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X-ray nanoprobe
After the major efforts made during 2015, swapping from start-up to routine operation of the three beamlines built within Phase I of the ESRF upgrade, all five XNP beamlines have been in full user operation in 2016. They provide a vast spectrum of techniques, imaging, diffraction and spectroscopy to our user community and offer nanobeams over an X-ray energy regime ranging from 2 to 35 keV. This flexibility in techniques is reflected in the great variety of scientific highlights ranging from hard condensed matter to biological and archaeological samples, and sample sizes ranging from individual nano-objects of 100 nm in size to samples of several centimetres.
Depending on the status of their development, the XNP beamlines have continued to polish their recently commissioned equipment or have launched ambitious refurbishment plans in accordance with the EBS project. The general trend shows a rapid increase in data recording speed and data dimensionality revealing the future challenges imposed by the treatment of huge amounts of data during experiments.
In this context, at ID01, we have started to implement sample environments such as high-temperature furnaces (up to 1000°C) and gas flow reactors in the Bragg coherent diffraction setup. These lightweight and compact environments can be carried by piezo scanners and scanned in the 100 nm beam in continuous motion to resolve structural changes on the sample or to monitor drift during temperature changes more easily. They reply as well to the ambitions of the full-field diffraction microscope, an endstation that became fully operational in 2016. For experiments requiring intense focused beams, the arrival of the KB mirrors in late 2016 should bring a decisive flux gain and will permit the use of the high-flux multilayer optics in nanofocusing mode. On the software side, a data analysis tool has been designed for ID01 with a graphical user interface able to handle the 5D datasets produced by the quick-mapping (K-MAP) of a sample in real (2D) and reciprocal space (3D).
At ID13, the integration of the EIGER 4M pixel array detector has progressed well allowing stable operation at up to 750 Hz. Based on this achievement, millimetre-scale fast continuous scanning with micrometre-scale resolution has become feasible. This enables scanning-SAXS/WAXS imaging of extended areas of square-millimetres yielding two-dimensional maps extracted from millions of diffraction patterns, i.e. resulting in megapixel raster images comparable in size to optical micrographs. The high frame rate of this detector is also being employed more often for time-resolved experiments close to one millisecond. Synchronisation with TTL-signal compatible user devices is possible. This offers many opportunities for fast in situ, in vivo, operando micro-/nano-beam studies on topics such as ultra-fast heating, mechanical testing, and micro-fluidics. Regarding nanobeam activities, ID13 has started operation of nanodiffraction with a sub 50 nm spot size for collaborators, with the aim of offering this option to all users by the end of 2017.
The nano-imaging beamline ID16A has successfully put into operation cryo-cooling of the sample stage. Analysing samples in the frozen hydrated state is a major milestone for the beamline and crucial to delay the effects of radiation damage in biological samples. A complete cryogenic workflow has been put in place, from fast sample freezing to analysis in the X-ray microscope. For room temperature analysis, the capacity of the sample changer has been increased from four to sixteen, leading to a significant improvement in the throughput of the instrument. All imaging modalities of the microscope, fluorescence analysis, magnified phase imaging, near-field and far-field ptychography, are now routinely used in two dimensions, but increasingly also in three dimensions through tomography techniques. The beamline offers a ‘low’ energy mode at 17 keV optimised for fluorescence analysis of biological samples and a ‘high’ energy mode at 34 keV more appropriate for materials science applications.
For ID16B, 2016 was mostly dedicated to the improvement of the in situ high-temperature nanotomography setup. The long-term stability has been much improved while both the spatial resolution range (from 35 to 300 nm) and the acquisition speed (< 20 s per tomographic scan) have been significantly increased. This paves the way to the nanoscale investigation of many high temperature driven heterogeneous dynamics in material science (such as nucleation, sintering, deformation, glass synthesis, growth of pores or cracks, etc.). In parallel, several operando experiments were successfully carried out, involving, for example, XBIC and/or XEOL measurements. Both in situ and operando experiments are being requested more often by users to study samples in their real or native environment, and so ID16B is trying to respond to this clear trend emerging from the user community and in-house research programme.
At ID21, the tender X-ray and infrared microspectroscopy beamline, an important effort was dedicated to preparing the beamline review and the conceptual design report for the upgrade of the beamline. Based on the feedback received from the users and the review panel, main priorities were identified as: a strong refurbishment of the main optics to obtain a smaller (~ 100 nm), more stable (in particular over the EXAFS energy range) and more intense beam, over a wider energy range (including Zn K-edge); a refurbishment of XRF detectors and electronics to collect XRF and XANES data faster (hence at reduced dose), on highly concentrated and highly diluted elements both present in complex matrices; an easy-to-install and easy-to-use cryo stage, in particular for the analysis of biological materials, which constitute a high proportion of the samples studied at ID21, particularly from the fields of life science, medicine and plant science. The design and implementation of some of this equipment is already on-going (new double mirror system, new double crystal monochromator, new SDD detectors and electronics) or has been recently completed (new cryo-stage) and should be of benefit to the users before the EBS long shutdown and even more after the complete refurbishment of the beamline.
T. Schülli