An in-vacuum diffractometer for resonant elastic soft x-ray scattering

We describe the design, construction, and performance of a 4-circle in-vacuum diffractometer for resonant elastic soft x-ray scattering. The diffractometer, installed on the resonant elastic and inelastic x-ray scattering beamline at the Canadian Light Source, includes 9 in-vacuum motions driven by in-vacuum stepper motors and operates in ultra-high vacuum at base pressure of 2 × 10(-10) Torr. Cooling to a base temperature of 18 K is provided with a closed-cycle cryostat. The diffractometer includes a choice of 3 photon detectors: a photodiode, a channeltron, and a 2D sensitive channelplate detector. Along with variable slit and filter options, these detectors are suitable for studying a wide range of phenomena having both weak and strong diffraction signals. Example measurements of diffraction and reflectivity in Nd-doped (La,Sr)(2)CuO(4) and thin film (Ga,Mn)As are shown.     

Bragg diffraction using a 100 ps 17.5 keV x-ray backlighter and the Bragg diffraction imager

A new diagnostic for measuring Bragg diffraction of petawatt-generated high-energy x rays off a laser-compressed crystal was designed and tested successfully at the Omega EP laser facility on static Mo and Ta (111) oriented single crystal samples using a 17.5 keV Mo?Kα backlighter. The Bragg diffraction imager consists of a heavily shielded enclosure and a precisely positioned beam block attached to the enclosure by an aluminum arm. Fuji image plates are used as the x-ray detectors. The diffraction from Mo and Ta (222) crystal planes was clearly detected with a high signal-to-noise. This technique will be applied to shock- and quasi-isentropically loaded single crystals on the Omega EP laser.     

Theory and application of Kossel x-ray diffraction in the scanning electron microscope

The application of Kossel x-ray diffraction to the SEM is reviewed with discussion of identification of structures, determination of orientation relationships between crystals, residual strain measurements, examination of fracture surfaces and semi-quantitative measurement of plastic strain. Geometrical theory of formation of the patterns is outlined and methods of analysis reviewed with emphasis on the techniques available when the pattern centre and specimen to film distance can be accurately determined. A recent method of obtaining the latter parameters is discussed. Pattern recognition techniques are discussed with references to F. C. Frank's model based on the intersection of an x-ray sphere of radius 1/2 with the Brillouin zone boundaries of the crystal and estimates are produced of the diffracting volume as a function of perfection of the crystal.     

The scanning low-energy electron microscope: First attainment of diffraction contrast in the scanning electron microscope

Using small Pb crystals deposited in situ on a partially contaminated Si (100) crystal, we demonstrate that a commercial scanning electron microscope (SEM) can easily be converted into a scanning low-energy electron microscope (SLEEM). Although the contrast mechanism is much more complicated than that in nonscanning LEEM because not only one diffracted monochromatic beam and its close environment are used for imaging, but several diffracted beams and a wide energy spectrum of electrons of different origin (secondary electrons, inelastically andelastically scattered electrons) are used, SLEEM is a valuable addition to the standard SEM because it provides an additional structure- and orientation-sensitive contrast mechanism in crystalline materials, a low sampling depth, and high intensity at low energies.     

A new correction method for high-resolution energy-dispersive x-ray analyses in the environmental scanning electron microscope

Spurious x-ray signals, which previously prevented high-resolution energy-dispersive x-ray analysis (EDS) in the environmental scanning electron microscope (ESEM), can be corrected using a simple method presented here. As the primary electron beam travels through the gas in the ESEM chamber, a significant fraction of the primary electrons is scattered during collisions with gas molecules. These scattered electrons form a broad skirt that surrounds the primary electron beam as it impacts the sample. The correction method assumes that changes in the width of the electron skirt with pressure are less important than changes in the skirt intensity; this method works as follows: The influence of the gas on the overall x-ray data is determined by acquiring EDS spectra at two pressures. Subtracting the two spectra provides us with a difference spectrum which is then used to correct the original data, using extrapolation, back to the x-ray spectrum expected under high-vacuum conditions. Low-noise data are required to resolve small spectral peaks; however, the principle should apply equally to x-ray maps and even to low-magnification images.     

An electron microscope for the aberration-corrected era

Improved resolution made possible by aberration correction has greatly increased the demands on the performance of all parts of high-end electron microscopes. In order to meet these demands, we have designed and built an entirely new scanning transmission electron microscope (STEM). The microscope includes a flexible illumination system that allows the properties of its probe to be changed on-the-fly, a third-generation aberration corrector which corrects all geometric aberrations up to fifth order, an ultra-responsive yet stable five-axis sample stage, and a flexible configuration of optimized detectors. The microscope features many innovations, such as a modular column assembled from building blocks that can be stacked in almost any order, in situ storage and cleaning facilities for up to five samples, computer-controlled loading of samples into the column, and self-diagnosing electronics. The microscope construction is described, and examples of its capabilities are shown.     

Interpretation of the fading of diffraction patterns from organic substances irradiated with 100 keV electrons at 10-300 K

The fading curves of Debye-Scherrer ring intensities have been recorded for evaporated films of some aliphatic and aromatic compounds at temperatures between T_s=14-66 K and room temperature. The lowest real specimen temperature T_s was calibrated by the condensation of different gas atoms and depends on the current density used, which has to be raised with increasing resistivity to radiation damage. The fading curves for the lowest specimen temperature were compared with a theory of Clark et al. modified by a multiple-hit model. By fitting the theory to experimental results, values of the cross-section σ for a single hit, the mean number m of hits necessary to destroy a sensitive unit and the ratio b of the damaged to the undamaged structure amplitude of a unit cell can be established. There are considerable differences in these quantities for different compounds. The temperature dependence of σ for tetracene and other compounds can be explained by an activation energy of the order of a few tens of one meV.     

Setup for in situ x-ray diffraction study of swift heavy ion irradiated materials

An in situ x-ray diffraction (XRD) setup is designed and installed in the materials science beam line of the Pelletron accelerator at the Inter-University Accelerator Centre for in situ studies of phase change in swift heavy ion irradiated materials. A high vacuum chamber with suitable windows for incident and diffracted X-rays is integrated with the goniometer and the beamline. Indigenously made liquid nitrogen (LN2) temperature sample cooling unit is installed. The snapshots of growth of particles with fluence of 90 MeV Ni ions were recorded using in situ XRD experiment, illustrating the potential of this in situ facility. A thin film of C60 was used to test the sample cooling unit. It shows that the phase of the C60 film transforms from a cubic lattice (at room temperature) to a fcc lattice at around T=255 K.     

Portable chamber for the study of UHV prepared electrochemical interfaces by hard x-ray diffraction

We report on a new electrochemical cell setup, combined with a portable UHV chamber, for in situ x-ray diffraction using synchrotron radiation. In contrast to more traditional electrochemical sample preparation schemes, atomically clean and well-ordered surfaces are routinely prepared by UHV methods, even in the case of reactive elements or alloys. Samples can be transferred from larger UHV systems into the portable chamber without exposure to ambient air. They can then be studied successively in UHV, in controlled gas atmospheres, and in contact with electrolyte solutions under applied electrochemical potential. The electrochemical setup employs a droplet geometry, which guarantees good electrochemical conditions during in situ x-ray measurements combined with voltammetry. We present first experimental results of Cu deposition on GaAs(001) and on freshly produced nanometric Pd(001) islands on Cu(0.83)Pd(0.17)(001), respectively.     

Accuracy and precision of quantitative energy-dispersive x-ray spectrometry in the environmental scanning electron microscope

The accuracy and precision of quantitative energy-dispersive x-ray spectrometry in the environmental scanning electron microscope have been estimated using a series of copper / gold alloys of known composition. The mean values (five to six replicate experiments) had relative errors within +/- 5%, and most were within +/- 3.5%. All relative standard deviations were < 5% and most were < 3%. Since the standard specimens were large (approximately 500 microm) in diameter, electron scattering in the 2 torr of water vapor above the specimen did not affect the results. This level of accuracy and precision was possible only by using a novel specimen surface charge neutralization scheme.     

Design and performance of a versatile curved-crystal spectrometer for high-resolution spectroscopy in the tender x-ray range

A complete in-vacuum curved-crystal x-ray emission spectrometer in Johansson geometry has been constructed for a 2-6 keV energy range with sub natural line-width energy resolution. The spectrometer is designed to measure x-ray emission induced by photon and charged particle impact on solid and gaseous targets. It works with a relatively large x-ray source placed inside the Rowland circle and employs position sensitive detection of diffracted x-rays. Its compact modular design enables fast and easy installation at a synchrotron or particle accelerator beamline. The paper presents main characteristics of the spectrometer and illustrates its capabilities by showing few selected experimental examples.     

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.     

A method for accurately determining lattice parameters using electron diffraction in a commercial electron microscope

In this paper an electron diffraction method is discussed by which the lattice constants of polycrystalline thin films can be accurately determined (0.1%). The method involves the sequential examination of a standard material and the unknown material mounted on separate grids. The error which can arise through the possible difference in height of the two grids can be corrected by means of height and tilting adjustments. The analytical approach of the dependence of the camera constant on the ring diameter as given in literature appears to be insufficient. An experimental correction factor for this dependence is introduced. The accuracy of this method, and the influence of relevant sources of error, are discussed and explained in terms of some experimental results.