A compact, light weight and relatively inexpensive μ-XRF instrument that allows for non-destructive and local analysis of sub-mm samples with minor/trace level sensitivity was developed. Two versions of this prototype instrument exist: a table-top version that can be used in a laboratory environment while for in situ measurements a readily transportable version was constructed. Polycapillary lenses are used to focus the primary X-ray beam down to the level of 70–100 μm in diameter. Relative detection limits of transition elements in biological and glass matrices are situated at the 10–100 ppm level. These instruments are useful for characterization of various materials from the cultural heritage and forensic sector.

Single fibers of poly(p-phenylene terephthalamide) (PPTA; trade names: Kevlar(29), Kevlar(49), and Kevlar(149)) have been scanned through a 3 mu m diameter X-ray beam and the degree of orientation (f(c)) determined at every point. All samples show a gradient in f(c) values from the skin to the core. The highest degree of orientation was found at the edges of the fibers. This effect is particularly strong for Kevlar(29). In addition, ripples in orientation were observed along the fiber axis for Kevlar(29), but on a smaller scale than the transversal gradient. Upon tensile deformation up to about 3 GPa applied stress, the transversal f(c) anisotropy is gradually reduced and disappears at the highest stress values. Kevlar(29) attains at about 1.5 GPa applied stress the same degree of orientation as Kevlar(49).

Wide angle X-ray scattering (WAXS) data recorded during the drawing of poly(ethylene terephthalate) (PET) under industrial processing conditions was analysed in terms of changes in the degree of polymer orientation and crystallinity over a wide range of draw temperatures and draw ratios. The actual draw rate and draw ratio at the region in the specimen from which X-ray data was recorded was determined independently with high consistency by direct video observation of strain and total X-ray scattering. In contrast to previous claims, the start of strain-induced crystallization coincided with the end of draw within the 40ms time-resolution of the investigation. Crystallization has been shown to follow first order kinetics and the rate constant was determined over a range of temperatures from 85°C–125°C. Above 125°C little orientation is observed with no evidence of strain-induced crystallization. A detailed determination was made of the critical value of draw ratio below which strain-induced crystallization does not occur and where a relaxation in molecular orientation is observed after the extension process. The implications of these experimental observations for existing theory of strain-induced polymer crystallization are discussed.

Keratinous tissues play two major roles in the adaptation of vertebrates to their environment: a strong mechanical support and a chemical barrier. In order to determine whether these properties may originate from different zones in the tissues, microdiffraction experiments on the micrometre scale have been carried out on feather shaft, horse and human hair, and porcupine quill samples. The existence of several structural layers has been revealed in all the tissues, some corresponding to highly ordered α- or β-type keratin and the others to more or less amorphous keratin. The existence of lipid granules has also been evidenced, mainly in the outer layers. This study shows one of the possibilities which are now offered by third-generation synchrotron sources for the structural microanalysis of biological tissues.

Abstract Three small-angle scattering cameras based on mirror/monochromator optics, a circular Bragg-Fresnel (BF) lens, and a microcollimation system combined with a double-focusing mirror have been tested for microfocusing applications. In order to reach a focal spot less than or equal to 10 μm. a microcollimation system provides a flexible solution for medium-resolution applications. When using a glass capillary as a collimation system, a minimum s-value of 5·10−2 nm−1 was attained. Scanning small-angle x-ray scattering (SAXS) patterns from a poly(tetramethyl-p-silphenylene)-siloxane spherulite and a 40-μm polyethyl-eneterephthalate fiber were obtained in a few seconds per pattern with a 4 μm diameter beam at a wavelength of λ = 0.095 nm.

This is the first report on a series of studies of the crystallinity of bone tissues. The measurements were done at the microfocused diffraction beamline at ERSF (European Synchrotron Radiation Facility) as a feasibility test on various aspects on microdiffraction analysis. Beside the crystal structure, crystallite size distribution and preferential orientation were also studied, with a spatial resolution of 7μm. The experiments were performed at the microfocus beam line 1 at European Synchrotron Radiation Facility (ESRF). The samples were longitudinal and transversal cuts from human femoral shafts. Over 65 diffraction lines from apatite structure could be identified. The results show that the bone crystallites seem to be oriented in two orthogonal directions, one parallel with the Haversian system and the other perpendicular following the lamella’s curvature. Peak width analysis shows that the crystallites are about 25–40nm along the c-axis with a width of about 10nm. The result also shows that the peak width is somewhat larger close to the haversian canal compared with the outer region of the osteon.

Using a detailed ray-tracing code for capillary optics, interpretation is given for parallel bore hole and tapered capillary generated far-field images. These images can be used to indicate the presence of various types of surface imperfections (i.e., surface roughness or waviness) or shape distortions of the optical device. The capillary output patterns were recorded at the optical beam line of the European Synchrotron Radiation Facility by using a monochromatic, highly parallel incident synchrotron beam. Capillaries of various dimensions were studied, with inlet diameters in the range of 30–70 μm, outlet diameters of 22–42 μm, and capillary length values ranging from 10 to 23 cm. The far-field images were taken at a distance of 10–11 cm from the capillary exit using a high resolution charge coupled device camera. By comparisons of simulated and experimental capillary output patterns, the effects of surface roughness/waviness, as well as axial distortions are studied with respect to the angular distribution of the generated capillary beam.

With the opening of the first real ;third-generation' synchrotron source in Grenoble, in fall 1994, X-ray sources of unprecedented brilliances and qualities became available to the scientific community. Different X-ray analytical techniques could now be applied on a level that was unimaginable only a decade ago. Here are some preliminary results from an experiment where different analytical techniques have been applied on a micrometer level carried out at the most powerful synchrotron microbeam currently available in the world, the microfocus beamline (BL1) at ESRF. This beamline can now provide micrometer-sized X-ray beams with a flux density up to 10(10) photons microm(-2) at an energy of 13 keV and with a bandwidth of 10(-4). In this experiment, X-ray diffraction and X-ray fluorescence have been combined in order to obtain a precise and comprehensive micro-analytical description of micrometer-sized fly ash particles. These types of particles are heavily inhomogeneous with a very irregular shape that makes them inaccessible to conventional micro-analysis. The experiment was performed in a scanning mode and two-dimensional images of different analytical information were reconstructed from the data recorded during the scan. The major features and limitations of this micro-analytical technique will be outlined and different examples on how the analytical information can be used for generating two-dimensional images of the sample will be demonstrated and discussed.

By simultaneously recording X-ray fluorescence intensities and X-ray diffraction pattern at a microscopic level highly heterogeneous samples of fly-ash particles have been analyzed. From the data achieved by this combined experiment, the main minerals in the particles have been identified and the size distributions of these minerals have also been determined. The distribution of heavy elements, recorded from their fluorescent intensity, is presented and the impact of sample surface topology and anomalous attenuation is discussed. Estimates of the concentration of the these heavy elements are given and correlation analysis has been performed indicating that most of these elements seem to appear at the surface of the fly-ash particles.

The microfocus X-ray beamline at the European Synchrotron Radiation Facility has been used to investigate the variation in molecular orientation and crystallinity in the wall of a container fabricated from poly(ethylene terephthalate). Two-dimensional wide-angle X-ray scattering patterns were recorded and displayed in real time as the specimen was tracked across the incident X-ray beam enabling the measurement of textural changes to be made with a spatial resolution of ~2 mum.

An analysis of the background at the exit of tapered borosilicate glass capillaries in synchrotron radiation scattering experiments suggests scattering due to short-range order at larger angles while low-angle scattering is attributed to phase separation in the glass. Background scattering can be largely suppressed by introducing a pinhole aperture at the exit of the capillary. The lowest background was obtained for a pinhole approaching the size of the exit beam. Background reduction is particularly important for wide- and small-angle scattering experiments on weakly scattering samples like thin polymeric fibers.

The use of borosilicate-glass-capillary optics at a chosen wavelength for low scattering has been explored using an undulator beam at the ESRF. With a 2.3 mum beam at 0.092 nm wavelength, a silver behenate powder sample was scanned in two dimensions with a 2 mum step width. Scattering from single crystallites with d(001) = 5.83 nm could be observed. The limit for observation, at low angles, was ca s approximately 0.1 nm(-1) (s = 1/d for d approximately 10 nm).

A new and improved type of x-ray capillary optics unit (ellipsoidal), is developed, tested, and characterized using a table-top x-ray microbeam setup. The beam profiles of the x-ray beams generated by the 7.5 μm ellipsoidal capillary were constructed from ‘‘knife-edge’’ scans across the beam. The detection limits for various elements were determined, and the spatial resolution, when the beam was used in scanning mode, was demonstrated.

The microfocus X-ray beamline at the European Synchrotron Radiation Facility has been used to investigate the variation in molecular orientation and crystallinity in spherulites of the organic polymer poly-3-hydroxybutyrate (PHB). This is the first report of the correlation of optical and X-ray measurements on spherulitic polymer films where X-ray diffraction patterns have been recorded and displayed continuously in real time while the specimen was tracked in steps of 10 mum across an incident X-ray beam with a diameter as small as 10 mum.

The fluorescence X-ray scanning 2D microprobe based on a Bragg-Fresnel multilayer lens (BFML) has been tested at the ESRF, Grenoble (France) for the first time. A single elliptical BFML has been used for two-dimensional focusing of the X-ray synchrotron beam of an undulator source in the energy range of 12 keV. A spatial resolution of 2.4 μm and a photon intensity of about 1010 photons per second have been measured using a Cr knife-edge test object.

Status and development possibilities of microfocusing experiments in wide- and small angle scattering at the ESRF microfocus beamline are reported. The routinely available beam sizes range from ≈ 200 μm to 7 μm using mirror/monochromator optics. For the smallest beam size post collimation is required. Optics based on glass capillary and Bragg-Fresnel elements have been tested for μm or subμm applications.

A water-cooled double W/Si-multilayer monochromator has been operated at an ESRF low-beta undulator beam. For a fixed distance of the two multilayers the first-order Bragg reflection was at ~8 keV. The peak power density of the beam at the exit of the multilayers was ~1 W mm(-2) and the flux density of the first order after a 10 mum collimator was 4 x 10(5) photons s(-1) mum(-2) mA(-1.) The performance of the beam in microbeam diffraction has been tested on a 20 mum W wire. The observed pseudo-Laue pattern is discussed with respect to the multilayer spectrum.

An x-ray fluorescence microprobe with circular Bragg–Fresnel lens was tested at the European Synchrotron Radiation Facility Microfocus beamline. A focal spot of 0.7 μm was observed using the knife-edge technique at the energy 7.6 keV (wavelength 1.6 Å). The intensity in the focal spot was measured to 108 ph/s in energy bandwidth of 10−5. The fluorescence microprobe was applied for mapping 100 μm size micrometeorite at 13.5 keV.