Microstructures and micromechanical behaviors of high -entropy alloys investigated by synchrotron X-ray and neutron diffraction techniques: A review

High-entropy alloys(HEAs)possess outstanding features such as corrosion resistance,irradiation resistance,and good mechan-ical properties.A few HEAs have found applications in the fields of aerospace and defense.Extensive studies on the deformation mech-anisms of HEAs can guide microstructure control and toughness design,which is vital for understanding and studying state-of-the-art structural materials.Synchrotron X-ray and neutron diffraction are necessary techniques for materials science research,especially for in situ coupling of physical/chemical fields and for resolving macro/microcrystallographic information on materials.Recently,several re-searchers have applied synchrotron X-ray and neutron diffraction methods to study the deformation mechanisms,phase transformations,stress behaviors,and in situ processes of HEAs,such as variable-temperature,high-pressure,and hydrogenation processes.In this review,the principles and development of synchrotron X-ray and neutron diffraction are presented,and their applications in the deformation mechanisms of HEAs are discussed.The factors that influence the deformation mechanisms of HEAs are also outlined.This review fo-cuses on the microstructures and micromechanical behaviors during tension/compression or creep/fatigue deformation and the application of synchrotron X-ray and neutron diffraction methods to the characterization of dislocations,stacking faults,twins,phases,and intergrain/interphase stress changes.Perspectives on future developments of synchrotron X-ray and neutron diffraction and on research directions on the deformation mechanisms of novel metals are discussed.

Towards adaptable synchrotron image restoration pipeline

Synchrotron microscopic data commonly suffer from poor image quality with degraded resolution incurred by instrumentation defects or experimental conditions.Image restoration methods are often applied to recover the reduced resolution,providing improved image details that can greatly facilitate scientific discovery.Among these methods,deconvolution techniques are straightforward,yet either require known prior information or struggle to tackle large experimental data.Deep learning(DL)-based super-resolution(SR)methods handle large data well,however data scarcity and model generalizability are problematic.In addition,current image restoration methods are mostly offline and inefficient for many beamlines where high data volumes and data complexity issues are encountered.To overcome these limitations,an online image-restoration pipeline that adaptably selects suitable algorithms and models from a method repertoire is promising.In this study,using both deconvolution and pretrained DL-based SR models,we show that different restoration efficacies can be achieved on different types of synchrotron experimental data.We describe the necessity,feasibility,and significance of constructing such an image-restoration pipeline for future synchrotron experiments.

Operando measurement of lattice deformation profiles of synchrotron radiation monochromator

This study presents a new method for characterizing the thermal lattice deformation of a monochromator with high precision under service conditions and first reports the operando measurements of nanoscale thermal lattice deformation on a double-crystal monochromator at different incident powers.The nanoscale thermal lattice deformation of the monochromator first crystal was obtained by analyzing the intensity of the distorted DuMond diagrams.DuMond diagrams of the 333 diffraction index,sensitive to lattice deformation,were obtained directly using a 2D detector and an analyzer crystal orthogonal to the monochromator.With increasing incident power and power density,the maximum height of the lattice deformation increased from 3.2 to 18.5 nm,and the deformation coefficient of the maximum height increased from 1.1 to 3.2 nm/W.The maximum relative standard deviation was 4.2%,and the maximum standard deviation was 0.1 nm.Based on the measured thermal deformations,the flux saturation phenomenon and critical point for the linear operation of the monochromator were predicted with increasing incident power.This study provides a simple solution to the problem of the lower precision of synchrotron radiation monochromator characterizations compared to simulations.

Insights into the hydrogen evolution reaction in vanadium redox flow batteries:A synchrotron radiation based X-ray imaging study

The parasitic hydrogen evolution reaction(HER)in the negative half-cell of vanadium redox flow batteries(VRFBs)causes severe efficiency losses.Thus,a deeper understanding of this process and the accompanying bubble formation is crucial.This benchmarking study locally analyzes the bubble distribution in thick,porous electrodes for the first time using deep learning-based image segmentation of synchrotron X-ray micro-tomograms.Each large three-dimensional data set was processed precisely in less than one minute while minimizing human errors and pointing out areas of increased HER activity in VRFBs.The study systematically varies the electrode potential and material,concluding that more negative electrode potentials of-200 m V vs.reversible hydrogen electrode(RHE)and lower cause more substantial bubble formation,resulting in bubble fractions of around 15%–20%in carbon felt electrodes.Contrarily,the bubble fractions stay only around 2%in an electrode combining carbon felt and carbon paper.The detected areas with high HER activity,such as the border subregion with more than 30%bubble fraction in carbon felt electrodes,the cutting edges,and preferential spots in the electrode bulk,are potential-independent and suggest that larger electrodes with a higher bulk-to-border ratio might reduce HER-related performance losses.The described combination of electrochemical measurements,local X-ray microtomography,AI-based segmentation,and 3D morphometric analysis is a powerful and novel approach for local bubble analysis in three-dimensional porous electrodes,providing an essential toolkit for a broad community working on bubble-generating electrochemical systems.

SAPT:a synchrotron-based proton therapy facility in Shanghai

Because of its excellent dose distribution,proton therapy is becoming increasingly popular in the medical application of cancer treatment.A synchrotron-based proton therapy facility was designed and constructed in Shanghai.The synchrotron,beam delivery system,and other technical systems were commissioned and reached their expected performances.After a clinical trial of 47 patients was finished,the proton therapy facility obtained a registration certificate from the National Medical Products Administration.The characteristics of the accelerator and treatment systems are described in this article.

The biosafety level-2 macromolecular crystallography beamline(BL10U2)at the Shanghai Synchrotron Radiation Facility

BL10U2 is an undulator-based macromolecular crystallography(MX)beamline located at the 3.5-GeV Shanghai Synchrotron Radiation Facility.BL10U2 is specifically designed for conducting routine and biosafety level-2(BSL-2)MX experiments utilizing high-flux tunable X-rays with energies from 7 to 18 keV,providing a beam spot size of 20μm(horizontal)×10μm(vertical)at the sample point.Certification by the Shanghai Pudong Municipal Health Commission confirmed the capability to perform BSL-2 MX experiments.The beamline is currently equipped with an Eiger X 16 M detector and two newly developed in-house high-precision diffractometers that can be switched to perform conventional or in situ crystal diffraction experiments.An automatic sample changer developed in-house allows fast sample exchange in less than 30 s,supporting high-throughput MX experimentation and rapid crystal screening.Data collection from both the diffractometer and detector was controlled by an in-house developed data collection software(Finback)with a user-friendly interface for convenient operation.This study presents a comprehensive overview of the facilities,experimental methods,and performance characteristics of the BL10U2 beamline.

BL02U1:the relocated macromolecular crystallography beamline at the Shanghai Synchrotron Radiation Facility

Macromolecular crystallography beamline BL17U1 at the Shanghai Synchrotron Radiation Facility has been relocated,upgraded,and given a new ID(BL02U1).It now delivers X-rays in the energy range of 6–16 keV,with a focused beam of 11.6μm×4.8μm and photon flux greater than 1012 phs/s.The high credibility and stability of the beam and good timing synchronization of the equipment significantly improve the experimental efficiency.Since June 2021,when it officially opened to users,over 4200 h of beamtime have been provided to over 200 research groups to collect data at the beamline.Its good performance and stable operation have led to the resolution of several structures based on data collected at the beamline.

Understanding Pseudocapacitance Mechanisms by Synchrotron X-ray Analytical Techniques

Pseudocapacitive materials that store charges via reversible surface or near-surface faradaic reactions are capable of overcoming the capacity limitations of electrical double-layer capacitors.Revealing the structure–activity relationship between the microstructural features of pseudocapacitive materials and their electrochemical performance on the atomic scale is the key to build high-performance capacitor-type devices containing ideal pseudocapacitance effect.Currently,the high brightness(flux),and spectral and coherent nature of synchrotron X-ray analytical techniques make it a powerful tool for probing the structure–property relationship of pseudocapacitive materials.Herein,we report a comprehensive and systematic review of four typical characterization techniques(synchrotron X-ray diffraction,pair distribution function[PDF]analysis,soft X-ray absorption spectroscopy,and hard X-ray absorption spectroscopy)for the study of pseudocapacitance mechanisms.In addition,we offered significant insights for understanding and identifying pseudocapacitance mechanisms(surface redox pseudocapacitance,intercalation pseudocapacitance,and the extrinsic pseudocapacitance phenomenon in battery materials)by combining in situ hard XAS and electrochemical analyses.Finally,a perspective for further depth of understanding into the pseudocapacitance mechanism using synchrotron X-ray analytical techniques is proposed.

The effect of temperature on load partitioning evolution in magnesium metal matrix composite reinforced with Ti particles using in-situ synchrotron radiation diffraction experiments

The load partitioning between the magnesium and titanium phases in an extruded Mg-15%Ti(vol.%) composite from room temperature up to 300 ℃ using synchrotron radiation diffraction during in-situ compression tests. During compression, the magnesium matrix composite deforms mainly by the activation of the extension twinning system up to 200 ℃. The volume fraction of twins increases with the plastic strain but decrease with the compression temperature. Hard titanium particles bear an additional load transferred by the soft magnesium matrix from room temperature up to 300 ℃. This effect is amplified after yield stress during plastic deformation. Additionally, twins within magnesium grains behaves as an additional reinforcement at low temperature(below 200 ℃) inducing an increase in the work hardening of the composite.

Thermal expansivity of geikielite and ilmenite utilizing in-situ synchrotron X-ray diffraction at high temperature

The unit-cell parameters and volumes of geikielite(MgTiO_(3))and ilmenite(FeTiO_(3))were investigated at high temperatures up to 700 K and ambient pressure,using in-situ angle-dispersive synchrotron X-ray diffraction.No phase transition was detected over the experimental temperature range.Using(Berman in J Petrol29:445-522,1988.10.1093/petrology/29.2.445)equations to fit the temperature-volume data,the volumetric thermal expansion coefficients at ambient conditions(α_(V0))of MgTiO_(3) and FeTiO_(3) were obtained as follows:2.55(6)×10^(-5)K^(-1)and 2.82(10)×10^(-5)K^(-1),respectively.We infer that the larger effective ionic radius of Fe^(2+)(Ⅵ)(0.78 A)than that of Mg^(2+)(Ⅵ)(0.72?)renders FeTiO_(3)has a larger volumetric thermal expansivity than MgTiO_(3).Simultaneously,the refined axial thermal expansion coefficients under ambient conditions areα_(a0)=0.74(3)×10^(-5)K^(-1)andα_(c0)=1.08(5)×10^(-5)K^(-1)for the aaxis and c-axis of MgTiO_(3),respectively,andα_(a0)=0.95(5)×10^(-5)K^(-1)andα_(c0)=0.92(12)×10^(-5)K^(-1)for the aaxis and c-axis of FeTiO_(3),respectively.The axial thermal expansivity of MgTiO_(3) is anisotropic,but that of FeTiO_(3) is nearly isotropic.We infer that the main reason for the different axial thermal expansivity between MgTiO_(3) and FeTiO_(3) is that the thermal expansion mode of the Mg-O bond in MgTiO_(3) is different from that of the Fe-O bonds in FeTiO_(3).

Ultrasmall CoS nanoparticles embedded in heteroatom-doped carbon for sodium-ion batteries and mechanism explorations via synchrotron X-ray techniques

Transition metal sulfides have been regarded as promising anode materials for sodium-ion batteries(SIB).However,they face the challenges of poor electronic conductivity and large volume change,which result in capacity fade and low rate capability.In this work,a composite containing ultrasmall CoS(~7 nm)nanoparticles embedded in heteroatom(N,S,and O)-doped carbon was synthesized by an efficient one-step sulfidation process using a Co(Salen)precursor.The ultrasmall CoS nanoparticles are beneficial for mechanical stability and shortening Na-ions diffusion pathways.Furthermore,the N,S,and O-doped defect-rich carbon provides a robust and highly conductive framework enriched with active sites for sodium storage as well as mitigates volume expansion and polysulfide shuttle.As anode for SIB,CoS@HDC exhibits a high initial capacity of 906 mA h g^(-1)at 100 mA g^(-1)and a stable long-term cycling life with over 1000 cycles at 500 mA g^(-1),showing a reversible capacity of 330 mA h g^(-1).Meanwhile,the CoS@HDC anode is proven to maintain its structural integrity and compositional reversibility during cycling.Furthermore,Na-ion full batteries based on the CoS@HDC anode and Na_(3)V_(2)(PO_(4))_(3)cathode demonstrate a stable cycling behavior with a reversible specific capacity of~200 m A h g^(-1)at least for 100 cycles.Moreover,advanced synchrotron operando X-ray diffraction,ex-situ X-ray absorption spectroscopy,and comprehensive electrochemical tests reveal the structural transformation and the Co coordination chemistry evolution of the CoS@HDC during cycling,providing fundamental insights into the sodium storage mechanism.

Design of a rapid-cycling synchrotron for flash proton therapy

The purpose of this study was to design a rapid-cycling synchrotron, making it capable of proton beam ultrahigh dose rate irradiation, inspired by laser accelerators. The design had to be cheap and simple. We consider our design from six aspects: the lattice, injection, extraction, space charge effects, eddy current effects and energy switching. Efficiency and particle quantity must be addressed when injected. The space charge effects at the injection could affect particles' number. The eddy current effects in the vacuum chambers would affect the magnetic field itself and generate heat, all of which need to be taken into account. Fast extraction can obtain 10^(10) protons/pulse, equal to instantaneous dose rate up to 10~7 Gy/s in a very short time, while changing various extraction energies rapidly and easily to various deposition depths. In the further research, we expect to combine a delivery system with this accelerator to realize the FLASH irradiation.

L-shell x-ray fluorescence relative intensities for elements with 62≤Z≤83 at 18 keV and 23 keV by synchrotron radiation

The relative intensities of L-subshell x-ray fluorescence(XRF)for elements with atomic numbers 62≤Z≤83 were measured at two excitation energies,18 keV and 23 keV,using a synchrotron radiation source at a beamline of the Synchrotron Light Center for Experimental Science and Applications in the Middle East(SESAME),Jordan.The experimentally measured results of the relative intensities were compared with the calculated results using the subshell fluorescence yield and the Coster-Kronig transition probabilities recommended by Campbell and the values based on the Dirac-Hartree-Slater model by Puri.The experimental and theoretical results are in agreement.In this work,L XRF relative intensities for the elements Sm,Gd,Tb,Er,Ta,W,Re,Hg,Pb and Bi at energies of 18 keV and 23 keV were measured.

In situ study on columnar-equiaxed transition and anaxial columnar dendrite growth of Al-15%Cu alloy by synchrotron radiography

Directional solidification of Al-15% （mass fraction） Cu alloy was investigated by in situ and real time radiography which was performed by Shanghai synchrotron radiation facility （SSRF）. The imaging results reveal that columnar to equiaxed transition （CET） is provoked by external thermal disturbance. The detaching and floating of fragments of dendrite arms are the prelude of the transition when the solute boundary layer in front of the solid-liquid interface is thin. And the dendrite triangular tip is the fracture sensitive zone. When the conditions are suitable, new dendrites can sprout and grow up. This kind of dendrite has no obvious stem and is named anaxial columnar dendrites.

Synchrotron radiation-based materials characterization techniques shed light on molten salt reactor alloys

From a safety point of view, it is important to study the damages and reliability of molten salt reactor structural alloy materials, which are subjected to extreme environments due to neutron irradiation, molten salt corrosion, fission product attacks, thermal stress, and even combinations of these. In the past few years, synchrotron radiation-based materials characterization techniques have proven to be effective in revealing the microstructural evolution and failure mechanisms of the alloys under surrogating operation conditions. Here, we review the recent progress in the investigations of molten salt corrosion,tellurium(Te) corrosion, and alloy design. The valence states and distribution of chromium(Cr) atoms, and the diffusion and local atomic structure of Te atoms near the surface of corroded alloys have been investigated using synchrotron radiation techniques, which considerably deepen the understandings on the molten salt and Te corrosion behaviors. Furthermore, the structure and size distribution of the second phases in the alloys have been obtained, which are helpful for the future development of new alloy materials.

In situ analysis of multi-twin morphology and growth using synchrotron polychromatic X-ray microdiffraction

Synchrotron polychromatic X-ray microdiffraction（micro-XRD） was applied to study in situ deformation twinning of commercially AZ31（Mg-3Al-1Zn） strip subjected to uniaxial tension.The morphology and growth of twins were analyzed in situ under the load level from 64 to 73 MPa.The X-ray microdiffraction data,collected on beamline 12.3.2 at the Advanced Light Source,were then used to map an area of 396μm x 200μm within the region of interest.The experimental set-up and X-ray diffraction microscopy with a depth resolution allow the position and orientation of each illuminated grain to be determined at the submicron size.A list of parent grains sorted by crystallographic orientation were selected to examine their twinning behavior.The results depict twin variant selection,local misorientation fluctuation and mosaic spread for multi-twins within the same parent grain.As load increases,the amplitude of misorientation fluctuation along twin trace keeps increasing.This is attributable to the accumulation of geometrically necessary dislocations.

The protein complex crystallography beamline(BL19U1)at the Shanghai Synchrotron Radiation Facility

The protein complex crystallographic beamline BL19U1 at the Shanghai Synchrotron Radiation Facility is one of the five beamlines dedicated to protein sciences operated by National Facility for Protein Science(Shanghai,China).The beamline,which features a small-gap invacuum undulator,has been officially open to users since March 2015.This beamline delivers X-ray in the energy range 7–15 keV.With its high flux,low divergence beam and a large active area detector,BL19U1 is designed for proteins with large molecular weight and large crystallographic unit cell dimensions.Good performance and stable operation of the beamline have allowed the number of Protein Data Bank(PDB)depositions and the number of articles published based on data collected at this beamline to increase steadily.To date,over 300 research groups have collected data at the beamline.More than 600 PDB entries have been deposited at the PDB(www.pdb.org).More than 300 papers have been published that include data collected at the beamline,including 21 research articles published in the top-level journals Cell,Nature,and Science.

Design of wide-range energy material beamline at the Shanghai Synchrotron Radiation Facility

We report the design of a wide-range energy material beamline(E-line) with multiple experimental techniques at the Shanghai Synchrotron Radiation Facility.The undulators consisted of an elliptically polarizing undulator and in-vacuum undulator that generate the soft and hard X-rays, respectively. The beamline covered a wide energy range from 130 to 18 ke V with both a high photon flux([ 10^(12) phs/s with exit silt 30 lm in soft X-ray and [ 5 9 10^(12) phs/s in hard X-ray within 0.1%BW bandwidth) and promising resolving power(maximum E/DE [ 15,000 in soft X-ray with exit silt 30 lm and [6000 in hard X-ray). Moreover, the beam spots from the soft and hard X-rays were focused to the same sample position with a high overlap ratio, so that the surfaces, interfaces, and bulk properties were characterized in situ by changing the probing depth.

Synchrotron radiation investigations of the Sr_2MgSi_2O_7:Eu^(2+),R^(3+) persistent luminescence materials

The electronic and defect energy level structure of polyerystalline Sr2MgSi2OT：Eu^2＋,R^3＋ persistent luminescence materials were studied with thermoluminescence and different synchrotron radiation spectroscopies （UV-VUV emission and excitation, X-ray absorption near-edge spectroscopy （XANES） and extended X-ray absorption f＇me structure （EXAFS））. Special attention was paid on the effect of the R3＋ co-dopants on the persistent luminescence properties of the materials. Theoretical calculations using the density functional theory （DFT） were carried out simultaneously with the experimental work. The experimental band gap energy （Eg） value of ca. 7.1 eV agreed very well with the DFT value of 6.7 eV. The variation of the Eg value was attempted to relate with the trap structure as well as with the different properties of the R3＋ co-dopants. The trap level energy distribution depended strongly on the R3＋ co-dopant except for the shallowest trap energy above the room temperature remaining practically the same, however. The different processes in the mechanism of persistent luminescence from Sr2MgSi2OT：Eu^2＋,R^3＋ were assembled and their contributions discussed.

Tuning control system of a third harmonic superconducting cavity in the Shanghai Synchrotron Radiation Facility

Beam lifetime is dominated by Touschek scattering at the Shanghai Synchrotron Radiation Facility(SSRF).Touschek loss rate is affected by probability for scattering beyond the RF acceptance and the volume charge density of the bench.In the phaseⅡupgrade of the SSRF,a third harmonic superconducting cavity will be used to enhance the Touschek lifetime by lengthening the bunches.The Touschek lifetime improvement factor is affected by the voltage of a harmonic cavity.To stabilize the cavity voltage,a tuning control system was designed to control it.The design of the tuning control system was based on the SSRF third-generation low-level RF control system.Some hardware and specialized algorithms were redesigned to fit the harmonic cavity control.The design of the tuning control system is complete,and the control system has been tested.The test result shows that the fluctuation of amplitude is<±0.34%within 1.5 h,which satisfies the stability requirement.