In-situ compression and shape recovery of Ceramic single grain micro-pillar

Most ceramic materials are known for high fracture toughness while reacting highly brittle to physical deformation. Some advancements were made by utilizing the transformation toughening effect of Yttria-doped Zirconia. However, finding a ceramic material demonstrating an effect analogous to the Shape Memory Effect (SME) in certain metals, that also allows for superelastic responses, remains a challenge. The underlying mechanism for SME and superelasticity is based on crystallographic variations within the material's grains, requiring sophisticated electron microscopy techniques for direct observation. The combination of a scanning electron microscope (SEM) with focused ion beam (FIB) milling, a Kleindiek Nanotechnik GmbH micro-manipulator with a 1.5 $μ$m diamond tip, and the ability to achieve in-situ heating up to 450 °C on a Kleindiek heating stage provides a robust platform for the preparation, deformation, and heating of micro-pillars made from ceramic materials. This setup enabled us to conduct detailed studies on the Zirconia-based ceramic, observing permanent deformation exceeding 4% strain, followed by shape recovery at 370 °C. The paper provides outlines the key experimental steps that facilitated these observations.