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 controlled to at least 1300 K. The probe characteristics are evaluated and the relative 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 crystalline monoclinic ZrO2 is clearly observed at similar to 700 K. These data represent the first in situ O-17 solid State NMR observation of the structural development of a sol-gel-produced oxide at elevated temperatures.