This study evaluated a novel approach for acoustic emission (AE) monitoring of nanoindentation. The technique utilizes a miniature AE sensor integrated into a calibrated diamond indenter tip on a commercial nanoindentation system. The evaluation focused on the yield-point phenomenon in W (100); MgO (100); and sapphire C (0001); R (1012); A (1210); and M (1010) single-crystal surfaces. The minimum amount of elastic energy release sufficient to produce AE signal detectable with the indenter tip sensor was nearly two orders of magnitude lower than the minimum energy level required for conventional AE sensors. Wave forms detected with the indenter tip sensor were independent of sample size. A linear relationship between released elastic energies and the corresponding AE energies was observed for all three evaluated materials. The scaling coefficient of the linear relationship was independent of indenter tip size/shape and indentation depth. The differences between the mechanisms of the initial stages of plasticity for the various crystallographic orientations of sapphire were reflected in the following aspects of AE activity: detection of a specific type of AE wave form that correlated to the presence of linear surface features near the indentation sites; AE signal associated with the yield point, consisting either of one or two distinct wave forms; and presence or absence of AE signals after the yield point. The possibility of plasticity onset in sapphire involving both slip and twinning is discussed.
A quasistatic nanoindentation technique, enhanced by scanning probe microscopy, was used to measure cuticle stiffness of live Drosophila melanogaster during its larval, pupal, and early adult development in vivo. Stiffness was defined as the reduced elastic modulus (E(r)), which is a material property related to the elastic modulus. E(r) was measured at the local contact while indenting the live sample at a constant loading rate using a spherical tip. E(r) was derived from the resultant force-displacement curves. Insect cuticle exhibits viscoelastic behavior. Constant loading rate quasistatic measurements were used so that the effects of viscosity and contact force adhesion introduced systematic measurement effects. E(r) values were as follows: larvae, mean (SE), 0.39 (0.01) MPa; the puparium without evidence of adult structures 15.43 (1.78) MPa; and the adult, measured in the puparium at the completion of metamorphosis, 4.37 (0.31) MPa. Thus, as expected, the puparium and adult cuticle were very much stiffer than larval cuticle. Results also indicated stiffness variation that related to developmental events. This study has shown that this quasistatic nanoindentation-scanning probe microscopy approach is a suitable method for analyzing live biological samples.
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