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.

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.

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.

Structural,magnetic and dielectric properties of nano-crystalline Ni-doped BiFeO_(3) ceramics formulated by self-propagating high-temperature synthesis

Ni-doped BiFeO_(3) powders with the composition BiFe_(1-x)Ni_(x)O_(3)(x=0.05,0.1 and 0.15)were prepared by a self-propagating high-temperature synthesis(SHS),using metal nitrates as oxidizers and glycine as fuel.The X-ray diffraction(XRD)patterns depict that Ni-doped BiFeO_(3) ceramics crystallize in a rhombhohedral phase.The scanning electron micrographs of Ni-doped BiFeO_(3) ceramics show a dense morphology with interconnected structure.It is found that,the room-temperature magnetization measurements in Ni-incorporated BiFeO_(3) ceramics give rise to nonzero magnetization.The magnetization of Ni-doped BiFeO_(3) ceramics is significantly enhanced when Ni doping concentration reaches to x=0.1 at 5 K.The variations of dielectric constant with temperature in BiFe_(0.95)Ni_(0.05)O_(3),BiFe_(0.9)Ni_(0.1)O_(3) and BiFe_(0.85)Ni_(0.15)O_(3) samples exhibit clear dielectric anomalies approximately around 450℃,425℃and 410℃respectively,which correspond to antiferromagnetic to paramagnetic phase transition of the parent compound BiFeO_(3).

Thermal equation of state of a natural kyanite up to 8.55 GPa and 1273 K

The thermal equation of state of a natural kyanite has been investigated with a DIA-type,cubic-anvil apparatus(SAM85)combined with an energy-dispersive synchrotron X-ray radiation technique up to 8.55 GPa and 1273 K.No phase transition was observed in the studied pressure-temperature(P-T)range.The Le Bail full profile refinement technique was used to derive the unit-cell parameters.By fixing the bulk modulus K 0 as 196 GPa and its pressure derivative K0 as 4,our P-V(volume)-T data were fitted to the high temperature BircheMurnaghan equation of state.The obtained parameters for the kyanite are:V_(0)=294.05(9)Å^(3),a=2.53(11)×10^(-5)K^(-1) and(K/T)P=-0.021(8)GPa∙K^(-1).These parameters have been combined with other experimentally-measured thermodynamic data for the relevant phases to calculate the P-T locus of the reaction kyanite¼stishoviteþcorundum.With this thermodynamically constrained phase boundary,previous high-pressure phase equi-librium experimental studies with the multi-anvil press have been evaluated.

Thermal Expansion of LaCoO_3

High-temperature X-ray diffraction (HTXRD) measurements of LaCoO_3 powder was carried out in a temperature range from 298 to 1273 K. The experimental data obtained were adopted to evaluate the lattice parameters and cell volume. In this temperature range, the linear and volume expansion coefficients calculated using these cell parameters are 24.160～23.610×10^(-6)·K^(-1) and 59.601～63.218×10^(-6)·K^(-1) respectively. There is no discontinuity found in the cell parameters through the proposed first-order transition at 1210 K.

Thermoelasticity and stability of natural epidote at high pressure and high temperature:Implications for water transport during cold slab subduction

Epidote is a typical hydrous mineral in subduction zones.Here,we report a synchrotron-based single-crystal X-ray diffraction(XRD)study of natural epidote[Ca1.97Al2.15Fe0.84(SiO4)(Si2O7)O(OH)]under simultaneously high pressure-temperature(high P-T)conditions to~17.7 GPa and 700 K.No phase transition occurs over this P-T range.Using the third-order Birch-Murnaghan equation of state(EoS),we fitted the pressure-volume-temperature(P-V-T)data and obtained the zero-pressure bulk modulus K_(0)=138(2)GPa,its pressure derivative K'_(0)=3.0(3),the temperature derivative of the bulk modulus((∂K/∂T)P=-0.004(1)GPa/K),and the thermal expansion coefficient at 300 K(α_(0)=3.8(5)×10^(-5)K^(-1)),as the zero-pressure unit-cell volume V_(0)was fixed at 465.2(2)Å^(3)(obtained by a single-crystal XRD experiment at ambient conditions).This study reveals that the bulk moduli of epidote show nonlinear compositional dependence.By discussing the stabilization of epidote and comparing its density with those of other hydrous minerals,we find that epidote,as a significant water transporter in subduction zones,may maintain a metastable state to~14 GPa along the coldest subducting slab geotherm and promote slab subduction into the upper mantle while favoring slab stagnation above the 410 km discontinuity.Furthermore,the water released from epidote near 410 km may potentially affect the properties of the 410 km seismic discontinuity.

The Aqueous Dispersions of Bicontinuous Cubic Phases Formed by Precursor Method

The morphologies and the microstructures of the dispersed particles of the cubic phase, which were formed by precursor method, were studied. The freeze-fracture TEM clearly showed that the aqueous dispersed particles have irregular cubic shapes. X-ray diffraction technique has been utilized to study the microstructure of the particles and it was found that these particles still retained the cubic character. The sizes of the particles were measured by dynamic light scattering, and the results showed that the sizes of the dispersed particles were between 200 ~ 400 nm under different conditions.

Multivariate MOF for optimizing atmospheric water harvesting

Atmospheric water harvesting offers a powerful and promising solution to address the problem of global freshwater scarcity.In the past decade,significant progress has been achieved in utilizing hydrolytically stable metal-organic frameworks as recyclable water-sorbent materials under low relative humidity,especially in those arid areas.Recently,Yaghi's group has employed a combined crystallographic and theoretical technique to decipher the water filling mechanism in MOF-303,where the polar organic linkers rather than the inorganic units of MOF are demonstrated as the key factor.Hence,the hydrophilic strength of the water-binding pocket in MOFs can be optimized through the approach of multivariate modulations,resulting in enhanced water harvesting properties.

Reversion of Incommensurate Modulation in Cubic Lazurite: Example of Reversible Forced Equilibrium?

The sample of cubic lazurite, collected in the Baikal region, with incommensurately 3D modulated (ITM) structure has been studied by the method of high-temperature X-ray powder diffraction. At short time of annealing in high-temperature diffraction experiment the modulation recovery proceeds during cooling down the sample to room temperature. The identity of the period of both initial and recovered modulation demonstrates that the system has a structural memory. The acquired results are interpreted through comparison of thermal behavior of lazurite, sodalite and quartz structures. It is supposed that two kinetically different and thermally activated processes proceed under heating: 1) reversible framework expansion due to Si-O-Al angle increase, and 2) equalizing of periodic local distortions via the diffusion-controlled transfer of cage ions between adjacent subcells. The second process seems to be much slower than the first one, especially at lower temperatures. With increasing temperature, both processes are activated. However, the framework expands more rapidly than the cage clusters migrate, and the periodic distortions of the framework are aligned. Under lower temperatures, the framework shrinks and again accommodates to the configuration of cage cations (clusters), which may be changed at high temperature and sufficient time or may not at lower temperature, short time, unfavorable SO2 fugacity values. In the first case the modulation disappears entirely, while in the second case it arises again. The probable reason for ITM formation is the balance of counteracting energetic terms: the elastic strain energy of structure deformation and the energy of cluster ordering providing the state of forced equilibrium. The excess free energy due to structure distortion is compensated by the increment associated with the cluster ordering process. However, no significant variations in sulphur anion speciation for different degrees of modulation retention were observed by XPS S 2p. This may be due to the ordering of Na- and Ca-containing clusters rather than the clusters with different sulphur species. ITM reversion is considered as an example of reversible forced equilibrium with completely reproducible forcing factor.

Remarks on the Erroneous Dispersion Surfaces From a Pair of a Hyperbolic Branch and An Elliptical Arc of the Intersected Two Laue Spheres Based on the Usual Crude Approximation

In almost all previous works, the hyperbolic dispersion surfaces of the central proper quadrics have been crudely derived from the degree of reduction from the bi-quadratic equation by use of some roughly indefinable approximate relations. Moreover, neglecting the high symmetry of the hyperbola, both the branches have been approximated on the asymmetric surfaces composed of a pair of a branch of the hyperbola and a vertex of the ellipse without the presentation of reasonable evidence. Based upon the same dispersion surfaces equation, a new original gapless dispersion surfaces could be rigorously introduced without crude omission of even a term in the bi-quadratic equation based upon usual analogy with the extended band theory of solid as the close approximation to the truth.

Designing a toroidal crystal for monochromatic X-ray imaging of a laser-produced He-like plasma

In this study,a toroidal quartz(2023)crystal is designed for monochromatic X-ray imaging at 72.3◦.The designed crystal produces excellent images of a laser-produced plasma emitting He-like Ti X-rays at 4.75 keV.Based on the simulations,the imaging resolutions of the spherical and toroidal crystals in the sagittal direction are found to be 15 and 5μm,respectively.Moreover,the simulation results show that a higher resolution image of the source can be obtained by using a toroidal crystal.An X-ray backlight imaging experiment is conducted using 4.75 keV He-like Ti X-rays,a 3×3 metal grid,an imaging plate and a toroidal quartz crystal with a lattice constant of 2d=0.2749 nm.The meridional and sagittal radii of the toroidalα-quartz crystal are 295.6 and 268.5 mm,respectively.A highly resolved image of the microgrid,with a spatial resolution of 10μm,is obtained in the experiment.By using similar toroidal crystal designs,the application of a spatially resolved spectrometer with high-resolution X-ray imaging ability is capable of providing imaging data with the same magnification ratio in the sagittal and meridional planes.

Low thermal conductivity and anisotropic thermal expansion of ferroelastic(Gd_(1−x)Y_(x))TaO_(4) ceramics

In this paper,(Gd_(1−x)Y_(x))TaO_(4) ceramics have been fabricated by solid-phase synthesis reaction.Each sample was found to crystallize in a monoclinic phase by X-ray diffraction(XRD).The properties of(Gd_(1−x)Y_(x))TaO_(4) were optimized by adjusting the ratio of Gd/Y.(Gd_(1−x)Y_(x))TaO_(4) had a low high-temperature thermal conductivity(1.37–2.05 W·m^(−1)·K^(−1)),which was regulated by lattice imperfections.The phase transition temperature of the(Gd_(1−x)Y_(x))TaO_(4) ceramics was higher than 1500℃.Moreover,the linear thermal expansion coefficients(TECs)were 10.5×10^(−6) K^(−1)(1200℃),which was not inferior to yttria-stabilized zirconia(YSZ)(11×10^(−6) K^(−1),1200℃).(Gd_(1−x)Y_(x))TaO_(4) had anisotropic thermal expansion.Therefore,controlling preferred orientation could minimize the TEC mismatch when(Gd_(1−x)Y_(x))TaO_(4) coatings were deposited on different substrates as thermal barrier coatings(TBCs).Based on their excellent properties,it is believed that the(Gd_(1−x)Y_(x))TaO_(4) ceramics will become the next generation of high-temperature thermal protective coatings.

Partitioning behavior and lattice misfit of γ/γ’phases in Ni-based superalloys with different Mo additions

A low-density single crystal(LDS) alloy with the composition of high Mo content was designed.The extra 1.5 wt% Mo was added in the Alloy A with the composition of Ni-6.5 Al-8.0 Mo-2.4 Cr-6.2 Ta-4.9 Co-1.5 Re-(0.01-0.05) Y(wt%) to study the influence of Mo on the lattice parameter and partitioning behavior.Scanning electron microscope(SEM) with energy-dispersive spectrometer(EDS),transmission electron microscopy(TEM)and high-temperature X-ray diffraction(HT-XRD) were used to observe the microstructure,analyze the elemental content and measure the lattice parameter of the alloys.The natural lattice misfit was calculated by lattice constants which were measured by HT-XRD at the temperature from 25 to 1150℃,and the results showed that the lattice misfit would be more and more negative with temperature increasing.It was found that 1.5 wt% addition of Mo will increase the absolute value of the lattice misfit of γ/γ’phases and the volume fraction of γ’,and at the same time,influence the elemental distribution in γ and γ’ phases,especially Re and Cr.Re has a higher partitioning ratio(k) after the addition of Mo.

Study on Phase-Formation Mechanism and Intergrowth for Bi(Pb)-Sr-Ca-Cu-O System

In this paper, the phase-formation mechanism of Bi-based superconductors was systematically investigated by using high-temperature X-ray diffraction, differential thermal analysis (DTA) and crystallization of amorphous state. The transformations among Bi-based 2201, 2212 and 2223 phases were observed, and the intergrown phenomenon of the 2201, 2212 and 2223 phases was explained. It was proposed that there exist a composition equilibrium between 2212 phase and Ca2CuO3 and a competition of thermody-namic stability among Ca2CuO3, 2212 and 2223 phases. This is why it is difficult to prepare the 2223 phase. After Pb was doped in Bi-Sr-Ca-Cu-O system, Ca2CuO3 phase in the Bi-Sr-Ca-Cu-O system was replaced by Ca2PbO4, so that the composition equilibrium and competition of thermodynamic stability mentioned above were avoided.