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.

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.

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.

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).

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.

Radiological and X-Ray Diffraction Characterization of Bauxite and Rutile Ore Contaminated Environment in Kanam and Wase Mineral Exploration Sites, Plateau State-Nigeria

Two non-destructive analytical techniques (gamma spectrometer and X-ray diffractometer) were employed in the analysis of bauxite and rutile ore and their vicinity soil and control sourced within the Kanam and Wase mineral exploration sites. The activity concentrations of natural radionuclides 238U, 232Th, and 40K in the soil samples received from bauxite and rutile mineral mining vicinities revealed high concentrations of 238U, 232Th, and 40K compared to the control soil samples sourced 500 m away from the mineral exploration vicinities. Radiological detriments RLI, AUI, Hin and Hex unveiled values exceeding the radiation standard concentration (>1) for soil. X-ray diffraction characterization of bauxite ore revealed the interlocking minerals of Bauxite (18)%, Albite (11)%, Garnet (15)%, Illite (6)% and Muscovite (43)% in various proportions obtained within the 2θ range (9.18 to 64.4) and a peak value (intensity, cps) of 3400. Pure bauxite percentage in the ore meets metallurgical grade (15 - 25)%. X-ray diffraction of rutile ore revealed the minerals of rutile (40)%, quartz (21.4)%, ilmenite (27)% and garnet (11.8)% found within the 2θ range (27.5 to 35.6) and a peak value intensity of 31.1 - 100.0 cps also meeting the metallurgical grade of 15% - 25%. The major environmental concern associated with the mineral-sands industry is the radiation hazards, pollution of ground-water sources from heavy metals, mineral transport with heavy equipment’s, dredging operations in fragile coastal area and clearing of vegetation.

Investigation on the 773 K isothermal section of La-Fe-Sn ternary systems by X-ray powder diffraction

The 773 K isothermal section of the La-Fe-Sn ternary system was investigated and constructed by X-ray powder diffraction（XRD）.The existence of two reported ternary intermetallic compounds,La6Fe13Sn and La3FeSn6,is confirmed in this work.Compared with other R-Fe-Sn phase diagrams（R = Pr and Sm）,the binary alloys Fe3Sn and Fe5Sn3 are not present.The compound Fe3Sn2 was observed from the XRD pattern of Fe3Sn2 samples,but it is not an equilibrium phase at 773 K and decomposes into Fe and FeSn phases completely for a longer heat treated time.Up to now,the crystal structure data of La2Sn3 has not been reported,so the X-ray pattern of La2Sn3 was only estimated.The phase relationship for this compound was drawn by a dotted line.

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.

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.

Structure of MgSO_4 in Concentrated Aqueous Solutions by X-Ray Diffraction

Detailed time-and-space-averaged structure of MgSO4 in the concentrated aqueous solutions was investigated via X-ray diffraction with an X’pert Pro θ-θ diffractometer at 298 K, yielding structural function and radial distribution function（RDF）. The developed KURVLR program was employed for the theoretical investigation in consideration of the ionic hydration and ion association. Multi-peaks Gaussian fitting method was applied to deconvolving the overlapping bands of Differential radial distribution function（DRDF）. The calculation of the geometric model shows that octahedrally six-coordinated Mg（H2O）62＋, with an Mg2＋…OW bond length of 0.201 nm dominates in the solutions. There exists contact ion-pair（CIP） in the more concentrated solution（1：18, H2O/salt molar ratio） with a coordination number of 0.8 and a characteristic Mg…S distance of 0.340 nm. The result indicates the hydrated SO42– ion happens in the solution. The S…OW bond distance was determined to be 0.382 nm with a coordination number of 13. The fraction of CIP increases significantly with the increasing concentration. The symmetry of the hydration structure of sulfate ion is lowered by forming complex with magnesium ion.

Investigation of Peak Separation for X-ray Diffraction Profiles of Spinodal Decomposition by a Kind of Optimized Voigt Function

The intensity and position of sidebands (satellites) on both sides of main diffraction peak in a great number of X-ray diffraction profiles of alloys always change with progress of aging. The sidebands position is determined by a newly optimized Voigt function in present investigation. Furthermore, for Cu-4 wt pet Ti alloy aged at 400℃ for 720 min and 1080 min, after introducing the weight factor of above two satellites intensity, the relative error between the fitting curves and X-ray diffraction profiles is less than 0.185%, which is more precise than the previously calculating result.

Rietveld refinement of powder X-ray diffraction,microstructural and mechanical studies of magnesium matrix composites processed by high energy ball milling

This research reports the processing of magnesium matrix composites reinforced with silicon carbide(SiC)and aluminium oxide(Al_(2)O_(3))using powder metallurgy technique through high energy milling.Samples of Mg-SiC and Mg-Al_(2)O_(3)composites subjected to high energy ball milling for different vol%of secondary particles 20,30 and 40%of SiC and Al_(2)O_(3)are studied by X-Ray diffraction technique.The rietveld method as implemented in the Fullprof program is applied in order to determine the quantities of the resulting crystalline phases and amorphous phases at each stage of the mechanical treatment.Microstructural examination is carried out using Scanning Electron Microscope(SEM).In addition,crystal structural analysis using appropriate size and strain models is performed in order to handle the distinctive anistrophy that is observed in convinced crystallographic directions for the magnesium composite.The results are furnished in terms of crystalline domains size enlargement of the magnesium composites phases upon prolonged milling duration and discussed in the light of up to date views and theories on crystal growth of nanocrystaline materials.The hardness of the composite samples is calculated by Vickers’s Hardness tester.Further,dry sling wear test and corrosion test are performed for the fabricated composites.Composite with 30%secondary particles incorporated magnesium composites exhibits better wear and corrosion resistance than the other composites.

In situ X-ray diffraction and thermal analysis of LiNi0.8Co0.15Al0.05O2 synthesized via co-precipitation method

LiNi0.9Co0.15Al0.05O2 （NCA） material is successfully synthesized with a modified co-precipitation method,in which NH3,H2O and EDTA are used as two chelating agents. The obtained LiNi0.9Co0.15Al0.05O2 materialhas well-defined layered structure and uniform element distribution, which reveals an enhanced electro-chemical performance with a capacity retention of 97.9% after 100 cycles at 0.2 C, and reduced thermalrunaway from the isothermal calorimetry test. In situ X-ray diffraction （XRD） was employed to capturethe structural changes during the charge-discharge process. The reversible evolutions of lattice parame-ters （a, b, c, and V） further verify the structural stability.

Ultrafast structural dynamics using time-resolved x-ray diffraction driven by relativistic laser pulses

Based on a femtosecond laser plasma-induced hard x-ray source with a high laser pulse energy(>100 mJ)at 10 Hz repetition rate,we present a time-resolved x-ray diffraction system on an ultrafast time scale.The laser intensity is at relativistic regime(2×10^(19)W/cm^(2)),which is essential for effectively generating K_(α)source in high-Z metal material.The produced copper K_(α)radiation yield reaches to 2.5×10^(8)photons/sr/shot.The multilayer mirrors are optimized for monochromatizating and two-dimensional beam shaping of Kαemission.Our experiment exhibits its ability of monitoring the transient structural changes in a thin film SrCoO_(2.5)crystal.It is demonstrated that this facility is a powerful tool to perform dynamic studies on samples and adaptable to the specific needs for different particular applications with high flexibility.

High pressure x-ray diffraction techniques with synchrotron radiation

This article summarizes the developments of experimental techniques for high pressure x-ray diffraction（XRD） in diamond anvil cells（DACs） using synchrotron radiation. Basic principles and experimental methods for various diffraction geometry are described, including powder diffraction, single crystal diffraction, radial diffraction, as well as coupling with laser heating system. Resolution in d-spacing of different diffraction modes is discussed. More recent progress, such as extended application of single crystal diffraction for measurements of multigrain and electron density distribution, timeresolved diffraction with dynamic DAC and development of modulated heating techniques are briefly introduced. The current status of the high pressure beamline at BSRF（Beijing Synchrotron Radiation Facility） and some results are also presented.

Powder x-ray diffraction and Rietveld analysis of (C_(2)H_(5)NH_(3))_(2)CuCl_(4)

Structural properties of the organic-inorganic hybrid(C_(2)H_(5)NH_(3))_(2)CuCl_(4) have been investigated by means of x-ray powder diffraction and Rietveld analysis. A structural phase transition from Pbca to Aba2 occurs at T_(4)= 240 K, which results in a paraelectric–ferroelectric phase transition. The release of the Jahn–Teller distortion with increasing temperature toward T_(4) is revealed by the structural analysis.

X-ray Multiple Diffraction Topographic Imaging Technique For Growth History Study of Habit Modifying Impurity Doped Crystals

A novel crystal characterization instrument has been built up in which a combination of X-ray multiple diffraction and X-ray topography is applied to enabling the cross-correlation between micro-crystallographic symmetry and its spatial dependence in relation to lattice defects. This facility is used to examine, in a self-consistent manner, growth sector-dependant changes to both the crystallographic structure and the lattice defects associated with the action of habit-modifying additives in a number of representative crystal growth systems. In addition, the new instrument can be used to probe micro-crystallographic aspects(such as distortion to crystal symmetry) and relate these in a spatially resolved manner to the crystal defect structure in crystals doped with known habit modifiers.