Monte Carlo strategy for SEM-EDS micro-nanoanalysis of geopolymer composites

The development, optimization and application of new geopolymer composite materials must necessarily go through a precise and accurate physico-chemical and mineralogical characterization down to the micro and nanoscale. In this regard, SEM-EDS X-ray microanalysis is widely and successfully employed by the scientific community and industry. However, the nano-to-micrometre sized architecture of many geopolymer composites introduces many difficulties and issues in SEM-EDS quantification, with potential large sources of error that should carefully be taken into account and investigated. In this work, a SEM-EDS Monte Carlo approach is proposed to study the complex physical phenomena at the basis of the quantification issues and errors, through the investigation of: (i) a not completely reacted sodium-poly(sialate-siloxo) geopolymer, and (ii) a geopolymer composite with a potassium-poly(sialate-siloxo) matrix and basalt-derived glass fibres reinforcement. The Monte Carlo simulation evinced a strong influence of the nano-microsized specimen architecture (e.g., basalt fibre size and shape, different elemental composition between fibre and matrix) on the measured X-ray intensity, with contributions also depending on the SEM electron beam energy. The proposed approach provided fundamental indications for selecting optimal operative conditions depending on the type of geopolymer sample, shape, size with the specific SEM-EDS setup and silicon drift EDS detector here used.