Crystallographic faceting of bulk tungsten surfaces observed during in situ heating in an environmental scanning electron microscope

Abstract

The surface faceting of metals has been studied for several decades, typically using experimental methods such as low-energy electron diffraction. In the current paper, surface faceting of tungsten pellets was studied during in situ heating inside an environmental scanning electron microscope (ESEM), which allowed for direct, high-fidelity observation of morphological changes in response to high-temperature annealing under a moderate vacuum (0.8 Torr). Additionally, a second set of tungsten samples was annealed in an ultrahigh vacuum chamber (10−8 Torr), albeit without direct observation via ESEM. This study revealed that oxygen plays a crucial role in tungsten surface faceting and in a morphological transition to vertex rounding. Furthermore, this paper discusses relevant techniques for identifying the crystallographic indices of surface facets. It is demonstrated that a combination of electron backscatter diffraction, tilted-sample imaging from multiple angles, and serial sectioning in a focused ion beam system can be effectively deployed to determine the geometry of faceting, which in turn can be verified with the aid of software for generating Wulff shapes. The influence of processing environment on tungsten surface faceting enables the possibility of designing and controlling the morphology and crystallographic facets of tungsten surfaces.