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.

Investigation on X-Radiation for 126 kV Vacuum Interrupters

When subjected to high voltages between opened contacts, vacuum interrupters may emit X-rays. In order to ensure that these are of an acceptable level, vacuum interrupters should comply with the limits for X-ray emission and the test procedures to be carried out to verify this based on relevant standards and specifications. In this paper, a comprehensive experimental study has been performed for 126 kV vacuum interrupters used in a transmission system to understand the X-radiation level and its influence by three main parameters, namely applied power-frequency voltage, contact gap and power=frequency voltage conditioning. The radiation instrument is an FJ347 radiometer and the X-radiation dose was measured at the power-frequency test voltage. These tests demonstrated that the X-radiation emission level for a 126 kV vacuum interrupter did not exceed the following： 5 μSv per hour at a rated voltage of 126 kV and 150 μSv per hour at a power-frequency voltage of 230 kV at 1 m distance. The X-radiation dose increased with the applied power-frequency voltage increasing and decreased with the contact gap increasing. The X- radiation dose for 126 kV vacuum interrupters decreased by 57% after the conditioning procedure with a certain power-frequency voltage. During the conditioning procedure, the average value of the X-radiation dose was 4.49 mSv, which means if a professional conditions 180 interrupters per year, it will be safe at the 6.4 m distance.

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.

Changes of hMSH2 and hMLH1 Expression in Nasopharyngeal Carcinoma Cells after X-Radiation

OBJECTIVE To study the effect of X-radiation on expression of hMSH2 and hMLH1 in nasopharyngeal carcinoma （NPC） CNE-1 cells, and explore the mechanism of DNA mismatch repair after radiation. METHODS The cells were divided into experimental and control groups. Experimental cells were exposed to 10 Gy radiation administered as 2 Gy per fraction. Control cells were not radiated. The distribution of cells in the cell cycle was analyzed using flow cytometry. The expression of hMSH2 and hMLH1 was examined by RT-PCR and Western blots. RESULTS The expression of hMSH2 mRNA in experimental cells was significantly greater compared to control cells at 0-3rd weeks and decreased at the 4th week following radiation （P〈0.01）. The expression of hMSH2 protein in experimental cells was up-regulated and significantly greater compared to control cells at the 2nd-4th weeks after radiation （P〈0.01）. There were no significant differences in hMLH1 mRNA and protein expression between experimental and control cells （P 〉0.05）. CONCLUSION Radiation induces hMSH2 expression; hMSH2 has a role in the process of DNA repair, which maybe responsible for reduction of radiosensitivity after radiation.

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.

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.

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).

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.

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.

同步辐射装置主信号源的扩展方法研究

主信号源是同步辐射装置的关键组成部分之一,它不仅用于产生同步辐射光源各子系统所需的稳定度极高的参考信号,还用于生成整个装置的控制系统所需的高精度工作时钟。一般使用射频信号源作为主信号源,而商业射频信号源一般只配备单输出通道,远远不能满足同步辐射装置的需要,使用传统功分器对主信号通道进行扩展又存在幅度衰减、精度下降且相位不一致的问题。为解决上述问题,利用射频芯片AD9361,研究了对主信号源的单路输出进行扩展的方法。该方法可根据用户需求完成相应数量的信号通道扩展,设计了AD9361芯片和FPGA主控模块相结合的硬件架构。搭建实验平台,开展了射频信号源在C波段扩展的实验研究,对所提出的扩展方法进行实验验证。实验结果表明,该方法能保证扩展信号的幅度、频率与相位与主信号保持高度一致。

第四代同步辐射光源加速器物理与技术

同步辐射光源是20世纪应用最广泛的高性能X射线源,已成为物理、化学、能源环境、生物医学、先进材料等领域前沿研究的重要工具。进入21世纪,基于电子储存环的同步辐射光源的发展前沿是第四代同步辐射光源(4GLS)。其采用紧凑型的多弯铁消色散结构,可以实现接近甚至达到X射线衍射极限的超低束流发射度,将光源亮度在第三代光源基础上进一步提升2—3个数量级。文章将重点介绍第四代同步辐射光源关键的加速器物理与技术,以及国际范围内第四代同步辐射光源装置的发展情况。

辉铜矿化学-生物溶解机制及浸出动力学进展

辉铜矿是最具生物冶金工业利用价值的含铜矿物之一,然而,其生物浸出效率仍有较大提升空间。为了更好地揭示辉铜矿的生物浸出过程,对辉铜矿化学-生物溶解机制和浸出动力学相关研究进展进行综述。系统阐述辉铜矿的晶体结构,总结辉铜矿的化学溶解机制、电化学溶解机制和生物溶解机制,讨论辉铜矿的浸出动力学以及不同浸出参数对辉铜矿浸出的影响,总结辉铜矿生物冶金在工业应用中存在的问题。尽管如此,辉铜矿生物浸出的精细过程和浸出机制仍有待进一步研究。未来可采用同步辐射等多种新型研究方法在化学-生物多学科交叉基础上探明次生硫化铜矿的精细氧化溶解机制,为辉铜矿高效环保提铜奠定基础。

第四代同步辐射光源的光束线站及其应用

随着第四代同步辐射光源的兴起,得益于X射线亮度和相干性的大幅度提升,同步辐射实验技术在谱学、散射和成像等方面取得了显著进步。这些技术能够探测复杂非均匀体系和动态变化过程中的物质结构、成分、化学价态、电子态和磁性等关键信息,在基础科学领域和应用基础研究中发挥关键作用。文章旨在介绍第四代同步辐射光源的线站技术优势,并结合具体例子探讨其在若干物理研究中的应用,同时也讨论了当前存在的工程技术挑战。希望人们能够了解第四代同步辐射光源的光束线站的特点和应用潜力,以促进其在各个科研领域的推广。

X射线超快成像原位表征激光增材制造过程研究进展

在增材制造过程中,熔池经历快速熔化、冷却、凝固的过程,其物理、化学、结构和应力等处于极端非平衡状态,容易导致孔隙、裂纹等缺陷产生,影响制件力学性能。同步辐射X射线具有高空间分辨率和时间分辨率,可以实现增材制造过程中熔池动力学和缺陷演化的原位表征。本文综述了近年来激光增材制造原位实验平台的搭建,并从熔池结构演化、缺陷形成机理和成形工艺优化三个方面介绍了同步辐射X射线原位表征激光增材制造过程的研究进展。最后基于目前增材制造原位观察的局限性,从表征系统改进、原料多样化和计算修正等方面对未来研究进行了展望。