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M n 2 Au is a bimetallic antiferromagnetic with an extraordinarily high Néel temperature of 1600 K. M n 2 Au has also been found to demonstrate Néel-order spin–orbit torque, allowing for electrical switching of the antiferromagnetic Néel vector. This has led to much interest in this material for spintronic applications. Here, we detail the growth of high quality M n 2 Au (110) thin films. The films were grown on a high quality Pt (111) buffer layer, which was grown on an A l 2 O 3 (0001) substrate. The M n 2 Au films have excellent crystalline quality as demonstrated by x-ray diffraction, x-ray reflection, and reflection high energy electron diffraction measurements. The M n 2 Au (110) films are found to grow with three equivalent in-plane rotation domains, caused by the Pt/ A l 2 O 3 substrate. [ABSTRACT FROM AUTHOR]

Atomic layer deposition (ALD) of multicomponent materials is challenging because the growth characteristics often deviate from what is expected due to the difference in surface characteristics of heterogeneous and single materials, resulting in undesired thickness or properties. For metal oxides, the growth characteristics highly rely on the surface hydroxyl groups, which play a role as the reactive site. Thus, studying the reaction mechanism of a precursor on hydroxyl-terminated heterogeneous surfaces is important for understanding the nonideal growth of ternary oxide. Here, we investigated the correlation between hydroxyl and the growth of ALD TiSiOx depending on temperature, analyzing infrared spectra, and chemical compositions. The results show that large amounts of hydroxyl are detected in TiSiOx deposited at 100 °C, where the adsorption of H2O on Ti–O–Si bonds is favorable. It leads to higher growth per cycle (GPC) than the estimated value. In contrast, the hydroxyl disappears at 200 °C due to dehydroxylation, resulting in lower GPC. Differences in hydroxyl also influence the film density as revealed in x-ray reflection spectra, which is related to the film qualities (e.g., elastic modulus and dry etch rates). This work provides insight into how to control hydroxyl in the ALD of ternary oxides, which is susceptible to hydroxyl incorporation, leading to undesired growth characteristics. [ABSTRACT FROM AUTHOR]

This work presents the results of the analysis of the temperature dependence of the x-ray reflection intensity from solid heavy nitrogen in the ordered phase. The temperature dependence of the behavior of the orientational order parameter and mean square displacement of 15N2 molecules obtained from x-ray data is plotted. Based on the dependencies obtained, the orientational order parameter was determined at 0 K, which is 12% higher than the orientational order parameter obtained in theoretical works. It was found that the heavy nitrogen molecule "freely" rotates in the crystal at temperatures above 45 K. [ABSTRACT FROM AUTHOR]

The search for multiferroic order in a single phase of bismuth pyrochlore has been unsuccessful so far. In this direction, our study unveiled the capability of a biphase of bismuth pyrochlore and spinel in hosting a multiferroic order at room temperature. A complex oxide biphase of cubic pyrochlore and cubic spinel crystals acquired in the Bi2O3-Nb2O5-2MnCO3-Fe2O3 system revealed the crystals of a spinel phase (Fe1.59(3)Mn1.39(3)O4.26(7)) intergrown in the dense pyrochlore (Bi1.35(1)Fe0.64(1)Nb1.26(1)Mn0.75(1)O6.39(5)) matrix. The average composition of the components of the investigated biphase was determined using an electron probe microanalyzer (EPMA). The structural features indicated the presence of large ionic displacements within the cubic pyrochlore phase as seen from the appearance of 442 reflection in the X-ray diffraction pattern and infrared active mode at ∼64 cm−1 in the Raman spectrum recorded at room temperature. The pyrochlore single-phase composition (Bi1.35(1)Fe0.64(1)Nb1.26(1)Mn0.75(1)O6.39(5)), as suggested from a thorough EPMA microstructural analysis, exhibited broad dielectric relaxation and an overall paramagnetic behavior. The observation of disordered superparamagnetism as well as dielectric relaxation in the biphase conformed to that of a relaxorlike multiferroic behavior at room temperature. Moreover, self-biased magnetoelectric voltage coefficients of 0.60 mV/cm Oe at 100 Hz and 5.54 mV/cm Oe at 1 kHz were detected between magnetization and electric polarization at room temperature. Therefore, the composite of such a pyrochlore and spinel with an inherent property of strong spin–orbit and spin–lattice coupling will be interesting from theoretical and experimental point of view in the arena of magnetoelectrics. [ABSTRACT FROM AUTHOR]

Time-resolved x-ray diffraction has been used to measure the low-temperature thermal transport properties of a Pt/Gd3Fe5O12//Gd3Ga5O12 metal/oxide heterostructure relevant to applications in spin caloritronics. A pulsed femtosecond optical signal produces a rapid temperature rise in the Pt layer, followed by heat transport into the Gd3Fe5O12 (GdIG) thin film and the Gd3Ga5O12 (GGG) substrate. The time dependence of x-ray diffraction from the GdIG layer was tracked using an accelerator-based femtosecond x-ray source. The ultrafast diffraction measurements probed the intensity of the GdIG (1 −1 2) x-ray reflection in a grazing-incidence x-ray diffraction geometry. The comparison of the variation of the diffracted x-ray intensity with a model including heat transport and the temperature dependence of the GdIG lattice parameter allows the thermal conductance of the Pt/GdIG and GdIG//GGG interfaces to be determined. Complementary synchrotron x-ray diffraction studies of the low-temperature thermal expansion properties of the GdIG layer provide a precise calibration of the temperature dependence of the GdIG lattice parameter. The interfacial thermal conductance of the Pt/GdIG and GdIG//GGG interfaces determined from the time-resolved diffraction study is of the same order of magnitude as previous reports for metal/oxide and epitaxial dielectric interfaces. The thermal parameters of the Pt/GdIG//GGG heterostructure will aid in the design and implementation of thermal transport devices and nanostructures. [ABSTRACT FROM AUTHOR]

AlN layers were grown on a c-plane sapphire substrate by metal–organic vapor phase epitaxy (MOVPE) at 1350 °C. The structural quality of the grown AlN layers was drastically improved by post-growth annealing in mixed hydrogen, ammonia, and trimethylgallium ambiance at 1350 °C. As a first step, we grew the AlN layers exhibiting a double-domain structure with an in-plane rotation angle of ∼4°. Then, the domain structure was changed from double to single by the post-growth annealing. After 20 min post-growth annealing, the surface possessed an atomically flat step-and-terrace structure with a root-mean-square value of ∼0.11 nm measured across 5 × 5 µm2. The full-width at half maximum values for 0002 and 10 1 ̄ 4 AlN reflections using x-ray diffraction were as small as ∼75 and ∼280 arcsec, respectively. Since this work provides a simple continuous MOVPE growth procedure to improve the structural quality of AlN/sapphire, it is advantageous to the industrial fabrication of AlxGa1−xN-based ultraviolet light-emitters. [ABSTRACT FROM AUTHOR]

By adjusting the incidence angle of incoming x rays near the critical angle of x-ray total reflection, photoelectron intensity is strongly modulated due to the variation of x-ray penetration depth. Photoelectron spectroscopy combined with near-total reflection exhibits tunable surface sensitivity, providing depth-resolved information. In this Review, we first describe the experimental setup and specific data analysis process. We then review three different examples that show the broad application of this method. The emphasis is on its applications correlated to oxide heterostructures, especially quantitative depth analyses of compositions and electronic states. In the last part, we discuss the limitations of this technique, mostly in terms of the range of samples that can be studied. [ABSTRACT FROM AUTHOR]

X-ray reflectivity is a promising technique for characterizing buried layers and interfaces in ultrathin films because of its ability to probe the electron density profile along the depth in a nondestructive manner. While routine X-ray reflectivity assumes the in-plane uniformity of the sample to be measured, it is also quite important to see buried inhomogeneous/patterned layers and interfaces. The present paper describes the addition of spatial resolution and imaging capability to an X-ray reflectivity technique to visualize surfaces and buried interfaces. To visualize quite wide viewing area size quickly, the image reconstruction scheme has been employed instead of the scanning of microbeam. Though the mathematics is quite close to X-ray computer tomography, the technique gives the image contrast caused by the difference in reflectivity at each in-plane point in the thin film sample. By choosing a grazing angle, the image gives inhomogeneity of X-ray reflectivity at the specific wavevector transfer. With a collimated monochromatic synchrotron X-ray beam of 0.05 mm (H) × 8 mm (V), the intensity profiles of X-ray reflection projections have been taken at many different in-plane rotation angles, from 0° to 180°. We have succeeded in visualizing buried layers and interfaces of the 8 mm dia area with the spatial resolution of better than 20 μm. Because of the brilliance of synchrotron radiation, the typical measuring time is shorter than 1 min. Three analytical cases have been discussed: (i) imaging of a buried layer and an interface covered by a protection layer, (ii) distinguishing different local parts of different thicknesses in an ultrathin film, and (iii) selective imaging of a specific metal in the thin film form. [ABSTRACT FROM AUTHOR]

The highly coherent and tightly focused x-ray beams produced by hard x-ray light sources enable the nanoscale characterization of the structure of electronic materials but are accompanied by significant challenges in the interpretation of diffraction and scattering patterns. X-ray nanobeams exhibit optical coherence combined with a large angular divergence introduced by the x-ray focusing optics. The scattering of nanofocused x-ray beams from intricate semiconductor heterostructures produces a complex distribution of scattered intensity. We report here an extension of coherent x-ray optical simulations of convergent x-ray beam diffraction patterns to arbitrary x-ray incident angles to allow the nanobeam diffraction patterns of complex heterostructures to be simulated faithfully. These methods are used to extract the misorientation of lattice planes and the strain of individual layers from synchrotron x-ray nanobeam diffraction patterns of Si/SiGe heterostructures relevant to applications in quantum electronic devices. The systematic interpretation of nanobeam diffraction patterns from semiconductor heterostructures presents a new opportunity in characterizing and ultimately designing electronic materials. [ABSTRACT FROM AUTHOR]

We study the effect of low-temperature post growth annealing on the Fe layer in an epitaxial Fe/GaAs(001) heterojunction. High resolution X-ray diffraction and X-ray reflectivity were used to probe the Fe layer before and after annealing. No change in morphological features like annealing induced intermixing and thickness variation of the Fe layer are observed. However, annealing leads to increase in the compressive strain and improves isotropy of the ferromagnetic layer as revealed by measuring both lateral and out-of-plane lattice components. [ABSTRACT FROM AUTHOR]

Microstructure and composition analysis of periodic multilayer structure consisting of a low electron density contrast (EDC) material combination by grazing incidence hard X-ray reflectivity (GIXR), resonant soft X-ray reflectivity (RSXR), and transmission electron microscopy (TEM) are presented. Measurements of reflectivity at different energies allow combining the sensitivity of GIXR data to microstructural parameters like layer thicknesses and interfacing roughness, with the layer composition sensitivity of RSXR. These aspects are shown with an example of 10-period C/B4C multilayer. TEM observation reveals that interfaces C on B4C and B4C on C are symmetric. Although GIXR provides limited structural information when EDC between layers is low, measurements using a scattering technique like GIXR with a microscopic technique like TEM improve the microstructural information of low EDC combination. The optical constants of buried layers have been derived by RSXR. The derived optical constants from the measured RSXR data suggested the presence of excess carbon into the boron carbide layer. [ABSTRACT FROM AUTHOR]

By using full three-dimensional particle-in-cell and Monte Carlo simulations, we investigate the generation of a high-brightness attosecond x-ray pulse train in a double-laser-driven cone target. The scheme makes use of two lasers: the first high-intensity laser with a laser peak intensity 1.37 × 1020W/cm2 irradiates the cone and produces overdense attosecond electron bunches; the second counterpropagating weakly relativistic laser with a laser peak intensity 4.932 × 1017W/cm2 interacts with the produced electron bunches and a bright x-ray pulse train is generated by Thomson backscattering of the second laser off the attosecond electron bunches. It is shown that the photon flux rises by 5 times using the cone target as compared with a normal channel. Meanwhile, the x-ray peak brightness increases significantly from 1.4 × 1021/(s mm2 mrad2 0.1 keV) to 6.0 × 1021/(s mm2 mrad2 0.1 keV), which is much higher than that of the Thomson x-ray source generated from traditional accelerators. We also discuss the influence of the laser and target parameters on the x-ray pulse properties. This compact bright x-ray source may have diverse applications, e.g., the study of electric dynamics and harmonics emission in the atomic scale. [ABSTRACT FROM AUTHOR]

We presented a focal construct geometry (FCG) method for high intensity energy dispersive X-ray diffraction by utilizing a home-made ellipsoidal single-bounce capillary (ESBC) and a polycapillary parallel X-ray lens (PPXRL). The ESBC was employed to focus the X-rays from a conventional laboratory source into a small focal spot and to produce an annular X-ray beam in the far-field. Additionally, diffracted polychromatic X-rays were confocally collected by the PPXRL attached to a stationary energy-resolved detector. Our FCG method based on ESBC and PPXRL had achieved relatively high intensity diffraction peaks and effectively narrowed the diffraction peak width which was helpful in improving the potential d-spacing resolution for material phase analysis. [ABSTRACT FROM AUTHOR]

We have determined the depth profile of YCrO3/CaMnO3 superlattices by hard x-ray photoemission spectroscopy in near total reflection conditions. YCrO3/CaMnO3 is prone to exhibit interesting magnetotransport properties owing to the large amount of electron transfer expected between Cr3+ and Mn4+. The depth profile was reconstructed by simulating the rocking curves of the different core levels using the YXRO software and fine-tuning the structural model. The results globally conform to scanning transmission electron microscopy and electron energy loss spectroscopy analysis, except for the top layer, whose structure and stoichiometry are found to be preserved in contrast to microscopy. [ABSTRACT FROM AUTHOR]

We report on the experimental realization of propagation-based x-ray microscopy with laboratory sources equipped with waveguides. We discuss about the experimental setup, the fabrication steps, and the characterization procedures of the waveguide optics. We demonstrate that the system enables high resolution attenuation imaging of poorly absorbing biological specimens. Furthermore, we report the successful realization of propagation-based phase contrast x-ray microscopy, enabling quantitative thickness estimation in homogeneous objects. Advantages and major limitations of the experimental scheme are presented and discussed. [ABSTRACT FROM AUTHOR]

We report on the relationship between structural and magnetic properties, as well as their Mnsubstitution dependence for ceramics Ba(CoCo1-xMnx)O3 (x=0.00-0.30) following an analysis using synchrotron X-ray spectroscopy. The crystal structure of samples of Ba(CoCo1-xMnx)O3 ceramics changed from 2H- to 10H- through 12H-type phases depending on composition ratio x. The saturation magnetization increased in the presence of the 12H-type phase, and decreased in the presence of the 10H-type phase; a maximum value of 2.49 μB/f.u. at 5K is obtained with composition ratio x=0.1. The correlation between structural and magnetic properties as well as their dependence on Mn substitution are explained by the preferential occupation of the cubic stacking sites by Mn ions. The 12H-type phase exhibited ferri-magnetic ordering attributed to the ferromagnetic superexchange coupling of Co4+(d5)-O2--Mn4+(d3) with a bonding angle of 180°; the 2H- and 10H-type phases exhibited anti-ferromagnetic ordering attributed to the anti-ferromagnetic super-exchange couplings of Co4+(d5) -O2--Co4+(d5) and Co4+(d5) -O2--Mn4+(d3), respectively, with a bonding angle of 90°. The saturation magnetization therefore increases with the presence of the ferromagnetic 12H-type phase, whereas it decreases in the presence of the anti-ferromagnetic 10H-type phase. [ABSTRACT FROM AUTHOR]

Rocking curve topography at the Advanced Photon Source's beamline 1-BM measures the x-ray reflection from large (many cm2) flat crystals on a sub-mm scale with microradian angular resolution. The (01 1 ̄ 1) reflection at 8 keV is uniform across the crystal and close to theory for three thick quartz wafers well-polished with increasingly finer grit. However, the reflection is non-uniform for some ∼0.1 mm thin, bendable crystals that are made flat by optical contact with a flat substrate. These thin crystals are bent to serve in certain x-ray diagnostics of plasmas, and similar non-uniformities could then occur in bent crystals as well. The same detail in x-ray reflection in bent crystals is unachievable with the existing topography setup: One way to get the desired resolution is with a standard microfocusing approach. [ABSTRACT FROM AUTHOR]

The soft x-ray Opacity Spectrometer (OpSpec) used on the National Ignition Facility (NIF) has recently incorporated an elliptically shaped crystal. The original OpSpec used two convex cylindrical crystals for time-integrated measurements of point-projection spectra from 540 to 2100 eV. However, with the convex geometry, the low-energy portion of the spectrum suffered from high backgrounds due to scattered x-rays as well as reflections from alternate crystal planes. An elliptically shaped crystal allows an acceptance aperture at the crossover focus between the crystal and the detector, which reduces background and eliminates nearly all reflections from alternate crystal planes. The current elliptical design is an improvement from the convex cylindrical design but has a usable energy range from 900 to 2100 eV. In addition, OpSpec is currently used on 18 NIF shots/year, in which both crystals are typically damaged beyond reuse, so efficient production of 36 crystals/year is required. Design efforts to improve the existing system focus on mounting reliability, reducing crystal strain to increase survivability between mounting and shot time, and extending the energy range of the instrument down to 520 eV. The elliptical design, results, and future options are presented. [ABSTRACT FROM AUTHOR]

NbO2 is a promising candidate for resistive switching devices due to an insulator-metal transition above room temperature, which is related to a phase transition from a distorted rutile structure to an undistorted one. However, the electrical resistivity of the NbO2 thin films produced so far has been too low to achieve high on-off switching ratios. Here, we report on the structural, electrical, and optical characterization of single-crystalline NbO2 (001) thin films grown by pulsed laser deposition on MgF2 (001) substrates. An annealing step reduced the full width at half maximum of the NbO2 (004) x-ray Bragg reflection by one order of magnitude, while the electrical resistivity of the films increased by two orders of magnitude to about 1 kΩcm at room temperature. Temperature-dependent resistivity measurements of an annealed sample revealed that below 650 K, two deep-level defects with activation energies of 0.25 eV and 0.37 eV dominate the conduction, while above 650 K, intrinsic conduction prevails. Optical characterization by spectroscopic ellipsometry and by absorption measurements with the electric field vector of the incident light perpendicular to the c-axis of the distorted rutile structure indicates the onset of fundamental absorption at about 0.76 eV at room temperature, while at 4 K, the onset shifts to 0.85 eV. These optical transitions are interpreted to take place across the theoretically predicted indirect bandgap of distorted rutile NbO2. [ABSTRACT FROM AUTHOR]

We investigated the microstructure of PbTiO3 films epitaxially grown on DyScO3 (110) substrates using synchrotron-based 3D reciprocal space mapping and X-ray reflection interface microscopy. The results show that an in-plane anisotropic mixture domain state (a* + a/c) exists in the PbTiO3 films, where a* domains reside between a/c twin stripe domains. Furthermore, when compared with traditional a domains in a/c twins, the a* domain is found to possess a similar in-plane lattice parameter but a much smaller out-of-plane lattice (∼0.5%). We also discovered a temperature-driven transition between a* and a/c pointing to potential applications in functional devices due to the huge mechanical response (4.85%) and polarization rotation between the a* and c domains. [ABSTRACT FROM AUTHOR]

The surface contamination of reflective X-ray optics has long been a serious problem that degrades beam quality. We evaluated the total organic content at the surface by gas chromatography to clarify the source of contamination. We found that various materials that can become contamination sources are used around the optical elements. After covering the optics with cleaned materials and applying synchrotron radiation cleaning during commissioning, the observed reflected intensity at the beamline has not reduced for 2.5 years. [ABSTRACT FROM AUTHOR]

Thermally activated selective topography equilibration (TASTE) enables the creation of 3D structures in resist using grayscale electron-beam lithography followed by a thermal treatment to induce a selective polymer reflow. A blazed grating topography can be created by reflowing repeating staircase patterns in resist into wedgelike structures. Motivated by astronomical applications, such patterns with periodicities 840 and 400 nm have been fabricated in 130 nm-thick poly(methyl methacrylate) using TASTE to provide a base for x-ray reflection gratings. A path forward to integrate this alternative blazing technique into grating fabrication recipes is discussed. [ABSTRACT FROM AUTHOR]

Atomic layer deposition (ALD) of mixed oxides has attracted increasing research attention in recent years due to its excellent capability of film composition tuning. This in turn highlights the importance of understanding the underlying surface chemistry which dictates how a film of desired composition is achieved. In this work, the authors examined the ability of atomic layer deposition to precisely control the film thickness and composition by studying the growth behavior of SnxTi1-xOy thin films deposited from an alkylamide Ti(IV) precursor, a β-diketonate Sn(II) precursor and ozone. A set of samples with various compositions were deposited by controlling the ALD cycle ratio (ALDCR) of tin oxide/titanium oxide using our custom-built, warm-wall reactor. Both alloy- and laminate-type of growths were attempted by changing numbers of ALD subcycles while maintaining the cycle ratio. Growth rates, calculated based on the thicknesses measured by spectroscopic ellipsometery and x-ray reflectivity, showed a deviating pattern from that of linear interpolation using binary ALD processes, marked by an almost constant ~0.06 nm/cycle. Film composition, determined by x-ray photoelectron spectroscopy, exhibited a concave upward dependence on ALDCR. The chemisorption density of each precursor was determined by x-ray reflectivity, and a linearly ALDCR-dependent decrease was observed. Structural analysis using x-ray diffraction showed a transition from anatase to SnO2 rutile when Sn content in the film was varied from 0 to 1, for O2 annealed samples. At ~17 at. % Sn, a mixture of anatase and rutile phases was found. Other factors, such as surface roughness and surface chemical species, were examined in the attempt to account for the decreased chemisorption. [ABSTRACT FROM AUTHOR]

Al2O3 dielectric films deposited by atomic layer deposition (ALD) were characterized using grazing-incidence small angle x-ray scattering (GISAXS). Unique to this method, the diffuse scattering from surface and interface roughnesses was calculated with surface parameters (root mean square roughness σ, lateral correlation length ξ and Hurst parameter h) obtained from atomic force microscopy and layer densities, surface grading and interface roughness/grading obtained from specular x-ray reflectivity (XRR) simulation. Pore scattering was determined with the measured total diffuse scattering intensity subtracted by the simulated diffuse scattering from roughnesses, from which the pore size distribution was obtained. This GISAXS method was validated with the scanning electron microscopy result of a porous indium phosphide single layer and was applied to two Al2O3 dielectric single layers deposited with different ALD parameters. Both porous and nonporous Al2O3 layers were revealed. The pore size in the porous Al2O3 single layer was determined to disperse in a range of several nanometers with an uncertainty of ~1 nm. The GISAXS results are correlated with other techniques including specular XRR measurements, spectroscopic ellipsometry and broadband optical reflectance measurements. Pore size distribution, along with layer thicknesses, densities and refractive indices, is key to understanding the role of deposition conditions in the optical and electrical properties of Al23 dielectric films. [ABSTRACT FROM AUTHOR]

We present time-resolved x-ray reflectivity measurements on laser excited coherent and incoherent surface deformations of thin metallic films. Based on a kinematical diffraction model, we derive the surface amplitude from the diffracted x-ray intensity and resolve transient surface excursions with sub-Å spatial precision and 70 ps temporal resolution. The analysis allows for decomposition of the surface amplitude into multiple coherent acoustic modes and a substantial contribution from incoherent phonons which constitute the sample heating. [ABSTRACT FROM AUTHOR]

A new method for fast x-ray reflectivity data acquisition is presented. The method is based on a fast rotating, slightly tilted sample reflecting to a stationary mounted position sensitive detector and it allows for measurements of reflectivity curves in a quarter of a second. The resolution in q-space mainly depends on the beam properties and the pixel size of the detector. Maximum qz-value of 1 Å-1 can be achieved. The time-temperature depending structure changes of poly(Nisopropylacrylamide) thin films were investigated in situ by applying the fast-reflectivity setup. The results are presented in this paper as illustration of the method and proof of principle. [ABSTRACT FROM AUTHOR]

A Particle X-ray Temporal Diagnostic (PXTD) has been implemented on OMEGA for simultaneous time-resolved measurements of several nuclear products as well as the x-ray continuum produced in High Energy Density Plasmas and Inertial Confinement Fusion implosions. The PXTD removes systematic timing uncertainties typically introduced by using multiple instruments, and it has been used to measure DD, DT, D3He, and T3He reaction histories and the emission history of the x-ray core continuum with relative timing uncertainties within ±10-20 ps. This enables, for the first time, accurate and simultaneous measurements of the x-ray emission histories, nuclear reaction histories, their time differences, and measurements of Ti(t) and Te(t) from which an assessment of multiple-ion-fluid effects, kinetic effects during the shock-burn phase, and ion-electron equilibration rates can be made. [ABSTRACT FROM AUTHOR]

The Advanced Light Source beamline-9.3.1 x-rays are used to calibrate the rocking curve of bent potassium acid phthalate (KAP) crystals in the 2.3-4.5 keV photon-energy range. Crystals are bent on a cylindrically convex substrate with a radius of curvature ranging from 2 to 9 in. and also including the flat case to observe the effect of bending on the KAP spectrometric properties. As the bending radius increases, the crystal reflectivity converges to the mosaic crystal response. The X-ray Oriented Programs (xop) multi-lamellar model of bent crystals is used to model the rocking curve of these crystals and the calibration data confirm that a single model is adequate to reproduce simultaneously all measured integrated reflectivities and rocking-curve FWHM for multiple radii of curvature in both 1st and 2nd order of diffraction. [ABSTRACT FROM AUTHOR]

Talbot-Lau X-ray deflectometry (TXD) has been developed as an electron density diagnostic for High Energy Density (HED) plasmas. The technique can deliver x-ray refraction, attenuation, elemental composition, and scatter information from a single Moiré image. An 8 keV Talbot-Lau interferometer was deployed using laser and x-pinch backlighters. Grating survival and electron density mapping were demonstrated for 25-29 J, 8-30 ps laser pulses using copper foil targets. Moiré pattern formation and grating survival were also observed using a copper x-pinch driven at 400 kA, ∼1 kA/ns. These results demonstrate the potential of TXD as an electron density diagnostic for HED plasmas. [ABSTRACT FROM AUTHOR]

We demonstrate that stacking several imaging plates (IPs) constitutes an easy method to increase hard x-ray detection efficiency. Used to record x-ray radiographic images produced by an intense-laser driven hard x-ray backlighter source, the IP stacks resulted in a significant improvement of the radiograph density resolution. We attribute this to the higher quantum efficiency of the combined detectors, leading to a reduced photon noise. Electron-photon transport simulations of the interaction processes in the detector reproduce the observed contrast improvement. Increasing the detection efficiency to enhance radiographic imaging capabilities is equally effective as increasing the x-ray source yield, e.g., by a larger drive laser energy. [ABSTRACT FROM AUTHOR]

The [Au(CN)2 -]3 trimer in water experiences a strong van der Waals interaction between the d10 gold atoms due to large relativistic effect and can serve as an excellent model system to study the bond formation process in real time. The trimer in the ground state (S0) exists as a bent structure without the covalent bond between the gold atoms, and upon the laser excitation, one electron in the antibonding orbital goes to the bonding orbital, thereby inducing the formation of a covalent bond between gold atoms. This process has been studied by various timeresolved techniques, and most of the interpretation on the structure and dynamics converge except that the structure of the first intermediate (S1) has been debated due to different interpretations between femtosecond optical spectroscopy and femtosecond X-ray solution scattering. Recently, the excitation wavelength of 267 nm employed in our previous scattering experiment was suggested as the culprit for misinterpretation. Here, we revisited this issue by performing femtosecond X-ray solution scattering with 310 nm excitation and compared the results with our previous study employing 267 nm excitation. The data show that a linear S1 structure is formed within 500 fs regardless of excitation wavelength and the structural dynamics observed at both excitation wavelengths are identical to each other within experimental errors. [ABSTRACT FROM AUTHOR]

Optical elements of soft x-ray beamlines usually have motorized translations and rotations that allow for the fine alignment of the beamline. This is to steer the photon beam at some positions and to correct the focus on slits or on sample. Generally, each degree of freedom of a mirror induces a change of several parameters of the beam. Inversely, several motions are required to actuate on a single optical parameter, keeping the others unchanged. We define optical pseudomotors as combinations of physical motions of the optical elements of a beamline, which allow modifying one optical parameter without affecting the others. We describe a method to obtain analytic relationships between physical motions of mirrors and the corresponding variations of the beam parameters. This method has been implemented and tested at two beamlines at ALBA, where it is used to control the focus of the photon beam and its position independently. [ABSTRACT FROM AUTHOR]

During the last ten years, deflectometric profilometers have become indispensable tools for the precision form measurement of optical surfaces. They have proven to be especially suitable for characterizing beam-shaping optical surfaces for x-ray beamline applications at synchrotrons and free electron lasers. Deflectometric profilometers use surface slope (angle) to assess topography and utilize commercial autocollimators for the contactless slope measurement. To this purpose, the autocollimator beam is deflected by a movable optical square (or pentaprism) towards the surface where a co-moving aperture limits and defines the beam footprint. In this paper, we focus on the precise and reproducible alignment of the aperture relative to the autocollimator's optical axis. Its alignment needs to be maintained while it is scanned across the surface under test. The reproducibility of the autocollimator's measuring conditions during calibration and during its use in the profilometer is of crucial importance to providing precise and traceable angle metrology. In the first part of the paper, we present the aperture alignment procedure developed at the Advanced Light Source, Lawrence Berkeley National Laboratory, USA, for the use of their deflectometric profilometers. In the second part, we investigate the topic further by providing extensive ray tracing simulations and calibrations of a commercial autocollimator performed at the Physikalisch-Technische Bundesanstalt, Germany, for evaluating the effects of the positioning of the aperture on the autocollimator's angle response. The investigations which we performed are crucial for reaching fundamental metrological limits in deflectometric profilometry. [ABSTRACT FROM AUTHOR]

We describe experiments with a 45-cm long x-ray deformable mirror (XDM) that have been conducted in End Station 2, Beamline 5.3.1 at the Advanced Light Source. A detailed description of the hardware implementation is provided. We explain our one-dimensional Fresnel propagation code that correctly handles grazing incidence and includes a model of the XDM. This code is used to simulate and verify experimental results. Initial long trace profiler metrology of the XDM at 7.5 keV is presented. The ability to measure a large (150-nm amplitude) height change on the XDM is demonstrated. The results agree well with the simulated experiment at an error level of 1 μrad RMS. Direct imaging of the x-ray beam also shows the expected change in intensity profile at the detector. [ABSTRACT FROM AUTHOR]

We present a comprehensive investigation of the systematic and random errors of the nanometrology instruments used to characterize synchrotron X-ray optics at Diamond Light Source. With experimental skill and careful analysis, we show that these instruments used in combination are capable of measuring state-of-the-art X-ray mirrors. Examples are provided of how Diamond metrology data have helped to achieve slope errors of <100 nrad for optical systems installed on synchrotron beamlines, including: iterative correction of substrates using ion beam figuring and optimal clamping of monochromator grating blanks in their holders. Simulations demonstrate how random noise from the Diamond-NOM's autocollimator adds into the overall measured value of the mirror's slope error, and thus predict how many averaged scans are required to accurately characterize different grades of mirror. [ABSTRACT FROM AUTHOR]

The European XFEL (X-ray Free Electron Laser) is a large facility under construction in Hamburg, Germany. It will provide a transversally fully coherent x-ray radiation with outstanding characteristics: high repetition rate (up to 2700 pulses with a 0.6 ms long pulse train at 10 Hz), short wavelength (down to 0.05 nm), short pulse (in the femtoseconds scale), and high average brilliance (1.6 ・ 1025 (photons s-1 mm-2 mrad-2)/0.1% bandwidth). The beam has very high pulse energy; therefore, it has to be spread out on a relatively long mirror (about 1 m). Due to the very short wavelength, the mirrors need to have a high quality surface on their entire length, and this is considered very challenging even with the most advanced polishing methods. In order to measure the mirrors and to characterize their interaction with the mechanical mount, we equipped a metrology laboratory with a large aperture Fizeau interferometer. The system is a classical 100 mm diameter commercial Fizeau, with an additional expander providing a 300 mm diameter beam. Despite the commercial nature of the system, special care has been taken in the polishing of the reference flats and in the expander quality. We report the first commissioning of the instrument, its calibration, and performance characterization, together with some preliminary results with the measurement of a 950 mm silicon substrate. The intended application is to characterize the final XFEL mirrors with nanometer accuracy. [ABSTRACT FROM AUTHOR]

For glancing-incidence optical systems, such as short-wavelength optics used for nano-focusing, incorporating physical factors in the calculations used for shape optimization can improve performance. Wavefront metrology, including the measurement of a mirror's shape or slope, is routinely used as input for mirror figure optimization on mirrors that can be bent, actuated, positioned, or aligned. Modeling shows that when the incident power distribution, distance from focus, angle of incidence, and the spatially varying reflectivity are included in the optimization, higher Strehl ratios can be achieved. Following the works of Marechal and Mahajan, optimization of the Strehl ratio (for peak intensity with a coherently illuminated system) occurs when the expectation value of the phase error's variance is minimized. We describe an optimization procedure based on regression analysis that incorporates these physical parameters. This approach is suitable for coherently illuminated systems of nearly diffraction-limited quality. Mathematically, this work is an enhancement of the methods commonly applied for ex situ alignment based on uniform weighting of all points on the surface (or a sub-region of the surface). It follows a similar approach to the optimization of apodized and non-uniformly illuminated optical systems. Significantly, it reaches a different conclusion than a more recent approach based on minimization of focal plane ray errors. [ABSTRACT FROM AUTHOR]

X-ray mirrors are needed for beam shaping and monochromatization at advanced research light sources, for instance, free-electron lasers and synchrotron sources. Such mirrors consist of a substrate and a coating. The shape accuracy of the substrate and the layer precision of the coating are the crucial parameters that determine the beam properties required for various applications. In principal, the selection of the layer materials determines the mirror reflectivity. A single layer mirror offers high reflectivity in the range of total external reflection, whereas the reflectivity is reduced considerably above the critical angle. A periodic multilayer can enhance the reflectivity at higher angles due to Bragg reflection. Here, the selection of a suitable combination of layer materials is essential to achieve a high flux at distinct photon energies, which is often required for applications such as microtomography, diffraction, or protein crystallography. This contribution presents the current development of a Ru/C multilayer mirror prepared by magnetron sputtering with a sputtering facility that was designed in-house at the Helmholtz-Zentrum Geesthacht. The deposition conditions were optimized in order to achieve ultra-high precision and high flux in future mirrors. Input for the improved deposition parameters came from investigations by transmission electron microscopy. The X-ray optical properties were investigated by means of X-ray reflectometry using Cu- and Mo-radiation. The change of the multilayer d-spacing over the mirror dimensions and the variation of the Bragg angles were determined. The results demonstrate the ability to precisely control the variation in thickness over the whole mirror length of 500 mm thus achieving picometer-precision in the meter-range. [ABSTRACT FROM AUTHOR]

Grazing incidence mirrors are used on most X-ray synchrotron beamlines to focus, collimate or suppress harmonics. Increasingly beamline users are demanding variable beam shapes and sizes at the sample position. We have now developed a new concept to rapidly vary the beam size and shape of a focused X-ray beam. The surface of an elliptically figured mirror is divided into a number of laterally separated lanes, each of which is given an additional longitudinal height profile calculated to shape the X-ray beam to a top-hat profile in the focal plane. We have now fabricated two prototype mirrors and present the results of metrology tests and measurements made with one of the mirrors focusing the X-rays on a synchrotron beamline. We envisage that such mirrors could be widely applied to rapid beam-size switching on many synchrotron beamlines. [ABSTRACT FROM AUTHOR]

X-ray magnetic circular dichroism spectroscopy using an X-ray free electron laser is demonstrated with spectra over the Fe L3,2-edges. The high brightness of the X-ray free electron laser combined with high accuracy detection of incident and transmitted Xrays enables ultrafast X-ray magnetic circular dichroism studies of unprecedented sensitivity. This new capability is applied to a study of all-optical magnetic switching dynamics of Fe and Gd magnetic sublattices in a GdFeCo thin film above its magnetization compensation temperature. [ABSTRACT FROM AUTHOR]

An experimental campaign aiming to investigate electron cyclotron resonance (ECR) plasma X-ray emission has been recently carried out at the ECRISs-Electron Cyclotron Resonance Ion Sources laboratory of Atomki based on a collaboration between the Debrecen and Catania ECR teams. In a first series, the X-ray spectroscopy was performed through silicon drift detectors and high purity germanium detectors, characterizing the volumetric plasma emission. The on-purpose developed collimation system was suitable for direct plasma density evaluation, performed "on-line" during beam extraction and charge state distribution characterization. A campaign for correlating the plasma density and temperature with the output charge states and the beam intensity for different pumping wave frequencies, different magnetic field profiles, and single-gas/gas-mixing configurations was carried out. The results reveal a surprisingly very good agreement between warm-electron density fluctuations, output beam currents, and the calculated electromagnetic modal density of the plasma chamber. A charge-coupled device camera coupled to a small pin-hole allowing X-ray imaging was installed and numerous X-ray photos were taken in order to study the peculiarities of the ECRIS plasma structure. [ABSTRACT FROM AUTHOR]

Films of the topological insulator Bi2Se3 are grown by molecular beam epitaxy with in-situ reflection high-energy electron diffraction. The films are shown to be high-quality by X-ray reflectivity and diffraction and atomic-force microscopy. Quantum interference control of photocurrents is observed by excitation with harmonically related pulses and detected by terahertz radiation. The injection current obeys the expected excitation irradiance dependence, showing linear dependence on the fundamental pulse irradiance and square-root irradiance dependence of the frequencydoubled optical pulses. The injection current also follows a sinusoidal relative-phase dependence between the two excitation pulses. These results confirm the third-order nonlinear optical origins of the coherently controlled injection current. Experiments are compared to a tight-binding band structure to illustrate the possible optical transitions that occur in creating the injection current. [ABSTRACT FROM AUTHOR]

Films of the topological insulator Bi2Se3 are grown by molecular beam epitaxy with in-situ reflection high-energy electron diffraction. The films are shown to be high-quality by X-ray reflectivity and diffraction and atomic-force microscopy. Quantum interference control of photocurrents is observed by excitation with harmonically related pulses and detected by terahertz radiation. The injection current obeys the expected excitation irradiance dependence, showing linear dependence on the fundamental pulse irradiance and square-root irradiance dependence of the frequencydoubled optical pulses. The injection current also follows a sinusoidal relative-phase dependence between the two excitation pulses. These results confirm the third-order nonlinear optical origins of the coherently controlled injection current. Experiments are compared to a tight-binding band structure to illustrate the possible optical transitions that occur in creating the injection current. [ABSTRACT FROM AUTHOR]

During layer-by-layer homoepitaxial growth, both the Reflection High-Energy Electron Diffraction (RHEED) intensity and the x-ray reflection intensity will oscillate, and each complete oscillation indicates the addition of one monolayer of material. However, it is well documented, but not well understood, that the phase of the RHEED oscillations varies from growth to growth and thus the maxima in the RHEED intensity oscillations do not necessarily occur at the completion of a layer. We demonstrate this by using simultaneous in situ x-ray reflectivity and RHEED to characterize layer-by-layer growth of SrTiO3. We show that we can control the RHEED oscillation phase by changing the pre-growth substrate annealing conditions, changing the RHEED oscillation phase by as much as 137°. In addition, during growth via pulsed laser deposition, the relaxation times between each laser pulse can be used to determine when a layer is complete, independent of the phase of the RHEED oscillation. [ABSTRACT FROM AUTHOR]

Surface-pressure versus molecular area isotherms, X-ray reflectivity, and X-ray near-total reflection fluorescence were used to study the properties of 1-(3-methoxycarbonyl)propyl-1-phenyl[6,6]C6i (PCBM) that was pre-mixed with cesium carbonate and spread as a film at the air-water interface. The pre-mixed PCBM with cesium carbonate demonstrated a strikingly strong effect on the organization of the film. Whereas films formed from pure PCBM solution were rough due to strong inter-molecular interactions, the films formed from the mixture were much smoother. This indicates that the cesium carbonate moderates the inter-molecular interactions among PCBM molecules, hinting that the cesium diffusion observed in inverted organic photovoltaic structures and the likely ensuing ionic Cs-PCBM interaction decrease aggregation tendency of PCBM. This implies that the use of cesium salts affects the morphology of the organic layer and consequently improves the efficiency of these devices. [ABSTRACT FROM AUTHOR]