Ray Barrett

Upgraded ESRF BM29 beamline for SAXS on macromolecules in solution

A description of the new ESRF BioSAXS beamline is given. The beamline presented is dedicated to small-angle X-ray scattering of macromolecules in solution operating with a high-throughput sample-changer robot and automated data analysis for quality control and feedback.

Ultra-high resolution zone-doubled diffractive X-ray optics for the multi-keV regime

X-ray microscopy based on Fresnel zone plates is a powerful technique for sub-100 nm resolution imaging of biological and inorganic materials. Here, we report on the modeling, fabrication and characterization of zone-doubled Fresnel zone plates for the multi-keV regime (4-12 keV). We demonstrate unprecedented spatial resolution by resolving 15 nm lines and spaces in scanning transmission X-ray microscopy, and focusing diffraction efficiencies of 7.5% at 6.2 keV photon energy. These developments represent a significant step towards 10 nm spatial resolution for hard X-ray energies of up to 12 keV.

Nanofocusing of hard X-ray free electron laser pulses using diamond based Fresnel zone plates

A growing number of X-ray sources based on the free-electron laser (XFEL) principle are presently under construction or have recently started operation. The intense, ultrashort pulses of these sources will enable new insights in many different fields of science. A key problem is to provide x-ray optical elements capable of collecting the largest possible fraction of the radiation and to focus into the smallest possible focus. As a key step towards this goal, we demonstrate here the first nanofocusing of hard XFEL pulses. We developed diamond based Fresnel zone plates capable of withstanding the full beam of the worlds most powerful x-ray laser. Using an imprint technique, we measured the focal spot size, which was limited to 320 nm FWHM by the spectral band width of the source. A peak power density in the focal spot of 4×1017 W/cm2 was obtained at 70 fs pulse length.

High-efficiency Fresnel zone plates for hard X-rays by 100 keV e-beam lithography and electroplating.

The efficiencies of several Fresnel zone plates, that were fabricated using a direct-write method with high-energy electrons, were measured over a wide range of photon energies.

The ID21 Scanning X-ray Microscope at ESRF

The ID21 Scanning X-ray Microscope (SXM) is optimized for micro-spectroscopy with submicron resolution in the 2 to 9.5 keV energy range. After a brief description of the microscope setup, we present here recent developments, in particular, the latest version of the compact Wavelength Dispersive Spectrometer and the refurbished cryo-stage.

High-resolution lenses for sub-100 nm x-ray fluorescence microscopy

We report on the design, fabrication, and testing of Fresnel zone plates for high-resolution x-ray fluorescence microscopy using the scanning x-ray microscope at the European Synchrotron Radiation Source. The germanium lenses were optimized for operation near the sulphur absorption edge at 2472 eV photon energy. The high measured diffraction efficiencies of up to 9.6% and the good match to the spatial coherence of the undulator beam resulted in a photon flux of about 4×108 photons per second within the bandwidth of a silicon 〈111〉 monochromator. Using a test object consisting of zinc sulphide nanostructures, we were able to image features in sulphur x-ray fluorescence mode with lateral dimensions down to below 100 nm.

High efficiency nano-focusing kinoform optics for synchrotron radiation.

Modern synchrotron sources have provided for decades intense beams of photons over a large energy spectrum. The availability of improved optics and detectors has opened up new opportunities for the study of matter at the micrometre and nanometre scale in many disciplines. Whilst exploitation of micro-focused beams occurs almost daily in many beamlines, the production of beams of 100 nm is achieved on few instruments which use specialised optics. Refractive lenses, zone plates, curved mirrors, multilayers, and multilayer Laue lenses, can all focus x-rays to less than 50 nm under strict beam stability conditions. Focusing the synchrotron radiation to beam sizes smaller than 10 nm is considered the ultimate goal for the current decade. Silicon micro-technology has so far provided some of the most advanced x-ray refractive lenses; we report on design and characterisation of a novel silicon kinoform lens that is capable of delivering nano-beams with high efficiency.

The ID21 X-ray and infrared microscopy beamline at the ESRF: status and recent applications to artistic materials

The ID21 beamline (European Synchrotron Radiation facility, France) is a multi micro-analytical platform combining X-ray and infrared micro-probes, for characterization of elements, species, molecular groups and crystalline structures in complex materials. Applications are mainly in the fields of cultural heritage, life science, environmental and earth sciences, materials sciences. Here, we first present the status of instruments: (i) the scanning micro-spectroscopy end-station, operating from 2.0 to 9.2 keV, under vacuum and offering cryo conditions, for the acquisition of 2D micro X-ray fluorescence (μXRF) maps, single point micro X-ray Absorption Near Edge Structure (μXANES) spectra and speciation maps with sub-micrometric resolution; (ii) the XANES full-field end-station, operating in the same vacuum and energy conditions, for the acquisition of hyper-spectral radiographs of thin concentrated samples, resulting in speciation maps with micrometric resolution and millimetric field of view; (iii) the scanning micro-X-ray diffraction (μXRD)/μXRF end-station, operating at 8.5 keV, in air, for the acquisition of 2D crystalline phase maps, with micrometric resolution; and (iv) the scanning infrared microscope, operating in the mid-infrared range for the acquisition of molecular maps and some structural maps with micrometric resolution. Recent hardware and software developments are presented, as well as new protocols for improved sample preparation of thin sections. Secondly, a review of recent applications for the study of cultural heritage is presented, illustrated by various examples: determination of the origin of the color in blue Chinese porcelains and in brown Sevres porcelains; detection of lead in ink on Herculaneum papyri; identification and degradation of modeling materials used by Auguste Rodin and of chrome yellow pigments used by Vincent van Gogh. Cryo capabilities are illustrated by the analysis of plants exposed to chromate solutions. These examples show the variety of materials analyzed, of questions tackled, and particularly the multiple advantages of the ID21 analytical platform for the analysis of ancient and artistic materials.

Current status of the Scanning X-ray Microscope at the ESRF

A short description of the Scanning X-ray Microscope of the ESRF ID21 X-ray microscopy beamline is given and the consequences of the relatively wide operating energy range discussed. The current capabilities of the instrument are demonstrated through images and spectra recorded from a variety of pilot experiments, including X-ray fluorescence imaging, microdiffraction and XANES measurements.

Scanning microscopy end station at the ESRF x-ray microscopy beamline

The ID21 x-ray microscopy beamline at the ESRF has two branchlines: one is dedicated to scanning microscopy techniques and the second to full-field imaging microscopy. The scanning x-ray microscope end station is designed for use over a relatively wide spectral range ranging from 0.2 to 8keV giving access to absorption edges from a wide range of elements of interest in both the biological and materials sciences. The microscope is operating initially with Fresnel zone plate optics and, apart from conventional absorption contrast imaging, is designed to accept a variety of complementary imaging modes. In particular considerable effort has been made to optimize the design for spectromicroscopy using both fluorescence imaging and scanning of the primary x-ray probe energy for XANES imaging. A brief overview of the beamline design is given. This is followed by a discussion of the implications of both the source characteristics and the required wide spectral range upon the optical design of the microscope and, leading from this, the technological choices which have been made. Preliminary results obtained with the microscope are presented.