Search results for: synchrotron

Authors: S. S. Sathiesh

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The aim of this project is to study the radiation mechanism synchrotron and Inverse Compton scattering. Theoretically, we discussed spectral energy distribution for both. Programming is done for plotting the graph of Power-law spectrum for synchrotron Radiation using fortran90. The importance of power law spectrum was discussed and studied to infer its physical parameters from the model fitting. We also discussed how to infer the physical parameters from the theoretically drawn graph, we have seen how one can infer B (magnetic field of the source), γ min, γ max, spectral indices (p1, p2) while fitting the curve to the observed data.

Keywords: blazars/quasars, beaming, synchrotron radiation, Synchrotron Self Compton, inverse Compton scattering, mrk421

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Authors: Giovanni Meloni

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Recent results are presented from experiments carried out at the Advanced Light Source (ALS) at the Chemical Dynamics Beamline of Lawrence Berkeley National Laboratory using multiplexed synchrotron photoionization mass spectrometry. The reaction mixture and a buffer gas (He) are introduced through individually calibrated mass flow controllers into a quartz slow flow reactor held at constant pressure and temperature. The gaseous mixture effuses through a 650 μm pinhole into a 1.5 mm skimmer, forming a molecular beam that enters a differentially pumped ionizing chamber. The molecular beam is orthogonally intersected by a tunable synchrotron radiation produced by the ALS in the 8-11 eV energy range. Resultant ions are accelerated, collimated, and focused into an orthogonal time-of-flight mass spectrometer. Reaction species are identified by their mass-to-charge ratios and photoionization (PI) spectra. Comparison of experimental PI spectra with literature and/or simulated curves is routinely done to assure the identity of a given species. With the aid of electronic structure calculations, potential energy surface scans are performed, and Franck-Condon spectral simulations are obtained. Examples of these experiments are discussed, ranging from new intermediates characterization to reaction mechanisms elucidation and biofuels oxidation pathways identification.

Keywords: mass spectrometry, reaction intermediates, synchrotron photoionization, oxidation reactions

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Authors: Sunil Dehipawala, Gayathrie Amarasuriya, N. Gadura, G. Tremberger Jr, D.Lieberman, Harry Gafney, Todd Holden, T. Cheung

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The iron environment in Fe-doped Vycor Anode was investigated with EXAFS using Brookhaven Synchrotron Light Source. The iron-reducing Shewanella oneidensis culture was grown in a microbial fuel cell under anaerobic respiration. The Fe bond length was found to decrease and correlate with the amount of biofilm growth on the Fe-doped Vycor Anode. The data suggests that Fe-doped Vycor Anode would be a good substrate to study the Shewanella oneidensis nanowire structure using EXAFS.

Keywords: EXAFS, fourier transform, Shewanella oneidensis, microbial fuel cell

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Authors: Sunil Dehipawala, Aregama Sirisumana, stephan Smith, P. Schneider, G. Tremberger Jr, D. Lieberman, Todd Holden, T. Cheung

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The arsenic and iron environments in different growth stages have been studied with EXAFS and XANES using Brookhaven Synchrotron Light Source. Collard Greens plants were grown and tissue samples were harvested. The project studied the EXAFS and XANES of tissue samples using As and Fe K-edges. The Fe absorption and the Fourier transform bond length information were used as a control comparison. The Fourier transform of the XAFS data revealed the coexistence of As (III) and As (V) in the As bonding environment inside the studied plant tissue samples, although the soil only had As (III). The data suggests that Collard Greens has a novel pathway to handle arsenic absorption in soil.

Keywords: EXAFS, fourier transform, metalloproteins, XANES

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Authors: S. Djaziri, F. Sket, A. Hynowska, S. Milenkovic

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The use of Fe-Al based intermetallics as an alternative to Cr/Ni based stainless steels is very promising for industrial applications that use critical raw materials parts under extreme conditions. However, the development of advanced Fe-Al based intermetallics with appropriate mechanical properties presents several challenges that involve appropriate processing and microstructure control. A processing strategy is being developed which aims at producing a net-shape porous Fe-based preform that is infiltrated with molten Al or Al-alloy. In the present work, porous Fe-based preforms produced by two different methods (selective laser melting (SLM) and Kochanek-process (KE)) are studied during infiltration with molten aluminum. In the objective to elucidate the mechanisms underlying the formation of Fe-Al intermetallic phases during infiltration, an in-house furnace has been designed for in situ observation of infiltration at synchrotron facilities combining x-ray radiography (XR) and x-ray diffraction (XRD) techniques. The feasibility of this approach has been demonstrated, and information about the melt flow front propagation has been obtained. In addition, reactive infiltration has been achieved where a bi-phased intermetallic layer has been identified to be formed between the solid Fe and liquid Al. In particular, a tongue-like Fe₂Al₅ phase adhering to the Fe and a needle-like Fe₄Al₁₃ phase adhering to the Al were observed. The growth of the intermetallic compound was found to be dependent on the temperature gradient present along the preform as well as on the reaction time which will be discussed in view of the different obtained results.

Keywords: combined synchrotron radiography and diffraction, Fe-Al intermetallic compounds, in-situ molten Al infiltration, porous solid Fe preforms

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Authors: Mohammad Reza Ghaani, Michele Catti

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The reduction of CoO/Fe₂O₃ oxides supported on carbon xerogels was studied to elucidate the effect of nano-size distribution of the catalyst in carbon matrices. Resorcinol formaldehyde xerogels were synthesized, impregnated with iron and cobalt nitrates, and subsequently heated to obtain the oxides. The mechanism of oxide reduction to metal was investigated by in-situ synchrotron X-ray diffraction in dynamic, non-isothermal conditions. Kinetic profiles of the reactions were obtained by plotting the diffraction intensities of selected Bragg peaks vs. temperature. The extracted Temperature-Programmed-Reduction (TPR) diagrams were analyzed by appropriate kinetic models, leading to best results with the Avrami-Erofeev model for all reduction reactions considered. The activation energies for the two-step reduction of iron oxide were 65 and 37 kJmol⁻¹, respectively. The average value for the reduction of CoO to Co was found to be around 21 kJ mol⁻¹. Such results may contribute to develop efficient and inexpensive non-noble metal-based catalysts in element form, e.g., Fe, Co, via heterogenization of metal complexes on mesoporous supports.

Keywords: non-isothermal kinetics, carbon aerogel, in-situ synchrotron X-ray diffraction, reduction mechanisms

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Authors: Amira Abdelrasoul

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This study aimed to ascertain the controlled permeability of biomimetic cellulose triacetate (CTA) membranes by investigating the electrical oscillatory behavior across impregnated membranes (IM). The biomimetic CTA membranes were infused with a fatty acid to induce electrical oscillatory behavior and, hence, to ensure controlled permeability. In situ synchrotron radiation micro-computed tomography (SR-μCT) at the BioMedical Imaging and Therapy (BMIT) Beamline at the Canadian Light Source (CLS) was used to evaluate the main morphology of IMs compared to neat CTA membranes to ensure fatty acid impregnation inside the pores of the membrane matrices. A monochromatic beam at 20 keV was used for the visualization of the morphology of the membrane. The X-ray radiographs were recorded by means of a beam monitor AA-40 (500 μm LuAG scintillator, Hamamatsu, Japan) coupled with a high-resolution camera, providing a pixel size of 5.5 μm and a field of view (FOV) of 4.4 mm × 2.2 mm. Changes were evident in the phase transition temperatures of the impregnated CTA membrane at the melting temperature of the fatty acid. The pulsations of measured voltages were related to changes in the salt concentration of KCl in the vicinity of the electrode. Amplitudes and frequencies of voltage pulsations were dependent on the temperature and concentration of the KCl solution, which controlled the permeability of the biomimetic membranes. The presented smart biomimetic membrane successfully combined porous polymer support and impregnating liquid not only imitate the main barrier properties of the biological membranes but could be easily modified to achieve some new properties, such as facilitated and active transport, regulation by chemical, physical and pharmaceutical factors. These results open new frontiers for the facilitation and regulation of active transport and permeability through biomimetic smart membranes for a variety of biomedical and drug delivery applications.

Keywords: biomimetic, membrane, synchrotron, permeability, morphology

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Authors: A. Al-Juboori, D. Wexler, H. Li, H. Zhu, C. Lu, A. McCusker, J. McLeod, S. Pannila, Z. Wang

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Squats are a type railhead defect related to rolling contact fatigue (RCF) damage and are considered serious problem affecting a wide range of railway networks across the world. Squats can lead to partial or complete rail failure. Formation mechanics of squats on the surface of rail steel is still a matter of debate. In this work, structural and microstructural observations from ex-service damaged rail both confirms the phases present in white etching layer (WEL) regions and relationship between cracking in WEL and squat defect formation. XRD synchrotron results obtained from the top surfaces of rail regions containing both WEL and squat defects reveal that these regions contain both martensite and retained austenite. Microstructural analysis of these regions revealed the occurrence cracks extending from WEL down into the rail through the squat region. These findings obtained from field rail specimen support the view that WEL contains regions of austenite and martensitic transformation product, and that cracks in this brittle surface layer propagate deeper into the rail as squats originate and grow.

Keywords: squat, white etching layer, rolling contact fatigue, synchrotron diffraction

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Authors: A. Alvaredo , R. Guzman De Villoria, P. Castell, Juan P. Fernandez-Blazquez

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Since graphene was discovered in 2004, has been considered as superb material, due to its outstanding mechanical, electrical and thermal properties. Graphene has been incorporated as reinforcement in several high performance polymers in order to obtain a good balance of properties and to get new properties as thermal or electric conductivity. As well known, the properties of semicrystalline polymer and its composites depends heavily on degree of crystallinity. In this context, our research group has studied the crystallization behavior from amorphous state of PEEK/GNP composites. The monitoring of cold crystallization processes studied by time-resolved simultaneous wide-angle X-ray scattering (WAXS) and small-angle X-ray scattering (SAXS). These techniques allowed to get an extremely relevant information about the evolution of the morphology of the PEEK/GNP composites. In addition, the thermal evolution of cold crystallization was followed by differential scanning calorimetry (DSC) as well. The experimental results showed changes in crystallization kinetics and c parameter unit cell when adding graphene. The main aim of this work is to produce PEEK/GNP composites and characterize their morphology, unit cell parameters and crystallization kinetic.

Keywords: PEEK, graphene, synchrotron, cold crystallization

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Authors: Michael Dole, Pierre Ninin, Denis Raffourt

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Most of the CERN’s facilities hosting particle accelerators are large, underground and radioactive areas. All fire detection systems installed in such areas, shall be carefully studied to cope with the particularities of this stringent environment. The detection equipment usually chosen by CERN to secure these underground facilities are based on air sampling technology. The electronic equipment is located in non-radioactive areas whereas air sampling networks are deployed in radioactive areas where fire detection is required. The air sampling technology provides very good detection performances and prevent the "radiation-to-electronic" effects. In addition, it reduces the exposure to radiations of maintenance workers and is permanently available during accelerator operation. In order to protect the Super Proton Synchrotron and its 7 km tunnels, a specific long distance aspirating smoke detector has been developed to detect smoke at up to 700 meters between electronic equipment and the last air sampling hole. This paper describes the architecture, performances and return of experience of the long distance fire detection system developed and installed to secure the CERN Super Proton Synchrotron tunnels.

Keywords: air sampling, fire detection, long distance, radioactive areas

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Authors: Seokyoon Moon, Yun-Ho Ahn, Heejoong Kim, Sujin Hong, Yunseok Lee, Youngjune Park

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Gas hydrate is a non-stoichiometric crystalline compound consisting of host water-framework and low molecular weight guest molecules. Small gaseous molecules such as CH₄, CO₂, and N₂ can be captured in the host water framework lattices of the gas hydrate with specific temperature and pressure conditions. The three well-known crystal structures of structure I (sI), structure II (sII), and structure H (sH) are determined by the size and shape of guest molecules. In this study, we measured the phase equilibria of binary (2,2-dimethyl-1-propanol + CO₂, CH₄, N₂) hydrates to explore their fundamental thermodynamic characteristics. We identified the structure of the binary gas hydrate by employing synchrotron high-resolution powder diffraction (HRPD), and the guest distributions in the lattice of gas hydrate were investigated via dispersive Raman and ¹³C solid-state nuclear magnetic resonance (NMR) spectroscopies. The end-to-end distance of 2,2-dimethyl-1-propanol was calculated to be 7.76 Å, which seems difficult to be enclathrated in large cages of sI or sII. However, due to the flexibility of the host water framework, binary hydrates of sI or sII types can be formed with the help of small gas molecule. Also, the synchrotron HRPD patterns revealed that the binary hydrate structure highly depends on the type of help gases; a cubic Fd3m sII hydrate was formed with CH₄ or N₂, and a cubic Pm3n sI hydrate was formed with CO₂. Interestingly, dispersive Raman and ¹³C NMR spectra showed that the unique tuning phenomenon occurred in binary (2,2-dimethyl-1-propanol + CO₂) hydrate. By optimizing the composition of NPA, we can achieve both thermodynamic stability and high CO₂ storage capacity for the practical application to CO₂ capture.

Keywords: clathrate, gas hydrate, neopentyl alcohol, CO₂, tuning phenomenon

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Authors: T. N. Tran Thi, J. Morse, C. Detlefs, P. K. Cook, C. Yıldırım, A. C. Jakobsen, T. Zhou, J. Hartwig, V. Zurbig, D. Caliste, B. Fernandez, D. Eon, O. Loto, M. L. Hicks, A. Pakpour-Tabrizi, J. Baruchel

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The ability to grow boron-doped diamond epilayers of high crystalline quality is a prerequisite for the fabrication of diamond power electronic devices, in particular high voltage diodes and metal-oxide-semiconductor (MOS) transistors. Boron and intrinsic diamond layers are homoepitaxially overgrown by microwave assisted chemical vapour deposition (MWCVD) on single crystal high pressure, high temperature (HPHT) grown bulk diamond substrates. Various epilayer thicknesses were grown, with dopant concentrations ranging from 1021 atom/cm³ at nanometer thickness in the case of 'delta doping', up 1016 atom/cm³ and 50µm thickness or high electric field drift regions. The crystalline quality of these overgrown layers as regards defects, strain, distortion… is critical for the device performance through its relation to the final electrical properties (Hall mobility, breakdown voltage...). In addition to the optimization of the epilayer growth conditions in the MWCVD reactor, other important questions related to the crystalline quality of the overgrown layer(s) are: 1) what is the dependence on the bulk quality and surface preparation methods of the HPHT diamond substrate? 2) how do defects already present in the substrate crystal propagate into the overgrown layer; 3) what types of new defects are created during overgrowth, what are their growth mechanisms, and how can these defects be avoided? 4) how can we relate in a quantitative manner parameters related to the measured crystalline quality of the boron doped layer to the electronic properties of final processed devices? We describe synchrotron-based techniques developed to address these questions. These techniques allow the visualization of local defects and crystal distortion which complements the data obtained by other well-established analysis methods such as AFM, SIMS, Hall conductivity…. We have used Grazing Incidence X-ray Diffraction (GIXRD) at the ID01 beamline of the ESRF to study lattice parameters and damage (strain, tilt and mosaic spread) both in diamond substrate near surface layers and in thick (10–50 µm) overgrown boron doped diamond epi-layers. Micro- and nano-section topography have been carried out at both the BM05 and ID06-ESRF) beamlines using rocking curve imaging techniques to study defects which have propagated from the substrate into the overgrown layer(s) and their influence on final electronic device performance. These studies were performed using various commercially sourced HPHT grown diamond substrates, with the MWCVD overgrowth carried out at the Fraunhofer IAF-Germany. The synchrotron results are in good agreement with low-temperature (5°K) cathodoluminescence spectroscopy carried out on the grown samples using an Inspect F5O FESEM fitted with an IHR spectrometer.

Keywords: synchrotron X-ray diffaction, crystalline quality, defects, diamond overgrowth, rocking curve imaging

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Authors: Disha Gupta

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The aim of this research is to conduct X-ray and e-beam characterization techniques on lithium-ion battery materials for the improvement of battery performance. The key characterization techniques employed are the synchrotron X-ray Absorption Spectroscopy (XAS) combined with X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) to obtain a more holistic approach to understanding material properties. This research effort provides additional battery characterization knowledge that promotes the development of new cathodes, anodes, electrolyte and separator materials for batteries, hence, leading to better and more efficient battery performance. Both ex-situ and in-situ synchrotron experiments were performed on LiFePO₄, one of the most common cathode material, from different commercial sources and their structural analysis, were conducted using Athena/Artemis software. This analysis technique was then further extended to study other cathode materials like LiMnxFe(₁₋ₓ)PO₄ and even some sulphate systems like Li₂Mn(SO₄)₂ and Li₂Co0.5Mn₀.₅ (SO₄)₂. XAS data were collected for Fe and P K-edge for LiFePO4, and Fe, Mn and P-K-edge for LiMnxFe(₁₋ₓ)PO₄ to conduct an exhaustive study of the structure. For the sulphate system, Li₂Mn(SO₄)₂, XAS data was collected at both Mn and S K-edge. Finite Difference Method for Near Edge Structure (FDMNES) simulations were also conducted for various iron, manganese and phosphate model compounds and compared with the experimental XANES data to understand mainly the pre-edge structural information of the absorbing atoms. The Fe K-edge XAS results showed a charge compensation occurring on the Fe atom for all the differently synthesized LiFePO₄ materials as well as the LiMnxFe(₁₋ₓ)PO₄ systems. However, the Mn K-edge showed a difference in results as the Mn concentration changed in the materials. For the sulphate-based system Li₂Mn(SO₄)₂, however, no change in the Mn K-edge was observed, even though electrochemical studies showed Mn redox reactions.

Keywords: li-ion batteries, electrochemistry, X-ray absorption spectroscopy, XRD

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Authors: Swapnil Kumar Singh

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Gamma-ray bursts (GRB's), short and intense pulses of low-energy γ rays, have fascinated astronomers and astrophysicists since their unexpected discovery in the late sixties. GRB'sare accompanied by long-lasting afterglows, and they are associated with core-collapse supernovae. The detection of delayed emission in X-ray, optical, and radio wavelength, or "afterglow," following a γ-ray burst can be described as the emission of a relativistic shell decelerating upon collision with the interstellar medium. While it is fair to say that there is strong diversity amongst the afterglow population, probably reflecting diversity in the energy, luminosity, shock efficiency, baryon loading, progenitor properties, circumstellar medium, and more, the afterglows of GRBs do appear more similar than the bursts themselves, and it is possible to identify common features within afterglows that lead to some canonical expectations. After an initial flash of gamma rays, a longer-lived "afterglow" is usually emitted at longer wavelengths (X-ray, ultraviolet, optical, infrared, microwave, and radio). It is a slowly fading emission at longer wavelengths created by collisions between the burst ejecta and interstellar gas. In X-ray wavelengths, the GRB afterglow fades quickly at first, then transitions to a less-steep drop-off (it does other stuff after that, but we'll ignore that for now). During these early phases, the X-ray afterglow has a spectrum that looks like a power law: flux F∝ E^β, where E is energy and beta is some number called the spectral index. This kind of spectrum is characteristic of synchrotron emission, which is produced when charged particles spiral around magnetic field lines at close to the speed of light. In addition to the outgoing forward shock that ploughs into the interstellar medium, there is also a so-called reverse shock, which propagates backward through the ejecta. In many ways," reverse" shock can be misleading; this shock is still moving outward from the restframe of the star at relativistic velocity but is ploughing backward through the ejecta in their frame and is slowing the expansion. This reverse shock can be dynamically important, as it can carry comparable energy to the forward shock. The early phases of the GRB afterglow still provide a good description even if the GRB is highly collimated since the individual emitting regions of the outflow are not in causal contact at large angles and so behave as though they are expanding isotropically. The majority of afterglows, at times typically observed, fall in the slow cooling regime, and the cooling break lies between the optical and the X-ray. Numerous observations support this broad picture for afterglows in the spectral energy distribution of the afterglow of the very bright GRB. The bluer light (optical and X-ray) appears to follow a typical synchrotron forward shock expectation (note that the apparent features in the X-ray and optical spectrum are due to the presence of dust within the host galaxy). We need more research in GRB and Particle Physics in order to unfold the mysteries of afterglow.

Keywords: GRB, synchrotron, X-ray, isotropic energy

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Authors: Raphaelle Guillou, Matthieu Le Saux, Jean-Christophe Brachet, Thomas Guilbert, Elodie Rouesne, Denis Menut, Caroline Toffolon-Masclet, Dominique Thiaudiere

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In some hypothetical accidental situations, such as during a Loss Of Coolant Accident (LOCA) in pressurized water reactors, fuel cladding tubes made of zirconium alloys can be exposed for a few minutes to steam at High Temperature (HT up to 1200°C) before being cooled and then quenched in water. Under LOCA-like conditions, the cladding undergoes a number of metallurgical changes (phase transformations, oxygen diffusion and growth of an oxide layer...) and is consequently submitted to internal stresses whose state evolves during the transient. These stresses can have an effect on the oxide structure and the oxidation kinetics of the material. They evolve during cooling, owing to differences between the thermal expansion coefficients of the various phases and phase transformations of the metal and the oxide. These stresses may result in the failure of the cladding during quenching, once the material is embrittled by oxidation. In order to progress in the evaluation of these internal stresses, X-ray diffraction experiments were performed in-situ under synchrotron radiation during HT oxidation and subsequent cooling on Zircaloy-4 sheet samples. First, structural evolutions, such as phase transformations, have been studied as a function of temperature for both the oxide layer and the metallic substrate. Then, internal stresses generated within the material oxidized at temperatures between 700 and 900°C have been evaluated thanks to the 2θ diffraction peak position shift measured during the in-situ experiments. Electron backscatter diffraction (EBSD) analysis was performed on the samples after cooling in order to characterize their crystallographic texture. Furthermore, macroscopic strains induced by oxidation in the conditions investigated during the in-situ X-ray diffraction experiments were measured in-situ in a dilatometer.

Keywords: APRP, stains measurements, synchrotron diffraction, zirconium allows

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Authors: A. Larrousi, M. Elkeurti, K. Amara, M. Zemouli, L. H. Coudert, I. R. Medvedev, F. C. De Lucia, Atsuko Maeda, R. W. C. McKellar, D. Appadoo

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Experimental and theoretical investigations of the microwave and far infrared spectra of CH3COD are reported. Two hundred twelve lines were identified in the far infrared spectrum recorded using the Canadian synchrotron radiation light source. Two thousand one hundred and sixty-eight lines in vt=0,1 and 216 in vt=2 have been measured in the microwave spectrum obtained using the fast scan submillimeter spectroscopic technique. A global analysis of the new data and of already available microwave lines has been carried out and yielded values for rotation–torsion parameters. The unitless weighted standard deviation of the fit is 1.6. 46 parameters and 216 lines were identified.

Keywords: CH3COD, torsion, the microwave spectra, far infrared spectra high resolution

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Authors: Daniel R. McDougall, Martin D. de Jonge, Gordon M. Miskelly, Duncan J. McGillivray, Andrew G. Jeffs

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The chelating agent ethylenediaminetetraacetic acid (EDTA) is commonly added as a cure-all to seawater in aquaculture hatcheries around the world to reduce heavy metal toxicity, significantly improve the survival of larval shellfish, and to therefore improve the overall production efficiency of the aquaculture industry. However, EDTA is not a biodegradable chemical and is considered to be a persistent organic pollutant, which will accumulate in the environment over time. This makes the use of EDTA unsustainable environmentally, and therefore alternatives should be considered. Ethylenediaminedisuccinic acid (EDDS) is a biodegradable alternative to EDTA with very similar metal chelation properties. This study investigates the effect of EDTA and EDDS at two different concentrations, on metal concentrations found within developing New Zealand green-lipped mussel (Perna canaliculus) larvae. P. canaliculus is New Zealand’s main shellfish aquaculture species, providing a major export for New Zealand’s economy, with excellent potential for increased production in the near future. It is well known that the early stages of bivalve development are the most vulnerable to metal toxicity and P. canaliculus is no exception. The commercially used concentration (12 µmol L⁻¹) of EDTA added to P. canaliculus larval rearing tanks often increases the yield of D-larvae by over 80%. This concentration of EDTA and EDDS will be tested in this study, along with a lower concentration (3 µmol L⁻¹). After 48 hours of larval development, the D-larvae will be analyzed for heavy metal content with Inductively Coupled Plasma Mass Spectrometry (ICP-MS) and heavy metal distribution with synchrotron X-ray Fluorescence Microscopy (XFM). In this study, we found that EDDS also improves the yield of P. canaliculus larvae and could be a viable alternative to EDTA in aquaculture. Furthermore, results suggest a higher concentration of chelating agent is more effective for improving the yield of developing P. canaliculus larvae. Metals with significant differences in concentration with the addition of EDTA were Cr, Cu, Zn, Cd and Pb (P < 0.05). We observed for the first time to the author’s best knowledge, metal distribution within 100 µm P. canaliculus D-larvae using synchrotron XFM and found changes in the distribution of metals with the addition of EDTA. XFM also has the potential to provide information about the chemical state of the metals within mussel larvae. This research provides greater insight into the reasons for the effectiveness of adding the chelating agent to aquaculture culture water, and a more environmentally conscious alternative to the currently used EDTA, which could be extremely valuable for the aquaculture industry.

Keywords: EDDS, EDTA, heavy metals, P. canaliculus, toxicity, water treatment

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Authors: Saad S. Alrwashdeh, Henning Markötter, Handri Ammari, Jan Haußmann, Tobias Arlt, Joachim Scholta, Ingo Manke

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In this investigation, synchrotron X-ray imaging is used to study water transport inside polymer electrolyte membrane fuel cells. Two measurement techniques are used, namely in-situ radiography and quasi-in-situ tomography combining together in order to reveal the relationship between the structures of the microporous layers (MPLs) and the gas diffusion layers (GDLs), the operation temperature and the water flow. The developed cell is equipped with a thick GDL and a high back pressure MPL. It is found that these modifications strongly influence the overall water transport in the whole adjacent GDM.

Keywords: polymer electrolyte membrane fuel cell, microporous layer, water transport, radiography, tomography

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Authors: Chetna Tyagi, Ambuj Tripathi, Devesh Avasthi

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Graphene oxide consists of sp³ hybridization along with sp² hybridization due to the presence of different oxygen-containing functional groups on its edges and basal planes. However, its sp³ / sp² hybridization can be tuned by various methods to utilize it in different applications, like transistors, solar cells and biosensors. Ion beam irradiation can also be one of the methods to optimize sp² and sp³ hybridization ratio for its desirable properties. In this work, graphene oxide films were irradiated with 100 keV Argon ions at different fluences varying from 10¹³ to 10¹⁶ ions/cm². Synchrotron X-ray diffraction measurements showed an increase in crystallinity at the low fluence of 10¹³ ions/cm². Raman spectroscopy performed on irradiated samples determined the defects induced by the ion beam qualitatively. Also, identification of different groups and their removal with different fluences was done using Fourier infrared spectroscopy technique.

Keywords: graphene oxide, ion beam irradiation, spectroscopy, X-ray diffraction

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Authors: Minas Balyan

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Nowadays X-ray nonlinear diffraction and nonlinear effects are investigated due to the presence of the third generation synchrotron sources and XFELs. X-ray third order nonlinear dynamical diffraction is considered as well. Using the nonlinear model of the usual visible light optics the third-order nonlinear Takagi’s equations for monochromatic waves and the third-order nonlinear time-dependent dynamical diffraction equations for X-ray pulses are obtained by the author in previous papers. The obtained equations show, that even if the Fourier-coefficients of the linear and the third order nonlinear susceptibilities are zero (forbidden reflection), the dynamical diffraction in the nonlinear case is related to the presence in the nonlinear equations the terms proportional to the zero order and the second order nonzero Fourier coefficients of the third order nonlinear susceptibility. Thus, in the third order nonlinear Bragg diffraction case a nonlinear analogue of the well-known Renninger effect takes place. In this work, the 'third order nonlinear Renninger effect' is considered theoretically.

Keywords: Bragg diffraction, nonlinear Takagi’s equations, nonlinear Renninger effect, third order nonlinearity

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Authors: Abdulrahman Sumayli

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Natural Zinc has many significant biological functions, including developments and sustainable of bones and wound healing. Metallic zinc has recently been explored as potential biomaterials that have preferable biodegradable, biocompatible, and mechanical properties. Pure metal zinc has a preferable physical and mechanical properties for biodegradable and biocompatible applications such as density and modulus of elasticity. The aim of the research is to make different Zn-based metallic alloys and test them effectively to be used as biocompatible and biodegradable materials in the field biomedical application. Microstructure study of the as-cast alloys will be examined using SEM (scanning electron microscope) followed by X-ray diffraction investigated so as to evaluate phase constitution of the designed alloys. After that, immersion test and electrochemical test will be applied to the designed alloys so as to study bio corrosion behaviour of the proposed alloys. Finally, in vitro cytocompatibility well conducted to study biocompatibility of the made alloys.

Keywords: Zn-based alloys, biodegradable and biocompatible materials, cytotoxicity test, neutron synchrotron imaging

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Authors: Bing Shi, Raymond A. Conley, Jun Qian, Xianbo Shi, Steve Heald, Lahsen Assoufid

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A pair of Kirkpatrick-Baez (KB) mirrors were designed and fabricated for experiments within a hard x-ray energy range lower than 20 kev at beamline 20-ID in a synchrotron radiation facility, Advanced Photon Source (APS). The KB mirrors were deposited with Rhodium thin films using a customized designed and self-built magnetron sputtering system. The purpose of these mirrors is to focus the x-ray beam down to 1 micron. This is the first pair of Rhodium-coated KB mirrors with elliptical shape that was fabricated using the profile coating technique. The profile coating technique is to coat the substrate with designed shape using masks during the deposition. The mirrors were equipped at the beamline and achieved the designed focusing requirement. The details of the mirror design, the fabrication process, and the customized magnetron sputtering deposition system will be discussed.

Keywords: magnetron-sputtering deposition, focusing optics, x-ray, rhodium thin film

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Authors: Till Fehlauer, Blanche Collin, Bernard Angeletti, Andrea Somogyi, Claire Lallemand, Perrine Chaurand, Cédric Dentant, Clement Levard, Jerome Rose

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Over the last decades, yttrium (Y) has gained importance in high-tech applications. It is an essential part of alloys and compounds used for lasers, displays, or cell phones, for example. Due to its chemical similarities with the lanthanides, Y is often considered a rare earth element (REE). Despite their increased usage, the environmental behavior of REEs remains poorly understood. Especially regarding their interactions with plants, many uncertainties exist. On the one hand, Y is known to have a negative effect on root development and germination, but on the other hand, it appears to promote plant growth at low concentrations. In order to understand these phenomena, a precise knowledge is necessary about how Y is absorbed by the plant and how it is handled once inside the organism. Contradictory studies exist, stating that due to a similar ionic radius, Y and the other REEs might be absorbed through Ca²⁺-channels, while others suspect that Y has a shared pathway with Al³⁺. In this study, laser ablation coupled ICP-MS, and synchrotron-based micro-X-ray fluorescence (µXRF, beamline Nanoscopium, SOLEIL, France) have been used in order to localize Y within the plant tissue and identify associated elements. The plant used in this study is Saxifraga paniculata, a rugged alpine plant that has shown an affinity for Y in previous studies (in prep.). Furthermore, Saxifraga paniculata performs guttation, which means that it possesses phloem sap secreting openings on the leaf surface that serve to regulate root pressure. These so-called hydathodes could provide special insights in elemental transport in plants. The plants have been grown on Y doped soil (500mg/kg DW) for four months. The results showed that Y was mainly concentrated in the roots of Saxifraga paniculata (260 ± 85mg/kg), and only a small amount was translocated to the leaves (10 ± 7.8mg/kg). µXRF analysis indicated that within the root transects, the majority of Y remained in the epidermis and hardly penetrated the stele. Laser ablation coupled ICP-MS confirmed this finding and showed a positive correlation in the roots between Y, Fe, Al, and to a lesser extent Ca. In the stem transect, Y was mainly detected in a hotspot of approximately 40µm in diameter situated in the endodermis area. Within the stem and especially in the hotspot, Y was highly colocalized with Al and Fe. Similar-sized Y hotspots have been detected in/on the leaves. All of them were strongly colocalized with Al and Fe, except for those situated within the hydathodes, which showed no colocalization with any of the measured elements. Accordingly, a relation between Y and Ca during root uptake remains possible, whereas a correlation to Fe and Al appears to be dominant in the aerial parts, suggesting common storage compartments, the formation of complexes, or a shared pathway during translocation.

Keywords: laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), Phytoaccumulation, Rare earth elements, Saxifraga paniculata, Synchrotron-based micro-X-ray fluorescence, Yttrium

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Authors: Majid Samavatian, Reza Gholamipour, Vahid Samavatian

Abstract:

This study addresses the role of rejuvenation on the fluctuation of atomic-level stresses and nanoscale topological heterogeneity in ZrCuNiAl bulk metallic glass (BMG). Based on atomic force microscopy (AFM) results, the rejuvenation process leads to an increase in nanoscale spatial heterogeneity manifested by the intensification of the local viscoelastic response of the BMG nanostructure. It means that the rejuvenation process induces more loose-packing structures which behave towards an external load in a viscoelastic way. Hence, it is suggested that the alteration of such heterogeneity may be attributed to the variation of positional atomic rearrangement during the evolution of structural rejuvenation. On the other side, the synchrotron X-ray diffraction (XRD) results indicate that the rejuvenation intensifies the variation of internal stresses at the atomic level. This conclusion unfolds that the increase of atomic-level stresses during rejuvenation induces structural disordering and nanoscale heterogeneity in the amorphous material.

Keywords: bulk metallic glass, heterogeneity, rejuvenation, nanostructure

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Authors: Masoume Ehsani, Ning Zhu, Huu Doan, Ali Lohi, Amira Abdelrasoul

Abstract:

Membrane fouling poses severe challenges in membrane-based wastewater treatment applications. Ultrasound (US) has been considered an effective fouling remediation technique in filtration processes. Bubble cavitation in the liquid medium results from the alternating rarefaction and compression cycles during the US irradiation at sufficiently high acoustic pressure. Cavitation microbubbles generated under US irradiation can cause eddy current and turbulent flow within the medium by either oscillating or discharging energy to the system through microbubble explosion. Turbulent flow regime and shear forces created close to the membrane surface cause disturbing the cake layer and dislodging the foulants, which in turn improve the cleaning efficiency and filtration performance. Therefore, the number, size, velocity, and oscillation pattern of the microbubbles created in the liquid medium play a crucial role in foulant detachment and permeate flux recovery. The goal of the current study is to gain in depth understanding of the influence of the US power intensity and frequency on the microbubble dynamics and its characteristics generated under US irradiation. In comparison with other imaging techniques, the synchrotron in-line Phase Contrast Imaging technique at the Canadian Light Source (CLS) allows in-situ observation and real-time visualization of microbubble dynamics. At CLS biomedical imaging and therapy (BMIT) polychromatic beamline, the effective parameters were optimized to enhance the contrast gas/liquid interface for the accuracy of the qualitative and quantitative analysis of bubble cavitation within the system. With the high flux of photons and the high-speed camera, a typical high projection speed was achieved; and each projection of microbubbles in water was captured in 0.5 ms. ImageJ software was used for post-processing the raw images for the detailed quantitative analyses of microbubbles. The imaging has been performed under the US power intensity levels of 50 W, 60 W, and 100 W, in addition to the US frequency levels of 20 kHz, 28 kHz, and 40 kHz. For the duration of 2 seconds of imaging, the effect of the US power and frequency on the average number, size, and fraction of the area occupied by bubbles were analyzed. Microbubbles’ dynamics in terms of their velocity in water was also investigated. For the US power increase of 50 W to 100 W, the average bubble number and the average bubble diameter were increased from 746 to 880 and from 36.7 µm to 48.4 µm, respectively. In terms of the influence of US frequency, a fewer number of bubbles were created at 20 kHz (average of 176 bubbles rather than 808 bubbles at 40 kHz), while the average bubble size was significantly larger than that of 40 kHz (almost seven times). The majority of bubbles were captured close to the membrane surface in the filtration unit. According to the study observations, membrane cleaning efficiency is expected to be improved at higher US power and lower US frequency due to the higher energy release to the system by increasing the number of bubbles or growing their size during oscillation (optimum condition is expected to be at 20 kHz and 100 W).

Keywords: bubble dynamics, cavitational bubbles, membrane fouling, ultrasonic cleaning

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Authors: Anil Kumar, Rajnish Kaur, Mateusz Czyzycki, Alessandro Migilori, Andreas Germanos Karydas, Sanjiv Puri

Abstract:

The radiative decay of Li(i=1-3) sub-shell vacancies produced through photoionization results in production of the characteristic emission spectrum comprising several X-ray lines, whereas non-radiative vacancy decay results in Auger electron spectrum. Accurate reliable data on the Li(i=1-3) sub-shell X-ray production (XRP) cross sections is of considerable importance for investigation of atomic inner-shell ionization processes as well as for quantitative elemental analysis of different types of samples employing the energy dispersive X-ray fluorescence (EDXRF) analysis technique. At incident photon energies in vicinity of the absorption edge energies of an element, the many body effects including the electron correlation, core relaxation, inter-channel coupling and post-collision interactions become significant in the photoionization of atomic inner-shells. Further, in case of compounds, the characteristic emission spectrum of the specific element is expected to get influenced by the chemical environment (coordination number, oxidation state, nature of ligand/functional groups attached to central atom, etc.). These chemical effects on L X-ray fluorescence parameters have been investigated by performing the measurements at incident photon energies much higher than the Li(i=1-3) sub-shell absorption edge energies using EDXRF spectrometers. In the present work, the cross sections for production of the Lk(k= γ2,3, γ4) X-rays have been measured for some compounds of 66Dy, namely, Dy2O3, Dy2(CO3)3, Dy2(SO4)3.8H2O, DyI2 and Dy metal by tuning the incident photon energies few eV above the L1 absorption-edge energy in order to investigate the influence of chemical effects on these cross sections in presence of the many body effects which become significant at photon energies close to the absorption-edge energies. The present measurements have been performed under vacuum at the IAEA end-station of the X-ray fluorescence beam line (10.1L) of ELETTRA synchrotron radiation facility (Trieste, Italy) using self-supporting pressed pellet targets (1.3 cm diameter, nominal thicknesses ~ 176 mg/cm2) of 66Dy compounds (procured from Sigma Aldrich) and a metallic foil of 66Dy (nominal thickness ~ 3.9 mg/cm2, procured from Good Fellow, UK). The present measured cross sections have been compared with theoretical values calculated using the Dirac-Hartree-Slater(DHS) model based fluorescence and Coster-Kronig yields, Dirac-Fock(DF) model based X-ray emission rates and two sets of L1 sub-shell photoionization cross sections based on the non-relativistic Hartree-Fock-Slater(HFS) model and those deduced from the self-consistent Dirac-Hartree-Fock(DHF) model based total photoionization cross sections. The present measured XRP cross sections for 66Dy as well as for its compounds for the L2,3 and L4 X-rays, are found to be higher by ~14-36% than the two calculated set values. It is worth to be mentioned that L2,3 and L4 X-ray lines are originated by filling up of the L1 sub-shell vacancies by the outer sub-shell (N2,3 and O2,3) electrons which are much more sensitive to the chemical environment around the central atom. The present observed differences between measured and theoretical values are expected due to combined influence of the many-body effects and the chemical effects.

Keywords: chemical effects, L X-ray production cross sections, Many body effects, Synchrotron radiation

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Authors: Amanda C. Evans

Abstract:

Enabling technologies such as continuous processing (CP) approaches can provide the tools needed to control and manipulate reactivities and transform chemical reactions into micro-controlled in-flow processes. Traditional synthetic approaches can be radically transformed by the application of CP, facilitating the pairing of chemical methodologies with technologies from other disciplines. CP supports sustainable processes that controllably generate reaction specificity utilizing supramolecular interactions. Continuous photochemical processing is an emerging field of investigation. The use of light to drive chemical reactivity is not novel, but the controlled use of specific and tunable wavelengths of light to selectively generate molecular structure under continuous processing conditions is an innovative approach towards chemical synthesis. This investigation focuses on the use of circularly polarized (cp) light as a sustainable catalyst for the CP generation of asymmetric molecules. Chiral photolysis has already been achieved under batch, solid-phase conditions: using synchrotron-sourced cp light, asymmetric photolytic selectivities of up to 4.2% enantiomeric excess (e.e.) have been reported. In order to determine the optimal wavelengths to use for irradiation with cp light for any given molecular building block, CD and anisotropy spectra for each building block of interest have been generated in two different solvents (water, hexafluoroisopropanol) across a range of wavelengths (130-400 nm). These spectra are being used to support a series of CP experiments using cp light to generate enantioselectivity.

Keywords: anisotropy, asymmetry, flow chemistry, active pharmaceutical ingredients

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Authors: Benhui Fan, Fahmi Bedoui, Jinbo Bai

Abstract:

Incorporated carbon nanotube-BaTiO₃ hybrids (H-CNT-BT) with core-shell structure, a better dispersion of CNTs can be achieved in a semi-crystalline polymeric matrix, polyvinylidene fluoride (PVDF). Carried by BT particles, CNTs are easy to mutually connect which helps to obtain an extremely low percolation threshold (fc). After thermal treatments, the dielectric constants (ε’) of samples further increase which depends on the conditions of thermal treatments such as annealing temperatures, annealing durations and cooling ways. Thus, in order to study more comprehensively about the influence of thermal treatments on composite’s dielectric behaviors, in situ synchrotron X-ray is used to detect re-crystalline behavior of PVDF. Results of wide-angle X-ray diffraction (WAXD) and small-angle X-ray scattering (SAXS) show that after the thermal treatment, the content of β polymorph (the polymorph with the highest ε’ among all the polymorphs of PVDF’s crystalline structure) has increased nearly double times at the interfacial region of CNT-PVDF, and the thickness of amorphous layers (La) in PVDF’s long periods (Lp) has shrunk around 10 Å. The evolution of CNT’s network possibly occurs in the procedure of La shrinkage, where the strong interfacial polarization may be aroused and increases ε’ at low frequency. Moreover, an increase in the thickness of crystalline lamella may also arouse more orientational polarization and improve ε’ at high frequency.

Keywords: dielectric properties, thermal treatments, carbon nanotubes, crystalline structure

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Authors: Sahar Heidary, Ramin Ghasemi Shayan

Abstract:

The overall goal Monte Carlo N-atom radioactivity transference PC program (MCNP4C) was done for the regeneration of x-ray groups in diagnostic radiology and mammography. The electrons were transported till they slow down and stopover in the target. Both bremsstrahlung and characteristic x-ray creation were measured in this study. In this issue, the x-ray spectra forecast by several computational models recycled in the diagnostic radiology and mammography energy kind have been calculated by appraisal with dignified spectra and their outcome on the scheming of absorbed dose and effective dose (ED) told to the adult ORNL hermaphroditic phantom quantified. This comprises practical models (TASMIP and MASMIP), semi-practical models (X-rayb&m, X-raytbc, XCOMP, IPEM, Tucker et al., and Blough et al.), and Monte Carlo modeling (EGS4, ITS3.0, and MCNP4C). Images got consuming synchrotron radiation (SR) and both screen-film and the CR system were related with images of the similar trials attained with digital mammography equipment. In sight of the worthy feature of the effects gained, the CR system was used in two mammographic inspections with SR. For separately mammography unit, the capability acquiesced bilateral mediolateral oblique (MLO) and craniocaudal(CC) mammograms attained in a woman with fatty breasts and a woman with dense breasts. Referees planned the common groups and definite absences that managed to a choice to miscarry the part that formed the scientific imaginings.

Keywords: mammography, monte carlo, effective dose, radiology

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Authors: Murtaza Adil, Sen Yang, Zhou Chao, Song Xiaoping

Abstract:

The morphotropic phase boundary (MPB) recently has attracted constant interest in ferromagnetic systems for obtaining enhanced large magnetoelastic response. In the present study, structural and magnetoelastic properties of MPB involved ferromagnetic Tb_1-xGd_xFe₂ (0≤x≤1) system has been investigated. The change of easy magnetic direction from <111> to <100> with increasing x up MPB composition of x=0.9 is detected by step-scanned [440] synchrotron X-ray diffraction reflections. The Gd substitution for Tb changes the composition for the anisotropy compensation near MPB composition of x=0.9, which was confirmed by the analysis of detailed scanned XRD, magnetization curves and the calculation of the first anisotropy constant K₁. The spin configuration diagram accompanied with different crystal structures for Tb_1-xGd_xFe₂ was designed. The calculated first anisotropy constant K₁ shows a minimum value at MPB composition of x=0.9. In addition, the large ratio between magnetostriction, and the absolute values of the first anisotropy constant │λ_S∕K₁│ appears at MPB composition, which makes it a potential material for magnetostrictive application. Based on experimental results, a theoretically approach was also proposed to signify that the facilitated magnetization rotation and enhanced magnetoelastic effect near MPB composition are a consequence of the anisotropic flattening of free energy of ferromagnetic crystal. Our work specifies the universal existence of MPB in ferromagnetic materials which is important for substantial improvement of magnetic and magnetostrictive properties and may provide a new route to develop advanced functional materials.

Keywords: free energy, magnetic anisotropy, magnetostriction, morphotropic phase boundary (MPB)

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