Characterization of single-pulse photon energy and photon energy jitter at the Shanghai soft X-ray Free-Electron Laser

The X-ray free-electron laser(XFEL),a new X-ray light source,presents numerous opportunities for scientific research.Self-amplified spontaneous emission(SASE)is one generation mode of XFEL in which each pulse is unique.In this paper,we propose a pinhole diffraction method to accurately determine the XFEL photon energy,pulses'photon energy jitter,and sample-to-detector distance for soft X-ray.This method was verified at Shanghai soft X-ray Free-Electron Laser(SXFEL).The measured average photon energy was 406.5 eV,with a photon energy jitter(root-mean-square)of 1.39 eV,and the sample-to-detector distance was calculated to be 16.61 cm.

State-of-the-Art Review of High-Throughput Statistical Spatial-Mapping Characterization Technology and Its Applications

Macroscopic materials are heterogeneous,multi-elementary,and complex.No material is homogeneous or isotropic at a certain small scale.Parts of the material that differ from one another can be termed"natural chips."At different spots on the material,the composition,structure,and properties vary slightly,and the combination of these slight differences establishes the overall material performance.This article presents a state-of-the-art review of research and applications of high-throughput statistical spatialmapping characterization technology based on the intrinsic heterogeneity within materials.Highthroughput statistical spatial-mapping uses a series of rapid characterization techniques for analysis from the macroscopic to the microscopic scale.Datasets of composition,structure,and properties at each location are obtained rapidly for practical sample sizes.Accurate positional coordinate information and references to a point-to-point correspondence are used to set up a database that contains spatialmapping lattices.Based on material research and development design requirements,dataset spatialmapping within required target intervals is selected from the database.Statistical analysis can be used to select a suitable design that better meets the targeted requirements.After repeated verification,genetic units that reflect the material properties are determined.By optimizing process parameters,the assembly of these genetic unit(s)is verified at the mesoscale,and quantitative correlations are established between the microscale,mesoscale,macroscale,practical sample,across-the-scale span composition,structure,and properties.The high-throughput statistical spatial-mapping characterization technology has been applied to numerous material systems,such as steels,superalloys,galvanization,and ferrosilicon alloys.This approach has guided the composition and the process optimization of various materials.

In situ characterizations of solid-solid interfaces in solid-state batteries using synchrotron X-ray techniques

The solid-solid electrode-electrolyte interface represents an important component in solid-state batteries(SSBs),as ionic diffusion,reaction,transformation,and restructuring could all take place.As these processes strongly influence the battery performance,studying the evolution of the solid-solid interfaces,particularly in situ during battery operation,can provide insights to establish the structure-property relationship for SSBs.Synchrotron X-ray techniques,owing to their unique penetration power and diverse approaches,are suitable to investigate the buried interfaces and examine structural,compositional,and morphological changes.In this review,we will discuss various surface-sensitive synchrotron-based scattering,spectroscopy,and imaging methods for the in situ characterization of solid-solid interfaces and how this information can be correlated to the electrochemical properties of SSBs.The goal is to overview the advantages and disadvantages of each technique by highlighting representative examples,so that similar strategies can be applied by battery researchers and beyond to study similar solid-solid interface systems.

Combinatorial synthesis and high-throughput characterization of copper-oxide superconductors

Fast synthesis and screening of materials are vital to the advance of materials science and are an essential component of the Materials Genome Initiative. Here we use copper-oxide superconductors as an example to demonstrate the power of integrating combinatorial molecular beam epitaxy synthesis with high-throughput electric transport measurements. Leveraging this method, we have generated a phase diagram with more than 800 compositions in order to unravel the doping dependence of interface superconductivity. In another application of the same method, we have studied the superconductorto-insulator quantum phase transition with unprecedented accuracy in tuning the chemical doping level.

Combinatorial Synthesis and High-Throughput Characterization of Microstructure and Phase Transformation in Ni-Ti-Cu-V Quaternary Thin-Film Library

Ni-Ti-based shape memory alloys(SMAs)have found widespread use in the last 70 years,but improving their functional stability remains a key quest for more robust and advanced applications.Named for their ability to retain their processed shape as a result of a reversible martensitic transformation,SMAs are highly sensitive to compositional variations.Alloying with ternary and quaternary elements to finetune the lattice parameters and the thermal hysteresis of an SMA,therefore,becomes a challenge in materials exploration.Combinatorial materials science allows streamlining of the synthesis process and data management from multiple characterization techniques.In this study,a composition spread of Ni-Ti-Cu-V thin-film library was synthesized by magnetron co-sputtering on a thermally oxidized Si wafer.Composition-dependent phase transformation temperature and microstructure were investigated and determined using high-throughput wavelength dispersive spectroscopy,synchrotron X-ray diffraction,and temperature-dependent resistance measurements.Of the 177 compositions in the materials library,32 were observed to have shape memory effect,of which five had zero or near-zero thermal hysteresis.These compositions provide flexibility in the operating temperature regimes that they can be used in.A phase map for the quaternary system and correlations of functional properties are discussed w让h respect to the local microstructure and composition of the thin-film library.

X-ray Computed Tomography Characterization of 3D Tufted Twill Textile Composite for Aerostructures

Damage assessments in three dimensional (3D) textile composites subjected to mechanical loading can be performed by non-destructive and destructive techniques.This paper applies the two techniques to investigate the fracture behavior of 3D tufted textile composites.X-ray computed tomography as a non-destructive evaluation method is appropriate to detect damage locations and identify their progression in 3D textile composites.Destructive methods such as sectioning toward observing damage provide valuable information about damage patterns.The results of this research could be utilized to evaluate the initial cause of rupture in 3D tufted composites used in aerospace structures and analyze fracture modes and damage progression.

X-ray Diffraction and Raman Spectroscopy Characterization of Isotropic Pyrocarbon Obtained by Hot Wall Chemical Vapor Deposition

Varying the flow rate of natural gas from 50 to 80 to 120 l/h, isotropic pyrocarbon produced by hot wall chemical vapor deposition at 1000 ℃ were examined by X-ray diffraction and Raman spectroscopy. The X-ray data were evaluated by Scherrer equation, and the intensity ratio of D to G band derived from Raman data was used to evaluate the lateral extension of isotropic pyrocarbon. The experimental results show that the d002-spacing of isotropic pyroearbon decreases from 0.3499 nm to 0.3451 nm, while the stack height increases from 6.5 to 8.4 nm with the increase of flow rate of natural gas. The intensity ratio of D to G band and lateral extension of isotropie pyrocarbon increases with natural gas flow rate increasing. After heat treatment, all the crystallite parameters （stack height, lateral extension, and d002-spacing） decrease, indicating the improvement of the arrangement of the basic structural units of isotropic pyrocarbon.

Detailed characterization of polycapillary focusing x-ray lenses by a charge-coupled device detector and a pinhole

A method to measure the detailed performance of polycapillary x-ray optics by a pinhole and charge coupled device(CCD)detector was proposed in this study.The pinhole was located between the x-ray source and the polycapillary x-ray optics to determine the illuminating region of the incident x-ray beam on the input side of the optics.The CCD detector placed downstream of the polycapillary x-ray optics ensured that the incident x-ray beam controlled by the pinhole irradiated a specific region of the input surface of the optics.The intensity of the output beam of the polycapillary x-ray optics was obtained from the far-field image of the output beam of the optics captured by CCD detector.As an application example,the focal spot size,gain in power density,transmission efficiency,and beam divergence of different parts of a polycapillary focusing x-ray lenses(PFXRL)were measured by a pinhole and CCD detector.Three pinholes with diameters of 500,1000,and 2000μm were used to adjust the diameter of the incident x-ray beam illuminating the PFXRL from 500μm to the entire surface of the input side of the PFXRL.The focal spot size of the PFXRL,gain in power density,transmission efficiency,and beam divergence ranged from 27.1μm to 34.6μm,400 to 3460,26.70%to 5.38%,and 16.8 mrad to 84.86 mrad,respectively.

IN SITU X-RAY DIFFRACTION CHARACTERIZATION OF SILVER/SOLUTION INTERFACES

In situ x-ray diffraction electrochemical method is used to study the activation of silver electrode in KCl solution and UPD lead on silver electrode surface. We found that the activation makes the silver crystal thicker in (111), and the arrangement of water molecules on the silver electrode surface with UPD lead is partially ordered.

Chemical Characterization of Auriferous Ores from the Brazilian State of Paraiba

One of the most important problems facing the gold industry is that the placer and free milling gold ores are almost terminating. Hence, the use of refractory ores has been increased during the recent years. In general, gold refractory ores occurs in various types of deposits associated with a range of minerals. Among the refractory ores, the sulfide type is the most common. The methodology employed in the mining process depends on the mode of occurrence of the ore and on the particle size, shape and degree of purity of the auriferous species. We have undertaken a mineralogical investigation of a representative sample of a complex gold mining ore collected in the municipality of Princesa Isabel, Paraiba, Brazil, using X-ray fluorescence spectrometry, X-ray diffractometry, infrared spectroscopy, inductively coupled plasma-atomic emission spectrometry and the Fire Assay. The results showed that the arsenic content of the ore was closely related to the gold content, and that the occurrence of “invisible gold” was associated primarily with pyrite and secondarily with arsenopyrite. The sulfur content of the ore was directly related to its refractoriness. It is concluded that gold mineralization in the study area is mainly of the gold-quartz-sulfide veins (lode gold), while the gold found in the mini-fractures of the deposits is probably associated with the hydrothermal processes that occurred in the region.

High-Throughput Powder Diffraction Using White X-Ray Beam and a Simulated Energy-Dispersive Array Detector

High-throughput powder X-ray diffraction(XRD)with white X-ray beam and an energy-dispersive detector array is demonstrated in this work on a CeO;powder sample on a bending magnet synchrotron beamline at the Shanghai Synchrotron Radiation Facility(SSRF),using a simulated energy-dispersive array detector consisting of a spatially scanning silicon-drift detector(SDD).Careful analysis and corrections are applied to account for various experimental hardware-related and diffraction angle-related factors.The resulting diffraction patterns show that the relative strength between different diffraction peaks from energy-dispersive XRD(EDXRD)spectra is consistent with that from angle-resolved XRD(ARXRD),which is necessary for analyzing crystal structures for unknown samples.The X-ray fluorescence(XRF)signal is collected simultaneously.XRF counts from all pixels are integrated directly by energy,while the diffraction spectra are integrated by d-spacing,resulting in a much improved peak strength and signal-to-noise(S/N)ratio for the array detector.In comparison with ARXRD,the diffraction signal generated by a white X-ray beam over monochromic light under the experimental conditions is about 104 times higher.The full width at half maximum(FWHM)of the peaks in q-space is found to be dependent on the energy resolution of the detector,the angle span of the detector,and the diffraction angle.It is possible for EDXRD to achieve the same or even smaller FWHM as ARXRD under the energy resolution of the current detector if the experimental parameters are properly chosen.

Non Destructive 3D, 4D Microscopy and Mineral Phase Characterization in Industrial Minerals, Composites to Construction Materials

Conventional electron and optical microscopy techniques require the sample to be sectioned, polished or etched to expose the internal surfaces for imaging. However, such sample preparation techniques have traditionally prevented the observation of the same sample over time, under realistic three-dimensional geometries and in an environment representative of real-world operating conditions. X-ray microscopy (XRM) is a rapidly emerging technique that enables non-destructive evaluation of buried structures within hard to soft materials in 3D, requiring little to no sample preparation. Furthermore in situ and 4D quantification of microstructural evolution under controlled environment as a function of time, temperature, chemistry or stress can be done repeatable on the same sample, using practical specimen sizes ranging from tens of microns to several cm diameter, with achievable imaging resolution from submicron to 50 nm. Many of these studies were reported using XRM in synchrotron beamlines. These include crack propagation on composite and construction materials; corrosion studies; microstructural changes during the setting of cement; flow studies within porous media to mention but a few.

Comparative Structural and Spectroscopic Characterization of M^ILn^IIITiO4 Ion-exchanged Phases,with M^I： Na, H, K

In this paper, a comparative study of the XRD characterization and FTIR spectroscopic behavior of some M^ILn^IIITiO4 phases with M^I： Na, H, K and Ln^III, the trivalent lanthanides elements： Sm, Eu, Er and Yb is reported. The H and K- oxides were obtained by ion-exchange from NaLnTiO4. These ternary oxides belong to the K2NiF4 structural type, with the M^I and Ln^III cations distributed in an ordered way on the K-sub lattice. The FTIR spectra of the materials were analyzed by comparison with structurally related materials. A close relationship with the parent NaLnTiO4 was found.

Phosphorus Based Ceramics for Positive Electrode Synthesis and Characterization

Historically, the LiCoO2 is the most used as active material for battery positive electrode because of its great potential (3.7 - 4.2 V), its interesting specific capacity (150 mA·h·g-1) and its excellent life cycle [1] 08D0C9EA79F9BACE118C8200AA004BA90B02000000080000000E0000005F005200650066003300390038003500370036003700340032000000 . However, its toxicity, the cobalt cost and its structural instability oriented research towards new materials more stable that can replace it. In another context, hybrid, electrical vehicles and communication (computers and mobile phones...) have increased the scientific and technological research for new materials capable of storing and return energy through a system called accumulator. And research has identified the phosphate olivine structure as the most prolific ceramic material for positive electrode. LiFePO4 is a promising cathode material for Lithium-ion batteries. It provides high thermal stability and is synthesized using low cost materials. Unfortunately LiFePO4 suffers from a low electrical conductivity, which is harmful to its electrochemical performance. Decreasing the particle size, coating the particles with carbon or doping with metal atoms can increase the conductivity of the material. In this paper, we present the synthesis, physico-chemical and electrical characterization of lithium and iron doped Al-phosphorrus-based ceramic. The NPK Fertiliser was used as Al and phosphorus precursors. The powder XRD spectrum shows a possible presence of LiFePO4 and Fe2(PO)3 in theheterostrcture. An important quantity of Al is found by EDX spectra which supposed that the most important based atom is Aluminum and not Phosphorus. This can explain the increase of the conductivity value 102 times more important than those found in the literature for LiFePO4.

Synthesis, Growth, Crystal Structure and Characterization of the o-Toluidinium Picrate

A new organic charge transfer molecular complex salt of o-toluidinium picrate (OTP) was synthesised and the single crystals were grown by the slow solvent evaporation solution growth technique using methanol as a solvent at room temperature. Formation of the new crystal has been confirmed by single crystal X-ray diffraction (XRD) and NMR spectroscopic techniques. The crystal structure determined by single crystal X-ray diffraction indicates that both the cation and the anion are interlinked to each other by three types of intermolecular hydrogen bonds, namely N(4)-H(4A)···O(7), N(4)-H(4B)···O(5) and N(4)-H(4C)···O(7). The title compound (OTP) crystallizes in monoclinic crystal system with the centrosymmetric space group P21/c. Fourier transform infrared (FT IR) spectral analysis was used to confirm the presence of various functional groups in the grown crystal. The optical properties were analyzed by the UV-Vis-NIR and fluorescence emission studies.

In situ studies of energy-related electrochemical reactions using Raman and X-ray absorption spectroscopy

Electrochemical energy conversion technologies involving processes such as water splitting and O_(2)/CO_(2) reduction,provide promising solutions for addressing global energy scarcity and minimizing adverse environmental impact.However,due to a lack of an in-depth understanding of the reaction mechanisms and the nature of the active sites,further advancement of these techniques has been limited by the development of efficient and robust catalysts.Therefore,in situ characterization of these electrocatalytic processes under working conditions is essential.In this review,recent applications of in situ Raman spectroscopy and X-ray absorption spectroscopy for various nano-and single-atom catalysts in energy-related reactions are summarized.Notable cases are highlighted,including the capture of oxygen-containing intermediate species formed during the reduction of oxygen and oxidation of hydrogen,and the detection of catalyst structural transformations occurring with the change in potential during the evolution of oxygen and reduction of CO_(2).Finally,the challenges and outlook for advancing in situ spectroscopic technologies to gain a deeper fundamental understanding of these energy-related electrocatalytic processes are discussed.

BL19U2:Small-angle X-ray scattering beamline for biological macromolecules in solution at SSRF

The BL19U2 at the Shanghai Synchrotron Radiation Facility is a small-angle X-ray scattering beamline dedicated to structural studies pertaining to biological macromolecules in solution.The beamline has been officially opened to users in March 2015,and since then,a series of technological innovations has been developed to optimize beamline performance,thereby significantly improving the data collection efficiency and broadening the application scope of biological small-angle X-ray scattering.BL19U2 is ideal for the high-throughput screening of weakly scattered proteins,protein assemblies,nucleic acids,inorganic nanomaterials,and organic drug molecules.This paper describes the design and overview of the BL19U2 beamline.Versatile sample environments at the experimental station and some recent scientific highlights are presented.

Introducing a Novel Approach for Oil-Oil Correlation based on Asphaltene Structure: X-ray Diffraction

Asphaltenes have always been an attractive subject for researchers.However,the application of this fraction of the geochemical field has only been studied in a limited way.In other words,despite many studies on asphaltene structure,the application of asphaltene structures in organic geochemistry has not so far been assessed.Oil-oil correlation is a wellknown concept in geochemical studies and plays a vital role in basin modeling and the reconstruction of the burial history of basin sediments,as well as accurate characterization of the relevant petroleum system.This study aims to propose the Xray diffraction(XRD)technique as a novel method for oil-oil correlation and investigate its reliability and accuracy for different crude oils.To this end,13 crude oil samples from the Iranian sector of the Persian Gulf region,which had previously been correlated by traditional geochemical tools such as biomarker ratios and isotope values,in four distinct genetic groups,were selected and their asphaltene fractions analyzed by two prevalent methods of XRD and Fouriertransform infrared spectroscopy(FTIR).For oil-oil correlation assessment,various cross-plots,as well as principal component analysis(PCA),were conducted,based on the structural parameters of the studied asphaltenes.The results indicate that asphaltene structural parameters can also be used for oil-oil correlation purposes,their results being completely in accord with the previous classifications.The average values of distance between saturated portions(d_(r))and the distance between two aromatic layers(d_(m))of asphaltene molecules belonging to the studied oil samples are 4.69Aand 3.54A,respectively.Furthermore,the average diameter of the aromatic sheets(L_(a)),the height of the clusters(L_(c)),the number of carbons per aromatic unit(C_(au)),the number of aromatic rings per layer(R_(a)),the number of sheets in the cluster(M_(e))and aromaticity(f_(a))values of these asphaltene samples are 10.09A,34.04A,17.42A,3.78A,10.61Aand 0.26A,respectively.The results of XRD parameters indicate that plots of dr vs.d_(m),d_(r) vs.M_(e),d_(r) vs.f_(a),d_(m) vs.L_(c),L_(c) vs.L_(a),and f_(a) vs.L_(a) perform appropriately for distinguishing genetic groups.A comparison between XRD and FTIR results indicated that the XRD method is more accurate for this purpose.In addition,decision tree classification,one of the most efficacious approaches of machine learning,was employed for the geochemical groups of this study for the first time.This tree,which was constructed using XRD data,can distinguish genetic groups accurately and can also determine the characteristics of each geochemical group.In conclusion,the obtaining of structural parameters for asphaltene by the XRD technique is a novel,precise and inexpensive method,which can be deployed as a new approach for oil-oil correlation goals.The findings of this study can help in the prompt determination of genetic groups as a screening method and can also be useful for assessing oil samples affected by secondary processes.

Time-resolved K-shell x-ray spectra of nanosecond laser-produced titanium tracer in gold plasmas

A study of a nanosecond laser irradiation on the titanium-layer-buried gold planar target is presented. The timeresolved x-ray emission spectra of titanium tracer are measured by a streaked crystal spectrometer. By comparing the simulated spectra obtained by using the FLYCHK code with the measured titanium spectra, the temporal plasma states, i.e.,the electron temperatures and densities, are deduced. To evaluate the feasibility of using the method for the characterization of Au plasma states, the deduced plasma states from the measured titanium spectra are compared with the Multi-1D hydrodynamic simulations of laser-produced Au plasmas. By comparing the measured and simulated results, an overall agreement for the electron temperatures is found, whereas there are deviations in the electron densities. The experiment–theory discrepancy may suggest that the plasma state could not be well reproduced by the Multi-1D hydrodynamic simulation, in which the radial gradient is not taken into account. Further investigations on the spectral characterization and hydrodynamic simulations of the plasma states are needed. All the measured and FLYCHK simulated spectra are given in this paper as datasets. The datasets are openly available at http://www.doi.org/10.57760/sciencedb.j00113.00032.

Synthesis, Spectroscopy and X-Ray Crystal Structure of 9-Methyl-3-Thiophen-2-Yl-Thieno [3, 2-e] [1, 2, 4] Triazolo [4, 3-c] Pyrimidine-8-Carboxylic Acid Ethyl Ester

The Preparation of 9-Methyl-3-thiophen-2-yl-thieno [3, 2-e] [1, 2, 4] triazolo [4, 3-c] pyrimi-dine-8-carboxylic acid ethyl ester is described. Elemental analysis, IR spectrum, 1H NMR, 13C NMR and X-ray crystal structure analyses were carried out to determine the composition and molecular structure of the title compound. There are two independent molecules in the asymmetric unit exhibiting intermolecular C-H…N, C-H…O interactions with additional π-π interaction that further helps in stabilizing the supramolecular structure. The results showed that the proposed method for synthesis is simple, precise and accurate which was further confirmed by crystal structure analysis.