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.

Direct visualization of laser-driven dynamic fragmentation in tin by in situ x-ray diffraction

We present a novel method for investigating laser-driven dynamic fragmentation in tin using in situ X-ray diffraction.Our experimental results demonstrate the feasibility of the method for simultaneously identifying the phase and temperature of fragments through analysis of the diffraction pattern.Surprisingly,we observe a deviation from the widely accepted isentropic release assumption,with the temperature of the fragments being found to be more than 100 K higher than expected,owing to the release of plastic work during dynamic fragmentation.Our findings are further verified through extensive large-scale molecular dynamics simulations,in which strain energies are found to be transferred into thermal energies during the nucleation and growth of voids,leading to an increase in temperature.Our findings thus provide crucial insights into the impact-driven dynamic fragmentation phenomenon and reveal the significant influence of plastic work on material response during shock release.

Intensity correlation properties of x-ray beams split with Laue diffraction

Beam splitting is one of the main approaches to achieving x-ray ghost imaging, and the intensity correlation between diffraction beam and transmission beam will directly affect the imaging quality. In this paper, we investigate the intensity correlation between the split x-ray beams by Laue diffraction of stress-free crystal. The analysis based on the dynamical theory of x-ray diffraction indicates that the spatial resolution of diffraction image and transmission image are reduced due to the position shift of the exit beam. In the experimental setup, a stress-free crystal with a thickness of hundredmicrometers-level is used for beam splitting. The crystal is in a non-dispersive configuration equipped with a double-crystal monochromator to ensure that the dimension of the diffraction beam and transmission beam are consistent. A correlation coefficient of 0.92 is achieved experimentally and the high signal-to-noise ratio of the x-ray ghost imaging is anticipated.Results of this paper demonstrate that the developed beam splitter of Laue crystal has the potential in the efficient data acquisition of x-ray ghost imaging.

Dispersion Relations in Diffraction in Time

In agreement with Titchmarsh’s theorem, we prove that dispersion relations are just the Fourier-transform of the identity, g(x′)=±Sgn(x′)g(x′), which defines the property of being a truncated functions at the origin. On the other hand, we prove that the wave-function of a generalized diffraction in time problem is just the Fourier-transform of a truncated function. Consequently, the existence of dispersion relations for the diffraction in time wave-function follows. We derive these explicit dispersion relations.

Surface diffraction beamline at the SSRF

BL02U2 of the Shanghai Synchrotron Radiation Facility is a surface diffraction beamline with a photon flux of 5.5×10^(12) photons/s at 10 keV and a beam size of 160µm×80µm at the sample site.It is dedicated to studying surfaces(solid-vacuum,solid-gas)and interfaces(solid-solid,solid-liquid,and liquid-liquid)in nanoscience,condensed matter,and soft matter systems using various surface scattering techniques over an energy range of 4.8-28 keV with transmission and reflection modes.Moreover,BL02U2 has a high energy resolution,high angular resolution,and low beam divergence,which can provide excellent properties for X-ray diffraction experiments,such as grazing incident X-ray diffraction,X-ray reflectivity,crystal truncation rods,and liquid X-ray scattering.Diversity of in situ environments can also be provided for the samples studied.This paper describes the setup of the new beamline and its applications in various fields.

A novel self-alignment method for high precision silicon diffraction microlens arrays preparation and its integration with infrared focal plane arrays

Silicon(Si)diffraction microlens arrays are usually used to integrating with infrared focal plane arrays(IRFPAs)to improve their performance.The errors of lithography are unavoidable in the process of the Si diffrac-tion microlens arrays preparation in the conventional engraving method.It has a serious impact on its performance and subsequent applications.In response to the problem of errors of Si diffraction microlens arrays in the conven-tional method,a novel self-alignment method for high precision Si diffraction microlens arrays preparation is pro-posed.The accuracy of the Si diffractive microlens arrays preparation is determined by the accuracy of the first li-thography mask in the novel self-alignment method.In the subsequent etching,the etched area will be protected by the mask layer and the sacrifice layer or the protective layer.The unprotection area is carved to effectively block the non-etching areas,accurately etch the etching area required,and solve the problem of errors.The high precision Si diffraction microlens arrays are obtained by the novel self-alignment method and the diffraction effi-ciency could reach 92.6%.After integrating with IRFPAs,the average blackbody responsity increased by 8.3%,and the average blackbody detectivity increased by 10.3%.It indicates that the Si diffraction microlens arrays can improve the filling factor and reduce crosstalk of IRFPAs through convergence,thereby improving the perfor-mance of the IRFPAs.The results are of great reference significance for improving their performance through opti-mizing the preparation level of micro nano devices.

Direct observation of shock-induced phase transformation in polycrystalline iron via in situ x-ray diffraction

Phase transition of polycrystalline iron compressed along the Hugoniot is studied by combining laser-driven shock with in situ x-ray diffraction technique.It is suggested that polycrystalline iron changes from an initial body-centered cubic structure to a hexagonal close-packed structure with increasing pressure(i.e.,a phase transition fromαtoε).The relationship between density and pressure for polycrystalline iron obtained from the present experiments is found to be in good agreement with the gas-gun Hugoniot data.Our results show that experiments with samples at lower temperatures under static loading,such as in a diamond anvil cell,lead to higher densities measured than those found under dynamic loading.This means that extrapolating results of static experiments may not predict the dynamic responses of materials accurately.In addition,neither the face-centered cubic structure seen in previous molecular-dynamics simulations or twophase coexistence are found within our experimental pressure range.

The Crystal Structure Study of CaSrFe0.75Co0.75Mn0.5O6−δ by Neutron Diffraction

The crystal structure of CaSrFe0.75Co0.75Mn0.5O6−δ is investigated through neutron diffraction techniques in this study. The material is synthesized using a solid-state synthesis method at a temperature of 1200˚C. Neutron diffraction data is subjected to Rietveld refinement, and a comparative analysis with X-ray diffraction (XRD) data is performed to unravel the structural details of the material. The findings reveal that the synthesized material exhibits a cubic crystal structure with a Pm-3m phase. The neutron diffraction results offer valuable insights into the arrangement of atoms within the lattice, contributing to a comprehensive understanding of the material’s structural properties. This research enhances our knowledge of CaSrFe0.75Co0.75Mn0.5O6−δ, with potential implications for its applications in various technological and scientific domains.

Tailoring electron vortex beams with customizable intensity patterns by electron diffraction holography

An electron vortex beam(EVB) carrying orbital angular momentum(OAM) plays a key role in a series of fundamental scientific researches, such as chiral energy-loss spectroscopy and magnetic dichroism spectroscopy. So far, almost all the experimentally created EVBs manifest isotropic doughnut intensity patterns. Here, based on the correlation between local divergence angle of electron beam and phase gradient along azimuthal direction, we show that free electrons can be tailored to EVBs with customizable intensity patterns independent of the carried OAM. As proof-of-concept, by using computer generated hologram and designing phase masks to shape the incident free electrons in the transmission electron microscope, three structured EVBs carrying identical OAM are tailored to exhibit completely different intensity patterns. Furthermore, through the modal decomposition, we quantitatively investigate their OAM spectral distributions and reveal that structured EVBs present a superposition of a series of different eigenstates induced by the locally varied geometries. These results not only generalize the concept of EVB, but also demonstrate an extra highly controllable degree of freedom for electron beam manipulation in addition to OAM.

Diffraction deep neural network-based classification for vector vortex beams

The vector vortex beam(VVB)has attracted significant attention due to its intrinsic diversity of information and has found great applications in both classical and quantum communications.However,a VVB is unavoidably affected by atmospheric turbulence(AT)when it propagates through the free-space optical communication environment,which results in detection errors at the receiver.In this paper,we propose a VVB classification scheme to detect VVBs with continuously changing polarization states under AT,where a diffractive deep neural network(DDNN)is designed and trained to classify the intensity distribution of the input distorted VVBs,and the horizontal direction of polarization of the input distorted beam is adopted as the feature for the classification through the DDNN.The numerical simulations and experimental results demonstrate that the proposed scheme has high accuracy in classification tasks.The energy distribution percentage remains above 95%from weak to medium AT,and the classification accuracy can remain above 95%for various strengths of turbulence.It has a faster convergence and better accuracy than that based on a convolutional neural network.

Numerical Study on the Effect of Gap Diffraction on the Hydrodynamic Performance of A Floating Breakwater

Two-dimensional(2D)flume experiments are useful in investigating the performances of floating breakwaters(FBs),including hydrodynamic performances,motion responses,and mooring forces.Designing a reasonable gap between the flume wall and the FBs is a critical step in 2D flume tests.However,research on the effect of the gap on the accuracy of 2D FB experimental results is scarce.To address this issue,a numerical wave tank is developed using CFD to estimate the wave-FB interaction of a moored dual-cylindrical FB,and the results are compared to experimental data from a previously published work.There is good agreement between them,indicating that the numerical model is sufficiently accurate.The numerical model is then applied to explore the effect of gap diffraction on the performance of FBs in2D experiments.It was discovered that the nondimensional gap length L_(Gap)/W_(Pool)should be smaller than 7.5%to ensure that the relative error of the transmission coefficient is smaller than 3%.The influence of the gap is also related to the entering wave properties,such as the wave height and period.

A Novel High Temperature Apparatus for in situ Synchrotron X-ray Diffraction Studies of Molten Salt

This study demonstrates the design and application of a novel high temperature rotatory apparatus for insitu synchrotron X-ray diffraction studies of molten salts,facilitating investigation into the interaction between various structural materials and molten salts.The apparatus enables accurate detection of every phase change during hightemperature experiments,including strong reaction processes like corrosion.Molten salts,such as chlorides or fluo⁃rides,together with the structure materials,are inserted into either quartz or boron nitride capillaries,where X-ray diffraction pattern can be continuously collected,as the samples are heated to high temperature.The replacement re⁃action,when molten ZnCl2 are etching Ti3AlC2,can be clearly observed through changes in diffraction peak intensity as well as expansion in c-axis lattice parameter of the hexagonal matrix,due to the larger atomic number and ionic ra⁃dius of Zn2+.Furthermore,we investigated the high-temperature corrosion process when GH3535 alloy is in FLiNaK molten salt,and can help to optimize its stability for potential applications in molten salt reactor.Additionally,this high temperature apparatus is fully compatible with the combined usage of X-ray diffraction and Raman technique,providing both bulk and surface structural information.This high temperature apparatus has been open to users and is extensively used at BL14B1 beamline of the Shanghai Synchrotron Radiation Facility.

基于蒙特卡罗模拟的透射式XRD背景的定量分析

XRD背景主要来源于空气、装置和样品中光子的散射,XRD分析需准确扣除背景,常用的扣背景方法具有一定的局限。蒙特卡罗模拟可实现光子的甄别与统计,因此可将其用于XRD背景来源的定量分析。相干散射的模拟中需考虑物质的Form Factor,这可由Baró等的拟合式、独立原子模型或德拜公式给出;在20 keV能量及透射几何模式下,通过对骨、尼龙、水等物质的XRD模拟,对探测器中光子来源进行了区分和统计。结果表明,德拜公式计算的空气背景大于独立原子模型;空气散射在小角度时背景占比大,随散射角的增加从100%减小至40%以下,而样品中康普顿散射的计数占比则从0增大至60%以上。该方法可对不同样品组成以及复杂装置结构的XRD背景进行定量分析。

Diffraction deep neural network based orbital angular momentum mode recognition scheme in oceanic turbulence

Orbital angular momentum(OAM)has the characteristics of mutual orthogonality between modes,and has been applied to underwater wireless optical communication(UWOC)systems to increase the channel capacity.In this work,we propose a diffractive deep neural network(DDNN)based OAM mode recognition scheme,where the DDNN is trained to capture the features of the intensity distribution of the OAM modes and output the corresponding azimuthal indices and radial indices.The results show that the proposed scheme can recognize the azimuthal indices and radial indices of the OAM modes accurately and quickly.In addition,the proposed scheme can resist weak oceanic turbulence(OT),and exhibit excellent ability to recognize OAM modes in a strong OT environment.The DDNN-based OAM mode recognition scheme has potential applications in UWOC systems.

基于XRD内标法测定LiF-BeF_2熔盐体系中UF_3含量

在氟化物熔盐相直接将UF6中转化为UF_4是熔盐堆燃料盐的合成及重构的候选工艺之一。其中,UF_(3)是该工艺过程的重要中间产物,其含量是开展工艺研究的关键参数之一。本文采用X射线衍射(X-ray Diffraction,XRD)内标法测量氟化物体系中的UF_(3)含量,分析了不同组分的固态熔盐样品,建立了UF_(3)含量的测量分析方法。首先以刚玉(α-Al_(2)O_(3))为内标,获得了UF_(3)在1.00~10.00 wt%含量范围时,LiF-BeF_(2)-UF_(3)熔盐的XRD峰高度内标曲线(R=0.986)和峰面积内标曲线(R=0.995)。然后应用这两条内标曲线测量已知含量的LiUF_(5)和UF_(3)固体混合样品,结果表明峰面积内标曲线具有更好的准确度,测量相对误差不大于8.7%。最后分别对快速冷却的LiF-BeF_(2)-UF_(3)固态熔盐样品和自然冷却的LiF-BeF_(2)-UF_(3)-LiUF_(5)固态熔盐样品进行测量,测量结果的相对误差不大于5.4%。以上结果表明:本文建立的XRD内标法可以用于混合氟盐样品的UF_(3)分析,并具有较好的测量精度和重复性。

偏光显微镜和XRD在南非Postmasburg锰矿定性分析中的应用

根据南非Postmasburg锰矿田BIF型矿体中的矿石分带和品位差异,识别出了富锰型矿石、砾岩型矿石以及铁质岩型矿石。为确定各类矿石的矿物成分,了解矿石类型与其矿物成分间的对应关系,以各类矿石为研究对象,对其中的矿物成分进行了研究。采用偏光显微鉴定技术结合X射线衍射物相分析,基于矿物偏光特征和特征衍射峰,对矿石中的矿物进行了定性。结果表明,富锰型矿石中的主量矿物为方铁锰矿和褐锰矿;砾岩型矿石中金属矿物几乎全为赤铁矿,黏土矿物以钠珠云母为主;含砾铁质岩中黏土矿物居多,以白云母为主,金属矿物多为赤铁矿。由此可见,偏光显微鉴定和XRD具有良好的一致性和互补性,尤其是对厚层的沉积型矿床,岩性和岩相具有一定变化序列的情况下,更适合二者相结合进行精确定性分析。

Tracking the phase transformation and microstructural evolution of Sn anode using operando synchrotron X-ray energy-dispersive diffraction and X-ray tomography

Tin(Sn)holds great promise as an anode material for next-generation lithium(Li)ion batteries but suffers from massive volume change and poor cycling performance.To clarify the dynamic chemical and microstructural evolution of Sn anode during lithiation and delithiation,synchrotron X-ray energydispersive diffraction and X-ray tomography are simultaneously employed during Li/Sn cell operation.The intermediate Li-Sn alloy phases during de/lithiation are identified,and their dynamic phase transformation is unraveled which is further correlated with the volume variation of the Sn at particle-and electrode-level.Moreover,we find that the Sn particle expansion/shrinkage induced particle displacement is anisotropic:the displacement perpendicular to the electrode surface(z-axis)is more pronounced compared to the directions(x-and y-axis)along the electrode surface.This anisotropic particle displacement leads to an anisotropic volume variation at the electrode level and eventually generates a net electrode expansion towards the separator after cycling,which could be one of the root causes of mechanical detachment and delamination of electrodes during long-term operation.The unraveled chemical evolution of Li-Sn and deep insights into the microstructural evolution of Sn anode provided here could guide future design and engineering of Sn and other alloy anodes for high energy density Li-and Na-ion batteries.

Pluggable multitask diffractive neural networks based on cascaded metasurfaces

Optical neural networks have significant advantages in terms of power consumption,parallelism,and high computing speed,which has intrigued extensive attention in both academic and engineering communities.It has been considered as one of the powerful tools in promoting the fields of imaging processing and object recognition.However,the existing optical system architecture cannot be reconstructed to the realization of multi-functional artificial intelligence systems simultaneously.To push the development of this issue,we propose the pluggable diffractive neural networks(P-DNN),a general paradigm resorting to the cascaded metasurfaces,which can be applied to recognize various tasks by switching internal plug-ins.As the proof-of-principle,the recognition functions of six types of handwritten digits and six types of fashions are numerical simulated and experimental demonstrated at near-infrared regimes.Encouragingly,the proposed paradigm not only improves the flexibility of the optical neural networks but paves the new route for achieving high-speed,low-power and versatile artificial intelligence systems.

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).

Analysis and Prediction of Effect of Turning Marks Diffraction on Image Quality of Optical System

Single-point diamond turning (SPDT) is widely used in the machining of infrared materials and metal-based mirrors. Diamond tips can scratch material, replicate the shape of the tip, and create annular turning marks on optical surfaces, which can have unpredictable adverse effects on imaging. In order to predict the effect of turning marks diffraction on the degradation of imaging quality, a model of the influence of SPDT processing parameters on the reduction of system imaging MTF under the influence of ideal grating turning marks diffraction was established. The results show that the depth of the turning mark will lead to the decline of MTF, especially the low frequency information. Finally, a method is proposed to reduce the effect of turning marks diffraction through changing the processing parameters. .