Online in situ x-ray diffraction setup for structural modification studies during swift heavy ion irradiation

The high energy density of electronic excitations due to the impact of swift heavy ions can induce structural modifications in materials. We present an x-ray diffractometer called ALIX ("Analyse en Ligne sur IRRSUD par diffraction de rayons X"), which has been set up at the low-energy beamline (IRRadiation SUD - IRRSUD) of the Grand Acce?le?rateur National d'Ions Lourds facility, to allow the study of structural modification kinetics as a function of the ion fluence. The x-ray setup has been modified and optimized to enable irradiation by swift heavy ions simultaneously to x-ray pattern recording. We present the capability of ALIX to perform simultaneous irradiation-diffraction by using energy discrimination between x-rays from diffraction and from ion-target interaction. To illustrate its potential, results of sequential or simultaneous irradiation-diffraction are presented in this article to show radiation effects on the structural properties of ceramics. Phase transition kinetics have been studied during xenon ion irradiation of polycrystalline MgO and SrTiO(3). We have observed that MgO oxide is radiation-resistant to high electronic excitations, contrary to the high sensitivity of SrTiO(3), which exhibits transition from the crystalline to the amorphous state during irradiation. By interpreting the amorphization kinetics of SrTiO(3), defect overlapping models are discussed as well as latent track characteristics. Together with a transmission electron microscopy study, we conclude that a single impact model describes the phase transition mechanism.     

外加电场制备CdS纳米线阵列、纳米带和纳米管

在外加电场的条件下利用物理热蒸发法成功制备出CdS纳米线阵列、纳米带和纳米管，纳米线阵列沿平行于电场方向生长。借助SEM、EDX和TEM以及XRD，研究了外加电场对CdS纳米线生长的影响。结果表明：外加电场大大促进了CdS纳米线定向排列生长；但是，低温区获得的CdS纳米带和纳米管没有任何方向性。     

Density measurements of noncrystalline materials at high pressure with diamond anvil cell

We describe an x-ray absorption method for in situ density measurement of non-crystalline materials in the diamond anvil cell using a monochromatic synchrotron x-ray microbeam. Sample thickness, which is indispensable in the absorption method, can be determined precisely by extrapolating the thickness profile of the gasket obtained by x-ray absorption and diffraction measurements. Diamond deformation across the sample chamber becomes noticeable at high pressures above 10 GPa, which can be monitored with a precision better than 1%, as demonstrated by measurements on crystalline Ag. We have applied the developed method to measure densities of the classic network-forming GeO(2) glass in octahedral form at pressures up to 56 GPa. The fit to the pressure-volume data with the Birch-Murnaghan equation from 13 to 56 GPa gives parameters of V(0)=23.2+/-0.4 cm(3)mol and K=35.8+/-3.0 GPa, assuming that K(')=4. This method could be applicable for in situ determination of the density of liquids and other noncrystalline materials using a diamond anvil cell up to ultrahigh pressures.     

The effect of exit beam phase aberrations on parallel beam coherent x-ray reconstructions

Diffraction artifacts from imperfect x-ray windows near the sample are an important consideration in the design of coherent x-ray diffraction measurements. In this study, we used simulated and experimental diffraction patterns in two and three dimensions to explore the effect of phase imperfections in a beryllium window (such as a void or inclusion) on the convergence behavior of phasing algorithms and on the ultimate reconstruction. A predictive relationship between beam wavelength, sample size, and window position was derived to explain the dependence of reconstruction quality on beryllium defect size. Defects corresponding to this prediction cause the most damage to the sample exit wave and induce signature error oscillations during phasing that can be used as a fingerprint of experimental x-ray window artifacts. The relationship between x-ray window imperfection size and coherent x-ray diffractive imaging reconstruction quality explored in this work can play an important role in designing high-resolution in situ coherent imaging instrumentation and will help interpret the phasing behavior of coherent diffraction measured in these in situ environments.     

Rapid qualitative phase analysis in highly textured thin films by x-ray diffraction

Phase analysis of highly out-of-plane textured specimens using x-ray diffraction is usually complicated due to the disappearance of most of the x-ray peaks in a common theta/2 theta diffraction geometry. In this paper, we propose a technique, where powderlike spectra of textured samples are obtained by multiaxial x-ray diffraction scans. This technique is a simple, yet powerful method which allows for significant improvement in thin film characterization and provides several types of information about the samples, such as the rapid qualitative identification of phases using common powder x-ray diffraction spectra databases, texture distribution, and quantitative residual stress analysis.     

Absolute x-ray energy calibration over a wide energy range using a diffraction-based iterative method

In this paper, we report a method of precise and fast absolute x-ray energy calibration over a wide energy range using an iterative x-ray diffraction based method. Although accurate x-ray energy calibration is indispensable for x-ray energy-sensitive scattering and diffraction experiments, there is still a lack of effective methods to precisely calibrate energy over a wide range, especially when normal transmission monitoring is not an option and complicated micro-focusing optics are fixed in place. It is found that by using an iterative algorithm the x-ray energy is only tied to the relative offset of sample-to-detector distance, which can be readily varied with high precision of the order of 10(-5) -10(-6) spatial resolution using gauge blocks. Even starting with arbitrary initial values of 0.1 A?, 0.3 A?, and 0.4 A?, the iteration process converges to a value within 3.5 eV for 31.122 keV x-rays after three iterations. Different common diffraction standards CeO(2), Au, and Si show an energy deviation of 14 eV. As an application, the proposed method has been applied to determine the energy-sensitive first sharp diffraction peak of network forming GeO(2) glass at high pressure, exhibiting a distinct behavior in the pressure range of 2-4 GPa. Another application presented is pair distribution function measurement using calibrated high-energy x-rays at 82.273 keV. Unlike the traditional x-ray absorption-based calibration method, the proposed approach does not rely on any edges of specific elements, and is applicable to the hard x-ray region where no appropriate absorption edge is available.     

Laser powered heating stage in a scanning electron microscope for microstructural investigations at elevated temperatures

A laser powered heating stage designed for application in high vacuum environment of a scanning electron microscope (SEM) is presented. It was developed to observe and characterize microstructural changes in crystalline materials at elevated temperatures up to 1000 degrees C. The approach utilizes the power output of a commercial infrared diode laser in order to heat up specimens without interference with the electronic system of the SEM. The heating stage can be used in combination with any standard characterization technique applicable for SEMs--electron backscatter diffraction, orientation contrast imaging, x-ray energy dispersive spectrometry, etc. The results of test measurements are presented.     

A laboratory based system for laue micro x-ray diffraction

A laboratory diffraction system capable of illuminating individual grains in a polycrystalline matrix is described. Using a microfocus x-ray source equipped with a tungsten anode and prefigured monocapillary optic, a micro-x-ray diffraction system with a 10 microm beam was developed. The beam profile generated by the ellipsoidal capillary was determined using the "knife edge" approach. Measurement of the capillary performance, indicated a beam divergence of 14 mrad and a useable energy bandpass from 5.5 to 19 keV. Utilizing the polychromatic nature of the incident x-ray beam and application of the Laue indexing software package X-Ray Micro-Diffraction Analysis Software, the orientation and deviatoric strain of single grains in a polycrystalline material can be studied. To highlight the system potential the grain orientation and strain distribution of individual grains in a polycrystalline magnesium alloy (Mg 0.2 wt % Nd) was mapped before and after tensile loading. A basal (0002) orientation was identified in the as-rolled annealed alloy; after tensile loading some grains were observed to undergo an orientation change of 30 degrees with respect to (0002). The applied uniaxial load was measured as an increase in the deviatoric tensile strain parallel to the load axis.     

Synchrotron-based ultrafast x-ray diffraction at high repetition rates

We present a setup for ultrafast x-ray diffraction (UXRD) based at the storage ring BESSY II, in particular, a pump laser that excites the sample using 250 fs laser-pulses at repetition rates ranging from 208 kHz to 1.25 MHz. We discuss issues connected to the high heat-load and spatio-temporal alignment strategies in the context of a UXRD experiment at high repetition rates. The spatial overlap between laser pump and x-ray probe pulse is obtained with 10 μm precision and transient lattice changes can be recorded with an accuracy of δa/a(0) = 10(-6). We also compare time-resolved x-ray diffraction signals from a laser excited LSMO/STO superlattice with phonon dynamics simulations. From the analysis we determine the x-ray pulse duration to 120 ps in standard operation mode and below 10 ps in low-α mode.     

Development of a laboratory EXAFS facility

The EXAFS technique is a powerful new structural tool, particularly useful for studies of disordered or otherwise complex materials for which x-ray diffraction techniques are difficult or unfeasible. At the present time, most EXAFS experiments are carried out at a synchrotron facility because of the larger fluxes available. We have developed an in-laboratory apparatus utilizing a focusing crystal technique which increases available fluxes two to three orders of magnitude over previous laboratory facilities, so that EXAFS measurements can be carried out quickly and accurately in the laboratory. We will discuss the principles of the focusing monochromator and we will also illustrate the experimental method with examples, including studies of chemical solutions, defect crystalline solids, and high-temperature superconductors.     

An instrument for 3D x-ray nano-imaging

We present an instrument dedicated to 3D scanning x-ray microscopy, allowing a sample to be precisely scanned through a beam while the angle of x-ray incidence can be changed. The position of the sample is controlled with respect to the beam-defining optics by laser interferometry. The instrument achieves a position stability better than 10 nm standard deviation. The instrument performance is assessed using scanning x-ray diffraction microscopy and we demonstrate a resolution of 18 nm in 2D imaging of a lithographic test pattern while the beam was defined by a pinhole of 3 μm in diameter. In 3D on a test object of copper interconnects of a microprocessor, a resolution of 53 nm is achieved.     

Time- and angle-resolved x-ray diffraction to probe structural and chemical evolution during Al-Ni intermetallic reactions

We present novel time- and angle-resolved x-ray diffraction (TARXD) capable of probing structural and chemical evolutions during rapidly propagating exothermic intermetallic reactions between Ni-Al multilayers. The system utilizes monochromatic synchrotron x-rays and a two-dimensional (2D) pixel array x-ray detector in combination of a fast-rotating diffraction beam chopper, providing a time (in azimuth) and angle (in distance) resolved x-ray diffraction image continuously recorded at a time resolution of ~30 μs over a time period of 3 ms. Multiple frames of the TARXD images can also be obtained with time resolutions between 30 and 300 μs over three to several hundreds of milliseconds. The present method is coupled with a high-speed camera and a six-channel optical pyrometer to determine the reaction characteristics including the propagation speed of 7.6 m/s, adiabatic heating rate of 4.0 × 10(6) K/s, and conductive cooling rate of 4.5 × 10(4) K/s. These time-dependent structural and temperature data provide evidences for the rapid formation of intermetallic NiAl alloy within 45 μs, thermal expansion coefficient of 1.1 × 10(-6) K for NiAl, and crystallization of V and Ag(3)In in later time.     

Phase identification of individual crystalline particles by electron backscatter diffraction

Recently, an electron backscatter diffraction (EBSD) system was developed that uses a 1024 × 1024 CCD camera coupled to a thin phosphor. This camera has been shown to produce excellent EBSD patterns. In this system, crystallographic information is determined from the EBSD pattern and coupled with the elemental information from energy or wavelength dispersive X-ray spectrometry. Identification of the crystalline phase of a sample is then made through a link to a commercial diffraction database. To date, this system has been applied almost exclusively to conventional, bulk samples that have been polished to a flat surface. In this investigation, we report on the application of the EBSD system to the phase identification analysis of individual micrometre and submicrometre particles rather than flat surfaces.     

Gas gun shock experiments with single-pulse x-ray phase contrast imaging and diffraction at the Advanced Photon Source

The highly transient nature of shock loading and pronounced microstructure effects on dynamic materials response call for in situ, temporally and spatially resolved, x-ray-based diagnostics. Third-generation synchrotron x-ray sources are advantageous for x-ray phase contrast imaging (PCI) and diffraction under dynamic loading, due to their high photon fluxes, high coherency, and high pulse repetition rates. The feasibility of bulk-scale gas gun shock experiments with dynamic x-ray PCI and diffraction measurements was investigated at the beamline 32ID-B of the Advanced Photon Source. The x-ray beam characteristics, experimental setup, x-ray diagnostics, and static and dynamic test results are described. We demonstrate ultrafast, multiframe, single-pulse PCI measurements with unprecedented temporal (<100 ps) and spatial (～2 μm) resolutions for bulk-scale shock experiments, as well as single-pulse dynamic Laue diffraction. The results not only substantiate the potential of synchrotron-based experiments for addressing a variety of shock physics problems, but also allow us to identify the technical challenges related to image detection, x-ray source, and dynamic loading.     

A methodology for measuring in situ lattice strain of bulk polycrystalline material under cyclic load

The material response of polycrystalline materials under cyclic loading is not fully understood. Even during uniaxial loading, individual grains embedded within the polycrystalline material can experience complicated strain histories. By quantifying the deformation state at the crystal level, we can begin to understand the conditions that lead to fatigue failure. An in situ powder diffraction method was developed and employed at the Cornell High Energy Synchrotron Source to measure the aggregate crystal response at various points in a material's life using synchrotron x ray. A set of experiments was conducted using a load frame capable of exerting cyclic uniaxial loads on a specimen. A high speed x-ray shutter was developed to synchronize the x-ray beam and the loading cycle. Using the high speed shutter, the evolution of the lattice strains for the families of crystallographic planes was measured while the aggregate was under cyclic uniaxial loading, thus monitoring a live evolution of lattice strain in a cyclically loaded specimen. The methodology is demonstrated using uniaxial cyclic specimens machined from oxygen free conductivity (OFHC) copper sheet.     

Development of an x-ray diffraction camera used in magnetic fields up to 10 T

A high-field x-ray diffraction (HF-XRD) camera was developed to observe structural changes of magnetic materials in magnetic fields up to 10 T. The instrument mainly consists of a Debye-Scherrer-type camera with a diameter of 80.1 mm, a 10-T cryocooled superconducting magnet with a 100-mm room-temperature bore, an x-ray source, a power supply, and a chiller for the x-ray source. An x-ray detector (image plate) in the HF-XRD camera can be taken out and inserted into the magnet without changing the sample position. The performance of the instrument was tested by measuring the HF-XRD for silicon and ferromagnetic MnBi powders. A change of x-ray diffraction pattern was observed due to the magnetic orientation of MnBi, showing that the instrument is useful for studying field-induced orientation processes and structural properties of field-controlled materials.     

Recrystallization of tungsten wire for fabrication of sharp and stable nanoprobe and field-emitter tips

Atomically sharp tungsten tips made from single crystal tungsten wire are superior to those made from cold-drawn polycrystalline wire but are rarely used due to their high price. We have devised a method of obtaining highly crystalline tungsten wire by recrystallizing cold-drawn wire. The effect of various heat treatments on the wire microstructure was observed using scanning electron microscopy and x-ray diffraction. A dramatic difference in the shapes of tips etched from cold-drawn and recrystallized wires was observed using transmission electron microscopy. The described annealing process is an inexpensive alternative to using single crystal wires.     

Grazing incidence wide angle x-ray scattering at the wiggler beamline BW4 of HASYLAB

We present an upgrade of the available measurement techniques at the wiggler beamline BW4 of the Hamburger Synchrotronstrahlungslabor (HASYLAB) to grazing incidence wide angle x-ray scattering (GIWAXS). GIWAXS refers to an x-ray diffraction method, which, based on the measurement geometry, is perfectly suited for the investigation of the material crystallinity of surfaces and thin films. It is shown that the overall experimental GIWAXS setup employing a movable CCD-detector provides the capability of reliable and reproducible diffraction measurements in grazing incidence geometry. Furthermore, the potential usage of an additional detector enables the simultaneous or successive measurement of GIWAXS and grazing incidence small angle x-ray scattering (GISAXS). The new capability is illustrated by the microbeam GIWAXS measurement of a thin film of the conjugated polymer poly(3-octylthiophene) (P3OT). The investigation reveals the semicrystalline nature of the P3OT film by a clear identification of the wide angle scattering reflexes up to the third order in the [100]-direction as well as the first order in the [010]-direction. The corresponding microbeam GISAXS measurement on the present morphology complements the characterization yielding the complete sample information from subnanometer up to micrometer length scales.     

A high-repetition rate scheme for synchrotron-based picosecond laser pump/x-ray probe experiments on chemical and biological systems in solution

We present the extension of time-resolved optical pump/x-ray absorption spectroscopy (XAS) probe experiments towards data collection at MHz repetition rates. The use of a high-power picosecond laser operating at an integer fraction of the repetition rate of the storage ring allows exploitation of up to two orders of magnitude more x-ray photons than in previous schemes based on the use of kHz lasers. Consequently, we demonstrate an order of magnitude increase in the signal-to-noise of time-resolved XAS of molecular systems in solution. This makes it possible to investigate highly dilute samples at concentrations approaching physiological conditions for biological systems. The simplicity and compactness of the scheme allows for straightforward implementation at any synchrotron beamline and for a wide range of x-ray probe techniques, such as time-resolved diffraction or x-ray emission studies.     

X-ray diffraction from shock-loaded polycrystals

X-ray diffraction was demonstrated from shock-compressed polycrystalline metals on nanosecond time scales. Laser ablation was used to induce shock waves in polycrystalline foils of Be, 25-125 microm thick. A second laser pulse was used to generate a plasma x-ray source by irradiation of a Ti foil. The x-ray source was collimated to produce a beam of controllable diameter, which was directed at the Be sample. X-rays were diffracted from the sample, and detected using films and x-ray streak cameras. The diffraction angle was observed to change with shock pressure. The diffraction angles were consistent with the uniaxial (elastic) and isotropic (plastic) compressions expected for the loading conditions used. Polycrystalline diffraction will be used to measure the response of the crystal lattice to high shock pressures and through phase changes.