SummaryThe contribution describes the implementation of a broad ion beam (BIB) polisher into a scanning electron microscope (SEM) functioning at cryogenic temperature (cryo). The whole system (BIB-cryo-SEM) provides a first generation of a novel multibeam electron microscope that combines broad ion beam with cryogenic facilities in a conventional SEM to produce large, high-quality cross-sections (up to 2 mm 2 ) at cryogenic temperature to be imaged at the state-of-the-art SEM resolution. Cryogenic method allows detecting fluids in their natural environment and preserves samples against desiccation and dehydration, which may damage natural microstructures. The investigation of microstructures in the third dimension is enabled by serial cross-sectioning, providing broad ion beam tomography with slices down to 350 nm thick. The functionalities of the BIB-cryo-SEM are demonstrated by the investigation of rock salts (synthetic coarse-grained sodium chloride synthesized from halite-brine mush cold pressed at 150 MPa and 4.5 GPa, and natural rock salt mylonite from a salt glacier at Qom Kuh, central Iran). In addition, results from BIB-cryo-SEM on a gas shale and Boom Clay are also presented to show that the instrument is suitable for a large range of sedimentary rocks. For the first time, g.desbois@ged.rwth-aachen.de pore and grain fabrics of preserved host and reservoir rocks can be investigated at nm-scale range over a representative elementary area. In comparison with the complementary and overlapping performances of the BIB-SEM method with focused ion beam-SEM and X-ray tomography methods, the BIB cross-sectioning enables detailed insights about morphologies of pores at greater resolution than X-ray tomography and allows the production of large representative surfaces suitable for FIB-SEM investigations of a specific representative site within the BIB cross-section.
Paleoclimate reconstructions based on reef corals require precise detection of diagenetic alteration. Secondary calcite can significantly affect paleotemperature reconstructions at very low amounts of ∼1%. X‐ray powder diffraction is routinely used to detect diagenetic calcite in aragonitic corals. This procedure has its limitations as single powder samples might not represent the entire coral heterogeneity. A conventional and a 2‐D X‐ray diffractometer were calibrated with gravimetric powder standards of high and low magnesium calcite (0.3% to 25% calcite). Calcite contents <1% can be recognized with both diffractometer setups based on the peak area of the calcite [104] reflection. An advantage of 2‐D‐XRD over convenient 1‐D‐XRD methods is the nondestructive and rapid detection of calcite with relatively high spatial resolution directly on coral slabs. The calcite detection performance of the 2‐D‐XRD setup was tested on thin sections from fossil Porites sp. samples that, based on powder XRD measurements, showed <1% calcite. Quantification of calcite contents for these thin sections based on 2‐D‐XRD and digital image analysis showed very similar results. This enables spot measurements with diameters of ∼4 mm, as well as systematic line scans along potential tracks previous to geochemical proxy sampling. In this way, areas affected by diagenetic calcite can be avoided and alternative sampling tracks can be defined. Alternatively, individual sampling positions that show dubious proxy results can later be checked for the presence of calcite. The presented calibration and quantification method can be transferred to any 2‐D X‐ray diffractometer.
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