High temperature oxidation resistance in titanium-niobium alloys

Titanium alloys are ideally suited for use as lightweight structural materials, but their use at high temperature is severely restricted by oxidation. Niobium is known to confer oxidation-resistance, and here we disprove the normal explanation, that Nb5+ ions trap oxygen vacancies. Using density functional theory calculation, scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) we show that Nb is insoluble in TiO2. In fact, the Ti–Nb surface has three-layer structure: the oxide itself, an additional Nb-depleted zone below the oxide and a deeper sublayer of enhanced Nb. Microfocussed X-ray diffraction also demonstrates recrystallization in the Nb-depleted zone. We interpret this using a dynamical model: slow Nb-diffusion leads to the build up of a Nb-rich sublayer, which in turn blocks oxygen diffusion. Nb effects contrast with vanadium, where faster diffusion prevents the build up of equivalent structures

Tomography of a Cryo-immobilized Yeast Cell Using Ptychographic Coherent X-Ray Diffractive Imaging

The structural investigation of noncrystalline, soft biological matter using x-rays is of rapidly increasing interest. Large-scale x-ray sources, such as synchrotrons and x-ray free electron lasers, are becoming ever brighter and make the study of such weakly scattering materials more feasible. Variants of coherent diffractive imaging (CDI) are particularly attractive, as the absence of an objective lens between sample and detector ensures that no x-ray photons scattered by a sample are lost in a limited-efficiency imaging system. Furthermore, the reconstructed complex image contains quantitative density information, most directly accessible through its phase, which is proportional to the projected electron density of the sample. If applied in three dimensions, CDI can thus recover the sample's electron density distribution. As the extension to three dimensions is accompanied by a considerable dose applied to the sample, cryogenic cooling is necessary to optimize the structural preservation of a unique sample in the beam. This, however, imposes considerable technical challenges on the experimental realization. Here, we show a route toward the solution of these challenges using ptychographic CDI (PCDI), a scanning variant of coherent imaging. We present an experimental demonstration of the combination of three-dimensional structure determination through PCDI with a cryogenically cooled biological sample—a budding yeast cell (Saccharomyces cerevisiae)—using hard (7.9 keV) synchrotron x-rays. This proof-of-principle demonstration in particular illustrates the potential of PCDI for highly sensitive, quantitative three-dimensional density determination of cryogenically cooled, hydrated, and unstained biological matter and paves the way to future studies of unique, nonreproducible biological cells at higher resolution