Kinga Nalepka

The reinforcement function of shell ribs depends not only on their vaulted morphology but also on their microstructure. They are part of the outer layer which, in the case of the Pinna nobilis bivalve, is built from almost monocrystalline calcitic prisms, always oriented perpendicular to the growth surfaces. Originally, prisms and their c-axes follow the radii of rib curvature, becoming oblique to the shell thickness direction. Later, prisms bend to reach the nacre layer perpendicularly, but their c-axes retain the initial orientation. Calcite grains form nonrandom boundaries. Most often, three twin disorientations arise, with two of them observed for the first time. Nano-indentation and impact tests demonstrate that the oblique orientation of c-axes significantly improves the hardness and fracture toughness of prisms. Moreover, compression tests reveal that the rib area achieves a unique strength of 700 MPa. The detection of the specific microstructure formed to toughen the shell is novel.

Investigations by electron backscatter diffraction (EBSD) and X-ray diffraction with the use of synchrotron radiation, as well as parallel extended finite element (XFEM) simulations, reveal the evolution of the 316L stainless steel microstructure in the vicinity of a macro-crack developing at the temperature of liquid helium (4.2 K). The fracture propagation induces a dynamic, highly localized phase transformation of face-centred cubic austenite into α’ martensite with a body-centred cubic structure. Synchrotron studies show that the texture of the primary phase controls the transition process. The austenite grains, tending to the stable Brass orientation, generate three mechanisms of the phase transformation. EBSD studies reveal that the secondary phase particles match the ordered austenitic matrix. Hence, interphase boundaries with the Pitsch disorientation are most often formed and α’ martensite undergoes intensive twinning. The XFEM simulations, based on the experimentally determined kinetics of the phase transformation and on the relevant constitutive relationships, reveal that the macro-crack propagates mainly in the martensitic phase. Synchrotron and EBSD studies confirm the almost 100% content of the secondary phase at the fracture surface. Moreover, they indicate that the boundaries formed then are largely random. As a result, the primary beneficial role of martensite as reinforcing particles is eliminated.

The mechanical properties such as compressive strength and nanohardness were investigated for Pinctada margaritifera mollusk shells. The compressive strength was evaluated through a uniaxial static compression test performed along the load directions parallel and perpendicular to the shell axis, respectively, while the hardness and Young modulus were measured using nanoindentation. In order to observe the crack propagation, for the first time for such material, the in-situ X-ray microscopy (nano-XCT) imaging (together with 3D reconstruction based on the acquired images) during the indentation tests was performed. The results were compared with these obtained during the micro-indentation test done with the help of conventional Vickers indenter and subsequent scanning electron microscopy observations. The results revealed that the cracks formed during the indentation start to propagate in the calcite prism until they reach a ductile organic matrix where most of them are stopped. The obtained results confirm a strong anisotropy of both crack propagation and the mechanical strength caused by the formation of the prismatic structure in the outer layer of P. margaritifera shell.

Temperature dependence of twinning stress associated with type I twin boundaries in the Ni_49.5Mn_38.4Sn_12.2 single crystal has been measured. At room temperature, the twinning stress amounts to 16.6 MPa, exceeding the typical values observed in the archetypical Ni-Mn-Ga alloys; nonetheless, it shows a remarkable sensitivity to temperature decreasing with a slope of 0.2498 MPa/K. This is a level of magnitude more than in Ni-Mn-Ga alloys. The remarkable sensitivity of twinning stress to temperature is primarily associated with the evolution of lattice parameters during heating. The type II twin boundaries in the same single crystal are activated at the twinning stress of 3.4 MPa, roughly one fifth of the twinning stress recorded for the type I twin boundaries. It is demonstrated that by careful compositional adjustments and thermomechanical training, it may be feasible to exercise magnetic field-induced strain due to twin variant rearrangement outside the Ni-Mn-Ga system.