attracting attention as a new material for Lithium (Li) ion secondary battery (LIB) to replace graphite which is widely used. Therefore, a chemical state analysis method using soft X-ray emission spectroscopy (SXES) has been reported for the purpose of structural analysis of the Si negative electrode active material in the charged state. However, since elemental mapping by SXES takes at least a few hours of processing time, it is not easy to compare the chemical state of each Si particle across the entire negative electrode layer. In this study, we combined a newly designed windowless EDS and SXES, and tried to establish a simple method to analyze the chemical state of Si negative electrodes in charged states.
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Battery note
Battery cells are essential in modern life as they are extensively used in mobile phones, personal computers, and even as the power source of some automobiles in recent years. In addition, the research and development of rechargeable batteries has become increasingly important in the endeavor to realize a low-carbon society.
The demand for fuel cells as hydrogen-based generators is also expected to grow, as fuel cells have already been widely applied to household equipment and automobiles.
JEOL believes that analyses and evaluations by using various high-performance evaluation instruments are required to improve both the performance and quality of these battery cells.
JEOL offers a wide variety of analytical instruments available for morphological observations, surface analyses, structure analyses, and chemical analyses at micro- to nano-scales for the purposes of research, development, and quality improvement.
This Battery Note has been created to provide solutions and reference information for research and development activities focused on lithium ion batteries (LIBs).
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Solid-state battery note
The shift to battery vehicles (BEV) is rapidly advancing worldwide in order to achieve carbon neutrality by 2050 which is to “reduce overall greenhouse gas emissions to zero ». The research and development on rechargeable battery cells that can be used repeatedly, are progressing for the use of power source of BEV and larger energy storage system (ESS). To improve both the performance and quality of these battery cells, analyses and evaluations by using various high-performance evaluation instruments are required. JEOL offers a wide variety of analytical instruments available for morphological observations, surface analyses, structure analyses, and chemical analyses at micro- to nano-scales for the purpose of research, development, and quality improvement.
This Solid-state battery Note has been created with the samples provided by Prof. Atsunori Matsuda, Toyohashi University of Technology (Department of Electrical and Electronic Information Engineering), to provide solutions and reference information for research and development of solid-state batteries evolving from the lithium ion batteries (LIBs).
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Cleanliness inspection of automotive lithium-ion batteries manufacture
For system components which cannot be cleaned after assembly, cleanliness inspection using VDA 19 part 2 (VDA19.2) is recommended. This guideline for Technical Cleanliness in assembly is designed to help protect against the entry of critical contamination via the environment during production. In automotive LIB assembly areas, the inspection of the manufacturing environment to comply with VDA19.2 should be applied.
JEOL’s Particle Contamination Inspection System (PCI System) can determine critical particulate contamination in LIB assembly areas for ensuring VDA 19.2 compliance. PCI System enables an easy daily routine for Cleanliness Inspection.
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