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.

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.

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.

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.

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).

Simple and universal method in designs of high-efficiency diffractive optical elements for spectrum separation and beam concentration

Diffractive optical elements（DOEs） with spectrum separation and beam concentration（SSBC） functions have important applications in solar cell systems. With the SSBC DOEs, the sunlight radiation is divided into several wave bands so as to be effectively absorbed by photovoltaic materials with different band gaps. A new method is proposed for designing high-efficiency SSBC DOEs, which is physically simple, numerically fast, and universally applicable. The SSBC DOEs are designed by the new design method, and their performances are analyzed by the Fresnel diffraction integral method.The new design method takes two advantages over the previous design method. Firstly, the optical focusing efficiency is heightened by up to 10%. Secondly, focal positions of all the designed wavelengths can be designated arbitrarily and independently. It is believed that the designed SSBC DOEs should have practical applications to solar cell systems.

A single diffractive optical element implementing spectrum-splitting and beam-concentration functions simultaneously with high diffraction efficiency

In this paper,a novel method is proposed and employed to design a single diffractive optical element（DOE） for implementing spectrum-splitting and beam-concentration（SSBC） functions simultaneously.We develop an optimization algorithm,through which the SSBC DOE can be optimized within an arbitrary thickness range according to the limitations of modern photolithography technology.Theoretical simulation results reveal that the designed SSBC DOE has a high optical focusing efficiency.It is expected that the designed SSBC DOE should have practical applications in high-efficiency solar cell systems.

Realizing high photovoltaic efficiency with parallel multijunction solar cells based on spectrum-splitting and-concentrating diffractive optical element

Based on the facts that multijunction solar cells can increase the efficiency and concentration can reduce the cost dramatically, a special design of parallel multijunction solar cells was presented. The design employed a diffractive optical element （DOE） to split and concentrate the sunlight. A rainbow region and a zero-order diffraction region were generated on the output plane where solar cells with corresponding band gaps were placed. An analytical expression of the light intensity distribution on the output plane of the special DOE was deduced, and the limiting photovoltaic efficiency of such parallel multijunction solar ceils was obtained based on Shockley-Queisser＇s theory. An efficiency exceeding the Shockley--Queisser limit （33%） can be expected using multijunction solar cells consisting of separately fabricated subcells. The results provide an important alternative approach to realize high photovoltaic efficiency without the need for expensive epitaxial technology widely used in tandem solar cells, thus stimulating the research and application of high efficiency and low cost solar cells.

Elemental composition x-ray fluorescence analysis with a TES-based high-resolution x-ray spectrometer

The accurate analysis of the elemental composition plays a crucial role in the research of functional materials.The emitting characteristic x-ray fluorescence(XRF)photons can be used for precisely discriminating the specified element.The detection accuracy of conventional XRF methodology using semiconductor detector is limited by the energy resolution,thus posing a challenge in accurately scaling the actual energy of each XRF photon.We adopt a novel high-resolution x-ray spectrometer based on the superconducting transition-edge sensor(TES)for the XRF spectroscopy measurement of different elements.Properties including high energy resolution,high detection efficiency and precise linearity of the new spectrometer will bring significant benefits in analyzing elemental composition via XRF.In this paper,we study the Ledge emission line profiles of three adjacent rare earth elements with the evenly mixed sample of their oxide components:terbium,dysprosium and holmium.Two orders of magnitude better energy resolution are obtained compared to a commercial silicon drift detector.With this TES-based spectrometer,the spectral lines overlapped or interfered by background can be clearly distinguished,thus making the chemical component analysis more accurate and quantitative.A database of coefficient values for the line strength of the spectrum can then be constructed thereafter.Equipped with the novel XRF spectrometer and an established coefficient database,a direct analysis of the composition proportion of a certain element in an unknown sample can be achieved with high accuracy.

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.

Design optimization of highly efficient spectrum-splitting and beam-concentrating diffractive optical element for lateral multijunction solar cells

Two improved algorithms are proposed to extend a diffractive optical element （DOE） to work under the broad spec- trum of sunlight. An optimum design has been found for the DOE, with a weighted average optical efficiency of about 6.8% better than that of the previous design. The optimization of designing high optical efficiency DOEs will pave the way for future designs of high-efficiency, low-cost lateral multijunction solar cells based on such a DOE.

Spectrum-Splitting Diffractive Optical Element of High Concentration Factor and High Optical Efficiency for Three-Junction Photovoltaics

A spectrum-splitting and beam-concentrating （SSBC） diffractive optical element （DOE） for three-junction pho- tovoltaics （PV） system is designed and fabricated by five-circ/e micro-fabrication. The incident solar light is efficiently split into three sub-spectrum ranges and strongly concentrated on the focal plane, which can be di- rectly utilized by suitable spectrum-matching solar cells. The system concentration factor reaches 12x. Moreover, the designed wavelengths （450nm, 550nm and 65Onto） are spatially distributed on the focal plane, in good agree- ment with the theoretical results. The average optical effic/ency of all the cells over the three designed wavelengths is 60.07%. The SSBC DOE with a high concentration factor and a high optical efficiency provides a cost-effective approach to achieve higher PV conversion efficieneies.

Design of Diffractive Optical Elements Used for Beam Shaping in the Fresnel Domain

In the Fresnel transform domain, an effective improvement to the conventional iterative algorithm for designing the diffractive optical elements (DOEs) used for spatial beam shaping has been proposed. The algorithm can successfully achieve to design DOEs for beam shaping. Compared with conventional algorithm, this algorithm can provide faster convergence, more powerful ability to overcome local minimum problem and better shaping quality. By computer simulation, the result has shown that the DOEs designed by this algorithm has snch advantages as high uniformity at the main lobe, low profile error and steep edge.

Subwavelength Diffractive Optical Elements

1 Introduction 1.1 Advantages of DOE 1)High diffraction efficiency; 2)Dispersive; 3)More selectivity of designing parameters; 4)More selectivity of primary materials; 5)Can make components miniature,forming array and integration. 1.2 1.3 megapixel triplet plastic mobile

A study on some elements and their phases in sediments of Changjiang Estuary by X-ray spectrometer and X-ray diffractometer

INTRODUCTIONThe studies on the quantitative distribution of the conventional elements and their phases in the sediments of the Changjiang Estuary are of great importance to the understanding of the chemical processes of ion exchange, absorption, desorption and flocculation in the estuary.

Evaluation on residual stresses of silicon-doped CVD diamond films using X-ray diffraction and Raman spectroscopy

The effect of silicon doping on the residual stress of CVD diamond films is examined using both X-ray diffraction (XRD) analysis and Raman spectroscopy measurements. The examined Si-doped diamond films are deposited on WC-Co substrates in a home-made bias-enhanced HFCVD apparatus. Ethyl silicate (Si(OC2H5)4) is dissolved in acetone to obtain various Si/C mole ratio ranging from 0.1% to 1.4% in the reaction gas. Characterizations with SEM and XRD indicate increasing silicon concentration may result in grain size decreasing and diamond [110] texture becoming dominant. The residual stress values of as-deposited Si-doped diamond films are evaluated by both sin2ψ method, which measures the (220) diamond Bragg diffraction peaks using XRD, with ψ-values ranging from 0° to 45°, and Raman spectroscopy, which detects the diamond Raman peak shift from the natural diamond line at 1332 cm-1. The residual stress evolution on the silicon doping level estimated from the above two methods presents rather good agreements, exhibiting that all deposited Si-doped diamond films present compressive stress and the sample with Si/C mole ratio of 0.1% possesses the largest residual stress of ~1.75 GPa (Raman) or ~2.3 GPa (XRD). As the silicon doping level is up further, the residual stress reduces to a relative stable value around 1.3 GPa.

Thermal expansion of kyanite at ambient pressure:An X-ray powder diffraction study up to 1000℃

The thermal expansion coefficients of kyanite at ambient pressure have been investigated by an X-ray powder diffraction technique with temperatures up to 1000 ℃. No phase transition was observed in the experimental temperature range. Data for the unit-cell parameters and temperatures were fitted empirically resulting in the following thermal expansion coefficients： αa = 5.8（3） × 10^-5, αb = 5.8 （1）× 10^-5, αc = 5.2（1）× 10^-5, and αv = 7.4（1） × 10^-3 ℃ 1 in good agreement with a recent neutron powder diffraction study. On the other hand, the variation of the unit-cell angles α, β and γ of kyanite with increase in temperature is very complicated, and the agreement among all studies is poor. The thermal expansion data at ambient pressure reported here and the compression data at ambient temperature from the literature suggest that, for the kyanite lattice, the most and least thermally expandable directions correspond to the most and least compressible directions, respectively.

SnO_2-based solid solutions for CH_4 deep oxidation: Quantifying the lattice capacity of SnO_2 using an X-ray diffraction extrapolation method

A series of SnO2‐based catalysts modified by Mn, Zr, Ti and Pb oxides with a Sn/M （M=Mn, Zr, Ti and Pb） molar ratio of 9/1 were prepared by a co‐precipitation method and used for CH4 and CO oxidation. The Mn3＋, Zr4＋, Ti4＋and Pb4＋cations are incorporated into the lattice of tetragonal rutile SnO2 to form a solid solution structure. As a consequence, the surface area and thermal stability of the catalysts are improved. Moreover, the oxygen species of the modified catalysts become easier to be reduced. Therefore, the oxidation activity over the catalysts was improved, except for the one modified by Pb oxide. Manganese oxide demonstrates the best promotional effects for SnO2. Using an X‐ray diffraction extrapolation method, the lattice capacity of SnO2 for Mn2O3 was 0.135 g Mn2O3/g SnO2, which indicates that to form stable solid solution, only 21%Sn4＋cations in the lattice can be maximally replaced by Mn3＋. If the amount of Mn3＋cations is over the capacity, Mn2O3 will be formed, which is not favorable for the activity of the catalysts. The Sn rich samples with only Sn‐Mn solid solution phase show higher activity than the ones with excess Mn2O3 species.

X-ray Diffraction of Dust Particles in Spring Beijing

X-ray diffractometry was utilized to study the mineralogical characteristics of the inhalable particles （PM10） sampled during two dust storms in Beijing city on March 18th and May 21st, 2008. We confirm, for the first time, that there stably exists ammonium chloride in the atmosphere when temperature is low. The total sulfates particles were affected by relative humidity. Both species and concentration of sulfates decreased first and then grew back by the end of each dust storm. Koninckite, a phosphate mineral never reported as particulate aerosol before, was identified. Meanwhile, our result shows that a chemical modification on dust minerals occurs during long range transportation. PM10 samples collected during the period of dust storms were dominated by crustal minerals such as quartz, illite/smectite, illite, chlorite, feldspar and calcite, and were notably higher in concentration than that in normal periods of time. The amounts of total sulfates, calcite and feldspar altered in each dust storm. It is derived from 24-hour isentropic backward trajectories that two dust events in spring 2008 originated in different sources.

MULTI-PEAK MATCH INTENSITY RATIO METHOD OF QUANTI-TATIVE X-RAY DIFFRACTION PHASE ANALYSIS

A new method for quantitative phase analysis is proposed by using X-ray diffraction multi-peak match intensity ratio. This method can obtain the multi-peak match intensity ratio among each phase in the mixture sample by using all diffraction peak data in the mixture sample X-ray diffraction spectrum and combining the relative intensity distribution data of each phase standard peak in JCPDS card to carry on the least square method regression analysis. It is benefit to improve the precision of quantitative phase analysis that the given single line ratio which is usually adopted is taken the place of the multi-peak match intensity ratio and is used in X-ray diffraction quantitative phase analysis of the mixture sample. By analyzing four-group mixture sample, adopting multi-peak match intensity ratio and X-ray diffraction quantitative phase analysis principle of combining the adiabatic and matrix flushing method, it is tested that the experimental results are identical with theory.