JEOL USA Blog

Japan Academy Prize for Electron Microscopy Goes to University of Tokyo Professor Yuichi Ikuhara and Professor Naoya Shibata

JEOL Collaborators renowned for their innovations with JEOL Electron Microscopes

JEOL USA congratulates University of Tokyo Professor Yuichi Ikuhara and Professor Naoya Shibata, recently awarded the Japan Academy Prize for development of State-of-the-Art Electron Microscopy and their contribution to Nano Interface Technology (Joint Research). As corroborators with JEOL, their work in developing the Magnetic-field-free Atomic-Resolution STEM (MARS), Annular Bright Field (ABF), and Optimum Bright Field STEM detector (OBF) is invaluable.

Ikuhara and Shibata have worked together to pioneer the cutting edge of scanning transmission electron microscopy (STEM) and to solve various problems in nanomaterials science, including:

Establishing quantitative evaluation methods for local atomic structures and electronic states such as interfaces and dislocations
Achieving the world's highest resolution of 40.5 pm using GaN[211], direct observation of light elements, high-resolution in-situ observation, etc.
Developing numerous sophisticated analysis methods using TEM, such as:

Determining the correlation between interfacial atomic/electronic structure and functional properties, the relationship between identification of atomic positions of light elements and physical properties, elucidation of dislocation core/lattice defect structure, elucidation of material deformation and fracture mechanism, ceramics grain boundary segregation mechanism
Direct observation of the electric field inside the atom/observation of the atomic magnetic field.

Ultimately, developing new STEM detectors including Annular Bright Field (ABF) and atomic resolution magnetic field-free electron microscopes (MARS)

Based on these series of research results, Ikuhara and Shibata are constructing the theory of nano-interface engineering leading to the design and creation of new materials focusing on the functions of interfaces and lattice defects.

Additional Reading:

Atomic resolution electron microscopy in a magnetic field free environment

Japanese Researchers Identify Magnetic Fields of Atoms with Nobel-Worthy Electron Microscope

Atomic Magnetism Finally Caught on Camera

Visualization of the origin of magnetic forces by atomic resolution electron microscopy

Microscopy Community Celebrates Wil Bigelow

Prof. Wil Bigelow with a detailed balloon model of the 2100F TEM column on his 100th birthday.

Friends of Prof. Wilbur (Wil) Bigelow, Professor Emeritus at University of Michigan and Fellow of the Microscopy Society of America, threw a surprise 100th birthday party for him at the University of Michigan’s Dept. of Materials Science & Engineering in Ann Arbor on March 16. (His actual birthday was March 18). Among his colleagues and past students that attended were renowned researchers Larry Allard and John Mardinly.

Larry Allard (Oak Ridge National Laboratory) reported that, “The department hired a local balloon artist to make the balloon model of the 2100F microscope, shown in the poster with a slightly younger Wil sitting in front. The picture was also placed in the cake. It was a total surprise to Wil. The balloon model took an entire day to construct...it was pretty unique. I did a presentation of some of his early history, including my training on the JEM-6A in 1963, through the early 70s, right after I returned to Ann Arbor after 2 years in Oak Ridge, when John Mardinly came into the lab, shortly after the 1st JSM-U3 SEM was acquired. John covered the next decade or so, which included acquisition of the 2nd JSM-U3 and the JEM-100CX AEM, and the naming of the EMAL (Electron Microprobe Analysis Laboratory). John Mansfield wrapped up with the final history of the EMAL, and the move of the lab from Main Campus to North Campus.”

Prof. Wil Bigelow honored with a special cake and the blue and gold theme of University of Michigan.

It's an honor to know these great researchers and we wish Wil all the best in his 100th year!

More about this legendary man:

Dr. Larry Allard (Oak Ridge), Pete Genovese (JEOL), and Prof. Wil Bigelow at JEOL’s 70th anniversary celebration in 2019.

PANIC 2023: Conference Notes & Recorded Symposium

PANIC 2023 Conference Notes

PANIC (Practical Applications of NMR industry Conference) started out in 2012 as a scientific conference seeking to promote real-world, practical solutions for modern NMR problems. PANIC seeks to address the daily problems that scientists encounter when they apply NMR to wide range of analytical problems.

This year, for their 11^th conference to date, scientists from across the world traveled to Nashville, TN, to learn, network, and share their latest discoveries in the field of NMR. Here at JEOL, we were excited to share our new ECZ Luminous series NMR spectrometer and some recent developments in the application of qNMR during our Mini Symposium on Sunday morning.

NMR Mini Symposium

Three speakers presented at the meeting. The first talk, given by Ronald Crouch of JEOL USA, was titled "Strategies to Evaluate Low-Sensitivity Experiments" and explored the use of older but underutilized experiments that are still very valuable, as well as using data that seems to be wrong at first glance.

Our second speaker, Iain Day from JEOL UK, gave an overview of current tools in JASON as well as some of the projects under development in his presentation "qNMR with JASON: The power of SMILEQ".

Lastly, Jessie Ochoa of Genentech summarized some methods and techniques developed and used in a real life industrial setting for quantitative NMR work. in her discussion of “Quantitative NMR of Small Molecule Pharmaceuticals”.

In case you missed it, you can view our NMR Mini Symposium on-demand:

Our new NMR ECZL G series is a flagship model for cutting-edge NMR methods. The footprint of the spectrometer has been reduced to less than 60% of ECZR, while maintaining the expandability needed to support a wide range of applications. It is flexible in terms of expansion, with support for three or more channels, high-power amplifiers, and high-output magnetic field gradients, allowing for future functional expansion even when installed in the minimum configuration. Learn more about the ECZL.

Designing Better Batteries through Innovative Microscopy Characterization and Analysis

The drive is on to improve the performance of Lithium-ion batteries, particularly to increase energy density, life cycle, and safety. However, during development and assessment of their performance, lithium-ion batteries can present unique challenges for characterization and analysis using electron microscopy.

The basic structure of Lithium-ion batteries (LIB) contains as many as 10 different thin films and at least that many solid−solid interfaces. These interfaces consist of thin layers of cathode material, insulating barriers, anode materials, metal current collectors, and the electrolyte. These various components are in the form of powders, sheets, and fluids and require assessment before and after assembly and after repeated charge/discharge operations. Researchers who are correlating electrochemical behavior to what is physically happening within the cell need to study the 3D microstructure of the battery components as well as the interfaces formed between those layers.

Cross Section of Lithium Ion Battery Layers

The efficiency of batteries and fuel cells is governed by the diffusion of ions, the transport of electrons and the chemical interactions of electrode/electrolyte materials. Engineers can routinely characterize the structure and properties of components that shed light on their behavior during electrochemical processes, including ion relocation, lattice expansion or contraction, phase transition and surface reconstruction.

However, since materials containing Li are reactive in ambient environments, being able to prepare, image, and analyze samples without exposing them to the atmosphere becomes vitally important. For that purpose, JEOL has established an air-isolated workflow from sample preparation using ion beam milling, to characterization and elemental analysis in the Scanning Electron Microscope (SEM) or Transmission Electron Microscope (TEM), without exposing the specimen to the atmosphere. JEOL ultrahigh resolution Field Emission SEMs, equipped with our new Gather-X Windowless EDS, detect ultra-low energy elements such as lithium (with Li K line of 54 eV) . Analyzing lithium and other light elements requires low kV imaging and analysis and often high beam current achievable in JEOL’s multipurpose or analytical high resolution SEMs.

Learn more about JEOL's air-isolated workflow, pristine sample preparation of sensitive samples, and high resolution imaging and analysis solutions at https://go.jeolusa.com/EM-LIB.

Petrochemical Analysis Using Soft- and Hard-Ionization | GCxGC-HRTOFMS

Petroleum accounts for a large percentage of the world's energy consumption and is an extraordinarily complex material composed of many types of hydrocarbons with a wide variety of properties, making them difficult to analyze.

Different types of hydrocarbons present different challenges to analysis: Aromatic hydrocarbons strongly absorb UV light, which is ideal for Photoionization (PI); saturated hydrocarbons can be analyzed by using traditional Electron Ionization (EI), but this technique can lead to complex fragmentation that does not occur in PI and Field Ionization (FI) experiments; and crude oil is a complex material that contains high boiling point compounds, thus making it difficult to analyze by GC-MS but making it ideal for direct probe analysis using Field Desorption (FD).

Comprehensive two-dimensional gas chromatography-high resolution time-of-flight mass spectrometry (GCxGC-HRTOFMS) with EI is a powerful method for characterizing complex mixtures such as base oils. However, EI data can often lack a strong molecular ion signal for many hydrocarbons, thus making them difficult to identify.

Field Ionization (FI) and Field Desorption (FD), however, are soft ionization techniques that are well suited for hydrocarbons analysis because they generate molecular ions for most compounds, including saturated hydrocarbons, with minimal fragmentation. The resulting mass spectra are dominated by molecular ions, whether from the GC output (FI) or from the emitter surface (FD).

In Dr. John Dane’s research on The Analysis of Petroleum Samples Measured by Using GCxGC-HRTOFMS, a high-resolution time-of-flight mass spectrometer (HRTOFMS) equipped with an electron ionization/field ionization/field desorption (EI/FI/FD) combination ion source and a GCxGC thermal modulator system was used to analyze petroleum samples. Additionally, the GC-MS interface was modified to increase the temperature in this region, so that higher boiling point compounds could be analyzed by the GCxGC-HRTOFMS system.

More specifically, Dr. Dane demonstrated JEOL’s AccuTOF GC-Alpha capabilities by pairing our optional EI/FI/FD combo source with GCxGC separation as a unique and powerful characterization tool for petrochemical mixtures. The GCxGC-EI data provides library searchable MS data while the GCxGC-FI data provides molecular ion accurate mass information to allow full characterization of compound families present in petroleum samples.

The combination of GCxGC, high resolution MS, and soft ionization provides the information needed to effectively analyze complex petrochemical samples. To learn more, stop by booth 2222!

NMR Analysis of Lithium Ion Batteries

LiB: Next Generation Energy Storage

Lithium-ion batteries (LIBs) are used to power portable electronics, electric vehicles, and grid storage solutions; they play a crucial role in driving sustainability and are an essential energy storage device. With the demand for electric vehicles and renewable energy sources continuing to rise, there is an increasing need to improve electrochemical storage. The search for new battery materials, alongside the drive to improve performance, and lower the cost of existing and new batteries, comes with its challenges.

Lithium has one of the highest electrochemical potentials compared to other metals, making it very active. Therefore, it releases the electron from the outer shell much faster than other metals, which makes it a good choice for battery research. 6/7Li are called ‘spin spies’ because they detect changes in structure, state of deterioration, Li-ion mobility, and quantitation during charging and discharging of the battery and have guided the synthesis of new anode, cathode and electrolyte materials.

A primary concern in finding new forms of electrolytes in secondary batteries is safety because electrolytes can leak in a battery and are very sensitive to temperature change, especially high temperatures.

Leveraging NMR for LiB Analysis

One method to observe lithium ions is nuclear magnetic resonance (NMR). NMR is one of the few analytical methods to characterize the local structure and ion dynamics of LIB materials. NMR spectroscopy is crucial in studying the electrochemical and physical properties of the LIB components. NMR applications are used for three of the components of LIBs: cathode, anode, and electrolyte. The material that is being analyzed will determine the appropriate NMR technique, such as solid-state NMR, in-situ NMR, and diffusion NMR.

Characterizing Li-ion cells and batteries can involve a galvanostatic cycle which can study the behavior of batteries being cycled. A current is applied to cause an electrochemical reaction, followed by a reverse reaction, and this is repeated until the battery degrades, usually because of temperature. NMR is used to determine the time this process will take.

NMR: Non-Destructive Analysis

The main benefits of NMR spectroscopy over alternative approaches are its non-destructive nature and ability to study a range of operating storage devices in situ. Further research will provide key observations that can lead to the development of more efficient, safer batteries in the future. Magic-angle spinning improves spectral resolution for solid-state samples by physically spinning the sample.

Ex-situ NMR can uncover the charging and discharging cycle during lithium-ion battery operation. It explored the new cathode material with a multi-layer structure with domains where lithium-ion is contained.

NMR is a valuable tool for researchers because of its high flexibility and chemical sensitivity whilst remaining non-invasive. NMR spectroscopy is a vital tool for investigating the chemical and physical properties and electrochemical performance of LIBs. It will help advance current research into finding more sustainable and efficient solutions to support the future of our planet. Further applications of NMR in battery research will support battery manufacturing and prevention of battery failures; furthermore, it will improve technologies to meet the demand for high efficiency, longer lifetime and lower costs.

To learn more about JEOL USA’s air-isolated microscopy workflow proving its value in advanced battery research and production, check our our press release on our Science of Energy theme at Pittcon 2023!

Super-Charged Mass Spectral Data Processing

Automated Structural Analysis using AI and GC-HRTOFMS

With the recent high-profile introduction of ChatGPT and Bard it’s no secret that artificial intelligence is here to stay. No matter how far this technology progresses, however, the most important software for any instrumentation will always be the scientist running the experiment. Looking to the future, AI will super-charge scientific analysis with high-speed identification of unknown compounds, and that future might be closer than we think.

At JEOL, Dr. Masaaki Ubukata’s recent work on Automated Structural Analysis for Real Unknown Compounds combines artificial intelligence (AI) with GC-HRTOFMS to rapidly provide analysis results of known mass spectra, automatically perform qualitative analysis of unknown chemical compounds, and provide high quality structural analysis results.

Prior to the development of our new software, structural analysis of real unknown compounds required significant knowledge, experience, and time: sorting through structural information for EI fragment ions, identifying higher-mass m/z ions as functional groups and substructures, looking at low-mass m/z fragment ions to classify compounds, and working through possible McLafferty rearrangement to derive structures from the fragmentation.

In this AI-assisted workflow, deconvolution of GC-MS data into mass spectrum, library search, molecular ion search, accurate mass analysis, isotope pattern matching, and structural analysis can all happen within minutes.

This newly developed automated structural analysis software, msFineAnalysis AI, two different AI programs: First, to predict chemical formulas from EI and SI (soft ionization) data and, second, to assign candidate structure matches by using our newly developed database for structure analysis.

Soft Ionization, but Smarter

Typically, despite being the most popular method used in gas chromatography-mass spectrometry (GC-MS), electron ionization (EI) results in weak or absent molecular ions in the mass spectral data, making it difficult to identify unknowns by EI alone. However, this technology leverages soft ionization data for molecular ion information with the large number of fragment ions observed in EI mass spectra to automatically interpret this data into potential structural formulas, even if the operator has no knowledge of mass spectrometry or AI.

Because of this, the predicted structural formula of a detected component is automatically obtained, with the ability to analyze the structures of up to 50 unknown compounds in 3 minutes or less. With less time required to perform qualitative analysis for a variety of sample types containing complex mixtures of structurally-similar compounds, scientists have more free time for running additional samples or getting started on their next experiment.

msFineAnalysis AI builds upon its predecessors, msFineAnalysis and msFineAnalysis iQ, but takes the analysis a step further by providing structural formula prediction for unknown compounds not registered in the NIST database. This technology is exclusively available on the JEOL AccuTOF™ GC-Alpha, our high-resolution GC-MS with best-in-class mass resolution, accurate mass measurement, and high mass accuracy. Stop by booth 2222 or download the software brochure to learn more about how AI software can energize your analysis!

Get to know JEOL de Mexico

For more than 30 years, the JEOL sales and service office in Mexico has been the resource for electron microscopes and microprobes, as well as NMR and Mass Spectrometers. We are proud to say that we partner with many well-known universities and organizations who are leading the way in research, and we are the preferred supplier for domestic industry.

JEOL de México continues our long history of dedication to providing support to our customers in education, research, and industry and encourage you to contact us at any time with your sales inquiries and service needs.

We are pleased to introduce our new Sales Manager, Erick Leyva. Erick is your primary contact for all sales enquiries regarding JEOL SEM, TEM, EPMA, Mass Spectrometers, and NMR Spectrometers, and manages our sales support organization. He has been with for JEOL for 4 years, and was promoted to Sales Manager of JEOL de México in 2022. He holds a Bachelor’s degree in Chemical Engineering from Universidad Nacional Autónoma de México (UNAM) with additional certificates from Harvard University and University of Michigan. He has also worked in sales at Anton Paar.

Alejandro Contreras is your primary contact for all service questions and requests for all JEOL instruments. Alejandro manages a department of 10 service engineers with expertise in JEOL instrumentation.

At JEOL de México we will continue to give the best support we can in our territory in sales, service and applications. By contacting Erick and Alejandro, JEOL de México customers can be confident they will have the best and fastest response time to their sales and service enquiries.

JEOL SALES

Ing. Erick Leyva Ramírez, Gerente de Ventas | LinkedIn

Teléfono: (55) 5448-5900 / 5211-4507 Ext. 101

Email: eleyva@jeol.com.mx

JEOL SERVICE

Alejandro Contreras

Teléfono: (55) 5448-5900

Email: service@jeol.com.mx

Elemental Analysis with Electron Microscopes

Electron Microscopy Excels at Elemental Analysis

Electron microscopes make it possible to see extraordinary details at ultrahigh magnifications, but they also make it possible to determine more details about the material you are investigating. Scanning Electron Microscopes (SEM) and Transmission Electron Microscopes (TEM) are essentially nanolabs when outfitted with multiple analytical detectors. For example, energy dispersive X-ray detectors (EDS or EDX) are used extensively to provide insight for analysis of elements ranging from Be to U. More specialized detectors enable detection of light elements like Li, or, in the case of TEM, fast elemental mapping up to atomic resolution.

Analytical SEM for EDS and SXES

EDS in general is considered a semi-quantitative elemental analysis technique. SEM-EDS provides information on the elements present, their relative concentrations and spatial distribution over very small volumes (micron and some instances nanometer scale).

With the analytical SEM you can view an EDS spectrum in real-time while also searching for the area of interest on the sample. JEOL EDS software makes it possible to perform Live Analysis, high resolution spectral mapping and quantitative mapping, drift compensation, line scan, and to produce large area montage maps. The fully-integrated EDS detector is capable of detecting elements from Be to U.

Gather-X, a new Windowless EDS from JEOL, provides even higher sensitivity and low-energy X-Ray detection, and can collect the entire X-ray range produced from the ultrahigh resolution Field Emission SEM, including low-energy X-rays down to Lithium. Collection provides clear, high count rate EDS maps with high spatial resolution.

For efficient and parallel collection of very low energy-rays a Soft X-ray Emission Spectrometer (SXES) provides the ultimate high spectral resolution (0.3eV). Ideal for Lithium Ion Battery research, it allows for the Nitrogen Kα and Titanium Lℓ line to be resolved with a separation of only 1.78eV, and also ultra-low energy, low-concentration sensitivity with the capability to detect Li even at low single digit weight percent concentration. An additional, and maybe its strongest asset, is its ability to do chemical state analysis. The spectrometer can detect subtle differences in emitted X-rays from conduction band and valence band which allows the distinction between bonding and crystal structure in samples containing the same elements.

TEM Analytical Capability at the Atomic Level

For Transmission Electron Microscopy, JEOL SDD detectors ranging from 60mm ² to 158mm ² deliver unparalleled EDX analytical results for a wide range of materials. Utilizing JEOL’s unique, on-the-fly “Lossless Drift Compensation”, large pixel EDX maps can be generated at up to atomic resolution, even for beam sensitive or 2D materials, at various accelerating voltages. In addition, JEOL’s spectrum imaging saves not only the entire spectrum data set but also each individual spectral slice, allowing for the specific summing of any number of frames collected during an experiment, which is useful for in-situ experiments.