This article presents a new technique for the characterization of low loss dielectric materials at high temperatures: the split cylinder resonator cavity. This technique allows the accurate characterization of the dimensional and electrical characteristics of the cavity and the electromagnetic properties of a dielectric material, simultaneously in one temperature cycle. To do this, the couple TE 011 +TE 013 is used to characterize the sample and the couple TE 012 +TE 014 is used to characterize

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... the cavity conductivity and dimensions. Measurements of conductivity and dimensions using the couple TE 012 +TE 014 for a loaded cavity at ambient temperature and during a thermal cycle show an agreement with the values obtained using the couple TE 011 +TE 013 for an unloaded cavity at ambient temperature and during a thermal cycle. The characterization of an Alumina sample during a thermal cycle performed using the new technique and the traditional one shows a good agreement for the permittivities and the loss tangents.