Summer is ending, and as kids head back to school, we look forward to cooler weather and a calm end to hurricane season. Rigaku's Summer 2024 Journal is out now, featuring the latest in SAXS, XRD, and more, plus a spotlight on our NEX LS analyzer.
Summer officially ends in the northern hemisphere in less than a month. Children are heading back to school, if they haven't already. In Texas, we hope the summer inferno has reached its peak and we look forward to gradually cooling weather and, hopefully, a quiet end to hurricane season, which still has a few months left to go.
Rigaku has released the Summer 2024 issue of the Rigaku Journal (Volume 40, No. 2). See below for links to the articles, which cover a wide range of subjects, from SAXS to XRD to electron diffraction to thermal analysis to WDXRF to X-ray CT.
September looks to be a busy month for trade shows and other events. JASIS, for example, is one of the largest analytical instrumentation conventions in the world. It is always interesting to contemplate how many things in our everyday lives were produced with the assistance of X-ray analytical instrumentation. You'd be hard pressed to come up with something that isn't! This kind of materials analysis can be used at every step from prospecting for new ideas to production of the final product.
Our featured product this month is the NEX LS, a scanning multi-element coating analyzer manufactured by our Applied Rigaku Technologies division in Austin, Texas. This instrument will be showcased at the upcoming Labelexpo Americas conference in Chicago. It is a fascinating, versatile instrument that uses EDXRF technology to non-destructively provide valuable information about a coating’s properties or composition. Check out the video below to see it in action. It's yet another example of how X-ray analytical instrumentation is involved in the production of a wide array of things people use all the time. You'll also find a link to an application note about the use of EDXRF in the analysis of silicone coating on paper, clay-coated paper, and plastic.
ICSCRM 2024 | Raleigh, NC| September 28, 2024 - October 3, 2024 |Website
Rigaku XRD Forum in Germany, September 3-5, 2024
Mark your calendar for the Rigaku XRD Forum - Semiconductors/Thin Films/Coatings, taking place at the headquarters of Rigaku Europe SE in Neu-Isenburg, Germany, from September 3-5, 2024.
Discover the latest in X-ray diffraction technology through hands-on experience with Rigaku SmartLab diffractometers and advanced software. Benefit from insights shared by leading experts in lectures and workshops, engage in discussions on XRD topics, present research in poster sessions, and network with peers and industry leaders.
Attendance is free but limited, so early registration is encouraged.
Controlling coating thickness or composition is vital to meeting end-use specifications for the release, metal finishing, and automotive industries. If coatings or composition are not in spec throughout the process, this could lead to product rejection or failure. NEX LS helps solve the challenges of coating and converting processes in real time. With continuous monitoring, you can quickly identify quality and uniformity issues related to the entire roll as it's being produced.
The NEX LS analytical head sweeps back and forth across a moving web or coil, transmitting measurements to a console box and industrial touchscreen computer. Real-time data is displayed as a graphical cross-direction and machine-direction profile. You can choose full scanning mode or user-defined fixed analysis positions.
Designed explicitly to meet the needs of challenging conditions found in coating and converting processes, NEX LS helps maintain routine quality control for web and coil applications. The NEX LS linear scanner provides real-time coat weight profiling of your process. Common applications include silicone release coaters, converters, denesting Si for vacuum-formed plastics, conversion coatings, fuel cell loadings, metalized plastic, top coatings on metal coil, and fire retardants on fabric.
August 14, 2024: Researchers used electron diffraction to studynanometer-sized, air-sensitive crystallites of compounds formed with the noble gas xenon. The researchers synthesized three xenon difluoride-manganese tetrafluoride compounds and successfully determined their three-dimensional structures, allowing them to determine xenon-fluoride bond lengths. The first compound with a xenon bond was synthesized more than 60 years ago, but its structure has yet to be elucidated.
August 18, 2024: Cement production accounts for approximately 8% of global CO₂ emissions, making it the largest single industrial emitter. A startup company recently demonstrateda sustainable cement production method on a commercial scale. The process utilizes electrochemical neutral water electrolysis to decarbonize CaCO3, CaCO₃ producing a high-purity O₂/CO₂ gas mixture at the anode and H₂ at the cathode.
August 19, 2024: Researchers are using machine learning to study performance data topredict the cycle lives of lithium-metal batteries. Analysis of charge, discharge and voltage relaxation data enabled them to accurately estimate the longevity of these batteries without making any assumptions about how the batteries degrade.
August 21, 2024:Single crystals of atomically thin sapphirehave been prepared at room temperature, which scientists previously thought to be impossible. A 1.25 nm layer of c-Al₂O₃ was formed on a single-crystalline Al surface at room temperature. These ultrathin materials could be used to develop next-gen transistors.
Featured Application Notes
Delamination in Lithium-ion Batteries
X-ray micro-CT is a powerful tool that allows researchers to look inside batteries in a non-destructive way. Swelling and delamination after repeated use can be visualized and quantified without opening the packages. In this example, lithium-ion battery packs were scanned using a micro-CT scanner,CT Lab HX.
This application note demonstrates the analysis of silicone coating on paper, clay-coated paper, and plastic using the Rigaku NEX QC. When the silicone coating is too heavy, silicone material is needlessly wasted, while too little coating may not meet the product specifications. At-line EDXRF is an excellent option for the quality control process in producing coated products. It provides an affordable means of optimizing quality while minimizing costs and helping to minimize product rejection and waste.
Small angle X-ray scattering study for investigating 3D nanoparticle packing structure of Pt catalyst on Gd-doped CeO₂ supports for fuel cells
Tomoyuki Iwata, Kazuhiko Omote and Katsuyoshi Kakinuma
A 3D real-space structural model for fuel cell catalysis systems, consisting of Pt and Gd-doped CeO₂ nanoparticles, was constructed to match simulated small angle X-ray scattering (SAXS) intensity and observed SAXS intensity using the reverse Monte–Carlo (RMC) method. The observed SAXS patterns were well reproduced by those of the simulations. The presented SAXS-RMC modeling can evaluate both local arrangement of the constituent primary particles and aggregated mesoscale structure.
Evaluation of stable and metastable forms of acetaminophen using a combination of X-ray diffraction, thermal analysis, and electron diffraction
Taiji Yamamoto, Yasuaki Masuda and Hiroyasu Sato
Acetaminophen has been reported to have multiple stable and metastable crystal polymorphs; however, the details of its crystallization control, evaluation methods, thermal behavior, and some crystal structure information are not known very well. In this article, a combination of several different evaluation methods using Rigaku technologies was applied to the analysis of crystal structures and physical properties of acetaminophen crystal polymorphs. As a result, the thermal behavior and crystal structure of acetaminophen were clarified.
There are three methods for lattice constant calculation: 1. a simple method using the Miller indices of one observed diffraction peak and the d value converted from the peak position using Bragg’s law; 2. the least-squares method using multiple diffraction peaks and the Miller indices of each peak; 3. the Whole Powder Pattern Fitting method using a wide range of diffraction patterns. There are external and internal standard methods, each with their own advantages and disadvantages. In-situ measurements are also possible using a temperature control attachment, where the temperature of the sample can be changed and the diffraction pattern is acquired in situ.
Analysis of liquid and powder samples by benchtop wavelength dispersive X-ray fluorescence spectrometer Supermini200 without helium gas
Natsumi Okazaki
In WDXRF analysis, liquid and some powder samples are usually measured under helium atmosphere while other samples are measured under vacuum atmosphere. The global shortage of helium gas has resulted in high prices and long delivery times, making analysis using helium gas difficult. Originally, thebenchtop WDXRF analyzer Supermini200measured samples while the sample chamber and optical chamber were either in vacuum or helium atmosphere. Rigaku has developed a new feature for the Supermini200 to measure all forms of samples, including solids, powders, and liquids, without helium gas. This paper describes the details of air/vacuum atmosphere measurement with the Supermini200 and introduces actual analysis examples.
Thenano3DXfrom Rigaku is a laboratory-based X-ray microscope that enables nondestructive observation of three-dimensional structures of a sample by CT reconstruction from X-ray projection images. As an example of biological applications of laboratory-based X-ray microscopy, the X-ray CT observation of kidney microstructure has been performed. By observing mouse kidney sections stained with heavy-element reagents and resin-embedded in sheet form, a three-dimensional rendering of nephrons, the functional units of the kidney, has been obtained successfully at micron-level spatial resolution. Furthermore, a detailed statistical analysis of CT images from five independent nephrons showed that heavy-element-stained proximal and distal tubules can be distinguished by brightness values.
TG-SPME Attachment: A simple approach to evolved gas analysis with solid phase microextraction
While TG-MS and TG-FTIR are effective for analyzing evolved gases, these techniques involve complex setups. They require the integration of STA with MS or FTIR instruments via transfer lines, which can pose challenges regarding the installation environment and associated costs. Additionally, they may not identify complex gases evolved during the pyrolysis of polymers and biomaterials due to their limited separation capabilities, unlike chromatography. We have proposed the TG-Solid Phase Microextraction (SPME) method to address these limitations. This simplified method enhances evolved gas analysis and is now available as the TG-SPME attachment for Rigaku’s STA.
Thermo Mass Photo Capillary Interface: New Interface Without Cold Points for High Boiling Point Gases Detection
TG-DTA-MS requires an interface for gas transport in order to accurately introduce the gas generated from the sample section of the TG-DTA analyzer into the MS instrument. In this new interface for Thermo Mass Photo, Rigaku succeeded in developing a capillary interface without cold points, enabling the detection of high boiling point gases at a wider range than ever before.
Beneath the Surface: X-ray Analyses of Battery Materials and Structures
Non-Destructive Elemental Analysis of Batteries Using XRF
Wednesday, October 16, 2024 1:00 PM CDT
Did you know you can non-destructively analyze the elemental composition of various battery components using the X-ray fluorescence (XRF) technique?
XRF does not require the digestion of samples. You can analyze powder and solid samples with minimal to no sample preparation and gain their elemental composition ranging in levels from ppm to percent. Wavelength dispersive XRF (WDXRF) spectrometers can analyze from beryllium to curium. Energy dispersive XRF (EDXRF) is cost-effective and fast, making it ideal for the analyses required for recycling and recovering raw materials. The fundamental parameter method enables standardless semi-quantitative analysis, while the conventional calibration method using standards can provide more accurate results, depending on the accuracy requirements.
XRF is perfect for quantifying the main elements of NCM (nickel, cobalt, and manganese) in the cathode, as well as impurities or foreign materials in coatings and the carbon anode. Appropriate sample preparation methods allow air and humidity-sensitive materials to be analyzed easily.
In this webinar, you will learn how to prepare different types of battery samples for WDXRF elemental analysis and see various application examples, as well as the use of EDXRF for the recycling of lithium battery black mass.
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