Energy Dispersive Detector Research Articles

Microstructure, wear behaviour and laser ablation behaviour of double glow plasma alloyed Ta[sbnd]W coating

TaW alloy is considered a crucial candidate for barrel protective coatings due to its high melting point, excellent high-temperature performance, and ablative resistance. In this study, TaW coating was deposited on the surface of PCrNi3MoVA gun steel by double glow plasma alloying (DGPA) technique. The morphology, phase structure, wear property, and laser ablation behaviour of the TaW deposited coating was studied and analyzed by means of scanning electron microscope (SEM), energy dispersive spectroscopy detector (EDS), X-ray diffractometer (XRD), ball-on-disk friction test, and laser pulse heating experiment. The results showed that the coating was dense and metallurgically bonded to the substrate. The coating was primarily composed of the α-Ta phase, and W was solidly dissolved in the Ta to form a mutual solution with solid-solution strengthening effect. The wear mechanisms of TaW coating were adhesive wear and oxidative wear. During the laser pulse heating (LPH) process, the transition region, center region, and splash region appeared successively in the ablation area of the coating. After 10 s of ablation, only a region with a diameter of 0.1 mm was penetrated, highlighting the effective protective role of the TaW infiltrated layer on the substrate.

In‐depth study of a speiss/matte sample from Castillo de Huarmey, North Coast of Peru, and its implications for the pre‐Columbian production of arsenic bronze in the Central Andes

AbstractThis study aims to characterize the phase composition and chemistry of the speiss/matte sample from the Metallurgist's Burial at Castillo de Huarmey and to use the information derived from these analyses to infer the temperatures, furnace conditions, and ores associated with the smelting processes, which created the speiss/matte sample. For this purpose, a number of geochemical analyses were performed on the spies/matte fragment: analysis of the general chemical composition (handheld X‐ray fluorescence spectrometry [hhXRF], X‐ray photoelectron spectroscopy [XPS]), analysis of the chemical composition in the micro area (field emission scanning electron microscope with an energy dispersive spectroscopy detector [FE‐SEM‐EDS], field emission electron probe microanalysis [FE‐EPMA]), analysis of the mineral composition (X‐ray diffraction [XRD]), and analysis of the phase composition (Raman spectroscopy). Chemical and mineralogical analyses of the speiss/matte specimen determined that the specimen is composed of distinct arsenide, arsenate, sulfide, and glass phases. During the smelting process, the charge material consisted mainly of Cu, Fe, and As sulfides. Arsenopyrite is the most likely candidate as the mineral source of arsenic. In addition, temperatures of at least 1200°C were achieved during the smelting process, with smelting occurring over a relatively short timeframe given that effective density separation of speiss and matte phases was not achieved.

Open the Window to Lithium Detection and Nanostructure Analysis

Abstract The features and benefits of a new cutting-edge windowless energy-dispersive detector (EDS) detector are introduced. This innovative technology provides fast results at high signal-to-noise with ultra-high analytical spatial resolution. The benefits are demonstrated through examples of nanostructures from various nanoscale devices including lithium metal anode specimens. Using windowless EDS detector technology allows for the efficient collection of EDS data under the same conditions used for high-resolution imaging (low accelerating voltage, low probe current, and short working distance). Examples include cross sections of lithium metal anode materials prepared with a broad argon ion beam and using an air-isolated workflow. The analyses of the cycled and pristine lithium-ion battery (LIB) materials are shown, along with the contrast results of crystal-shaped impurities found within these materials.

Process and mechanism of recovery of lepidolite and spodumene by flotation with synergistic action of alkali corrosion and Mg(II)

How to efficiently extract lithium resources from raw ore plays an important role in promoting the development of new energy fields dominated by lithium. Therefore, this paper proposes a co-flotation process for lepidolite and spodumene. The process involves synergistic alkaline corrosion treatment synergistic with magnesium (Mg2+) ion activation. Micro-flotation experiments had proven the high efficiency of the process for recovering the two main lithium-containing minerals in this paper. Alkaline corrosion and Mg2+ synergistic action could effectively promote the adsorption of the collectors on the mineral surface using adsorption capacity detection, X-ray photoelectron spectroscopy detections, and zeta potential measurement. At the same time, there were adsorption differences between the two minerals under different treatment conditions. Additionally, the influence of alkali corrosion conditions on the morphology of the two minerals, the flocculation state after synergistic activation, and the mechanism and difference of adsorption morphology were explored through particle size analysis, scanning electron microscope measurements, energy dispersive spectrometer detection, and atomic force microscope detection.

Diffraction, spectroscopic and microscopic studies of the sand from the amber deposit

QUARTZ sand plays a crucial role in the production of float glass, as it is the main source of silicon dioxide, which is necessary for the production of glass. The research was conducted on two samples of QUARTZ sand from the Oleksiivka amber deposit. The aim of this study was to investigate the morphology and chemical composition of QUARTZ sand samples. The identification methods such as infrared spectroscopy, X-ray diffraction, and electron microscopy with the Energy Dispersive X-ray Spectrometer detector were presented. Applied methods allowed to identify crystalline phases and non-crystalline components of the tested samples.

Ru-Ce0.7Zr0.3O2-δ as an Anode Catalyst for the Internal Reforming of Dimethyl Ether in Solid Oxide Fuel Cells.

The development of direct dimethyl ether (DME) solid oxide fuel cells (SOFCs) has several drawbacks, due to the low catalytic activity and carbon deposition of conventional Ni-zirconia-based anodes. In the present study, the insertion of 2.0 wt.% Ru-Ce0.7Zr0.3O2-δ (ruthenium-zirconium-doped ceria, Ru-CZO) as an anode catalyst layer (ACL) is proposed to be a promising solution. For this purpose, the CZO powder was prepared by the sol-gel synthesis method, and subsequently, nanoparticles of Ru (1.0-2.0 wt.%) were synthesized by the impregnation method and calcination. The catalyst powder was characterized by BET-specific surface area, X-ray diffraction (XRD), field emission scanning electron microscopy with an energy-dispersive spectroscopy detector (FESEM-EDS), and transmission electron microscopy (TEM) techniques. Afterward, the catalytic activity of Ru-CZO catalyst was studied using DME partial oxidation. Finally, button anode-supported SOFCs with Ru-CZO ACL were prepared, depositing Ru-CZO onto the anode support and using an annealing process. The effect of ACL on the electrochemical performance of cells was investigated under a DME and air mixture at 750 °C. The results showed a high dispersion of Ru in the CZO solid solution, which provided a complete DME conversion and high yields of H2 and CO at 750 °C. As a result, 2.0 wt.% Ru-CZO ACL enhanced the cell performance by more than 20% at 750 °C. The post-test analysis of cells with ACL proved a remarkable resistance of Ru-CZO ACL to carbon deposition compared to the reference cell, evidencing the potential application of Ru-CZO as a catalyst as well as an ACL for direct DME SOFCs.

Application of a metallic-magnetic calorimeter for high-resolution x-ray spectroscopy of Fe at an EBIT

In this work, we present an experiment conducted at the S-EBIT-I ion trap of GSI. It involved the study of ion-electron collisions of Fe and Ba ions in various charge states with the electron beam. Characteristic x-ray radiation emitted during the continuous interaction was recorded utilizing an energy-dispersive maXs-30 detector based on metallic-magnetic calorimeter (MMC) technology. Optimizations to the applied sensitivity-drift correction and energy calibration procedures significantly improved the achieved energy resolution compared to previous applications of a similar detector. This made it possible to individually resolve and identify overlapping x-ray lines of iron and barium in a wide spectral range. As a demonstration of the outstanding detector performance, we used the recorded spectral data to extract an estimate of the charge state distribution of Fe ions in the trap. This experiment campaign marks an important milestone in the ongoing effort to enable the deployment of MMC detectors for future high-precision measurements in fundamental physics experiments.

Insight into effects of terbium on cell growth, sporulation and spore properties of Bacillus subtilis.

Recovery of rare earth elements (REEs) from wastewater with Bacillus subtilis(B. subtilis)during culture is promising due to its environmental benefits. However, the effects of REEs in the culture media on B. subtilis are poorly understood. This study aims to investigate the effects of the terbium (Tb(III)), a typical rare earth element, on the cell growth, sporulation, and spore properties of B. subtilis. Tb(III) can suppress bacterial growth while enhancing spore tolerance to wet heat. Spore germination and content of dipicolinic acid (DPA) were promoted at low concentrations of Tb(III) while inhibited at a high level, but an inverse effect on initial sporulation appeared. Scanning electron microscope and energy dispersive spectrometer detection indicated that Tb(III) complexed cells or spores and certain media components simultaneously. The germination results of the spores after elution revealed that Tb(III) attached to the spore surface was a key effector of spore germination. In conclusion, Tb(III) directly or indirectly regulated both the nutrient status of the media and certain metabolic events, which in turn affected most of the properties of B. subtilis. Compared to the coat-deficient strain, the wild-type strain grew faster and was more tolerant to Tb(III), DPA, and wet heat, which in turn implied that it was more suitable for the recovery of REEs during cultivation. These findings provide fundamental insights for the recovery of rare earths during the culture process using microorganisms.

Magnetic microcalorimeter with paramagnetic temperature sensors and integrated dc-SQUID readout for high-resolution x-ray emission spectroscopy

We present two variants of a magnetic microcalorimeter with paramagnetic temperature sensors and integrated dc-superconducting quantum interference device readout for high-resolution x-ray emission spectroscopy. Each variant employs two overhanging gold absorbers with a sensitive area of 150 × 150 μm2 and a thickness of 3 μm, thus providing a thickness related quantum efficiency of >98% for photons up to 5 keV and >50% for photons up to 10 keV. The first variant operated nominally but suffered from Joule power dissipation of the Josephson junction shunt resistors, athermal phonon loss, and slew rate limitations of the overall setup. Overall, it only achieved an energy resolution of ΔEFWHM=8.9 eV for 5.9 keV photons. In the second variant, we introduced an innovative tetrapod absorber geometry as well as a membrane technique for diverting dissipated heat away from the temperature sensors. When all mitigations are applied optimally, the second variant achieves an energy resolution of ΔEFWHM=1.25(18) eV for 5.9 keV photons and hence provides the present best energy resolving power E/ΔEFWHM among all existing energy-dispersive detectors for soft and tender x-rays.

Enhanced time resolution with a room-temperature energy dispersive X-ray PIN photodiode detector

Enhanced time resolution with a room-temperature energy dispersive X-ray PIN photodiode detector

Nanoscopic lignin mapping on cellulose nanofibers via scanning transmission electron microscopy and atomic force microscopy

Cellulose has been developed as an alternative to petrochemical materials. By comparison with refined nanofibers (RCNFs), lignocellulose nanofibers (LCNFs) show particular promise because it is produced from biomass using only mild pretreatment. The mechanical properties of LCNFs depend on the contained lignin. However, the microscopic location of the lignin contained in LCNFs has not been determined. Thus, we developed two methods to detect and visualize lignin. One uses a scanning transmission electron microscope (STEM) equipped with an energy dispersive X-ray spectroscopy detector. The other method uses an atomic force microscope (AFM) equipped with a cantilever coated with an aromatic molecule. Both methods revealed that the lignin in LCNFs covers a thin cellulose fiber and is precipitated in a grained structure. In particular, the AFM system was able to determine the nanoscopic location of lignin-rich areas. The present study establishes a strong tool for analyzing the characteristics of lignin-containing materials.Graphical abstract

Superconductivity of Li doped BSCCO mesoscopic fiber

Mesoscopic Li doped BSCCO fibres are synthesized by the electrospinning technology and the sequent sintering treatment. With the assistance of high resolution energy-dispersive x-ray spectroscopy detector in the Aberration-corrected transmission electron microscopy, we discovered hidden CuO grains and separated Bi-2212 phases, which is proved by the existence of fishtail effect in the magnetization loops. The electric measurement is fulfilled via four probe method with the help of focus ion beam operation. A non-trivial resistance behaviour appears, which can be attributed to its polycrystalline and superconducting phase separation features.

Influence of Mechanical Torsion on MgCa1 Corrosion Behavior in Simulated Body Fluid

In this paper, the influence of mechanical torsion on the corrosion of MgCa1 alloy in simulated body fluid (SBF) is presented. The corrosion behavior is examined by microstructural observations, including a scanning electron microscope equipped with an energy dispersive spectroscopy detector and electrochemical studies, mainly impedance spectroscopy measurements and polarization curves. The experiments were performed for different time durations (4 h to 8 h) with and without torsion applied (within elastic deformation range in the form of rotary movements) to assign the differences between the corrosion behavior of the samples. It is shown that mechanical torsion (rotations) promotes the leaching of calcium from the grain boundaries in the samples, which decreases the overall alloy corrosion rate. On the other hand, grain boundaries leached out of calcium compounds influence the sample microstructure by enabling cracks formation and propagation. Therefore, rotated samples corroded at a lower rate but were more susceptible to catastrophic failure. It was then concluded that MgCa1 alloy may be a promising biodegradable material for medical implants, however, its durability in SBF with torsion applied is far from being satisfactory.

High-energy interference-free K-lines synchrotron X-ray fluorescence microscopy of rare earth elements in hyperaccumulator plants.

Synchrotron-based micro-X-ray fluorescence analysis (µXRF) is a non-destructive and highly sensitive technique. However, element mapping of rare earth elements (REEs) under standard conditions requires care, since energy-dispersive detectors are not able to differentiate accurately between REEs L-shell X-ray emission lines overlapping with K-shell X-ray emission lines of common transition elements of high concentrations. We aim to test REE element mapping with high-energy interference-free excitation of the REE K-lines on hyperaccumulator plant tissues and compare with measurements with REE L-shell excitation at the microprobe experiment of beamline P06 (PETRA III, DESY). A combination of compound refractive lens optics (CRLs) was used to obtain a micrometre sized focussed incident beam with an energy of 44 keV and an extra-thick silicon drift detector (SDD) optimised for high-energy X-ray detection to detect the K-lines of yttrium (Y), lanthanum (La), cerium (Ce), praseodymium (Pr) and neodymium (Nd) without any interferences due to line overlaps. High-energy excitation from La to Nd in the hyperaccumulator organs was successful but compared to L-line excitation less efficient and therefore slow (∼10-fold slower than similar maps at lower incident energy) due to lower flux and detection efficiency. However, REE K-lines do not suffer significantly from self-absorption, which makes XRF-tomography of millimetre-sized frozen-hydrated plant samples possible. The K-line excitation of REEs at the P06 CRL setup has scope for application in samples that are particularly prone to REE interfering elements, such as soil samples with high concomitant Ti, Cr, Fe, Mn, Ni concentrations.

Simultaneous MMC Readout Using a Tailored $\mu$MUX Based Readout System

Magnetic microcalorimeters (MMCs) are cryogenic, energy-dispersive single-particle detectors providing excellent energy resolution, intrinsically fast signal rise time, quantum efficiency close to 100%, large dynamic range as well as almost ideal linear response. One of the remaining challenges to be overcome to ultimately allow for the utilization of large-scale MMC based detector arrays with thousands to millions of individual pixels is the realization of a SQUID based multiplexing technique particularly tailored for MMC readout. Within this context, we report on the first demonstration of a frequency-division multiplexed readout of an MMC based detector array using both, a custom microwave SQUID multiplexer as well as a dedicated software-defined radio (SDR) readout electronics. We successfully performed a simultaneous readout up to eight multiplexer channels, each monitoring two detector pixels. We show that the signal shape is not changed as compared to a dc-SQUID readout and that similar values for the energy resolution can be obtained. Nevertheless, we observed an influence of the internal quality factor of the microwave resonators used for frequency encoding on the energy resolution that affects the resolution of the co-added sum spectrum.

Strength, Mineralogy, Microstructure, and Statistical Analysis of Alkali-Activated Sugarcane Bagasse Ash–Eggshell Lime Pastes

Portland cement production is an energy-intensive process, and more sustainable substitutes are needed, e.g., alkali-activated binders originated from industrial wastes. Thus, this paper analyzes the combination of sugarcane bagasse ash (SCBA) and hydrated eggshell lime (HEL) as precursors for an alkali-activated binary system, a combination, to our best knowledge, not studied in past research. The mechanical and microstructural behavior of the SCBA-HEL alkali-activated pastes has been discussed through unconfined strength tests, and x-ray fluorescence, x-ray diffraction (XRD), Fourier transform infrared spectroscopy, and scanning electron microscopy (SEM) and energy-dispersive detector (EDS) microstructural analysis. In addition, an analysis of variance was applied to investigate the impact of a three-factor combination, i.e., SCBA/HEL ratio, NaOH concentration, and water/binder ratio (W/B), on the paste’s compressive strength. The highest compressive strength is associated with 80% of SCBA and 20% of HEL (ratio equals 4), 1 M molarity, and W/B relation of 0.8 (2.61% of Na2O). A C─ (N)─ A─ S─ H gel is observed in the form of an amorphous hump through the XRD pattern. SEM images show that the material synthesized from alkali-activation has a cementing effect, with a structure less dense and more porous than that of conventional cementing materials. The EDS display areas are rich in Ca, Si, Na, and Al. The bands found for the alkali-activated paste are consistent with vibrations characteristic of C─ A─ S─ H and N─ A─ S─ H gels.

HpMCA: a Python-based graphical program for energy-dispersive X-ray diffraction data collection and analysis

ABSTRACT Energy-dispersive X-ray diffraction (EDXD) at synchrotron beamlines is commonly used for the study of material properties under high pressure and/or high temperature. Experimenters typically rely on the availability of robust data collection and analysis at a beamline, but this has become increasingly difficult, especially with the introduction of multi-element detectors that generate complex, multi-dimensional data sets. These data sets have energy resolution, and they can also be resolved in relation to sample position, diffraction angle, or different external stimuli. We report a new Python-based graphical program, hpMCA, for EDXD data collection and analysis that streamlines the experimental process for the beamline users. The program features a user-friendly interface, capability for online viewing and analyzing data from multi-element energy-dispersive detectors, and includes features useful for working with samples under high pressure and/or high temperature, such as crystal phase identification, real-time unit cell lattice refinement, and pressure determination based on an equation of state.

Influence of Mn content on the magnetic properties of the hexagonal Mn(Co,Ge)2 phase

Herein, we report on the effect of Mn content on the magnetic properties of the hexagonal Mn(Co,Ge)2 with composition Mn36+xCo49-xGe15.This compound was previously described as Mn2Co3Ge (MgZn2-type structure), but later as Mn(Co,Ge)2 with its own structure type, all samples in this work follow the same superstructure model. Samples were synthesized by induction melting, the crystal structures were evaluated using a combination of X-ray diffraction together with scanning electron microscopy equipped and an energy dispersive X-ray spectroscopy detector. The Curie temperature (TC) is shifted towards lower temperature as the Mn content is increased. On the other hand, the spin reorientation temperature (TSRT) increases and the magnetic moment decreases as the Mn content is increased. The magnetocaloric properties were investigated for the x=1 alloy, Mn37Co48Ge15. It was found that the isothermal entropy change is 2 J kg−1 K−1 at room temperature for an applied field of 5 T.

Analysis of Degradation Products of Biodegradable ZnMgY Alloy.

Biodegradable metallic materials are increasingly gaining ground in medical applications. Zn-based alloys show a degradation rate between those recorded for Mg-based materials with the fastest degradation rate and Fe-based materials with the slowest degradation rate. From the perspective of medical complications, it is essential to understand the size and nature of the degradation products developed from biodegradable materials, as well as the stage at which these residues are eliminated from the body. This paper presents investigations conducted on the corrosion/degradation products of an experimental material (ZnMgY alloy in cast and homogenized state) after immersion tests in three physiological solutions (Dulbecco's, Ringer's and simulated body fluid (SBF)). Scanning electron microscopy (SEM) was used to highlight the macroscopic and microscopic aspects of corrosion products and their effects on the surface. An X-ray energy dispersive detector (EDS), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) provided general information about the compounds based on their non-metallic character. The pH of the electrolyte solution was recorded for 72 h during immersion. The pH variation of the solution confirmed the main reactions proposed for the corrosion of ZnMg. The agglomerations of corrosion products were on the micrometer scale, mainly oxides, hydroxides and carbonates or phosphates. The corrosion effects on the surface were homogeneously spread, with a tendency to connect and form cracks or larger corrosion zones, transforming the pitting corrosion pattern into a generalized one. It was noticed that the alloy's microstructure strongly influences the corrosion characteristics.

Petrographic studies and mineralogical characterization of the Dellen impactites

AbstractThe impact origin of the Early Cretaceous (140.82 ± 0.51 Ma) 20‐km diameter Dellen structure was proven in the late 60s based on the discovery of planar deformation features (PDFs) in quartz grains. Although decades have passed, impactites found from the crater have not received much attention. Thus, this study provides a detailed petrological and mineralogical description of impactites from Dellen. Impactites were classified based on mineralogical observations using the latest recommendations of nomenclature. The studied samples include impact melt rocks (clast rich, clast poor, and clast free), suevitic impact breccias, shocked and unshocked granite, and a shatter cone. Altogether, 16 samples with different lithologies were studied using a polarization microscope. Selected samples were studied with an energy dispersive spectroscopy detector attached to the scanning electron microscopy. PDFs were indexed using a four‐axis universal stage from seven samples. Selected samples for PDF studies consisted of clast‐rich impact melt rocks (DEL10, DEL13, D99), suevitic impact breccias (DEL14, DEL16, DEL24), and shocked granite target rock (DEL17). A total of 197 PDF sets in 113 quartz grains were studied, and 186 sets resulted in rational crystallographic orientations. Common orientations include π{101̅2}, ω{101̅3}, z{101̅1}, ξ{112̅2}, and {101̅4}. In suevitic impact breccias and impact melt rocks, ballen silica and plagioclase with checkerboard texture were abundant. The petrographic results in Dellen impactites indicate a range of shock pressures from at least 2 to over 60 GPa, based on diagnostic shock metamorphic features in minerals and the occurrence of impact melt rock.