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.

Deformation behavior of Mg-Y-Ni alloys containing different volume fraction of LPSO phase during tension and compression through in-situ synchrotron diffraction

The deformation behavior of the as-extruded Mg-Y-Ni alloys with different volume fraction of long period stacking ordered(LPSO)phase during tension and compression was investigated by in-situ synchrotron diffraction.The micro-yielding,macro-yielding,tension-compression asymmetry and strain hardening behavior of the alloys were explored by combining with deformation mechanisms.The micro-yielding is dominated by basal slip of dynamic recrystallized(DRXed)grains in tension,while it is dominated by extension twinning of non-dynamic recrystallized(non-DRXed)grains in compression.At macro-yielding,the non-DRXed grains are still elastic deformed in tension and the basal slip of DRXed grains in compression are activated.Meanwhile,the LPSO phase still retains elastic deformation,but can bear more load,so the higher the volume fraction of hard LPSO phase,the higher the tensile/compressive macro-yield strength of the alloys.Benefiting from the low volume fraction of the non-DRXed grains and the delay effect of LPSO andγphases on extension twinning,the as-extruded alloys exhibit excellent tension-compression symmetry.When the volume fraction of LPSO phase reaches∼50%,tension-compression asymmetry is reversed,which is due to the fact that the LPSO phase is stronger in compression than in tension.The tensile strain hardening behavior is dominated by dislocation slip,while the dominate mechanism for compressive strain hardening changes from twinning in theα-Mg grains to kinking of the LPSO phase with increasing volume fraction of LPSO phase.The activation of kinking leads to the constant compressive strain hardening rate of∼2500 MPa,which is significantly higher than the tensile strain hardening rate.

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.

Mg-Ti hybrid joints:Surface modification,corrosion studies and 3D-pore investigation using synchrotron-based microtomography

A new direction toward the future of orthopedic implants is to combine biodegradable Mg alloys with permanent Ti to produce selectively biodegradable hybrid joints for advanced tissue engineering.However,the strong galvanic corrosion between Mg and Ti is a major issue to be considered.This work aims to explore plasma electrolytic oxidation(PEO)as a single-step coating treatment to allow for an acceptable degradation behavior of MgTi hybrid systems.To this end,MgTi hybrid joints were produced through the heat treatment of Mg-0.6Ca and commercially pure Ti specimens at 640°C for 8 h.A single-step PEO treatment was then employed to create a protective layer on the surface of hybrid couples.Even though the scanning electron microscopy(SEM)images showed only a porosity of 6%and 12%within the PEO layers on single Mg and MgTi couples,3D investigation of the synchrotron-based microtomography data demonstrated a porosity of 18%and 30%with a considerable number of interconnected pores.According to the electrochemical impedance spectroscopy measurements,the impedance modulus at all frequencies on coated MgTi coupled specimens was lower than that on the coated single Mg-0.6Ca and pure Ti.However,the application of PEO treatment significantly decreased the strong galvanic degradation of Mg-0.6Ca in contact with Ti.The results of hydrogen evolution tests revealed that PEO-treated MgTi couples showed a similar degradation behavior as the single alloy during the first day of immersion.

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.

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.

Discrimination of foodborne pathogenic bacteria using synchrotron FTIR microspectroscopy

Traditional Fourier transform infrared(FTIR)spectroscopy has been recognized as a valuable method to characterize and classify kinds of microorganisms.In this study,combined with multivariate statistical analysis,synchrotron radiation-based FTIR(SR-FTIR) microspectroscopy was applied to identify and discriminate ten foodborne bacterial strains.Our results show that the whole spectra(3000-900 cm^(-1)) and three subdivided spectral regions(3000-2800,1800-1500 and 1200-900 cm^(-1),representing lipids,proteins and polysaccharides,respectively) can be used to type bacteria.Either the whole spectra or the three subdivided spectra are good for discriminating the bacteria at levels of species and subspecies,but the whole spectra should be given preference at the genus level.The findings demonstrate that SR-FTIR microspectroscopy is a powerful tool to identify and classify foodborne pathogenic bacteria at the genus,species and subspecies level.

The application of synchrotron X-ray techniques to the study ofrechargeable batteries

The increased use of rechargeable batteries in portable electronic devices and the continuous develop-ment of novel applications （e.g. transportation and large scale energy storage）, have raised a strong de-mand for high performance batteries with increased energy density, cycle and calendar life, safety andlower costs. This triggers significant efforts to reveal the fundamental mechanism determining batteryperformance with the use of advanced analytical techniques. However, the inherently complex character-istics of battery systems make the mechanism analysis sophisticated and difficult. Synchrotron radiationis an advanced collimated light source with high intensity and tunable energies. It has particular ad-vantages in electronic structure and geometric structure （both the short-range and long-range structure）analysis of materials on different length and time scales. In the past decades, synchrotron X-ray tech-niques have been widely used to understand the fundamental mechanism and guide the technologicaloptimization of batteries. In particular, in situ and operando techniques with high spatial and temporalresolution, enable the nondestructive, real time dynamic investigation of the electrochemical reaction,and lead to significant deep insights into the battery operation mechanism. This review gives a brief introduction of the application of synchrotron X-ray techniques to the inves-tigation of battery systems. The five widely implicated techniques, including X-ray diffraction （XRD）, PairDistribution Function （PDF）, Hard and Soft X-ray absorption spectroscopy （XAS） and X-ray photoelectronspectroscopy （XPS） will be reviewed, with the emphasis on their in situ studies of battery systems during cycling.

Research progress on solidification structure of alloys by synchrotron X-ray radiography: A review

The synchrotron radiation technology has recently emerged as a powerful tool to characterize the real-time microstructure evolution during solidification of alloys.Compared with other methods,the synchrotron radiation technology,along with its unique advantages of strong brightness,high energy,excellent resolution,and good monochromaticity,allows for capturing the dendrite evolution behavior of alloys in real time and can be dynamically coordinated with high-resolution CCD(Charge-coupled Device)imaging systems.This paper briefly reviews the recent advances in developing synchrotron radiation for solidification of alloys with low,medium,and high melting points,and under the external electric,magnetic,and ultrasonic fields.Furthermore,a series of microstructural features and behaviors such as dendrite morphology,growth orientation,dendrite fracture,and rotation are described in detail.Finally,the development trends and application prospects of synchrotron radiation technology in alloy solidification are forecasted.

Small-angle X-ray scattering investigation of aging behavior of Al-Cu-Mg-Ag alloys using synchrotron radiation

The aging behavior of Al-Cu-Mg-Ag alloys with high Cu/Mg was studied by transmission electron microscopy (TEM) and small-angle X-ray scattering (SAXS) using synchrotron radiation. TEM study reveals that the major strengthening phases of the alloy after aging at 160?C for 10 h are Ω and less θ′. SAXS study shows that the scattering patterns are composed of several concentric circles at the beginning of aging process, which is replaced by the butterfly-wings scattering patterns with the increase of aging time. The butterfly-wings scattering patterns are composed of several branches. The angles between the branches are roughly equal to that between the habit planes of precipitates. The evolution of Guinier radius with aging time indicates the good coarsening resistance of the precipitates. The evolution of integrated intensity is consistent with the classical two-step precipitation process.

Internal Structure of Cambrian Fossil Embryo Markuelia Revealed in the Light of Synchrotron Radiation X-ray Tomographic Microscopy

In the light of Synchrotron Radiation X-ray Tomographic Microscopy （SRXTM）, the internal structure of Markuelia hunanensis is revealed. In one example, vitrification and peeling show the annuli hidden under the chorion. Sectioning and 3-D reconstruction display an intact digestive tract from the inverted introvert to the terminal anus. The inverted introvert forms a rugby cavum. The following digestive tract is rope-like coiling, parallel to the body axis, about 650 μm in length, and uniform in diameter （-80 μm）. An exquisitely preserved pipe-like structure is hidden in the middle of the rope-like structure, diameter 20--40 lam, with a length of -120 μm. We interpret this pipe-like structure as the possible epidermis of the gut and its surroundings as the possible residue of musculature, similar to that in Priapulans. The two symmetrical rod-shape structures connecting the body wall and digestive tract are interpreted as the possible retractor muscles. After comparing the well preserved Left-form and Right-form Body of Markuelia, we suggest that they may represent a dimorphism. Counted directly, one sample of Markuelia hunanensis possesses 62 annulations and the other 68.

Polycapillary X-ray lens for the secondary focusing Beijing synchrotron radiation source

According to intensity distribution of the synchrotron radiation source focused by a toroidal mirror at the Beijing synchrotron radiation biological macromolecule station, theoretical modeling of the Beijing synchrotron radiation source is developed for capillary optics. Using this theoretical modeling, the influences of the configuration curve of the polycapillary X-ray lens on transmission efficiency and working distance are analyzed. The experimental results of the transmission efficiency and working distance at the biological macromolecule station are in good agreement with the theoretical results.

Three-dimensional morphology of the Sinocyclocheilus hyalinus(Cypriniformes: Cyprinidae) horn based on synchrotron X-ray microtomography

Sinocyclocheilus is a cave-dwelling cyprinid genus endemic to southwest China. Several species possess a conspicuous horn on their head, which has been suggested as a constructive troglomorphic trait but lacks substantial evidence. We used non- invasive, high spatial resolution synchrotron X-ray microtomography to investigate the three-dimensional （3D） morphology of the horn of Sinocyclocheilus hyalinus, one of eight such troglobiotic species. 3D renderings demonstrated the osteological components, which were comprised of a rear wall comprised of the supraoccipital bone, a remaining frontal wall with numerous fenestrae, and the bottom continuous with the parietal and epiotic. A horn cavity occurred within the horn. The fenestrae in the frontal wall were continuous in the horn cavity and showed elaborate channeling, and were, connected to the cranial cavity by soft tissue. We tentatively called this configuration the ＂otocornual connection＂ due to its anatomic and putative functional similarity to the otolateralic connection in clupeids and loricariids, which provide an indirect pathway to enhance perception of underwater sound signals. This study provides a functional morphology context for further histological and physiological investigations of such horn structures in Sinocyclocheilus cavefish, and we suggest that the horn might enhance acoustic perception to compensate for visual loss in subterranean life, which warrants future physiological examination as lab-reared S. hyalinus become available.