Cyclic nanoindentation allows characterizing the influence of single phases and their interactions on fatigue mechanisms. Herein, a method for high cycle fatigue testing by nanoindentation is presented. By combining high‐ and low‐frequency indentation modes, high cycle numbers are achieved while obtaining sufficient data points to reconstruct force–displacement hysteresis loops. A challenge is the stochastic course of thermal drift which is addressed by measuring drift rate in regular low‐force holding segments. Drift rates are used to correct the displacement values, yielding reproducible cyclic deformation data as it is shown for two very different materials, a ductile metal and a brittle ceramic.
The objective of this study is the investigation of nanomechanical properties using nanoindentation of extruded and heat-treated Mg-Dy-Nd-Zn-Zr, with an emphasis on the transformation of long-period stacking-ordered (LPSO) phases. Solution heat treatment was performed with different heat treatment for durations on hot extruded Mg-Dy-Nd-Zn-Zr to monitor the transformation of LPSO phases, as well as to keep track of microstructural changes. The initial fine-grained microstructure, with blocky and lamellar LPSO structures within the matrix, first transformed into coarser grains with fewer LPSO lamellae, which then increased in amount again at higher annealing duration. The blocky LPSO phases, which have the highest hardness compared to the matrix grains with and without LPSO lamellae, consistently decrease in quantity, as so does the trend in their hardness value. The Mg matrix grains with LPSO lamellae show a lower hardness compared to the Mg matrix grains without or with a just few lamellar LPSO phases, and increase in quantity at long annealing durations. The overall hardness of the microstructure is essentially determined by the LPSO lamellae-containing grains and reaches a peak at 24 h. There is another peak found for the grain size values; however, this is at later annealing duration, at 72 h. The reduction in grain size towards longer annealing durations goes along with a reactivated formation of LPSO lamellae.
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