The combined use of a X-ray diffractometer and a high temperature chamber allows in-situ determination of microstructure during heat treatment. X-ray diffractograms are recorded during tempering of high speed steels. The Rietveld method is used in connection with size-strain analysis. Lattice parameters of austenite and martensite are utilized for estimating the change of car-bon content that has massive influence on the secondary hardening. Nevertheless, it was shown that the heat treatment of deep-frozen high speed steel cannot be deduced a priori from the applied tempering process under conventional quenching conditions. The differently conditioned microstructures are based on different phase amounts and microstrain-situations.

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