Studies on electrical and thermal properties of dental glass ionomer cement
A commercially available dental Glass Ionomer Cement (GIC) was studied after setting at room temperature (300 K) to understand its DC electrical conductivity, dielectric and thermal properties. The dental GIC’s are supposed to have free mobile charge carriers like F- ions. Interestingly this material loses its conductivity above 80°C and behaves like a non-polar substance. The frequency dependent dielectric studies also indicate the loss of mobile charge carriers in the samples annealed at 80°C. The DSC and TGA studies indicate that the material loses H2O exothermically at 100°C. This is attributed to the onset of a secondary setting reaction.
MAS-NMR spectroscopy studies in the setting reaction of glass ionomer cements.
OBJECTIVES
The main objective is the characterisation of the setting reaction in glass ionomer cements based on experimental ionomer glasses with different fluorine content and a commercial glass ionomer cement liquid by using 13C CP/MAS-NMR, 29Si, 27Al and 31P MAS-NMR spectroscopy in order to receive information specifically about the cross-linking process.


METHODS
Different fluorine containing glass compositions based on 4.5SiO2-3Al2O3-1.5P2O5-(5-z)CaO-zCaF(2) where z=0-3, were mixed with a commercially available polymer liquid to form glass ionomer cements. The cements were subjected to 27Al, 13C CP/MAS, 29Si, and 31P MAS-NMR analysis.


RESULTS
The 27Al spectra showed clearly the formation of six-fold coordinate Al(VI), that may crosslink the carboxyl groups in the poly-acid molecules. A shift towards to more positive values of the carboxyl peak in the 13C CP/MAS-NMR spectra showed clearly the proton dissociation of the carboxyl groups. A shift towards more negative values was observed in the 29Si MAS-NMR spectra, suggesting formation of hydrated silica gel and consequently formation of additional Si-O-Si bonds. 31P MAS-NMR spectra also reflected changes in the coordination state around a PO4(3-) tetrahedron. Increasing the fluorine content of the glasses resulted generally in increased reactivity during setting, due to promoting cross-linking and repolymerisation of the silicate phase, followed by clear changes in the MAS-NMR spectra.


CONCLUSIONS
The cross-linking process during the setting reaction of glass ionomer cements can be followed by MAS-NMR spectroscopy observing the conversion of Al(IV) to Al(VI). The acid base setting reaction is completed in 1 day and no further significant changes in the MAS-NMR spectra can be observed. Further study is required in order to understand the role of phosphorus.
Neutron Residual Stress Measurements on Rail Sections for Different Production Conditions
Rail sectioning with subsequent neutron diffraction experiments has been used to assess residual stresses in the rails. In this study we present the results of neutron stress measurements performed at the NIST Center for Neutron Research (NCNR) on rail sections from rails that were produced under various conditions. Specifically, these are air-cooled, air-cooled and roller-straightened, head-hardened and head-hardened and roller-straightened. More significantly, a head-hardened and roller-straightened rail was also studied after service to elucidate evolution of the service-induced residual stresses. In the latter case both a transverse-cut slice and the central region of a 0.53 m long piece were studied. Measurements on this piece are the first in which triaxial stresses have been determined for an intact rail. Neutron strain measurements with 3×3×3 mm3 spatial resolution were successfully employed for transversally cut slices to verify the difference in the stress state depending on the production process. Although examination of slices allows determination of only two-dimensional stresses in the plane of the slice, additional measurements on obliquely-cut slices, which were also carried out, and utilization of FEM gives the possibility of reconstructing the full triaxial stress distribution. Together, these approaches provide a better understanding of rail fabrication and the possibility of improving the durability and safety of rails in the future.Copyright © 2004 by ASME