Structural characterization of Al_(0.55)Ga_(0.45)N epitaxial layer determined by high resolution x-ray diffraction and transmission electron microscopy

Structural characteristics of Alo.55 Gao.45N epilayer were investigated by high resolution x-ray diffraction（HRXRD）and transmission electron microscopy（TEM）;the epilayer was grown on GaN/sapphire substrates using a high-temperature A1 N interlayer by metal organic chemical vapor deposition technique.The mosaic characteristics including tilt,twist,heterogeneous strain,and correlation lengths were extracted by symmetric and asymmetric XRD rocking curves as well as reciprocal space map（RSM）.According to Williamson-Hall plots,the vertical coherence length of AlGaN epilayer was calculated,which is consistent with the thickness of AlGaN layer measured by cross section TEM.Besides,the lateral coherence length was determined from RSM as well.Deducing from the tilt and twist results,the screw-type and edge-type dislocation densities are 1.0×10~8 cm^（-2） and 1.8×10^（10） cm^（-2）,which agree with the results observed from TEM.

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).

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.

An in situ high-pressure X-ray diffraction experiment on hydroxyapophyllite

The compression behavior of a natural hydroxyapophyllite is investigated up to about 10.01 GPa at 300 K using in situ angle-dispersive X-ray diffraction and a diamond anvil cell at the High Pressure Experiment Station, Beijing Synchrotron Radiation Facility （BSRF）. Over this pressure range, no phase change or disproportionation is observed. The isothermal equation of state is determined for the first time. The values of zero-pressure volume V0, isothermal bulk modulus K0, and K0＇ refined with a third-order Birch-Mumaghan equation of state are V0 = 1276.3 ± 0.9 A3, K0 = 71± 3 GPa, and K0＇ = 8 ±1. Furthermore, we confirm that the values of linear compressibility β along the a and c directions of hydroxyapophyllite are elastically anisotropic.

High-pressure effect on inverse spinel LiCuVO_4:X-ray diffraction and Raman scattering

The effect of external quasi-hydrostatic pressure on the inverse spinel structure of LiCuVO4 was studied in this paper. High-pressure synchrotron X-ray diffraction and Raman spectroscopy measurements were carried out at room temperature up to 35.7 and 40.3 GPa, respectively. At a pressure of about 20 GPa, both Raman spectra and X-ray diffraction results indicate that LiCuVO4 was transformed into a monoclinic phase, which remained stable up to at least 35.7 GPa. Upon release of pressure, the high-pressure phase returned to the initial phase. The pressure dependence of the volume of low pressure orthorhombic phase and high-pressure monoclinic phase were described by a second-order Birch-Murnaghan equation of state, which yielded bulk modulus values of B0 = 197 （5） and 232（8） GPa, respectively. The results support the empirical suggestion that the oxide spinels have similar bulk modulus around 200 GPa.

In-Situ High Temperature X-Ray Diffraction Study of Structure and Phase Transformation of Nd-FePt Alloys

The structure and disorder-order transformation of NdxFe60.5-x Pt39.5（x = 0, 0.5, 1.0, 1.5） alloys were investigated in situ by high temperature X-ray diffraction. The results show that the lattice parameter a of disordered γ phase （FCC, Al structure type） and the lattice parameter ratio c/a of ordered γ1 phase （FCT, L10 structure type） increase linearly with increasing Nd concentration, whereas the c/a ratio decreases with increasing temperature. The transition temperature from ordered FCT to disordered FCC decreases with increasing Nd concentration, but for alloys quenched rapidly from γ phase region into ice-water it increases with increasing Nd.

Synchrotron X-Ray Diffraction Studies on the New Generation Ferromagnetic Semiconductor Li(Zn,Mn)As under High Pressure

The pressure effect on the crystalline structure of the I-II- V semiconductor Li（Zn,Mn）As ferromagnet is studied using in situ high-pressure x-ray diffraction and diamond anvil cell techniques. A phase transition starting at -11.6GPa is found. The space group of the high-pressure new phase is proposed as Pmca. Fitting with the Birch-Murnaghan equation of state, the bulk modulus B0 and its pressure derivative B0 of the ambient pressure structure with space group of F43m are B0 = 75.4 GPa and B0 = 4.3, respectively.

The interface of SiO_2/ZnS films studied by high resolution X-ray photoluminescence

Sharp interfaces in optoelectronic devices are key for proper band alignment. Despite its benefits as buffer layer, ZnS deposited via atomic layer deposition(ALD) renders intermixed interfaces to its substrate, which can be detrimental for device performance. Here, we are attempting to elucidate the chemical species deriving from this metal-oxide to metal-sulfide transition studying ultrathin film ZnS on SiO_2 using high resolution X-ray photoluminescence spectroscopy(XPS).Regarding the S 2p spectra after a deposition of only three cycles of ZnS, we discover the many different chemical species in which S is present. These include intermediate oxides such as SO_4^(2-).These species become more obvious as we tilt the sample in the XPS chamber to shallower angles.Comparing the Si 2p and S 2p high resolution peaks in the depth profile, one can clearly uncover the confinement of SO_4^(2-) to the interface of the underlying substrate. This may indicate that SiO_2/ZnS interfaces contain interfacial sulphates that likely alter the electronic configuration of this interface.

High-pressure investigations on Piplia Kalan eucrite meteorite using in-situ X-ray diffraction and ^(57)Fe Mssbauer spectroscopic technique up to 16 GPa

We report here high-pressure investigations on Piplia Kalan eucrite-a member of HED （Howardite -Eucrite-Diogenite） family from asteroid 4-Vesta based on synchrotron X-ray diffraction （up to 16 GPa） and ^57Fe Mossbauer spectroscopy （up to 8 GPa）. Dominant with anorthite-rich plagioclase, pigeonite-rich pyroxene and clino-ferrosilite, the sample displayed various phase transitions attaining amorphous character at 16 GPa. These phase transitions of individual components could be explained simultaneously through variations in high-pressure XRD patterns and the Mossbauer parameters. Most prominent P21/c to C2/c transition of pigeonite and ferrosilite was exhibited both as sudden variation in Mossbauer parameters and population inversion of Fe^2＋ in M1 and M2 sites between 2.9 and 3.8 GPa and variation in intensity profile in XRD patterns at 3.56 GPa. Anorthite seemed to respond more to such impact than other components in the sample. Complete amorphization in anorthite which occurred at lower pressure of - 12 GPa implied residual stress experienced due to shock impact. The presence of high pressure （monoclinic） phase of pigeonite and ferrosilite at ambient condition in this eucrite sample confirmed earlier suggestions of an early shock event. This report is an attempt to emphasize the role of anorthite in the determination of the residual stress due to impact process in the parent body thus to understand the behavioral differences amongst HED members.

X-ray diffraction investigation of amorphous calcium phosphate and hydroxyapatite under ultra-high hydrostatic pressure

The changes in the crystal structures of synthetically prepared amorphous calcium phosphate（ACP） and hydroxyapatite（HAP） in water（1：1 mass ratio） were studied by synchrotron X-ray diffraction（XRD） under ultra-high hydrostatic pressures as high as 2.34 GPa for ACP and 4 GPa for HAP. At ambient pressure, the XRD patterns of the ACP and HAP samples in capillary tubes and their environmental scanning electron micrographs indicated amorphous and crystalline characteristics for ACP and HAP, respectively. At pressures greater than 0.25 GPa, an additional broad peak was observed in the XRD pattern of the ACP phase, indicating a partial phase transition from an amorphous phase to a new high-pressure amorphous phase. The peak areas and positions of the ACP phase, as obtained through fitting of the experimental data, indicated that the ACP exhibited increased pseudo-crystalline behavior at pressures greater than 0.96 GPa. Conversely, no structural changes were observed for the HAP phase up to the highest applied pressure of 4 GPa. For HAP, a unit-cell reduction during compression was evidenced by a reduction in both refined lattice parameters a and c. Both ACP and HAP reverted to their original structures when the pressure was fully released to ambient pressure.

Neutron powder diffraction and high-pressure synchrotron x-ray diffraction study of tantalum nitrides

Tantalum nitride （TAN） compact with a Vickers hardness of 26 GPa is prepared by a high-pressure and high- temperature （HPHT） method. The crystal structure and atom occupations of WC-type TaN have been investigated by neutron powder diffraction, and the compressibility of WC-type TaN has been investigated by using in-situ high-pressure synchrotron x-ray diffraction. The third-order Birch-Murnaghan equation of state fitted to the x-ray diffraction pressure- volume （P-V） sets of data, collected up to 41 GPa, yields ambient pressure isothermal bulk moduli of B0 = 369（2） GPa with pressure derivatives of B~ = 4 for the WC-type TaN. The bulk modulus of WC-type TaN is not in good agreement with the previous result （Bo = 351 GPa）, which is close to the recent theoretical calculation result （Bo = 378 GPa）. An analysis of the experiment results shows that crystal structure of WC-type TaN can be viewed as alternate stacking of Ta and N layers along the c direction, and the covalent Ta-N bonds between Ta and N layers along the c axis in the crystal structure play an important role in the incompressibility and hardness of WC-type TaN.

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.

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.

Novel high-voltage cathode for aqueous zinc ion batteries:Porous K_(0.5)VOPO_(4)·1.5H_(2)O with reversible solid-solution intercalation and conversion storage mechanism

Cathode materials that possess high output voltage,as well as those that can be mass-produced using facile techniques,are crucial for the advancement of aqueous zinc-ion battery(ZIBs)applications,Herein,we present for the first time a new porous K_(0.5)VOPO_(4)·1.5H_(2)O polyanionic cathode(P-KIVP)with high output voltage(above 1.2 V)that can be manufactured at room temperature using straightforward coprecipitation and etching techniques.The P-KVP cathode experiences anisotropic crystal plane expansion via a sequential solid-solution intercalation and phase co nversion pathway throughout the Zn^(2+)storage process,as confirmed by in-situ synchrotron X-ray diffraction and ex-situ X-ray photoelectron spectroscopy.Similar to other layered vanadium-based polyanionic materials,the P-KVP cathode experiences a progressive decline in voltage during the cycle,which is demonstrated to be caused by the irreversible conversion into amorphous VO_(x).By introducing a new electrolyte containing Zn(OTF)_(2) to a mixed triethyl phosphate and water solution,it is possible to impede this irreversible conversion and obtain a high output voltage and longer cycle life by forming a P-rich cathode electrolyte interface layer.As a proof-of-concept,the flexible fiber-shaped ZIBs based on modified electrolyte woven into a fabric watch band can power an electronic watch,highlighting the application potential of P-KVP cathode.

A COMPARISON OF FOUR RECENT NUMERICAL SCHEMES GIViNG HIGH RESOLUTION OF SHOCK WAVE AND CONCENTRATED VORTEX

In recent ten years high resolution difference schenies for the computation of thefull unsteady Eulerian system of equations for invisid compressible gas finds celebratedprogress. This paper tests furtherly, by a complex two-dimensional unsteady problem,four recent schemes. to them attentions are paid. The test problem is the initial stageof a two-dimensional diffraction and reflection of a plane shock wave, impinging on arectangular obstacle. At whose top side there are two sharp corners, near which flow.parameters finds severe variation. There is occurrence of expansion fan with a centerand also concentrated vortices. To simulate them well, the schemes should have goodadaptivity. The special shock Mach number M,=2.068 is so chosen, that at this M,the partical velocity behind impinging shock in fixed coordinate system is just equal tothe speed of sound there, this condition also occurs along a curve in the region ofexpansion fan with a center at the corner. This can clarify the computational featureof different schemes in case,when one of the eigenvalues is just zero. Zero eigenvaluemay spoil some schemes locally. Graphical visualization of the computational resultsmay, show features of the tested schemes about the shock wave resolution, schemeviscosity, expansion wave and the ability. to simulate the process of the generation ofunsteadv concentrated vortex.

Study of Oxidation Kinetics in Air of Zircaloy-4 by <i>in Situ</i>X-Ray Diffraction

The zircaloy-4 is an alloy of zirconium, which has a very weak thermal neutron absorption, satisfactory mechanical properties and good corrosion resistance at high temperature. For these reasons, zircaloy-4 is used as a material of cladding fuel rod of nuclear reactors. In this environment, it is submitted to different severe conditions of temperature and pressure. The objective of this work is to study the oxidation kinetics of zircaloy-4 in air by the X-ray diffraction technique. The experiments were realized in a “HTK1200” furnace installed as a sample holder in the diffractometer at different temperatures;25°C, 350°C, 500°C, 830°C and 1000°C. The results show that the monoclinic and the tetragonal phases are formed at 350°C temperature. The volume fraction of these phases increased with the temperature until 1000°C where the α phase disappears completely. For simulating the case of loss-of-coolant-accident (LOCA), we have done x-ray diffraction of Zry-4 samples water quenched at 1050°C with different ageing times at this temperature. At 10 seconds and more, there is an important evolution of monoclinic and tetragonal zirconias, which leads to the degradation of zircaloy-4 properties.

Measurement of integral diffraction coefficients of crystals on beamline 4B7 of Beijing Synchrotron Radiation Facility

Integral diffraction coefficients of the crystal are the essential data of a crystal spectrometer which is extensively used to measure quantitative x-ray spectra of high temperature plasmas in kilo-electron-volt region. An experimental method has been developed to measure the integral diffraction coefficients of crystals on beamline 4B7 of Beijing Synchrotron Radiation Facility. The integral diffraction coefficients of several crystals including polyethylene terephthalate （PET）, thallium acid phthalate （T1AP） and rubidium acid phthalate （RAP） crystals have been measured in the x-ray energy range 2100-5600 eV and compared with the calculations of the ＇Darwin Prins＇ and the ＇Mosaic＇ models. It is shown that the integral diffraction coefficients of these crystals are between the calculations of the ＇Darwin Prins＇ and the ＇Mosaic＇ models, but more close to the ＇Darwin Prins＇ model calculations.

Test of a High Throughput Detector on the X-ray Crystal Spectrometer of the EAST

An attempt was made to improve the spatio-temporal resolution of the tangen- tial X-ray crystal spectrometer （XCS） on the Experimental Advanced Superconducting Tokamak （EAST） by evaluating experimentally the applicability of a novel X-ray photon detection tech- nology for measuring the satellite spectra of Ar XVII with a high counting rate. High-resolution experimental data on the profiles of ion temperature and plasma rotation velocity facilitate the studies of the mechanisms underlining important physical phenomena, such as plasma heating, L-H transition and momentum transport. Based on silicon diode array and single-photon counting technology, a relatively small area （83.8 x 33.5 mm~） two-dimensional detector was successfully in- stalled and tested in the recent EAST campaign. X-ray photon counting rate higher than 20 MHz was observed for the first time, and high quality satellite spectra were recorded for ion temperature and plasma rotation measurement, indicating that the new technology is suitable for the next-step high-resolution XCS on EAST, and the deployment of a detector array with a much larger X-ray sensing area is planned for better plasma coverage.

Tb^(3+)-doped borosilicate glass scintillators for highresolution X-ray imaging

Scintillators are the vital component in X-ray perspective image technology that is applied in medical imaging,industrial nondestructive testing,and safety testing.But the high cost and small size of single-crystal commercialized scintillators limit their practical application.Here,a series of Tb^(3+)-doped borosilicate glass(BSG)scintillators with big production size,low cost,and high spatial resolution are designed and fabricated.The structural,photoluminescent,and scintillant properties are systematically investigated.Benefiting from excellent transmittance(87%at 600 nm),high interquantum efficiency(60.7%),and high X-ray excited luminescence(217%of Bi4Ge3O12),the optimal sample shows superhigh spatial resolution(exceeding 20 lp/mm).This research suggests that Tb^(3+)-doped BSG scintillators have potential applications in the static X-ray imaging field.

Combined use of fly ash and silica to prevent the long-term strength retrogression of oil well cement set and cured at HPHT conditions

The long-term strength retrogression of silica-enriched oil well cement poses a significant threat to wellbore integrity in deep and ultra-deep wells, which is a major obstacle for deep petroleum and geothermal energy development. Previous attempts to address this problem has been unsatisfactory because they can only reduce the strength decline rate. This study presents a new solution to this problem by incorporating fly ash to the traditional silica-cement systems. The influences of fly ash and silica on the strength retrogression behavior of oil well cement systems directly set and cured under the condition of 200°C and 50 MPa are investigated. Test results indicate that the slurries containing only silica or fly ash experience severe strength retrogression from 2 to 30 d curing, while the slurries containing both fly ash and silica experience strength enhancement from 2 to 90 d. The strength test results are corroborated by further evidences from permeability tests as well as microstructure analysis of set cement. Composition of set cement evaluated by quantitative X-ray diffraction analyses with partial or no known crystal structure(PONKCS) method and thermogravimetry analyses revealed that the conversion of amorphous C-(A)-S-H to crystalline phases is the primary cause of long-term strength retrogression.The addition of fly ash can reduce the initial amount of C-(A)-S-H in the set cement, and its combined use with silica can prevent the crystallization of C-(A)-S-H, which is believed to be the working mechanism of this new admixture in improving long-term strength stability of oil well cement systems.