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.

BL03HB: a Laue microdiffraction beamline for both protein crystallography and materials science at SSRF

A Laue microdiffraction beamline(BL03HB) was constructed at the Shanghai Synchrotron Radiation Facility(SSRF).This beamline features two consecutive focusing points in two different sectors within its end station, the first dedicated to protein crystallography and the other tailored to materials science applications. Based on a superbend dipole magnet with a magnetic field of 2.29 T, a two-stage focusing design was implemented with two sets of Kirkpatrick-Baez mirrors to achieve a micro white beam as small as 4.2 μ m ×4.3 μ m at the first sector and 0.9 μ m ×1.3 μ m at the second sector in the standard beamline operation mode at SSRF. The X-ray microbeam in the two sectors can be easily switched between monochromatic and white beams by moving a four-bounce monochromator in or out of the light path, respectively. In the protein crystallography sector, white-beam Laue microdiffraction was demonstrated to successfully determine the structure of protein crystals from only a few images of diffraction data collected by a Pilatus 2 M area detector. In the materials science sector,the white-beam Laue diffraction was collected in a reflection geometry using another Pilatus 2 M area detector, which could map the microstructural distribution on the sample surface by scanning the samples. In general, the BL03HB beamline promotes the application of Laue microdiffraction in both protein crystallography and materials science. This paper presents a comprehensive overview of the BL03HB beamline, end station, and the first commission results.

High-precision X-ray polarimeter based on channel-cut crystals

We report on using synthetic silicon for a high-precision X-ray polarimeter comprising a polarizer and an analyzer,each based on a monolithic channel-cut crystal used at multiple Brewster reflections with a Bragg angle very close to 45°.Experiments were performed at the BL09B bending magnet beamline of the Shanghai Synchrotron Radiation Facility using a Si(800)crystal at an X-ray energy of 12.914 keV.A polarization purity of 8.4×10^(-9)was measured.This result is encouraging,as the measured polarization purity is the best-reported value for the bending magnet source.Notably,this is the firstly systematic study on the hard X-ray polarimeter in China,which is crucial for exploring new physics,such as verifying vacuum birefringence.

Identification of optimal composition with superior electrochemical properties along the zero Mn^(3+)line in Na_(0.75)(Mn-Al-Ni)O_(2)pseudo ternary system

Biphasic layered oxide cathodes,known for their superior electrochemical performance,are prime candidates for commercializing in Na-ion batteries.Herein,we unveil a series of P3/P2 monophasic and biphasic Al-substituted Na_(3/4)Mn_(5-x/8)Al_(2x/8)Ni_(3-x/8)O_(2)layered oxide cathodes that lie along the‘zero Mn^(3+)line’in the Na_(3/4)(Mn-Al-Ni)O_(2)pseudo-ternary system.The structural analysis showed a larger Na^(+)conduction bottleneck area in both P3 and P2 structures with a higher Al3+content,which enhanced their rate performance.In each composition,the P3/P2 biphasic compound with nearly equal fractions of P3 and P2 phases outperformed their monophasic counterparts in almost all electrochemical performance parameters.Operando synchrotron XRD measurements obtained for the monophasic P3 and biphasic P2/P3 samples revealed the absence of the O3 phase during cycling.The high structure stability and faster Na^(+)transport kinetics in the biphasic samples underpins the enhancement of electrochemical properties in the Al-substituted P3/P2 cathodes.These results highlight fixed oxidation state lines as a novel tool to identify and design layered oxide cathodes for Na-ion batteries in pseudo-ternary diagrams involving Jahn-Teller active cations.

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.

Time-resolved ultra-small-angle X-ray scattering beamline(BL10U1)at SSRF

The construction of a new beamline,BL10U1,was completed at the Shanghai synchrotron radiation facility in 2020.This multipurpose beamline was designed to provide X-ray scattering techniques such as ultra-small-angle X-ray scattering(USAXS),small-angle X-ray scattering(SAXS),wide-angle X-ray scattering,and microfocus SAXS(μSAXS)for a broad user community.To realize fast time-resolved USAXS experiments,the beamline adopted an in-vacuum undulator with a total length of 1.6 m as the photon source.An in-house cryogenic-cooled double multilayer monochromator was installed to deliver a photon flux of approximately 10^(13) photons/s at a photon energy of 10 keV.The three-year successful operation of this beamline demonstrated that the monochromator operated smoothly,as expected.BL10U1 has three end stations in succession:USAXS end station,μSAXS end station,and end station for industrial applications.The minimum scattering vector q~0.0042 nm^(-1) at 10 keV can be achieved at the USAXS end station equipped with a 28 m-long and 1.8 m-diameter vacuum flight tube.At theμSAXS end station,a beam spot of less than 10×8μm was achieved for micro-SAXS experiments.In contrast,in situ experimental instruments up to 5 m high and 8 m wide can be mounted at the industrial application end station,which offers industrial scientists the opportunity to use their large industrial equipment.BL10U1 opens up a new capability to investigate phenomena such as non-equilibrium and dynamic processes of materials with a wide length scale from angstroms to micrometers with millisecond time resolution.In this paper,we also report beamline design considerations and commissioning results.

The SLEGS beamline of SSRF

The Shanghai Laser Electron Gamma Source(SLEGS, located in BL03SSID) beamline at the Shanghai Synchrotron Radiation Facility(SSRF) is a Laser Compton Scattering(LCS) gamma source used for the investigation of nuclear structure, which is in extensive demand in fields such as nuclear astrophysics, nuclear cluster structure, polarization physics, and nuclear energy. The beamline is based on the inverse Compton scattering of 10640 nm photons on 3.5 GeV electrons and a gamma source with variable energy by changing the scattering angle from 20° to 160°. γ rays of 0.25-21.1 MeV can be extracted by the scheme consisting of the interaction chamber, coarse collimator, fine collimator, and attenuator. The maximum photon flux for 180° is approximately 10~7 photons/s at the target at 21.7 MeV, with a 3-mm-diameter beam. The beamline was equipped with four types of spectrometers for experiments in( γ,γ'),( γ,n),( γ,p), and( γ,α). At present, Nuclear Resonance Fluorescence(NRF) spectrometry, Flat-Efficiency neutron Detector(FED) spectrometry, neutron Time-Of-Flight(TOF) spectrometry, and Light-Charged Particle(LCP) spectrometry methods have been developed.

High-precision X-ray characterization for basic materials in modern high-end integrated circuit

Semiconductor materials exemplify humanity's unwavering pursuit of enhanced performance,efficiency,and functionality in electronic devices.From its early iterations to the advanced variants of today,this field has undergone an extraordinary evolution.As the reliability requirements of integrated circuits continue to increase,the industry is placing greater emphasis on the crystal qualities.Consequently,conducting a range of characterization tests on the crystals has become necessary.This paper will examine the correlation between crystal quality,device performance,and production yield,emphasizing the significance of crystal characterization tests and the important role of high-precision synchrotron radiation X-ray topography characterization in semiconductor analysis.Finally,we will cover the specific applications of synchrotron radiation characterization in the development of semiconductor materials.

Quick-scanning X-ray absorption fine structure beamline at SSRF

The layout and characteristics of the hard X-ray spectroscopy beamline(BL11B)at the Shanghai synchrotron radiation facility are described herein.BL11B is a bending-magnet beamline dedicated to conventional and millisecond-scale quick-scanning X-ray absorption fine structures.It is equipped with a cylindrical collimating mirror,a double-crystal monochromator comprising Si(111)and Si(311),a channel-cut quick-scanning Si(111)monochromator,a toroidal focusing mirror,and a high harmonics rejection mirror.It can provide 5-30 keV of X-rays with a photon flux of~5×10^(11)photons/s and an energy resolution of~1.31×10^(-4)at 10 keV.The performance of the beamline can satisfy the demands of users in the fields of catalysis,materials,and environmental science.This paper presents an overview of the beamline design and a detailed description of its performance and capabilities.

Novel high-voltage cathode for aqueous zinc ion batteries:Porous K_(0.5)VOPO_(4)·1.5H_(2)O with reversible solid-solution intercalation and conversion storage mechanism

Cathode materials that possess high output voltage,as well as those that can be mass-produced using facile techniques,are crucial for the advancement of aqueous zinc-ion battery(ZIBs)applications,Herein,we present for the first time a new porous K_(0.5)VOPO_(4)·1.5H_(2)O polyanionic cathode(P-KIVP)with high output voltage(above 1.2 V)that can be manufactured at room temperature using straightforward coprecipitation and etching techniques.The P-KVP cathode experiences anisotropic crystal plane expansion via a sequential solid-solution intercalation and phase co nversion pathway throughout the Zn^(2+)storage process,as confirmed by in-situ synchrotron X-ray diffraction and ex-situ X-ray photoelectron spectroscopy.Similar to other layered vanadium-based polyanionic materials,the P-KVP cathode experiences a progressive decline in voltage during the cycle,which is demonstrated to be caused by the irreversible conversion into amorphous VO_(x).By introducing a new electrolyte containing Zn(OTF)_(2) to a mixed triethyl phosphate and water solution,it is possible to impede this irreversible conversion and obtain a high output voltage and longer cycle life by forming a P-rich cathode electrolyte interface layer.As a proof-of-concept,the flexible fiber-shaped ZIBs based on modified electrolyte woven into a fabric watch band can power an electronic watch,highlighting the application potential of P-KVP cathode.

Infrared microspectroscopy beamline BL06B at SSRF

The infrared microspectroscopy beamline(BL06B) is a phase Ⅱ beamline project at the Shanghai Synchrotron Radiation Facility(SSRF). The construction and optical alignment of BL06B were completed by the end of 2020. By 2021, it became accessible to users. The synchrotron radiation infrared(SRIR) source included edge radiation(ER) and bending magnet radiation(BMR). The extracted angles in the horizontal and vertical directions were 40 and 20 mrad, respectively. The photon flux, spectral resolution, and focused spot size were measured at the BL06B endstation, and the experimental results were consistent with theoretical calculations. SRIR light has a small divergence angle, high brightness, and a wide wavelength range. As a source of IR microscopy, it can easily focus on a diffraction-limited spatial resolution with a high signal-to-noise ratio(SNR). The BL06B endstation can be applied in a wide range of research fields, including materials, chemistry, biology, geophysics, and pharmacology.

Ultrahard X-ray multifunctional application beamline at the SSRF

The ultrahard X-ray multifunctional application beamline(BL12SW)is a phase-II beamline project at the Shanghai Syn-chrotron Radiation Facility.The primary X-ray techniques used at the beamline are high-energy X-ray diffraction and imaging using white and monochromatic light.The main scientific objectives of ultrahard X-ray beamlines are focused on two research areas.One is the study of the structural properties of Earth’s interior and new materials under extreme high-temperature and high-pressure conditions,and the other is the characterization of materials and processes in near-real service environments.The beamline utilizes a superconducting wiggler as the light source,with two diamond windows and SiC discs to filter out low-energy light(primarily below 30 keV)and a Cu filter assembly to control the thermal load entering the subsequent optical components.The beamline is equipped with dual monochromators.The first was a meridional bending Laue monochromator cooled by liquid nitrogen,achieving a full-energy coverage of 30-162 keV.The second was a sagittal bending Laue monochromator installed in an external building,providing a focused beam in the horizontal direction with an energy range of 60-120 keV.There were four experimental hutches:two large-volume press experimental hutches(LVP1 and LVP2)and two engineering material experimental hutches(ENG1 and ENG2).Each hutch was equipped with various near-real service conditions to satisfy different requirements.For example,LVP1 and LVP2 were equipped with a 200-ton DDIA press and a 2000-ton dual-mode(DDIA and Kawai)press,respectively.ENG1 and ENG2 provide in situ tensile,creep,and fatigue tests as well as high-temperature conditions.Since June 2023,the BL12SW has been in trial operation.It is expected to officially open to users by early 2024.

The hard X-ray nanoprobe beamline at the SSRF

The hard X-ray nanoprobe beamline BL13U is a phase-Ⅱ beamline project at the Shanghai Synchrotron Radiation Facility.The beamline aims to enable comprehensive experiments at high spatial resolutions ranging from 50 to 10 nm. The X-ray energy range of the beamline, 5–25 keV, can detect most elements in the periodic table. Two operating modes were designed to accommodate the experimental requirements of high-energy resolution or high photon flux, respectively. X-ray nanofluorescence, nanodiffraction, and coherent diffraction imaging are developed as the main experimental techniques for BL13U. This paper describes the beamline optics, end station configurations, experimental methods under development, and preliminary test results. This comprehensive overview aims to provide a clear understanding of the beamline capabilities and potential applications.

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.

Highly coupled off-resonance lattice design in diffraction-limited light sources

The round-beam operation presents many benefits for scientific experiments regarding synchrotron radiation and the weak-ening influences of intra-beam scattering in diffraction-limited synchrotron light sources.A round-beam generation method based on the global setting of skew quadrupoles and the application of a non-dominated sorting genetic algorithm was pro-posed in this study.Two schemes,including large-emittance coupling introduced via betatron coupling and vertical disper-sion,were explored in a candidate lattice for an upgrade-proposal of the Shanghai synchrotron radiation facility.Emittance variations with lattice imperfections and their influence on the beam dynamics of beam optic distortions were investigated.The results demonstrated that a precise coupling control ranging from 10 to 100%was achieved under low optical distortion,whereas full-coupling generation and its robustness were achieved by our proposed method by adjusting the skew quadrupole components located in the dispersion-free sections.The Touschek lifetime increased by a factor of 2–2.5.

NEUTRINO BEAM LINES AT HIGH-ENERGY PROTON SYNCHROTRONS

Revised September 2013 with numbers verified by representatives of the synchrotrons （contact C.-J. Lin, LBNL）. For existing （future） neutrino beam lines the latest achieved （design） values are given.

ARCADE 2 Spatial Roar, What Theory of Relation Reveals

The theory of Relation provides an explanation for the Arcade 2 excess. It assumes that the isotropic radio emission measured by the Arcade 2 Collaboration, which is 5 - 6 times brighter than the expected contributions from known extra-galactic sources, is the residue of an immense primitive energy of ordinary matter released by a relativistic bang almost 100 million years after the big bang, which gave the mass-energy the missing gravity to activate contraction. This relativistic bang, via a Lorentz energy transformation, would have released enormous energy held to be the source of the powerful radio noise detected by the NASA researchers. This transformation would have simultaneously triggered the formation of the first stars from dense gas and the reionization of less dense neutral gas. This departs from the idea that continuous reionization began after the formation of the first stars. We emphasize the importance of primordial magnetic fields, which would have generated significant density fluctuations during recombination and acted as a direct seed for cosmic structures. The first stars and galaxies were bathed in strong magnetic fields that gave rise to the radio microwave din (boom) discovered by Arcade 2. These intense magnetic fields alter the trajectory of charged particles zooming near the speed of light, triggering the space roar and emitting radiation that forms a synchrotron radio background. The theory of Relation offers an alternative to the Lambda-CDM cosmological model, which has become the standard model of the big bang, which leads straight to the vacuum catastrophe.

Study of a magnetic alloy-loaded cavity for compact synchrotrons

Magnetic alloy（MA）-loaded cavities have been widely used in compact proton and heavy-ion synchrotrons,and the MA core is the key issue in their development.Chinese-produced MA has never yet been adopted as core material for an MA-loaded cavity.To use Chinese-produced MA as the core material,it is necessary to study its properties,and compare with MA material produced elsewhere.In this paper,the properties of several MA cores made of Chinese-produced material are measured.Based on the measured results,a schematic design is produced for a cavity which could obtain 1 kV gap voltage with less than 1.5 kW power dissipation in the frequency range of0.5-7 MHz.The difference between resonant frequencies obtained from simulation and analytical results is less than10%.

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.