New Approach of Using Cryo-Soft X-ray Tomography for beam-sensitive materials
Abstract
Abstract Cryo-soft X-ray tomography (cryo-SXT) is emerging as a promising characterisation technique for imaging nanomaterials in the solid state and in material science. This capability is demonstrated through high-resolution 2D and 3D imaging of nanomaterials, enabling analysis of particle size distributions, nanoscale topography, volumetric distribution, heterogeneity, and clustering behaviour, while providing non-destructive characterisation of newly synthesised structures. A novel, rapid synthesis method producing magnetite (Fe 2.8 O 4 ) in water, in the tetragonal inverse-spinel Fe 2.8 O 4 lattice, was achieved using KOH/ethanol at 80°C. Zerovalent iron Fe(0) nanoparticles were synthesised using Dodecylamine (DDA) in a microwave reactor within 30 s. The face-centred cubic (FCC) crystal structure and phase purity were verified by powder X-ray diffraction (PXRD). The unit-cell parameter and crystal domain size were studied using Pawley refinements. Fe(0) and Fe 2.8 O 4 are beam-sensitive materials, and imaging using cryo-SXT was compared with conventional methods. Additionally, the size and shape of Fe 2.8 O 4 and Fe(0) nanoparticles were determined by scanning electron microscopy (SEM), high-resolution scanning transmission electron microscopy (HR-STEM), and simulation of cryo-SXT images using Fiji/ImageJ. Fourier transform infrared (FT-IR) spectroscopy, thermogravimetric analysis (TGA), and cryo-SXT indicated the presence of a trace of DDA on the surface of the Fe(0)…
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