Diffractive–refractive optics: (+,−,−,+) X‐ray crystal monochromator with harmonics separation

A new kind of two channel‐cut crystals X‐ray monochromator in dispersive (+,?,?,+) position which spatially separates harmonics is proposed. The diffracting surfaces are oriented so that the diffraction is inclined. Owing to refraction the diffracted beam is sagittally deviated. The deviation depends on wavelength and is much higher for the first harmonics than for higher harmonics. This leads to spatial harmonics separation. The idea is supported by ray‐tracing simulation.     

High‐power‐load DCLM monochromator for a computed tomography program at BMIT at energies of 25–150 keV

The research program at the biomedical imaging facility requires a high‐flux hard‐X‐ray monochromator that can also provide a wide beam. A wide energy range is needed for standard radiography, phase‐contrast imaging, K‐edge subtraction imaging and monochromatic beam therapy modalities. The double‐crystal Laue monochromator, developed for the BioMedical Imaging and Therapy facility, is optimized for the imaging of medium‐ and large‐scale samples at high energies with the resolution reaching 4 µm. A pair of 2 mm‐thick Si(111) bent Laue‐type crystals were used in fixed‐exit beam mode with a 16 mm vertical beam offset and the first crystal water‐cooled. The monochromator operates at energies from 25 to 150 keV, and the measured size of the beam is 189 mm (H) × 8.6 mm (V) at 55 m from the source. This paper presents our approach in developing a complete focusing model of the monochromator. The model uses mechanical properties of crystals and benders to obtain a finite‐element analysis of the complete assembly. The modeling results are compared and calibrated with experimental measurements. Using the developed analysis, a rough estimate of the bending radius and virtual focus (image) position of the first crystal can be made, which is also the real source for the second crystal. On the other hand, by measuring the beam height in several points in the SOE‐1 hutch, the virtual focus of the second crystal can be estimated. The focusing model was then calibrated with measured mechanical properties, the values for the force and torque applied to the crystals were corrected, and the actual operating parameters of the monochromator for fine‐tuning were provided.     

X‐ray analyzer‐based phase‐contrast computed laminography

X‐ray analyzer‐based phase‐contrast imaging is combined with computed laminography for imaging regions of interest in laterally extended flat specimens of weak absorption contrast. The optics discussed here consist of an asymmetrically cut collimator crystal and a symmetrically cut analyzer crystal arranged in a nondispersive (+, ?) diffraction geometry. A generalized algorithm is given for calculating multi‐contrast (absorption, refraction and phase contrast) images of a sample. Basic formulae are also presented for laminographic reconstruction. The feasibility of the method discussed was verified at the vertical wiggler beamline BL‐14B of the Photon Factory. At a wavelength of 0.0733 nm, phase‐contrast sectional images of plastic beads were successfully obtained. Owing to strong circular artifacts caused by a sample holder, the field of view was limited to about 6 mm in diameter.     

Possibility of X‐ray pulse compression using an asymmetric or inclined double‐crystal monochromator

It is shown theoretically that the asymmetric or inclined double‐crystal X‐ray monochromator may be used for X‐ray pulse compression if the pulse is properly chirped. By adjusting the mutual distance of the two asymmetric or inclined crystals it should be possible to achieve even a sub‐femtosecond compression of a chirped free‐electron laser pulse. The small d‐spacing of the crystal enables a more compact scheme compared with the currently used grating compression scheme. The asymmetric cut of the crystal enables the acceptance of a larger bandwidth. The inclined cut has larger tunability.     

Collimating Montel mirror as part of a multi‐crystal analyzer system for resonant inelastic X‐ray scattering

Advances in resonant inelastic X‐ray scattering (RIXS) have come in lockstep with improvements in energy resolution. Currently, the best energy resolution at the Ir L₃‐edge stands at ～25 meV, which is achieved using a diced Si(844) spherical crystal analyzer. However, spherical analyzers are limited by their intrinsic reflection width. A novel analyzer system using multiple flat crystals provides a promising way to overcome this limitation. For the present design, an energy resolution at or below 10 meV was selected. Recognizing that the angular acceptance of flat crystals is severely limited, a collimating element is essential to achieve the necessary solid‐angle acceptance. For this purpose, a laterally graded, parabolic, multilayer Montel mirror was designed for use at the Ir L₃‐absorption edge. It provides an acceptance larger than 10 mrad, collimating the reflected X‐ray beam to smaller than 100 µrad, in both vertical and horizontal directions. The performance of this mirror was studied at beamline 27‐ID at the Advanced Photon Source. X‐rays from a diamond (111) monochromator illuminated a scattering source of diameter 5 µm, generating an incident beam on the mirror with a well determined divergence of 40 mrad. A flat Si(111) crystal after the mirror served as the divergence analyzer. From X‐ray measurements, ray‐tracing simulations and optical metrology results, it was established that the Montel mirror satisfied the specifications of angular acceptance and collimation quality necessary for a high‐resolution RIXS multi‐crystal analyzer system.     

Utilizing broadband X‐rays in a Bragg coherent X‐ray diffraction imaging experiment

A method is presented to simplify Bragg coherent X‐ray diffraction imaging studies of complex heterogeneous crystalline materials with a two‐stage screening/imaging process that utilizes polychromatic and monochromatic coherent X‐rays and is compatible with in situ sample environments. Coherent white‐beam diffraction is used to identify an individual crystal particle or grain that displays desired properties within a larger population. A three‐dimensional reciprocal‐space map suitable for diffraction imaging is then measured for the Bragg peak of interest using a monochromatic beam energy scan that requires no sample motion, thus simplifying in situ chamber design. This approach was demonstrated with Au nanoparticles and will enable, for example, individual grains in a polycrystalline material of specific orientation to be selected, then imaged in three dimensions while under load.     

Design and performance of an ultra‐high‐vacuum‐compatible artificial channel‐cut monochromator

The design and performance of a novel ultra‐high‐vacuum‐compatible artificial channel‐cut monochromator that has been commissioned at undulator beamline 8‐ID‐I at the Advanced Photon Source are presented. Details of the mechanical and optical design, control system implementation and performance of the new device are given. The monochromator was designed to meet the challenging stability and optical requirements of the X‐ray photon correlation spectroscopy program hosted at this beamline. In particular, the device incorporates a novel in‐vacuum sine‐bar drive mechanism for the combined pitch motion of the two crystals and a flexure‐based high‐stiffness weak‐link mechanism for fine‐tuning the pitch and roll of the second crystal relative to the first crystal. The monochromator delivers an exceptionally uniform and stable beam and thereby improved brilliance preservation.     

Spectrometer for hard X‐ray free‐electron laser based on diffraction focusing

X‐ray free‐electron lasers (XFELs) generate sequences of ultra‐short spatially coherent pulses of X‐ray radiation. A diffraction focusing spectrometer (DFS), which is able to measure the whole energy spectrum of the radiation of a single XFEL pulse with an energy resolution of ΔE/E? 2 × 10^?6, is proposed. This is much better than for most modern X‐ray spectrometers. Such resolution allows one to resolve the fine spectral structure of the XFEL pulse. The effect of diffraction focusing occurs in a single‐crystal plate due to dynamical scattering, and is similar to focusing in a Pendry lens made from a metamaterial with a negative refraction index. Such a spectrometer is easier to operate than those based on bent crystals. It is shown that the DFS can be used in a wide energy range from 5 keV to 20 keV.     

Spatial structure of a focused X‐ray beam diffracted from crystals

The spatial structure of a beam focused by a planar refractive lens and Bragg diffracted from perfect silicon crystals was experimentally studied at the focal plane using a knife‐edge scan and a high‐resolution CCD camera. The use of refractive lenses allowed for a detailed comparison with theory. It was shown that diffraction leads to broadening of the focused beam owing to the extinction effect and, for a sufficiently thin crystal, to the appearance of a second peak owing to reflection from the back surface. It was found that the spatial structure of the diffracted beam depends on whether the crystal diffracts strongly (dynamically) or weakly (kinematically). The results help to understand the physical origin of the diffracted intensity recorded in a typical microbeam diffraction experiment.     

Silicon nitride transmission X‐ray mirrors

Transmission X‐ray mirrors have been fabricated from 300–400 nm‐thick low‐stress silicon nitride windows of size 0.6 mm × 85 mm. The windows act as a high‐pass energy filter at grazing incidence in an X‐ray beam for the beam transmitted through the window. The energy cut‐off can be selected by adjusting the incidence angle of the transmission mirror, because the energy cut‐off is a function of the angle of the window with respect to the beam. With the transmission mirror at the target angle of 0.22°, a 0.3 mm × 0.3 mm X‐ray beam was allowed to pass through the mirror with a cut‐off energy of 10 keV at the Cornell High Energy Synchrotron Source. The energy cut‐off can be adjusted from 8 to 12 keV at an angle of 0.26° to 0.18°, respectively. The observed mirror transmittance was above 80% for a 300 nm‐thick film.     

On aberrations in saw‐tooth refractive X‐ray lenses and on their removal

The X‐ray lens, which is composed of opposing canted saw‐tooth structures, originally assembled from cut‐out pieces from long‐playing records, is understood by recognizing that an incident plane X‐ray wave will traverse a varying number of triangular prisms in them. The refraction will deflect any beam towards the prism tips and the variation of the deflection angle, which grows linearly with the number of traversed prisms, can result in X‐ray focusing. The structure offers focusing flexibility by simply changing the taper angle. This report will discuss the aberrations arising in the saw‐tooth structure in its simplest form with identical prisms. It is found that the saw‐tooth structures in low‐Z materials with focal length below 1 m provide less flux density in the focal spot than stacks of one‐dimensionally focusing refractive lenses with identical transmission function. This is due to excessive aberrations in the regular structure, which are absent in stacks of concave lenses, and which limit the focusing to spot sizes of just submicrometre dimensions, as measured experimentally for some lenses. It will be shown that this limitation can be overcome by appropriately modifying the prism shape. Then the image size could be reduced by about an order of magnitude to the diffraction limit with competitive numbers even below 0.1 µm. Microfabrication techniques are identified as the appropriate means for producing the structures.     

A microfocus X‐ray fluorescence beamline at Indus‐2 synchrotron radiation facility

A microfocus X‐ray fluorescence spectroscopy beamline (BL‐16) at the Indian synchrotron radiation facility Indus‐2 has been constructed with an experimental emphasis on environmental, archaeological, biomedical and material science applications involving heavy metal speciation and their localization. The beamline offers a combination of different analytical probes, e.g. X‐ray fluorescence mapping, X‐ray microspectroscopy and total‐external‐reflection fluorescence characterization. The beamline is installed on a bending‐magnet source with a working X‐ray energy range of 4–20 keV, enabling it to excite K‐edges of all elements from S to Nb and L‐edges from Ag to U. The optics of the beamline comprises of a double‐crystal monochromator with Si(111) symmetric and asymmetric crystals and a pair of Kirkpatrick–Baez focusing mirrors. This paper describes the performance of the beamline and its capabilities with examples of measured results.     

IDATEN and G‐SITENNO: GUI‐assisted software for coherent X‐ray diffraction imaging experiments and data analyses at SACLA

Using our custom‐made diffraction apparatus KOTOBUKI‐1 and two multiport CCD detectors, cryogenic coherent X‐ray diffraction imaging experiments have been undertaken at the SPring‐8 Angstrom Compact free electron LAser (SACLA) facility. To efficiently perform experiments and data processing, two software suites with user‐friendly graphical user interfaces have been developed. The first is a program suite named IDATEN, which was developed to easily conduct four procedures during experiments: aligning KOTOBUKI‐1, loading a flash‐cooled sample into the cryogenic goniometer stage inside the vacuum chamber of KOTOBUKI‐1, adjusting the sample position with respect to the X‐ray beam using a pair of telescopes, and collecting diffraction data by raster scanning the sample with X‐ray pulses. Named G‐SITENNO, the other suite is an automated version of the original SITENNO suite, which was designed for processing diffraction data. These user‐friendly software suites are now indispensable for collecting a large number of diffraction patterns and for processing the diffraction patterns immediately after collecting data within a limited beam time.     

X‐ray focusing by the system of refractive lens(es) placed inside asymmetric channel‐cut crystals

An X‐ray one‐dimensionally focusing system, a refracting–diffracting lens (RDL), composed of Bragg double‐asymmetric‐reflecting two‐crystal plane parallel plates and a double‐concave cylindrical parabolic lens placed in the gap between the plates is described. It is shown that the focal length of the RDL is equal to the focal distance of the separate lens multiplied by the square of the asymmetry factor. One can obtain RDLs with different focal lengths for certain applications. Using the point‐source function of dynamic diffraction, as well as the Green function in a vacuum with parabolic approximation, an expression for the double‐diffracted beam amplitude for an arbitrary incident wave is presented. Focusing of the plane incident wave and imaging of a point source are studied. The cases of non‐absorptive and absorptive lenses are discussed. The intensity distribution in the focusing plane and on the focusing line, and its dependence on wavelength, deviation from the Bragg angle and magnification is studied. Geometrical optical considerations are also given. RDLs can be applied to focus radiation from both laboratory and synchrotron X‐ray sources, for X‐ray imaging of objects, and for obtaining high‐intensity beams. RDLs can also be applied in X‐ray astronomy.     

Transmission of an X‐ray beam through a two‐dimensional photonic crystal and the Talbot effect

Results of computer simulations of the transmission of an X‐ray beam through a two‐dimensional photonic crystal as well as the propagation of an X‐ray beam in free space behind the photonic crystal are reported. The photonic crystal consists of a square lattice of silicon cylinders of diameter 0.5 µm. The amount of matter in the path of the X‐ray beam rapidly decreases at the sides of the cylinder projections. Therefore the transmission is localized near the boundaries, and appears like a channeling effect. The iterative method of computer simulations is applied. This method is similar to the multi‐slice method that is widely used in electron microscopy. It allows a solution to be obtained with acceptable accuracy. A peculiarity in the intensity distribution inside the Talbot period z_T in free space was found when the intensity is approximately equal to the initial value at a distance 0.46z_T, and it is shifted by half a period at distance 0.5z_T. The reason for this effect is the existence of a periodic phase of the wavefunction of radiation inside the intensity peaks. Simulations with zero phase do not show this effect. Symmetry rules for the Talbot effect are discussed.     

The first microbeam synchrotron X‐ray fluorescence beamline at the Siam Photon Laboratory

The first microbeam synchrotron X‐ray fluorescence (µ‐SXRF) beamline using continuous synchrotron radiation from Siam Photon Source has been constructed and commissioned as of August 2011. Utilizing an X‐ray capillary half‐lens allows synchrotron radiation from a 1.4 T bending magnet of the 1.2 GeV electron storage ring to be focused from a few millimeters‐sized beam to a micrometer‐sized beam. This beamline was originally designed for deep X‐ray lithography (DXL) and was one of the first two operational beamlines at this facility. A modification has been carried out to the beamline in order to additionally enable µ‐SXRF and synchrotron X‐ray powder diffraction (SXPD). Modifications included the installation of a new chamber housing a Si(111) crystal to extract 8 keV synchrotron radiation from the white X‐ray beam (for SXPD), a fixed aperture and three gate valves. Two end‐stations incorporating optics and detectors for µ‐SXRF and SXPD have then been installed immediately upstream of the DXL station, with the three techniques sharing available beam time. The µ‐SXRF station utilizes a polycapillary half‐lens for X‐ray focusing. This optic focuses X‐ray white beam from 5 mm × 2 mm (H × V) at the entrance of the lens down to a diameter of 100 µm FWHM measured at a sample position 22 mm (lens focal point) downstream of the lens exit. The end‐station also incorporates an XYZ motorized sample holder with 25 mm travel per axis, a 5× ZEISS microscope objective with 5 mm × 5 mm field of view coupled to a CCD camera looking to the sample, and an AMPTEK single‐element Si (PIN) solid‐state detector for fluorescence detection. A graphic user interface data acquisition program using the LabVIEW platform has also been developed in‐house to generate a series of single‐column data which are compatible with available XRF data‐processing software. Finally, to test the performance of the µ‐SXRF beamline, an elemental surface profile has been obtained for a piece of ancient pottery from the Ban Chiang archaeological site, a UNESCO heritage site. It was found that the newly constructed µ‐SXRF technique was able to clearly distinguish the distribution of different elements on the specimen.     

Multiple‐element spectrometer for non‐resonant inelastic X‐ray spectroscopy of electronic excitations

A multiple‐analyser‐crystal spectrometer for non‐resonant inelastic X‐ray scattering spectroscopy installed at beamline ID16 of the European Synchrotron Radiation Facility is presented. Nine analyser crystals with bending radii R = 1 m measure spectra for five different momentum transfer values simultaneously. Using a two‐dimensional detector, the spectra given by all analysers can be treated individually. The spectrometer is based on a Rowland circle design with fixed Bragg angles of about 88°. The energy resolution can be chosen between 30–2000 meV with typical incident‐photon energies of 6–13 keV. The spectrometer is optimized for studies of valence and core electron excitations resolving both energy and momentum transfer.     

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/B₄C), 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.     

X‐ray dynamical diffraction Fraunhofer holography

An X‐ray dynamical diffraction Fraunhofer holographic scheme is proposed. Theoretically it is shown that the reconstruction of the object image by visible light is possible. The spatial and temporal coherence requirements of the incident X‐ray beam are considered. As an example, the hologram recording as well as the reconstruction by visible light of an absolutely absorbing wire are discussed.     

Coherent X‐ray diffractive imaging of protein crystals

The technique of coherent X‐ray diffraction imaging (CXDI) has recently shown great promise for the study of inorganic nanocrystals. In this work the CXDI method has been applied to the study of micrometer‐size protein crystals. Finely sampled diffraction patterns of single crystals were measured and iterative phase‐retrieval algorithms were used to reconstruct the two‐dimensional shape of the crystal. The density maps have limited reproducibility because of radiation damage, but show clear evidence for crystal facets. Qualitative analysis of a number of single‐crystal diffraction peaks indicates the presence of inward surface contraction on 2 µm size crystals. A survey of several hundred diffraction patterns yielded a number of examples with dramatic single‐sided streaks, for which a plausible model is constructed.