Through the Cryo-FIB-SEM facility located at the University of Edinburgh, ECFP has access to a Zeiss Crossbeam 550 focused ion beam-scanning electron microscope (FIB-SEM) with a variety of associated attachments. This microscope is capable of individual particle resolution down to around 1nm and therefore offers the possibility of using captured images to determine particle size distribution. Using SEM to carry out this analysis has the advantage of providing three results in one: particle size distribution, detailed images of the particles’ surface morphology, and composition analysis via the Energy Dispersive X-ray Spectroscopy attachment. This 3-in-1 approach is therefore particularly informative for multicomponent systems, such as cement powders.
Once SEM images have been acquired, ImageJ can be utilised for analysis to determine particle size distribution. Below, this is illustrated using calcite particles. Using ImageJ, 128 particles were identified and a mean particle size of 5.8µm was determined, close to the supplier’s estimate of ≈5µm. The minimum particle size was ~2.7µm, and the maximum ~15.8µm. The major advantage of determining particle size using imaging, over other methods such as laser diffraction, is that measurements can be readily checked by manual inspection.
A common issue that can lead to inaccurate results when sizing particles is agglomeration. When processing images, larger particles can be scrutinised to determine if it is a single particle or multiple neighbouring particles. If agglomeration proves to be an issue, the quantity of sample loaded into the chamber of the particle disperser can be reduced. The efficacy of this approach is illustrated below, where 0.03g of sample was loaded on the left and 0.003g on the right. In the right-hand image, the agglomeration has been greatly reduced, allowing for greater accuracy when calculating the particle size distribution.
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Case Study – Lamellar Biomedical
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