Focusing synchrotron radiation using a polycapillary half‐focusing X‐ray lens for imaging

An imaging system based on a polycapillary half‐focusing X‐ray lens (PHFXRL) and synchrotron radiation source has been designed. The focal spot size and the gain in power density of the PHFXRL were 22 µm (FWHM) and 4648, respectively, at 14.0 keV. The spatial resolution of this new imaging system was better than 5 µm when an X‐ray charge coupled device with a pixel size of 10.9 × 10.9 µm was used. A fossil of an ancient biological specimen was imaged using this system.     

High‐energy X‐ray optics with silicon saw‐tooth refractive lenses

Silicon saw‐tooth refractive lenses have been in successful use for vertical focusing and collimation of high‐energy X‐rays (50–100 keV) at the 1‐ID undulator beamline of the Advanced Photon Source. In addition to presenting an effectively parabolic thickness profile, as required for aberration‐free refractive optics, these devices allow high transmission and continuous tunability in photon energy and focal length. Furthermore, the use of a single‐crystal material (i.e. Si) minimizes small‐angle scattering background. The focusing performance of such saw‐tooth lenses, used in conjunction with the 1‐ID beamline's bent double‐Laue monochromator, is presented for both short (～1:0.02) and long (～1:0.6) focal‐length geometries, giving line‐foci in the 2 µm–25 µm width range with 81 keV X‐rays. In addition, a compound focusing scheme was tested whereby the radiation intercepted by a distant short‐focal‐length lens is increased by having it receive a collimated beam from a nearer (upstream) lens. The collimation capabilities of Si saw‐tooth lenses are also exploited to deliver enhanced throughput of a subsequently placed small‐angular‐acceptance high‐energy‐resolution post‐monochromator in the 50–80 keV range. The successful use of such lenses in all these configurations establishes an important detail, that the pre‐monochromator, despite being comprised of vertically reflecting bent Laue geometry crystals, can be brilliance‐preserving to a very high degree.     

Large‐aperture prism‐array lens for high‐energy X‐ray focusing

A new prism‐array lens for high‐energy X‐ray focusing has been constructed using an array of different prisms obtained from different parabolic structures by removal of passive parts of material leading to a multiple of 2π phase variation. Under the thin‐lens approximation the phase changes caused by this lens for a plane wave are exactly the same as those caused by a parabolic lens without any additional corrections when they have the same focal length, which will provide good focusing; at the same time, the total transmission and effective aperture of this lens are both larger than those of a compound kinoform lens with the same focal length, geometrical aperture and feature size. This geometry can have a large aperture that is not limited by the feature size of the lens. Prototype nickel lenses with an aperture of 1.77 mm and focal length of 3 m were fabricated by LIGA technology, and were tested using CCD camera and knife‐edge scan method at the X‐ray Imaging and Biomedical Application Beamline BL13W1 at Shanghai Synchrotron Radiation Facility, and provided a focal width of 7.7 µm and a photon flux gain of 14 at an X‐ray energy of 50 keV.     

Improvement of spatial resolution of µ‐XRF by using a thin metal filter

An improvement of spatial resolution of µ‐XRF by using a thin metal filter was investigated. The size of the x‐ray beam focused by the polycapillary x‐ray lens depended on the energy of the characteristic x‐rays. Original spot sizes at the focal point were 48 µm for CrKα, 41 µm for NiKα, and 28 µm for MoKα, respectively. To make the x‐ray beam size small, Ti? Cu thin foil was placed between the output of the lens and the focal point as a metal filter to reduce the continuous x‐rays. Finally, the x‐ray microbeam size was improved to 30 µm by applying a filter. Clear 2D mapping images of Cr, Fe, and Ni in 300‐mesh stainless steel could be obtained by applying this filter. Copyright © 2008 John Wiley & Sons, Ltd.     

High‐flux hard X‐ray microbeam using a single‐bounce capillary with doubly focused undulator beam

A pre‐focused X‐ray beam at 12 keV and 9 keV has been used to illuminate a single‐bounce capillary in order to generate a high‐flux X‐ray microbeam. The BioCAT undulator X‐ray beamline 18ID at the Advanced Photon Source was used to generate the pre‐focused beam containing 1.2 × 10¹³ photons s^?1 using a sagittal‐focusing double‐crystal monochromator and a bimorph mirror. The capillary entrance was aligned with the focal point of the pre‐focused beam in order to accept the full flux of the undulator beam. Two alignment configurations were tested: (i) where the center of the capillary was aligned with the pre‐focused beam (`in‐line') and (ii) where one side of the capillary was aligned with the beam (`off‐line'). The latter arrangement delivered more flux (3.3 × 10¹² photons s^?1) and smaller spot sizes (≤10 µm FWHM in both directions) for a photon flux density of 4.2 × 10¹⁰ photons s^?1µm^?2. The combination of the beamline main optics with a large‐working‐distance (approximately 24 mm) capillary used in this experiment makes it suitable for many microprobe fluorescence applications that require a micrometer‐size X‐ray beam and high flux density. These features are advantageous for biological samples, where typical metal concentrations are in the range of a few ng cm^?2. Micro‐XANES experiments are also feasible using this combined optical arrangement.     

Detective quantum efficiency,modulation transfer function and energy resolution comparison between CdTe and silicon sensors bump‐bonded to XPAD3S

XPAD3S is a single‐photon‐counting chip developed in collaboration by SOLEIL Synchrotron, the Institut Louis Néel and the Centre de Physique de Particules de Marseille. The circuit, designed in the 0.25 µm IBM technology, contains 9600 square pixels with 130 µm side giving a total size of 1 cm × 1.5 cm. The main features of each pixel are: single threshold adjustable from 4.5 keV up to 35 keV, 2 ms frame rate, 10⁷ photons s^?1 mm^?2 maximum local count rate, and a 12‐bit internal counter with overflow allowing a full 27‐bit dynamic range to be reached. The XPAD3S was hybridized using the flip‐chip technology with both a 500 µm silicon sensor and a 700 µm CdTe sensor with Schottky contacts. Imaging performances of both detectors were evaluated using X‐rays from 6 keV up to 35 keV. The detective quantum efficiency at zero line‐pairs mm^?1 for a silicon sensor follows the absorption law whereas for CdTe a strong deficit at low photon energy, produced by an inefficient entrance layer, is measured. The modulation transfer function was evaluated and it was shown that both detectors present an ideal modulation transfer function at 26 keV, limited only by the pixel size. The influence of the Cd and Te K‐edges of the CdTe sensor was measured and simulated, establishing that fluorescence photons reduce the contrast transfer at the Nyquist frequency from 60% to 40% which remains acceptable. The energy resolution was evaluated at 6% with silicon using 16 keV X‐rays, and 8% with CdTe using 35 keV X‐rays. A 7 cm × 12 cm XPAD3 imager, built with eight silicon modules (seven circuits per module) tiled together, was successfully used for X‐ray diffraction experiments. A first result recently obtained with a new 2 cm × 3 cm CdTe imager is also presented.     

Focusing,collimation and flux throughput at the IMCA‐CAT bending‐magnet beamline at the Advanced Photon Source

The IMCA‐CAT bending‐magnet beamline was upgraded with a collimating mirror in order to achieve the energy resolution required to conduct high‐quality multi‐ and single‐wavelength anomalous diffraction (MAD/SAD) experiments without sacrificing beamline flux throughput. Following the upgrade, the bending‐magnet beamline achieves a flux of 8 × 10¹¹ photons s^?1 at 1 Å wavelength, at a beamline aperture of 1.5 mrad (horizontal) × 86 µrad (vertical), with energy resolution (limited mostly by the intrinsic resolution of the monochromator optics) δE/E = 1.5 × 10^?4 (at 10 kV). The beamline operates in a dynamic range of 7.5–17.5 keV and delivers to the sample focused beam of size (FWHM) 240 µm (horizontally) × 160 µm (vertically). The performance of the 17‐BM beamline optics and its deviation from ideally shaped optics is evaluated in the context of the requirements imposed by the needs of protein crystallography experiments. An assessment of flux losses is given in relation to the (geometric) properties of major beamline components.     

BioCARS: a synchrotron resource for time‐resolved X‐ray science

BioCARS, a NIH‐supported national user facility for macromolecular time‐resolved X‐ray crystallography at the Advanced Photon Source (APS), has recently completed commissioning of an upgraded undulator‐based beamline optimized for single‐shot laser‐pump X‐ray‐probe measurements with time resolution as short as 100 ps. The source consists of two in‐line undulators with periods of 23 and 27 mm that together provide high‐flux pink‐beam capability at 12 keV as well as first‐harmonic coverage from 6.8 to 19 keV. A high‐heat‐load chopper reduces the average power load on downstream components, thereby preserving the surface figure of a Kirkpatrick–Baez mirror system capable of focusing the X‐ray beam to a spot size of 90 µm horizontal by 20 µm vertical. A high‐speed chopper isolates single X‐ray pulses at 1 kHz in both hybrid and 24‐bunch modes of the APS storage ring. In hybrid mode each isolated X‐ray pulse delivers up to ～4 × 10¹⁰ photons to the sample, thereby achieving a time‐averaged flux approaching that of fourth‐generation X‐FEL sources. A new high‐power picosecond laser system delivers pulses tunable over the wavelength range 450–2000 nm. These pulses are synchronized to the storage‐ring RF clock with long‐term stability better than 10 ps RMS. Monochromatic experimental capability with Biosafety Level 3 certification has been retained.     

Point focusing with flat and wedged crossed multilayer Laue lenses

Point focusing measurements using pairs of directly bonded crossed multilayer Laue lenses (MLLs) are reported. Several flat and wedged MLLs have been fabricated out of a single deposition and assembled to realise point focusing devices. The wedged lenses have been manufactured by adding a stress layer onto flat lenses. Subsequent bending of the structure changes the relative orientation of the layer interfaces towards the stress‐wedged geometry. The characterization at ESRF beamline ID13 at a photon energy of 10.5 keV demonstrated a nearly diffraction‐limited focusing to a clean spot of 43 nm × 44 nm without significant side lobes with two wedged crossed MLLs using an illuminated aperture of approximately 17 µm × 17 µm to eliminate aberrations originating from layer placement errors in the full 52.7 µm × 52.7 µm aperture. These MLLs have an average individual diffraction efficiency of 44.5%. Scanning transmission X‐ray microscopy measurements with convenient working distances were performed to demonstrate that the lenses are suitable for user experiments. Also discussed are the diffraction and focusing properties of crossed flat lenses made from the same deposition, which have been used as a reference. Here a focal spot size of 28 nm × 33 nm was achieved and significant side lobes were noticed at an illuminated aperture of approximately 23 µm × 23 µm.     

Model‐independent structure factors from powder X‐ray diffraction: a novel approach

Under the experimental condition that all Bragg peaks in a powder X‐ray diffraction (PXRD) pattern have the same shape, one can readily obtain the Bragg intensities without fitting any parameters. This condition is fulfilled at the P02.1 beamline at PETRA III using the seventh harmonic from a 23 mm‐period undulator (60 keV) at a distance of 65 m. For grain sizes of the order of 1 µm, the Bragg peak shape in the PXRD is entirely determined by the diameter of the capillary containing the powder sample and the pixel size of the image plate detector, and consequently it is independent of the scattering angle. As an example, a diamond powder has been chosen and structure factors derived which are in accordance with those calculated from density functional theory methods of the WIEN2k package to within an accuracy that allows a detailed electron density analysis.     

Kirkpatrick–Baez mirrors to focus hard X‐rays in two dimensions as fabricated,tested and installed at the Advanced Photon Source

The micro‐focusing performance for hard X‐rays of a fixed‐geometry elliptical Kirkpatrick–Baez (K–B) mirrors assembly fabricated, tested and finally implemented at the micro‐probe beamline 8‐BM of the Advanced Photon Source is reported. Testing of the K–B mirror system was performed at the optics and detector test beamline 1‐BM. K–B mirrors of length 80 mm and 60 mm were fabricated by profile coating with Pt metal to produce focal lengths of 250 mm and 155 mm for 3 mrad incident angle. For the critical angle of Pt, a broad bandwidth of energies up to 20 keV applies. The classical K–B sequential mirror geometry was used, and mirrors were mounted on micro‐translation stages. The beam intensity profiles were measured by differentiating the curves of intensity data measured using a wire‐scanning method. A beam size of 1.3 µm (V) and 1.2 µm (H) was measured with monochromatic X‐rays of 18 keV at 1‐BM. After installation at 8‐BM the measured focus met the design requirements. In this paper the fabrication and metrology of the K–B mirrors are reported, as well as the focusing performances of the full mirrors‐plus‐mount set‐up at both beamlines.     

Theoretical consideration of an X‐ray Bragg‐reflection lens using the eikonal approximation

On the basis of the eikonal approximation, X‐ray Bragg‐case focusing by a perfect crystal with parabolic‐shaped entrance surface is considered theoretically. Expressions for focal distances, intensity gain and distribution around the focus spot as well as for the focus spot sizes are obtained. The condition of point focusing is presented. The experiment can be performed using X‐ray synchrotron radiation sources (particularly free‐electron lasers).     

A desktop X‐ray monochromator for synchrotron radiation based on refraction in mosaic prism lenses

Focusing planar refractive mosaic lenses based on triangular prism microstructures have been used as an alternative approach for wide‐bandpass monochromatization of high‐energy X‐rays. The strong energy dependence of the refractive index of the lens material leads to an analogous energy dependence of the focal length of the lens. The refractive mosaic lens, in comparison with the refractive lens of continuous parabolic profile, is characterized by a higher aperture because of reduced passive material. In combination with a well defined pinhole aperture in the focal plane, the transmittance of photons of an appropriate energy can be relatively high and photons of deviating energy can be efficiently suppressed. The photon energy can be tuned by translating the pinhole along the optical axis, and the bandwidth changed by selecting appropriate pinhole aperture and beam stop. This method of monochromatization was realised at the ANKA FLUO beamline using a mosaic lens together with a 20 µm pinhole and beam stop. An energy resolution of 2.0% at 16 keV has been achieved.     

A simple optical system delivering a tunable micrometer pink beam that can compensate for heat‐induced deformations

The radiation from an undulator reflected from one or more optical elements (usually termed `pink‐beam') is used in photon‐hungry experiments. The optical elements serve as a high‐energy cutoff and for focusing purposes. One of the issues with this configuration is maintaining the focal spot dimension as the energy of the undulator is varied, since this changes the heat load absorbed by the first optical element. Finite‐element analyses of the power absorbed by a side water‐cooled mirror exposed to the radiation emitted by an undulator at the Advanced Photon Source (APS) and at the APS after the proposed upgrade (APSU) reveals that the mirror deformation is very close to a convex cylinder creating a virtual source closer to the mirror than the undulator source. Here a simple optical system is described based on a Kirkpatrick–Baez pair which keeps the focus size to less than 2 µm (in the APSU case) with a working distance of 350 mm despite the heat‐load‐induced change in source distance. Detailed ray tracings at several photon energies for both the APS and APSU show that slightly decreasing the angle of incidence on the mirrors corrects the change in the `virtual' position of the source. The system delivers more than 70% of the first undulator harmonic with very low higher‐orders contamination for energies between 5 and 10 keV.     

Mini‐beam collimator enables microcrystallography experiments on standard beamlines

The high‐brilliance X‐ray beams from undulator sources at third‐generation synchrotron facilities are excellent tools for solving crystal structures of important and challenging biological macromolecules and complexes. However, many of the most important structural targets yield crystals that are too small or too inhomogeneous for a `standard' beam from an undulator source, ～25–50 µm (FWHM) in the vertical and 50–100 µm in the horizontal direction. Although many synchrotron facilities have microfocus beamlines for other applications, this capability for macromolecular crystallography was pioneered at ID‐13 of the ESRF. The National Institute of General Medical Sciences and National Cancer Institute Collaborative Access Team (GM/CA‐CAT) dual canted undulator beamlines at the APS deliver high‐intensity focused beams with a minimum focal size of 20 µm × 65 µm at the sample position. To meet growing user demand for beams to study samples of 10 µm or less, a `mini‐beam' apparatus was developed that conditions the focused beam to either 5 µm or 10 µm (FWHM) diameter with high intensity. The mini‐beam has a symmetric Gaussian shape in both the horizontal and vertical directions, and reduces the vertical divergence of the focused beam by 25%. Significant reduction in background was achieved by implementation of both forward‐ and back‐scatter guards. A unique triple‐collimator apparatus, which has been in routine use on both undulator beamlines since February 2008, allows users to rapidly interchange the focused beam and conditioned mini‐beams of two sizes with a single mouse click. The device and the beam are stable over many hours of routine operation. The rapid‐exchange capability has greatly facilitated sample screening and resulted in several structures that could not have been obtained with the larger focused beam.     

Ultra‐thin optical grade scCVD diamond as X‐ray beam position monitor

Results of measurements made at the SIRIUS beamline of the SOLEIL synchrotron for a new X‐ray beam position monitor based on a super‐thin single crystal of diamond grown by chemical vapor deposition (CVD) are presented. This detector is a quadrant electrode design processed on a 3 µm‐thick membrane obtained by argon–oxygen plasma etching the central area of a CVD‐grown diamond plate of 60 µm thickness. The membrane transmits more than 50% of the incident 1.3 keV energy X‐ray beam. The diamond plate was of moderate purity (～1 p.p.m. nitrogen), but the X‐ray beam induced current (XBIC) measurements nevertheless showed a photo‐charge collection efficiency approaching 100% for an electric field of 2 V µm^?1, corresponding to an applied bias voltage of only 6 V. XBIC mapping of the membrane showed an inhomogeneity of more than 10% across the membrane, corresponding to the measured variation in the thickness of the diamond plate before the plasma etching process. The measured XBIC signal‐to‐dark‐current ratio of the device was greater than 10⁵, and the X‐ray beam position resolution of the device was better than a micrometer for a 1 kHz sampling rate.     

Polycapillary‐optics‐based micro‐XANES and micro‐EXAFS at a third‐generation bending‐magnet beamline

A focusing system based on a polycapillary half‐lens optic has been successfully tested for transmission and fluorescence µ‐X‐ray absorption spectroscopy at a third‐generation bending‐magnet beamline equipped with a non‐fixed‐exit Si(111) monochromator. The vertical positional variations of the X‐ray beam owing to the use of a non‐fixed‐exit monochromator were shown to pose only a limited problem by using the polycapillary optic. The expected height variation for an EXAFS scan around the Fe K‐edge is approximately 200 µm on the lens input side and this was reduced to ～1 µm for the focused beam. Beam sizes (FWHM) of 12–16 µm, transmission efficiencies of 25–45% and intensity gain factors, compared with the non‐focused beam, of about 2000 were obtained in the 7–14 keV energy range for an incoming beam of 0.5 × 2 mm (vertical × horizontal). As a practical application, an As K‐edge µ‐XANES study of cucumber root and hypocotyl was performed to determine the As oxidation state in the different plant parts and to identify a possible metabolic conversion by the plant.     

Design of an ultrahigh‐energy‐resolution and wide‐energy‐range soft X‐ray beamline

A new ultrahigh‐energy‐resolution and wide‐energy‐range soft X‐ray beamline has been designed and is under construction at the Shanghai Synchrotron Radiation Facility. The beamline has two branches: one dedicated to angle‐resolved photoemission spectroscopy (ARPES) and the other to photoelectron emission microscopy (PEEM). The two branches share the same plane‐grating monochromator, which is equipped with four variable‐line‐spacing gratings and covers the 20–2000 eV energy range. Two elliptically polarized undulators are employed to provide photons with variable polarization, linear in every inclination and circular. The expected energy resolution is approximately 10 meV at 1000 eV with a flux of more than 3 × 10¹⁰ photons s^?1 at the ARPES sample positions. The refocusing of both branches is based on Kirkpatrick–Baez pairs. The expected spot sizes when using a 10 µm exit slit are 15 µm × 5 µm (horizontal × vertical FWHM) at the ARPES station and 10 µm × 5 µm (horizontal × vertical FWHM) at the PEEM station. The use of plane optical elements upstream of the exit slit, a variable‐line‐spacing grating and a pre‐mirror in the monochromator that allows the influence of the thermal deformation to be eliminated are essential for achieving the ultrahigh‐energy resolution.     

A dedicated small‐angle X‐ray scattering beamline with a superconducting wiggler source at the NSRRC

At the National Synchrotron Radiation Research Center (NSRRC), which operates a 1.5 GeV storage ring, a dedicated small‐angle X‐ray scattering (SAXS) beamline has been installed with an in‐achromat superconducting wiggler insertion device of peak magnetic field 3.1 T. The vertical beam divergence from the X‐ray source is reduced significantly by a collimating mirror. Subsequently the beam is selectively monochromated by a double Si(111) crystal monochromator with high energy resolution (ΔE/E? 2 × 10^?4) in the energy range 5–23 keV, or by a double Mo/B₄C multilayer monochromator for 10–30 times higher flux (～10¹¹ photons s^?1) in the 6–15 keV range. These two monochromators are incorporated into one rotating cradle for fast exchange. The monochromated beam is focused by a toroidal mirror with 1:1 focusing for a small beam divergence and a beam size of ～0.9 mm × 0.3 mm (horizontal × vertical) at the focus point located 26.5 m from the radiation source. A plane mirror installed after the toroidal mirror is selectively used to deflect the beam downwards for grazing‐incidence SAXS (GISAXS) from liquid surfaces. Two online beam‐position monitors separated by 8 m provide an efficient feedback control for an overall beam‐position stability in the 10 µm range. The beam features measured, including the flux density, energy resolution, size and divergence, are consistent with those calculated using the ray‐tracing program SHADOW. With the deflectable beam of relatively high energy resolution and high flux, the new beamline meets the requirements for a wide range of SAXS applications, including anomalous SAXS for multiphase nanoparticles (e.g. semiconductor core‐shell quantum dots) and GISAXS from liquid surfaces.     

Performance of a collimating L‐shaped laterally graded multilayer mirror for the IXS analyzer system at NSLS‐II

The L‐shaped laterally graded multilayer mirror is a vital part of the ultrahigh‐energy and momentum‐resolution inelastic X‐ray scattering spectrometer at the National Synchrotron Light Source II. This mirror was designed and implemented as a two‐dimensional collimating optic for the analyzer system. Its performance was characterized using a secondary large‐divergence source at the 30‐ID beamline of the Advanced Photon Source, which yielded an integrated reflectivity of 47% and a collimated beam divergence of 78 µrad with a source size of 10 µm. Numerical simulations of the mirror performance in tandem with the analyzer crystal optics provided details on the acceptance sample volume in forward scattering and defined the technical requirements on the mirror stability and positioning precision. It was shown that the mirror spatial and angular stability must be in the range <8.4 µm and <21.4 µrad, respectively, for reliable operation of the analyzer.