Indentation tests with loads between 0.5 and 10 mN were performed on fused quartz, (0001) oriented sapphire and (001) oriented barium titanate. The resulting submicron cracks were used to determine the fracture toughness KIC of the tested samples. The indentation crack length method was applicable, but a c/a dependency of the constant of proportionality was found. In addition, a very effective and simple approach—using the extra penetration of the indenter, due to the formation of cracks, so called pop-in—was used to determine KIC.

Nanoindentation tests in an aa-in-plane domain area of an {001} oriented barium titanate single crystal were performed using a conical indenter with a tip radius of 800 nm. The topography and the polarization vectors of the area after indentation were imaged afterwards by both atomic force and piezoresponse force microscopy (PFM), respectively. Two perpendicular oriented cracks in the {110} planes were identified in the topographic image. An unexpected considerable uplift occurs inside the residual impression, which was correlated with a sharp pop-out-like behavior observed in the force-displacement curve just prior to unloading. Furthermore, PFM revealed an almost a twofold symmetric arrangement of the domains around the indent, which can be explained by residual circumferential tensile stresses around a residual impression and was unambiguously correlated to the crystal orientation.

We believe these data are also a valuable contribution to understand the mechanical behavior of enamel and to develop nanoscale biomimetic materials.

Nanoindentation tests in an 90°-ac-domain area of an {001} orientated barium titanate single crystal were performed using four different indenters (two with cube corner and two with spherical shape) with tip radii from 61nm to 1.9μm. Extensive calibrations of the tips on fused quartz and sapphire defined the penetration depth range for approximately spherical contact prior to indentation of barium titanate (BaTiO3). The measured elastic modulus is independent of the different indenters. The measurements showed plastic deformation after “pop-in”. The calculated mean pressure remained constant for each indenter, but clearly depends upon the indenter radius. The indenter radius dependence of the hardness support the concept of “geometrically necessary dislocations”, proposed by W. D. Nix and H. Gao [J. Mech. Phys. Sol., 46, 411 (1998)] and its extension to spherical tipped indenters [J. G. Swadener, E. P. George, G. M. Pharr, J. Mech. Phys. Solids, 50, 681 (2002)]. The results show this concept fits the data generated with indenter radii which are at least an order of magnitude lower than investigated by Swadener. Furthermore, the results agree with estimates of the statistically stored dislocation density determined for BaTiO3.

Articles you may be interested inNanoindentation-induced plastic deformation and fracture behavior difference between a -and c -domains of BaTiO 3 single crystal J. Appl. Phys.Plastic behavior during loading of ferroelectric bulk materials is commonly explained by domain switching processes. In this study the authors show that dislocation induced deformation also occurs during nanoindentation of BaTiO 3 . Studies were conducted using a spheroconical shaped indenter together with observations using atomic force microscopy ͑AFM͒ and focussed ion beam cross sections for transmission electron microscopy ͑TEM͒ of the contact areas. Force/displacement measurements showed the sudden appearance of "pop-in" events, which AFM/TEM observations revealed were associated with plastic deformation and dislocation arrays at the surface. TEM cross sections of the indents showed paired parallel slip lines with 45°to the original surface.