X-ray Powder Diffraction of Portland Cement Clinker
The benefits of using XRDynamic 500 for qualitative and quantitative phase analysis of Port-land cement clinker is investigated under ambient conditions. Quantification of the amorphous and crystalline phases is notoriously difficult for cementitious materials due to the complexity of the mineral phases present in the mixes and the significant peak overlap that occurs. By using a standard measurement configuration, excellent results could be obtained through Rietveld refinement of the measured sample. This can be further improved using a primary multilayer divergent beam Kα1,2 monochromator instead of a traditional Kβ filter.
Introduction
Since its first reported use almost 2000 years ago by the Roman Empire (albeit slightly different to the form we use today), cement has become the most prevalent man-made material on earth and has been the focus topic of many subsequent studies of its composition and uses. (1) Arguably, X-ray diffraction (XRD) is considered one of most important analytical methods utilized today to identify and quantify mineral phases in cement and concrete mixtures. This characterization is of particular significance due to the complexity of the composition and interactions between the many polycrystalline minerals found in the material.
Unlike X-ray fluorescence (XRF) spectroscopy, that is used to determine the chemical composition in these sample types, XRD is the go-to method to provide information about the microstructure and characteristic crystalline phases that originate from the clinker and cement manufacturing processes. Modern XRD instrumentation also provides the possibility to perform in-situ investigations of the phase changes and reactions during cement hydration by incorporating non-ambient attachments into the instrumental setup.
For this report, a standard reference Portland cement sample (SRM 2688) from the National Institute of Standards and Technology (NIST) was analyzed under ambient conditions. (2)
References:
1. History of cement, Britannica www.britannica.com/technology/cement-building-material/Strength, Access on 06/06/2023
2. NIST SRM 2688, 2017, Portland Cement Clinker, National Institute of Standards and Technology, www-s.nist.gov
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