Development of in situ characterization techniques in molecular beam epitaxy

Ex situ characterization techniques in molecular beam epitaxy(MBE)have inherent limitations,such as being prone to sample contamination and unstable surfaces during sample transfer from the MBE chamber.In recent years,the need for improved accuracy and reliability in measurement has driven the increasing adoption of in situ characterization techniques.These techniques,such as reflection high-energy electron diffraction,scanning tunneling microscopy,and X-ray photoelectron spectroscopy,allow direct observation of film growth processes in real time without exposing the sample to air,hence offering insights into the growth mechanisms of epitaxial films with controlled properties.By combining multiple in situ characterization techniques with MBE,researchers can better understand film growth processes,realizing novel materials with customized properties and extensive applications.This review aims to overview the benefits and achievements of in situ characterization techniques in MBE and their applications for material science research.In addition,through further analysis of these techniques regarding their challenges and potential solutions,particularly highlighting the assistance of machine learning to correlate in situ characterization with other material information,we hope to provide a guideline for future efforts in the development of novel monitoring and control schemes for MBE growth processes with improved material properties.

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.

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.

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.

Development of a high-repetition-rate lumped-inductance kicker magnet prototype for the beam switchyard of SHINE

The Shanghai high-repetition-rate X-ray free-electron laser and extreme light facility(SHINE)operates at a maximum repetition rate of 1 MHz.Kicker magnets are key components that distribute electron bunches into three different undulator lines in a bunch-by-bunch mode.The kicker field width must be less than the time interval between bunches.A lumpedinductance kicker prototype was developed using a vacuum chamber with a single-turn coil.The full magnetic field strength was 0.005 T.This paper presents the requirements,design considerations,design parameters,magnetic field calculations,and measurements of the kicker magnets.The relevant experimental results are also presented.The pulse width of the magnetic field was approximately 600 ns,and the maximum operation repetition rate was 1 MHz.The developed kicker satisfies the requirements for the SHINE project.Finally,numerous recommendations for the future optimization of kicker magnets are provided.

Scintillation characterization for multiple incoherent uplink Gaussian beams

By means of numerical simulations, we analyze the scintillation characterization for multiple incoherent uplink Gaussian beams under weak fluctuations cases. Because truly independent beams are difficult to create, we present a more general but approximate model for the multiple of beams traveling through partially correlated paths. This model compares with wave-optics simulations and highlights the reduced correlation coefficient as the beam separation is increased. The scintillation index of three and six incoherent uplink Gaussian beams is also induced. The result shows that the scintillation index decreases with the increase of beams amount and beam separation. When the beams amount and strength of atmospheric turbulence are fixed, the reduction of scintillation index is affected by the ratio of beams separation and the Fried length. The corresponding ohvsical mechanisms for the results are discussed.

Growth and Characterization of AlInAs on InP Substrate by Molecular Beam Epitaxy

AlxIn1-xAs with 0.47&lex&le0.62 onto (100) oriented InP substrate was grown by molecular beam epitaxy (MBE) and characterized with X-ray double crystal diffraction, low temperature photoluminescence and an electron probe. Results show their high qualities. Strain and residual stress were studied in detail.

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.

Beam and image experiment of beam deflection electron gun for distributed X-ray sources

Distributed X-ray sources comprise a single vacuum chamber containing multiple X-ray sources that are triggered and emit X-rays at a specific time and location. This process facilitates an application for innovative system concepts in X-ray and computer tomography. This paper proposes a novel electron beam focusing, shaping,and deflection electron gun for distributed X-ray sources.The electron gun uses a dispenser cathode as an electron emitter, a mesh grid to control emission current, and two electrostatic lenses for beam shaping, focusing, and deflection. Novel focusing and deflecting electrodes were designed to increase the number of focal spots in the distributed source. Two identical half-rectangle opening electrodes are controlled by adjusting the potential of the two electrodes to control the electron beam trajectory, and then, multifocal spots are obtained on the anode target. The electron gun can increase the spatial density of the distributed X-ray sources, thereby improving the image quality. The beam experimental results show that the focal spot sizes of the deflected(deflected amplitude 10.5 mm)and non-deflected electron beams at full width at half maximum are 0.80 mm 90.50 mm and 0.55 mm 90.40 mm, respectively(anode voltage 160 kV; beam current 30 mA). The imaging experimental results demonstrate the excellent spatial resolution and time resolution of an imaging system built with the sources, which has an excellent imaging effect on a field-programmable gate array chip and a rotating metal disk.

Ultrasonic characterization of modified Cr_2O_3 coatings by reflection coefficient spectroscopy

Pores,microcracks and density of plasma sprayed Cr2O3 coatings before and after high-intensity pulsed ion beam(HIPIB) irradiation were investigated using the ultrasonic reflection coefficient spectroscopy(URCS).The URCS was analyzed based on an acoustic transmission model for the multi-layered structure.The longitudinal velocity in the coatings was calculated from the experimental URCS,and the attenuation coefficient expression was deduced by comparing the experimental and numerical fitting amplitude spectral lines.The longitudinal velocity of as-sprayed Cr2O3 coating is 2 002 m/s,and increases to 2 099 and 2 148 m/s after being irradiated by HIPIB with 1 and 5 shots.Correspondingly,the factor A changes from 0.046 to 0.026 and 0.020 and n from 1.702 to 1.658 and 1.649 in the attenuation coefficient expression of α=Af n.It is observed that the surface morphology of Cr2O3 coatings changes from rough and porous to smooth and uniform with the increase of shot number,which accords with the ultrasonic analyses reasonably.The URCS seems to provide a convenient and nondestructive method to characterize surface modification of the plasma sprayed coatings.

Nanofabrication of 50 nm zone plates through e-beam lithography with local proximity effect correction for x-ray imaging

High resolution Fresnel zone plates for nanoscale three-dimensional imaging of materials by both soft and hard x-rays are increasingly needed by the broad applications in nanoscience and nanotechnology.When the outmost zone-width is shrinking down to 50 nm or even below,patterning the zone plates with high aspect ratio by electron beam lithography still remains a challenge because of the proximity effect.The uneven charge distribution in the exposed resist is still frequently observed even after standard proximity effect correction(PEC),because of the large variety in the line width.This work develops a new strategy,nicknamed as local proximity effect correction(LPEC),efficiently modifying the deposited energy over the whole zone plate on the top of proximity effect correction.By this way,50 nm zone plates with the aspect ratio from 4:1 up to 15:1 and the duty cycle close to 0.5 have been fabricated.Their imaging capability in soft(1.3 keV)and hard(9 keV)x-ray,respectively,has been demonstrated in Shanghai Synchrotron Radiation Facility(SSRF)with the resolution of 50 nm.The local proximity effect correction developed in this work should also be generally significant for the generation of zone plates with high resolutions beyond 50 nm.

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.

Energy band alignment at Cu2O/ZnO heterojunctions characterized by in situ x-ray photoelectron spectroscopy

With the increasing interest in Cu2O-based devices for photovoltaic applications,the energy band alignment at the Cu2O/ZnO heterojunction has received more and more attention.In this work,a high-quality Cu2O/ZnO heterojunction is fabricated on a c-Al2 O3 substrate by laser-molecular beam epitaxy,and the energy band alignment is determined by x-ray photoelectron spectroscopy.The valence band of ZnO is found to be 1.97 eV below that of Cu2O.A type-II band alignment exists at the Cu2O/ZnO heterojunction with a resulting conduction band offset of 0.77 eV,which is especially favorable for enhancing the efficiency of Cu2O/ZnO solar cells.

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.

Carbon-Ion Beams Efficiently Induce Cell Killing in X-Ray Resistant Human Squamous Tongue Cancer Cells

In order to see whether carbon ion (C-ion) beams have a biological advantage over X-rays, studies were designed to examine the effects of C-ion beams on radiosensitivity in X-ray resistant cells. Clinically relevant X-ray resistant SAS-R cells derived from human tongue cancer SAS cells were used. The cells were exposed to X-rays or Spread-Out Bragg peak (SOBP) beam C-ions. Cell survival was measured using a modified high-density survival assay. Cell survival signaling and cell death signaling were analyzed using flow cytometry. The cells were labeled with putative cancer stem cell markers such as CD44 and CD326. SAS-R cells were 1.6 times more radioresistant than SAS cells after exposure to X-rays. Cell survival was similar in each cell line after exposure to C-ion beams. SAS-R cells displayed enhanced cell survival signaling when compared to SAS cells under normal conditions. On the other hand, the phosphorylation of AKT-related proteins decreased and polycaspase activities were enhanced when cells were irradiated with C-ion beams in both cell lines. More CD44 and CD326 positive cells were seen in SAS-R cells than in SAS cells. Moreover, the marker positive cell numbers significantly decreased after exposure to C-ion beams when compared to X-rays at iso-survival doses in SAS-R cells. C-ion beams efficiently induced cell killing in X-ray resistant cells which displayed activated cell survival signaling and contained more numerous cancer stem-like cells.

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.