Effects of time and temperature of firing on Fe-rich ceramics studied by Mossbauer spectroscopy and two-dimensional 1H-nuclear magnetic resonance relaxometry

The combined effects of firing temperature and soaking time on the microstructure of iron-rich porous ceramics have been studied by Fe-57-Mossbauer spectroscopy and 2D H-1 nuclear magnetic resonance (NMR) relaxometry using a single-sided probe. Examining water-saturated ceramics using the relaxation correlation method, where longitudinal (T-1) and transverse (T-2) relaxation times are measured concurrently, provides information about firing-induced changes in both porosity (related to T-1) and magnetic properties (related to T-2). Comparing the information obtained from H-1-NMR analyses with that obtained from Mossbauer spectroscopy (which characterizes changes in iron-bearing species) shows that the T-1-T-2 NMR correlation technique is very sensitive to even subtle modifications in the magnetic behavior of Fe-bearing species. Moreover, the single-sided NMR approach allows us to perform millimeter-scale depth-resolved measurements, which can be used to non-invasively study the microstructural heterogeneities associated with non-uniform firing effects inside ceramics. This is in contrast to Mossbauer spectroscopy, which requires that the ceramic samples be ground. (C) 2012 American Institute of Physics. [http://dx.doi.org/10.1063/1.4759316]