An in situ electrochemical soft X-ray spectromicroscopy investigation of Fe galvanically coupled to Au.

In this paper we report a pioneering electrochemical study of the galvanic coupling of Au and Fe in neutral aqueous solutions containing sulphate and fluoride ions, carried out by synchrotron-based in situ soft X-ray imaging and X-ray absorption microspectroscopy. The investigation was performed at the TwinMic X-ray Microscopy station at Elettra synchrotron facility combining X-ray imaging with µ-XAS with sub-micron lateral resolution. Using a purposely developed model thin-layer wet cell the morphology and chemical evolution of Fe electrodes in contact with aqueous solutions containing Na2SO4 and NaF have been investigated. The obtained results shed light on fundamental aspects regarding stability of Fe-based metallic bipolar plates in different electrochemical environments, an important issue for durability of polymer-electrolyte fuel cells. Imaging morphological features typical of the relevant electrochemical processes with chemical contrast, yields details on the spatial distribution and speciation of Fe resulting from corrosion of the Fe electrodes in the working fuel cells.

The Neanderthalian molar from Hunas, Germany.

In this paper, we present a well-preserved isolated human molar found in 1986 in the Hunas cave ruin, south-east Bavaria. The tooth was located at the bottom of layer F2, which belongs to a long stratigraphic sequence comprising faunal remains as well as archaeological levels (Mousterian). A stalagmite from layer P at the base of the stratigraphic sequence was recently dated to 79.373+/-8.237 ka (base) and 76.872+/-9.686 ka (tip) by TIMS-U/Th (Stanford University). We identified the tooth as a right (possibly third) mandibular molar. Characteristic parameters such as crown and root morphology, fissure pattern, enamel thickness, occlusal and interproximal wear, dental dimensions and indices, and radiological features indicate that the Hunas molar represents the tooth of a Neanderthal. This is corroborated by both the palaeontological and archaeological findings (Mousterian) of layer F2.

Soft X-ray spectromicroscopy using ptychography with randomly phased illumination.

Ptychography is a form of scanning diffractive imaging that can successfully retrieve the modulus and phase of both the sample transmission function and the illuminating probe. An experimental difficulty commonly encountered in diffractive imaging is the large dynamic range of the diffraction data. Here we report a novel ptychographic experiment using a randomly phased X-ray probe to considerably reduce the dynamic range of the recorded diffraction patterns. Images can be reconstructed reliably and robustly from this setup, even when scatter from the specimen is weak. A series of ptychographic reconstructions at X-ray energies around the L absorption edge of iron demonstrates the advantages of this method for soft X-ray spectromicroscopy, which can readily provide chemical sensitivity without the need for optical refocusing. In particular, the phase signal is in perfect registration with the modulus signal and provides complementary information that can be more sensitive to changes in the local chemical environment.

Imaging with spectroscopic micro-analysis using synchrotron radiation.

Recent developments of element-specific microscopy techniques using synchrotron radiation are opening new opportunities for the analytical investigation of various heterogeneous materials. This article provides a general description of the operational principles of different microscopes allowing chemical and structural imaging combined with micro-spot spectroscopic analysis. Several selected examples are used to illustrate the potential of the synchrotron-based methods in terms of imaging and chemical sensitivity for identification of spatial variations in the composition of morphologically complex and nano-structured inorganic and organic materials, including biological samples.