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Although the concept, first demonstration, and potential applications of X-ray transmission mirrors (XTMs) were initially described over 30 years ago, only a few implementations exist in the literature. This is attributed to the unsolved challenge of a thick frame supporting a thin, reflecting membrane which does not itself block the transmitted beam. Here, we introduce a novel approach to solve this problem by employing silicon microfabrication. A robust XTM frame has been fabricated by using a novel two-step etch process, which secures the thin-film membrane without blocking the transmitted beam. Specifically, we have fabricated delicate XTM optics with 90% yield, which consist of 280-nm-thick low-stress silicon nitride membrane windows that are 1.5 mm wide and 125 mm long on silicon substrates. The XTM optics have been demonstrated to be a more efficient high-pass X-ray filter; for example, when configured for 40% transmission of 11.3 keV photons, we measure the reduction of 8.4 keV photons by a factor of 56.
The I13 transmission X-ray microscope at Diamond Light Source (DLS) has been designed to cover a broad range of energies and field of views. The beamline operates on an undulator source, and a multilayer monochromator can be used to work at a larger bandwidth to enable faster acquisitions. The experimental design includes large working distances for the optics to allow installing in situ sample environments. This paper presents the current state of the experimental system and shows some of the latest results.
The giant gypsum crystals of Naica cave have fascinated scientists since their discovery in 2000. Human activity has changed the microclimate inside the cave, making scientists wonder about the potential environmental impact on the crystals. Over the last 9 years, we have studied approximately 70 samples. This paper reports on the detailed chemical–structural characterization of the impurities present at the surface of these crystals and the experimental simulations of their potential deterioration patterns. Selected samples were studied by petrography, optical and electronic microscopy, and laboratory X-ray diffraction. 2D grazing incidence X-ray diffraction, X-ray μ-fluorescence, and X-ray μ-absorption near-edge structure were used to identify the impurities and their associated phases. These impurities were deposited during the latest stage of the gypsum crystal formation and have afterward evolved with the natural high humidity. The simulations of the behavior of the crystals in microclimatic chambers produced crystal dissolution by 1–4% weight fraction under high CO2 concentration and permanent fog, and gypsum phase dehydration under air and CO2 gaseous environment. Our work suggests that most surface impurities are of natural origin; the most significant anthropogenic damage on the crystals is the extraction of water from the caves.
The speciation of vanadium in the electrolyte of vanadium redox flow batteries (VRFBs) is important to determine the state of charge of the battery. To obtain a better understanding of the transport of the different vanadium species through the separator polymer electrolyte membranes, it is necessary to be able to determine concentration and species of the vanadium ions inside the nanoscopic water body of the membranes. The speciation of V in the electrolyte of VRFBs has been performed by others at the synchrotron by X-ray absorption near-edge structure analysis (XANES). However, the concentrations are quite high and not necessarily justify the use of a large-scale facility. Here, we show that vanadium species in the electrolyte and inside the ionomeric membranes can be determined by laboratory XANES. We were able to determine V species in the 1.6 M electrolyte with a measurement time of 2.3 h and V species having a concentration of 9.8 g kg−1 inside the membranes (178 µm thick) with a measurement time of 5 h. Our results show that laboratory XANES is an appropriate tool to study these kind of samples.
A commercial Empyrean X-ray diffractometer was adapted for combined grazing incidence X-ray fluorescence analysis (GIXRF) measurements with X-ray reflectivity (XRR) measurements. An energy-dispersive silicon drift detector was mounted and integrated in the angle-dependent data acquisition of the Empyrean. Different monochromator/X-ray optics units have been compared with the values obtained by the Atominstitut GIXRF + XRR spectrometer. Data evaluation was performed by JGIXA, a special software for combined GIXRF + XRR data fitting, developed at Atominstitut. A sample consisting of a ~50 nm nickel layer on a silicon substrate was used to compare the performance criteria (i.e. divergence and intensity) of the incident beam optics. An Empyrean X-ray diffractometer was successfully refitted to measure both GIXRF and XRR data.
A provisional setup for X-ray microprobe experiments at 35 keV is described. It is based on compound refractive lenses (CRLs) for nanofocusing and a Vortex silicon drift detector with 2 mm sensor thickness for increased sensitivity at high energies. The Microprobe experiment (PETRA III) generally uses Kirkpatrick-Baez mirrors for submicrometer focusing in the energy range of 5–21 keV. However, various types of scanning X-ray microscopy experiments require higher excitation energies. The CRL optics were characterized by X-ray ptychography and X-ray fluorescence (XRF) knife edge scans on a siemens star pattern and showed beam sizes down to 110 nm. The performance of the new setup for microscopic X-ray diffraction (XRD)–XRF scanning X-ray microscopy measurements at 35 keV is demonstrated on a cross-section of a painting fragment.
Precious ornaments from the Museum Royal Tombs of Sipán were analyzed by X-ray computed microtomography (microCT). The ornaments analyzed were golden earrings produced by the Moche culture that flourished along the north coast of present-day Peru between approximately 100 and 600 AD. Sipán, also known as Huava Rajada, is a mochica archaeological complex in the north of Peru. In particular, the spectacular jewelry, mainly composed of gold, silver, and copper alloys, gilded copper, and tumbaga, from the Museum “Royal Tombs of Sipán,” in Lambayeque, north of Peru, are some of the most sophisticated metalworking ever produced of pre-Columbian America. A portable microCT system consisting of a high-resolution flat panel detector and a mini X-ray tube were used for the structural analysis of these ornaments. The microCT images show parts of the internal structure, highlighting the manufacturing technique and gold sheets joining techniques of the Moche artisans. Furthermore, the advantage of using the portable microCT system for nondestructive testing is clear when the sample cannot be taken to the laboratory.