Measurement of the horizontal beam emittance of undulator radiation by tandem-double-slit optical system.

A tandem-double-slit optical system was constructed to evaluate the practical beam emittance of undulator radiation. The optical system was a combination of an upstream slit (S1) and downstream slit (S2) aligned on the optical axis with an appropriate separation. The intensity distribution after the double slits, I(x1, x2), was measured by scanning S1 and S2 in the horizontal direction. Coordinates having 1/\sqrt e intensity were extracted from I(x1, x2), whose contour provided the standard deviation ellipse in the x1-x2 space. I(x1, x2) was converted to the corresponding distribution in the phase space, I(x1, x1'). The horizontal beam emittance was evaluated to be 3.1 nm rad, which was larger than the value of 2.4 nm rad estimated by using ray-tracing. It was found that the increase was mainly due to an increase in beam divergence rather than size.

Inverse-phase composite zone plate providing deeper focus than the normal diffraction-limited depth of X-ray microbeams.

A novel type of zone plate (ZP), termed an inverse-phase composite ZP, is proposed to gain a deeper focus than the standard diffraction-limited depth of focus, with little reduction in spatial resolution. The structure is a combination of an inner ZP functioning as a conventional phase ZP and an outer ZP functioning with third-order diffraction with opposite phase to the inner ZP. Two-dimensional complex amplitude distributions neighboring the focal point were calculated using a wave-optical approach of diffraction integration with a monochromatic plane-wave illumination, where one dimension is the radial direction and the other dimension is the optical-axis direction. The depth of focus and the spatial resolution were examined as the main focusing properties. Two characteristic promising cases regarding the depth of focus were found: a pit-intensity focus with the deepest depth of focus, and a flat-intensity focus with deeper depth of focus than usual ZPs. It was found that twice the depth of focus could be expected with little reduction in the spatial resolution for 10 keV X-ray energy, tantalum zone material, 84 nm minimum fabrication zone width, and zone thickness of 2.645 µm. It was also found that the depth of focus and the spatial resolution were almost unchanged in the photon energy range from 8 to 12 keV. The inverse-phase composite ZP has high potential for use in analysis of practical thick samples in X-ray microbeam applications.

Atmospheric coherent X-ray diffraction imaging for in situ structural analysis at SPring-8 Hyogo beamline BL24XU.

Coherent X-ray diffraction imaging (CXDI) is a promising technique for non-destructive structural analysis of micrometre-sized non-crystalline samples at nanometre resolutions. This article describes an atmospheric CXDI system developed at SPring-8 Hyogo beamline BL24XU for in situ structural analysis and designed for experiments at a photon energy of 8 keV. This relatively high X-ray energy enables experiments to be conducted under ambient atmospheric conditions, which is advantageous for the visualization of samples in native states. The illumination condition with pinhole-slit optics is optimized according to wave propagation calculations based on the Fresnel-Kirchhoff diffraction formula so that the sample is irradiated by X-rays with a plane wavefront and high photon flux of ∼1 × 1010 photons/16 µmø(FWHM)/s. This work demonstrates the imaging performance of the atmospheric CXDI system by visualizing internal voids of sub-micrometre-sized colloidal gold particles at a resolution of 29.1 nm. A CXDI experiment with a single macroporous silica particle under controlled humidity was also performed by installing a home-made humidity control device in the system. The in situ observation of changes in diffraction patterns according to humidity variation and reconstruction of projected electron-density maps at 5.2% RH (relative humidity) and 82.6% RH at resolutions of 133 and 217 nm, respectively, were accomplished.

Note: Measurement of synchrotron radiation phase-space beam properties to verify astigmatism compensation in Fresnel zone plate focusing optics.

The intensity distribution in phase space of an X-ray synchrotron radiation beamline was measured using a pinhole camera method, in order to verify astigmatism compensation by a Fresnel zone plate focusing optical system. The beamline is equipped with a silicon double crystal monochromator. The beam size and divergence at an arbitrary distance were estimated. It was found that the virtual source point was largely different between the vertical and horizontal directions, which is probably caused by thermal distortion of the monochromator crystal. The result is consistent with our astigmatism compensation by inclining a Fresnel zone plate.

Point spread function measurement of an X-ray beam focused by a multilayer zone plate with narrow annular aperture.

The experimental procedure for obtaining the point spread function (PSF) of a focusing beam generated using an X-ray multilayer zone plate (MZP) with a narrow annular aperture has been developed. It was possible to reconstruct the PSF by applying the tomographic process to the measured dataset consisting of line spread functions (LSFs) in every radial direction on the focal plane. The LSFs were measured by a knife-edge scanning method of detecting scattered intensity. In the experimental work, quasi-monochromatic undulator radiation with a first harmonic energy of 20 keV was directly focused without a monochromator by the MZP, and the PSF was measured using this procedure. As a result, a near diffraction-limited focused beam size of 46 nm full width at half-maximum was obtained.

Micro-CT observations of the 3D distribution of calcium oxalate crystals in cotyledons during maturation and germination in Lotus miyakojimae seeds.

The cotyledon of legume seeds is a storage organ that provides nutrients for seed germination and seedling growth. The spatial and temporal control of the degradation processes within cotyledons has not been elucidated. Calcium oxalate (CaOx) crystals, a common calcium deposit in plants, have often been reported to be present in legume seeds. In this study, micro-computed tomography (micro-CT) was employed at the SPring-8 facility to examine the three-dimensional distribution of crystals inside cotyledons during seed maturation and germination of Lotus miyakojimae (previously Lotus japonicus accession Miyakojima MG-20). Using this technique, we could detect the outline of the embryo, void spaces in seeds and the cotyledon venation pattern. We found several sites that strongly inhibited X-ray transmission within the cotyledons. Light and polarizing microscopy confirmed that these areas corresponded to CaOx crystals. Three-dimensional observations of dry seeds indicated that the CaOx crystals in the L. miyakojimae cotyledons were distributed along lateral veins; however, their distribution was limited to the abaxial side of the procambium. The CaOx crystals appeared at stage II (seed-filling stage) of seed development, and their number increased in dry seeds. The number of crystals in cotyledons was high during germination, suggesting that CaOx crystals are not degraded for their calcium supply. Evidence for the conservation of CaOx crystals in cotyledons during the L. miyakojimae germination process was also supported by the biochemical measurement of oxalic acid levels.

Circular multilayer zone plate for high-energy x-ray nano-imaging.

A circular multilayer zone plate (MZP) was fabricated and its focusing performance was evaluated using 20-keV x-rays. MoSi(2) and Si layers were alternately deposited by DC magnetron sputtering on a wire core; all the interfaces satisfied the Fresnel zone condition. The measured line spread function was converted to a point spread function by tomographic reconstruction. The results suggest that the MZP has the potential to realize the diffraction-limited resolving power, which is calculated to be 35 nm using the diffraction integral. Furthermore, scanning transmission microscopy using the MZP could resolve a 50-nm line-and-space pattern.

A simple hard x-ray "nanoslit" for measuring wavefront intensity.

A new method is proposed for nanoscale hard x-ray measurements. This method uses a reflection on a heavy-metal wire that functions as a single slit with a nanoscale aperture for a parallel x-ray beam. This "nanoslit" can be used to perform high-spatial-resolution measurements of the intensity distribution of a wavefront that diverges from an aperture. In experiments, Fresnel fringes generated by a rectangular aperture were measured using a 300-microm-diameter platinum wire as the nanoslit. In these experiments, the finest fringes with a period of 26 nm could be successfully resolved.

Crystallinity estimation of thin silicon-on-insulator layers by means of diffractometry using a highly parallel X-ray microbeam.

An X-ray microbeam with a small angular divergence and a narrow energy bandwidth has been produced at BL24XU at SPring-8. The beam size was measured to be 3.1 microm and 1.6 microm in the horizontal and vertical directions, respectively, and the horizontal angular divergence was 4.0 arcsec. Using this microbeam the crystallinity estimation of thin layers on silicon-on-insulator (SOI) wafers is demonstrated. In reciprocal-space maps the lattice tilt variations were 80 arcsec and more than 220 arcsec in the SOI layers on bonded and SIMOX wafers, respectively. In equi-tilt maps, the typical equi-tilt areas of the SOI layers were 7 microm and 4 microm in size on the bonded and SIMOX wafers, respectively.

Trace elemental analysis of drugs of abuse using synchrotron radiation total reflection X-ray fluorescence analysis (SR-TXRF).

Synchrotron radiation total reflection X-ray fluorescence spectroscopy (SR-TXRF) was utilized to analyze various trace elements in small amounts of drugs of abuse. Sample amounts of 1 microL solutions containing 10 microg of drugs (methamphetamine, amphetamine, 3,4-methylenedioxymethamphetamine, cocaine, and heroin) were spotted on silicon wafers for direct analysis. In addition, a leaflet of marijuana was set directly on a silicon wafer, and opium in the form of a soft lump was smeared on another silicon wafer for analysis. In these experiments, about 10 pg of contaminant elements could be detected. For example, in a seized methamphetamine sample, iodine was found, which could be indicative of synthetic route. In seized 3,4-methylenedioxymethamphetamine samples, variable amounts of phosphorus, calcium, sulfur, and potassium were found, which could not be detected in a control 3,4-methylenedioxymethamphetamine sample. For marijuana and opium, two spectral patterns were obtained that were far different from each other and could be easily discriminated. Using SR-TXRF, pg amounts of each trace element in 10 microg of various drugs can be easily detected, which is not the case either for a standard TXRF experimental system or for other elemental analysis techniques.

High-resolution hard X-ray phase-contrast microscopy with a large-diameter and high-numerical-aperture zone plate.

An imaging transmission hard X-ray microscope has been constructed at beamline BL24XU of SPring-8. It makes use of a phase zone plate made of tantalum with a diameter of 1 mm and an outer-most zone width of 50 nm, aiming at a wide field of view and a high spatial resolution. The performance test was carried out at a photon energy of 10 keV. A field of view as wide as approximately 200 microm in diameter was achieved. The spatial resolution was measured to be 220 nm by analyzing a knife-edge image. Further, a line-and-space pattern as fine as 100 nm could be imaged. By placing a phase plate made of gold in the back focal plane of the zone plate, phase-contrast microscopy using Zernike's method was also carried out. The feasibility of phase-contrast microscopy for observing transparent samples was successfully demonstrated by imaging small polystyrene particles.