Inca 350 edx system 80 mm x max sdd detector

Images of the lattice structure of the calcite particles were obtained using HRTEM imaging of thin sections prepared by FIB Milling . FIB to electron transparency was performed using an FEI Dual Beam system equipped with a 30 kV Ga beam and a field emission electron gun operated at 5 kV. The samples were then analysed with a FEI Tecnai TF20 FEG-TEM fitted with an Oxford Instruments INCA 350 EDX system/80 mm X-Max SDD detector and a Gatan Orius SC600A CCD camera operating at 200 kV. In order to minimize electron beam related damage during the recording of images and diffraction patterns recording, a 10-μm condenser lens and the smallest spot size were used.

The structure of the calcite/NP composite crystals and the distribution of the Au NPs was investigated using TEM and associated SAED using an FEI Tecnai TF20 FEG-TEM field emission gun TEM/STEM operating at 200 kV and fitted with an HAADF detector, an Oxford Instruments INCA 350 EDX system/80 mm X-Max SDD detector and a Gatan Orius SC600A CCD camera. Thin lamellae were prepared from the nanocomposite crystals using FIB as described above, and lift-out was performed in situ using a Keindiek micromanipulator, to transfer the lamella to a copper TEM grid. The distribution of Au NPs was further confirmed using a HAADF-STEM imaging mode, and energy dispersive X-ray (EDX) analysis mapping of Ca and Au was performed. The collection angle of the HAADF-STEM imaging was 80–240 mrad. Gold NPs were also characterised using TEM, where samples were prepared by placing a couple of drops of the NP solution on carbon-coated TEM grids, and allowing them to dry in air.

The CaCO₃ particles were analysed using SEM, high-resolution TEM (HRTEM), optical microscopy, Raman microscopy, infrared spectroscopy, thermogravimetric analysis, surface area analysis (BET), atomic absorption spectroscopy and EBSD. Selected samples were also analysed using synchrotron PXRD and SAXS. For SEM, particles were typically transferred onto glass coverslips that were subsequently mounted on aluminium stubs using carbon sticky pads. Samples were then coated with 5 nm Pt/Pd using an Agar High Resolution Sputter Coater and were examined using a LEO 1530 Gemini FEG-SEM operating at 3 kV using an in-lens detector mode. For TEM analysis, an FEI Tecnai TF20 FEG-TEM fitted with Oxford Instruments INCA 350 EDX system/80 mm X-Max SDD detector and Gatan Orius SC600A CCD camera operating at 200 kV was used. Raman microscopy and infrared spectroscopy were used to further confirm the polymorph and internal structure change of crystal particles with Raman being carried out using a Renishaw 2000 Raman microscope operating with a 785-nm diode laser, and infrared being performed with a PerkinElmer ATR-IR. The Co content of samples was analysed using a PerkinElmer Atomic Absorption Spectrometer, AAnalyst 400 with an air-acetylene flame after dissolving samples in dilute HNO₃.