Particle sizing and composition analysis of cement powders 

Equipment Case Study - Particle Sizing

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.

To develop this capability, Dr Rory O’Neill from ECFP has designed a portable device to prepare dry powders or solid particle samples for analysis. An SEM stub plate can be secured within the custom designed chamber and the sample loaded into the bottom of the cavity. Compressed air can then be passed through the chamber to evenly disperse the sample on to the stub. The compressed air can be delivered through a controllable supply or simply an air can, making the dispenser efficient and mobile, as SEM stubs can be prepared in any lab or facility and sent for imaging. The effectiveness of this dispersal method can be seen in the images below with a sample of calcium phosphate particles. All were well dispersed using this technique, with particles down to around 1µm identifiable.
SEM image of well-dispersed calcium phosphate particles

Particle size distribution analysis

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.

ImageJ analysis of calcite particles

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.

A smaller amount of sample can be used (right) to navigate agglomeration issues (left)

Composition analysis

Industrial powders such as cements are often multicomponent systems. Using the above approach in combination with Energy Dispersive X-ray Spectroscopy (EDX) allows for element analysis to be conducted, facilitating identification of particle composition. Below are two images of a Portland cement-based powder, going back and forth between a normal SEM image and an EDX overlay. It is known that the bulk powder is a mix of Portland cement (containing calcium silicates), limestone (calcium carbonate) and gypsum (a sulphate mineral). The layered EDX image highlights the occurrence of silica (pink), sulphur (blue) and calcium (yellow). Particles that appear mainly pink in colour can be inferred to be Portland cement, those yellow in colour indicate limestone and the blue particles can be assumed to be gypsum. Therefore, the proportions of individual materials in a multicomponent powder can be determined. The variation in shape and size between the different types of particles can also be established, facilitating investigations into the influence of the individual components on the characteristics of the bulk powder.
SEM image with an EDX overlay, with the latter highlighting the occurrence of silica (pink), sulphur (blue) and calcium (yellow) (Portland cement, gypsum and limestone particles, respectively)

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