A novel high temperature NMR probe design: application to O-17 studies of gel formation of zirconia

A novel optically heated high temperature, water-cooled NMR probe design is described in detail. The sample temperature is easily and accurately contr olled to at least 1300 K. The probe characteristics are evaluated and the r elative merits of the design discussed. Its operation is illustrated by in situ measurement of the O-17 static NMR spectra and spin-lattice relaxation times (T-1) of gel-formed zirconia (ZrO2). A characteristic doublet of cry stalline monoclinic ZrO2 is clearly observed at similar to 700 K. These dat a represent the first in situ O-17 solid State NMR observation of the struc tural development of a sol-gel-produced oxide at elevated temperatures.