Refraction and ultra-small-angle scattering of X-rays in a single-crystal diamond compound refractive lens.

In this work a double-crystal setup is employed to study compound refractive lenses made of single-crystal diamond. The point spread function of the lens is calculated taking into account the lens transmission, the wavefront aberrations, and the ultra-small-angle broadening of the X-ray beam. It is shown that, similarly to the wavefront aberrations, the ultra-small-angle scattering effects can significantly reduce the intensity gain and increase the focal spot size. The suggested approach can be particularly useful for the characterization of refractive X-ray lenses composed of many tens of unit lenses.

Correlated Three-Dimensional Imaging of Dislocations: Insights into the Onset of Thermal Slip in Semiconductor Wafers.

Correlated x-ray diffraction imaging and light microscopy provide a conclusive picture of three-dimensional dislocation arrangements on the micrometer scale. The characterization includes bulk crystallographic properties like Burgers vectors and determines links to structural features at the surface. Based on this approach, we study here the thermally induced slip-band formation at prior mechanical damage in Si wafers. Mobilization and multiplication of preexisting dislocations are identified as dominating mechanisms, and undisturbed long-range emission from regenerative sources is discovered.

Erratum: Lattice Dynamics of EuO: Evidence for Giant Spin-Phonon Coupling [Phys. Rev. Lett. 116, 185501 (2016)].

This corrects the article DOI: 10.1103/PhysRevLett.116.185501.

Anomalous Lattice Dynamics of EuSi_{2} Nanoislands: Role of Interfaces Unveiled.

We report a systematic lattice dynamics study of EuSi_{2} films and nanoislands by in situ nuclear inelastic scattering on ^{151}Eu and ab initio theory. The Eu-partial phonon density of states of the nanoislands exhibits anomalous excess of phonon states at low and high energies, not present in the bulk and at the EuSi_{2}(001) surface. We demonstrate that atomic vibrations along the island-substrate interface give rise to phonon states both at low and high energies, while atomic vibrations across the island-island interface result in localized high-energy phonon modes.

Lattice Dynamics of EuO: Evidence for Giant Spin-Phonon Coupling.

Comprehensive studies of lattice dynamics in the ferromagnetic semiconductor EuO have been performed by a combination of inelastic x-ray scattering, nuclear inelastic scattering, and ab initio calculations. A remarkably large broadening of the transverse acoustic phonons was discovered at temperatures above and below the Curie temperature T_{C}=69 K. This result indicates a surprisingly strong momentum-dependent spin-phonon coupling induced by the spin dynamics in EuO.

Local strain and defects in silicon wafers due to nanoindentation revealed by full-field X-ray microdiffraction imaging.

Quantitative characterization of local strain in silicon wafers is critical in view of issues such as wafer handling during manufacturing and strain engineering. In this work, full-field X-ray microdiffraction imaging using synchrotron radiation is employed to investigate the long-range distribution of strain fields in silicon wafers induced by indents under different conditions in order to simulate wafer fabrication damage. The technique provides a detailed quantitative mapping of strain and defect characterization at the micrometer spatial resolution and holds some advantages over conventional methods.

Laboratory-based multi-modal X-ray microscopy and micro-CT with Bragg magnifiers.

We report on the successful demonstration of X-ray phase contrast microscopy and micro computed tomography (CT) with a Bragg magnifier microscope (BMM) in a laboratory setup. The Bragg magnifiers, constituted by two channel-cut crystals in asymmetric diffraction, produced a 15X magnification of the X-ray beam, thus enabling high resolution imaging to be attained. The angular sensitivity of the crystals was used to implement analyzer-based phase contrast imaging: acquiring images at different angular positions and the three parametric images (apparent absorption, differential phase and scattering) have been obtained. Micro-CT, with resolution of about 5 µm is demonstrated with the same system. The main limitations, as well as the ways to mitigate them, are discussed with the aid of the experimental data. The technique demonstrated herein extends high-resolution, multi-modal, x-ray imaging and micro-CT to compact laboratory setups, with the potential of broadening the reach of these techniques outside the community of synchrotron users.

Retrieval of the atomic displacements in the crystal from the coherent X-ray diffraction pattern.

The retrieval of spatially resolved atomic displacements is investigated via the phases of the direct(real)-space image reconstructed from the strained crystal's coherent X-ray diffraction pattern. It is demonstrated that limiting the spatial variation of the first- and second-order spatial displacement derivatives improves convergence of the iterative phase-retrieval algorithm for displacements reconstructions to the true solution. This approach is exploited to retrieve the displacement in a periodic array of silicon lines isolated by silicon dioxide filled trenches.

X-ray Bragg magnifier microscope as a linear shift invariant imaging system: image formation and phase retrieval.

We present the theoretical description of the image formation with the in-line germanium Bragg Magnifier Microscope (BMM) and the first successful phase retrieval of X-ray holograms recorded with this imaging system. The conditions under which the BMM acts as a linear shift invariant system are theoretically explained and supported by the experiment. Such an approach simplifies the mathematical treatment of the image formation and reconstruction as complicated propagation of the wavefront onto inclined planes can be avoided. Quantitative phase retrieval is demonstrated using a test sample and a proof of concept phase imaging of a spider leg is also presented.

Physical properties and biocompatibility of UHMWPE-derived materials modified by synchrotron radiation.

The applications of synchrotron radiation (SR) in medical imaging have become of great use, particularly in angiography, bronchography, mammography, computed tomography, and X-ray microscopy. Thanks to recently developed phase contrast imaging techniques non-destructive preclinical testing of low absorbing materials such as polymers has become possible. The focus of the present work is characterization and examination of UHMWPE-derived materials widely used in medicine, before and after their exposure to SR during such testing. Physical properties, such as wettability, surface energy, IR-spectroscopy, roughness, optical microscopy, microhardness measurements of UHMWPE samples were studied before and after SR. The relationship between a growth of UHMWPE surface hydrophilicity after SR and surface colonization by stromal cells was studied in vitro. Obtained results demonstrate that SR may be used as prospective direction to examine bulk (porous) structure of polymer materials and/or to modify polymer surface and volume for tissue engineering.

Comparative study of multilayers used in monochromators for synchrotron-based coherent hard X-ray imaging.

A systematic study is presented in which multilayers of different composition (W/Si, Mo/Si, Pd/B(4)C), periodicity (from 2.5 to 5.5 nm) and number of layers have been characterized. In particular, the intrinsic quality (roughness and reflectivity) as well as the performance (homogeneity and coherence of the outgoing beam) as a monochromator for synchrotron radiation hard X-ray micro-imaging are investigated. The results indicate that the material composition is the dominating factor for the performance. By helping scientists and engineers specify the design parameters of multilayer monochromators, these results can contribute to a better exploitation of the advantages of multilayer monochromators over crystal-based devices; i.e. larger spectral bandwidth and high photon flux density, which are particularly useful for synchrotron-based micro-radiography and -tomography.

Synchrotron-based radioscopy employing spatio-temporal micro-resolution for studying fast phenomena in liquid metal foams.

Investigations of pore coalescence and individual cell wall collapse in an expanding liquid metal foam by means of X-ray radioscopy with spatio-temporal micro-resolution are reported. By using white synchrotron radiation for imaging, the rupture of a film and the subsequent merger of two neighbouring bubbles could be recorded with a time sampling rate of 40000 frames s(-1) (25 micros exposure time) and a spatial sampling rate of 20 microm. The rupture time of a cell wall was found to be in the range of 300 micros. This value is in agreement with theoretical considerations which assume an inertia-dominated rupture time of cell walls in liquid metal foams.

Piezoelectric 3-D Fibrous Poly(3-hydroxybutyrate)-Based Scaffolds Ultrasound-Mineralized with Calcium Carbonate for Bone Tissue Engineering: Inorganic Phase Formation, Osteoblast Cell Adhesion, and Proliferation.

Elaboration of novel biocomposites providing simultaneously both biodegradability and stimulated bone tissue repair is essential for regenerative medicine. In particular, piezoelectric biocomposites are attractive because of a possibility to electrically stimulate cell response. In the present study, novel CaCO3-mineralized piezoelectric biodegradable scaffolds based on two polymers, poly[( R)3-hydroxybutyrate] (PHB) and poly[3-hydroxybutyrate- co-3-hydroxyvalerate] (PHBV), are presented. Mineralization of the scaffold surface is carried out by the in situ synthesis of CaCO3 in the vaterite and calcite polymorphs using ultrasound (U/S). Comparative characterization of PHB and PHBV scaffolds demonstrated an impact of the porosity and surface charge on the mineralization in a dynamic mechanical system, as no essential distinction was observed in wettability, structure, and surface chemical compositions. A significantly higher (4.3 times) piezoelectric charge and a higher porosity (∼15%) lead to a more homogenous CaCO3 growth in 3-D fibrous structures and result in a two times higher relative mass increase for PHB scaffolds compared to that for PHBV. This also increases the local ion concentration incurred upon mineralization under U/S-generated dynamic mechanical conditions. The modification of the wettability for PHB and PHBV scaffolds from hydrophobic (nonmineralized fibers) to superhydrophilic (mineralized fibers) led to a pronounced apatite-forming behavior of scaffolds in a simulated body fluid. In turn, this results in the formation of a dense monolayer of well-distributed and proliferated osteoblast cells along the fibers. CaCO3-mineralized PHBV surfaces had a higher osteoblast cell adhesion and proliferation assigned to a higher amount of CaCO3 on the surface compared to that on PHB scaffolds, as incurred from micro-computed tomography (µCT). Importantly, a cell viability study confirmed biocompatibility of all the scaffolds. Thus, hybrid biocomposites based on the piezoelectric PHB polymers represent an effective scaffold platform functionalized by an inorganic phase and stimulating the growth of the bone tissue.

Analysis of spatial cross-correlations in multi-constituent volume data.

We investigate spatial cross-correlations between two constituents, both belonging to the same microstructure. These investigations are based on two approaches: one via the measurement of the cross-correlation function and the other uses the spatial distances between the constituents. The cross-correlation function can be measured using the fast Fourier transform, whereas the distances are determined via the Euclidean distance transform. The characteristics are derived from volume images obtained by synchrotron microtomography. As an example we consider pore formation in metallic foams, knowledge of which is important to control the foam production process. For this example, we discuss the spatial cross-correlation between the pore space and the blowing agent particles in detail.

Fresnel diffractograms from pure-phase wave fields under perfect spatio-temporal coherence: Non-linear/non-local aspects and far-field behavior.

Recently, the diffractogram, that is, the Fourier transform of the intensity contrast induced by Fresnel free-space propagation of a given (exit) wave field, was investigated non-perturbatively in the phase-scaling factor S (controlling the strength of phase variation) for the special case of a Gaussian phase of width [Formula: see text]. Surprisingly, an additional low-frequency zero σ* = σ*(S, F) >0 emerges critically at small Fresnel number F (σ proportional to square of 2D spatial frequency). Here, we study the S-scaling behavior of the entire diffractogram. We identify a valley of maximum S-scaling linearity in the F - σ plane corresponding to a nearly universal physical frequency ξml = (0:143 ± 0.001)w -1/2. Large values of F (near field) are shown to imply S-scaling linearity for low σ but nowhere else (overdamped non-oscillatory). In contrast, small F values (far field) entail distinct, sizable s-bands of good S-scaling linearity (damped oscillatory). These bands also occur in simulated diffractograms induced by a complex phase map (Lena). The transition from damped oscillatory to overdamped non-oscillatory diffractograms is shown to be a critical phenomenon for the Gaussian case. We also give evidence for the occurrence of this transition in an X-ray imaging experiment. Finally, we show that the extreme far-field limit generates a σ-universal diffractogram under certain requirements on the phase map: information on phase shape then is solely encoded in S-scaling behavior.

Optimizing structural and mechanical properties of cryogel scaffolds for use in prostate cancer cell culturing.

Prostate cancer (PCa) currently is the second most diagnosed cancer in men and the second most cause of cancer death after lung cancer in Western societies. This sets the necessity of modelling prostatic disorders to optimize a therapy against them. The conventional approach to investigating prostatic diseases is based on two-dimensional (2D) cell culturing. This method, however, does not provide a three-dimensional (3D) environment, therefore impeding a satisfying simulation of the prostate gland in which the PCa cells proliferate. Cryogel scaffolds represent a valid alternative to 2D culturing systems for studying the normal and pathological behavior of the prostate cells thanks to their 3D pore architecture that reflects more closely the physiological environment in which PCa cells develop. In this work the 3D morphology of three potential scaffolds for PCa cell culturing was investigated by means of synchrotron X-ray computed micro tomography (SXCµT) fitting the according requirements of high spatial resolution, 3D imaging capability and low dose requirements very well. In combination with mechanical tests, the results allowed identifying an optimal cryogel architecture, meeting the needs for a well-suited scaffold to be used for 3D PCa cell culture applications. The selected cryogel was then used for culturing prostatic lymph node metastasis (LNCaP) cells and subsequently, the presence of multi-cellular tumor spheroids inside the matrix was demonstrated again by using SXCµT.

Hard X-ray index of refraction tomography of a whole rabbit knee joint: A feasibility study.

We report results of the computed tomography reconstruction of the index of refraction in a whole rabbit knee joint examined at the photon energy of 51keV. Refraction based images make it possible to delineate the bone, cartilage, and soft tissues without adjusting the contrast window width and level. Density variations, which are related to tissue composition and are not visible in absorption X-ray images, are detected in the obtained refraction based images. We discuss why refraction-based images provide better detectability of low contrast features than absorption images.

Potential use of V-channel Ge(220) monochromators in X-ray metrology and imaging.

While channel-cut crystals, in which the diffracting surfaces in an asymmetric cut are kept parallel, can provide beam collimation and spectral beam shaping, they can in addition provide beam compression or expansion if the cut is V-shaped. The compression/expansion ratio depends in this case on the total asymmetry factor. If the Ge(220) diffraction planes and a total asymmetry factor in excess of 10 are used, the rocking curves of two diffractors will have a sufficient overlap only if the second diffractor is tuned slightly with respect to the first one. This study compares and analyses several ways of overcoming this mismatch, which is due to refraction, when the Cu Kα1 beam is compressed 21-fold in a V21 monochromator. A more than sixfold intensity increase was obtained if the matching was improved either by a compositional variation or by a thermal deformation. This provided an intensity gain compared with the use of a simple slit in a symmetrical channel-cut monochromator. The first attempt to overcome the mismatch by introducing different types of X-ray prisms for the required beam deflection is described as well. The performance of the V-shaped monochromators is demonstrated in two applications. A narrow collimated monochromatic beam obtained in the beam compressing mode was used for high-resolution grazing-incidence small-angle X-ray scattering measurements of a silicon sample with corrupted surface. In addition, a two-dimensional Bragg magnifier, based on two crossed V15 channel monochromators in beam expansion mode and tuned by means of unequal asymmetries, was successfully applied to high-resolution imaging of test structures in combination with a Medipix detector.

A portable molecular beam epitaxy system for in situ x-ray investigations at synchrotron beamlines.

A portable synchrotron molecular beam epitaxy (MBE) system is designed and applied for in situ investigations. The growth chamber is equipped with all the standard MBE components such as effusion cells with shutters, main shutter, cooling shroud, manipulator, reflection high energy electron diffraction setup, and pressure gauges. The characteristic feature of the system is the beryllium windows which are used for in situ x-ray measurements. An UHV sample transfer case allows in vacuo transfer of samples prepared elsewhere. We describe the system design and demonstrate its performance by investigating the annealing process of buried InGaAs self-organized quantum dots.

On the implementation of computed laminography using synchrotron radiation.

Hard x rays from a synchrotron source are used in this implementation of computed laminography for three-dimensional (3D) imaging of flat, laterally extended objects. Due to outstanding properties of synchrotron light, high spatial resolution down to the micrometer scale can be attained, even for specimens having lateral dimensions of several decimeters. Operating either with a monochromatic or with a white synchrotron beam, the method can be optimized to attain high sensitivity or considerable inspection throughput in synchrotron user and small-batch industrial experiments. The article describes the details of experimental setups, alignment procedures, and the underlying reconstruction principles. Imaging of interconnections in flip-chip and wire-bonded devices illustrates the peculiarities of the method compared to its alternatives and demonstrates the wide application potential for the 3D inspection and quality assessment in microsystem technology.