Kadda Medjoubi

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 microm IBM technology, contains 9600 square pixels with 130 microm side giving a total size of 1 cm x 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, 10(7) 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 microm silicon sensor and a 700 microm 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 x 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 x 3 cm CdTe imager is also presented.

Development of fast, simultaneous and multi-technique scanning hard X-ray microscopy at Synchrotron Soleil

A distributed fast-acquisition system for synchronized multi-technique experiments is presented, in which the collection of metadata and the asynchronous merging of large data volumes from multiple detectors are managed as part of the data collection process. This fast continuous scanning scheme, named FLYSCAN, enables measurement of microscopy data on a timescale of milliseconds per pixel. Proof-of-principle multi-technique experiments, namely scanning X-ray fluorescence spectrometry combined with absorption, differential phase contrast and dark-field imaging, have been performed on biological and geological samples.

Diffraction studies under in situ electric field using a large-area hybrid pixel XPAD detector

A new experimental approach to perform in situ electric field diffraction on single crystals using an on-then-off pump–probe mode in situ (i.e. the field-switching method) with a synchrotron or a laboratory X-ray source is presented. Taking advantage of the fast readout of the XPAD hybrid pixel two-dimensional detector and its programmable functionalities, the operation mode of the detector has been customized to significantly increase the efficiency of the method. The very weak electric field-induced structural response of a piezoelectric crystal can be accurately measured. This allows the piezoelectric tensor to be precisely obtained from Δθ shifts while the structural variations can be modelled using a full set of ΔI/I data. The experimental method and methodology are detailed and tested as a case study on pure piezoelectric compounds belonging to the α-quartz family (SiO2 and GaAsO4 single crystals). Using the two scan modes developed, it is demonstrated that tiny Bragg angle shifts can be measured as well as small field-induced Bragg intensity variations (<1%). The relevance of measurements performed with an X-ray laboratory source is demonstrated: partial data sets collected at synchrotrons can be completed, but more interestingly, a large part of the study can now be realized in the laboratory (medium to strong intensity reflections) in a comparable data collection time.

Reduction of radiation damage and other benefits of short wavelengths for macromolecular crystallography data collection

Circumventing radiation damage remains a major problem for X-ray macromolecular crystallography. Analysis of diffraction data collected from normal-sized cryocooled lysozyme crystals shows that the dose required to collect a data set of prescribed resolution and signal-to-noise ratio, assuming an ideally efficient detector, decreases with increasing photon energy in the investigated 6.5–33 keV range. For example, the data collection efficiency is increased by a factor of ∼8 from 8 to 33 keV. Monte Carlo simulations on lysozyme crystals in the range 5–80 keV, taking into account electron escape from samples of different size, also show a positive effect of high energy (albeit less pronounced than in experiments), especially for micrometre-sized samples, and suggest that the optimum energy range is ∼24–41 keV, depending on crystal size. The importance of counting pixel detectors with a good efficiency at high energy is underlined. Macromolecular crystallography beamlines should be modified, or purposely designed, in order to benefit from higher-energy radiation through reduction of global radiation damage, better data accuracy and extension of phasing by anomalous dispersion.

MMX-I: data-processing software for multimodal X-ray imaging and tomography

The MMX-I open-source software has been developed for processing and reconstruction of large multimodal X-ray imaging and tomography datasets. The recent version of MMX-I is optimized for scanning X-ray fluorescence, phase-, absorption- and dark-field contrast techniques. This, together with its implementation in Java, makes MMX-I a versatile and friendly user tool for X-ray imaging.

A new paradigm for macromolecular crystallography beamlines derived from high-pressure methodology and results

Macromolecular crystallography at high pressure (HPMX) is a mature technique. Shorter X-ray wavelengths increase data collection efficiency on cryocooled crystals. Extending applications and exploiting spin-off of HPMX will require dedicated synchrotron radiation beamlines based on a new paradigm.

Patterns of metal distribution in hypersaline microbialites during early diagenesis: Implications for the fossil record

The use of metals as biosignatures in the fossil stromatolite record requires understanding of the processes controlling the initial metal(loid) incorporation and diagenetic preservation in living microbialites. Here, we report the distribution of metals and the organic fraction within the lithifying microbialite of the hypersaline Big Pond Lake (Bahamas). Using synchrotron-based X-ray microfluorescence, confocal, and biphoton microscopies at different scales (cm-μm) in combination with traditional geochemical analyses, we show that the initial cation sorption at the surface of an active microbialite is governed by passive binding to the organic matrix, resulting in a homogeneous metal distribution. During early diagenesis, the metabolic activity in deeper microbialite layers slows down and the distribution of the metals becomes progressively heterogeneous, resulting from remobilization and concentration as metal(loid)-enriched sulfides, which are aligned with the lamination of the microbialite. In addition, we were able to identify globules containing significant Mn, Cu, Zn, and As enrichments potentially produced through microbial activity. The similarity of the metal(loid) distributions observed in the Big Pond microbialite to those observed in the Archean stromatolites of Tumbiana provides the foundation for a conceptual model of the evolution of the metal distribution through initial growth, early diagenesis, and fossilization of a microbialite, with a potential application to the fossil record.

Simultaneous fast scanning XRF, dark field, phase-, and absorption contrast tomography

Scanning hard X-ray nanoprobe imaging provides a unique tool for probing specimens with high sensitivity and large penetration depth. Moreover, the combination of complementary techniques such as X-ray fluorescence, absorption, phase contrast and dark field imaging gives complete quantitative information on the sample structure, composition and chemistry. The multi-technique “FLYSCAN” data acquisition scheme developed at Synchrotron SOLEIL permits to perform fast continuous scanning imaging and as such makes scanning tomography techniques feasible in a time-frame well-adapted to typical user experiments. Here we present the recent results of simultaneous fast scanning multi-technique tomography performed at Soleil. This fast scanning scheme will be implemented at the Nanoscopium beamline for large field of view 2D and 3D multimodal imaging.

Silicon Absolute X‐Ray Detectors

The responsivity of silicon photodiodes having no loss in the entrance window, measured using synchrotron radiation in the 1.75 to 60 keV range, was compared to the responsivity calculated using the silicon thickness measured using near‐infrared light. The measured and calculated responsivities agree with an average difference of 1.3%. This enables their use as absolute x‐ray detectors.

Arsenic distribution and valence state variation studied by fast hierarchical length-scale morphological, compositional, and speciation imaging at the Nanoscopium, Synchrotron Soleil

The understanding of real complex geological, environmental and geo-biological processes depends increasingly on in-depth non-invasive study of chemical composition and morphology. In this paper we used scanning hard X-ray nanoprobe techniques in order to study the elemental composition, morphology and As speciation in complex highly heterogeneous geological samples. Multivariate statistical analytical techniques, such as principal component analysis and clustering were used for data interpretation. These measurements revealed the quantitative and valance state inhomogeneity of As and its relation to the total compositional and morphological variation of the sample at sub-μm scales.