Abstract

Electron backscatter diffraction (EBSD) was used for the analysis of multiple cyclic twins in cassiterite (SnO2), which form during sintering of SnO2 with small additions of CoO and Nb2O5. Grain misorientation analysis has shown that about one third of all grains contain {101} twin boundaries (TBs). The majority of these grains are contact twins, whereas a small fraction of grains are multiple, mainly cyclic twins. A procedure was developed in MTEX [Bachmann, Hielscher & Schaeben (2010). Solid State Phenom. 160, 63-88] for automated identification of crystallographically different types of cyclic twins and found two main types: coplanar twins composed of three or four domains with a common [010] axis and alternating twins composed of three to seven domains oriented along the [111] axis. Both types of cyclic twins have a characteristic common origin (nucleus) of all TBs, which is positioned eccentric relative to the grain section and the cycle is closed with a shorter non-crystallographic contact between the first and the last twin domain. The morphology of cyclic twins suggests that they form by nucleation in the initial stages of grain growth. The average size of twinned grains increases with the number of twin domains indicating the influence of TBs formation on the growth of composite grains.

Highlights

  • The sintering of SnO2 with small amounts of Coand Nb-oxides results in the development of a polycrystalline ceramic microstructure composed of randomly oriented cassiterite grains with a fairly large fraction of grains containing {101} twin boundaries (TBs) (Tominc et al, 2018)

  • In our previous study we focused on the functional properties of the ceramics and densification in relation to the specific charge compensation mechanisms in cassiterite with the addition of aliovalent dopants, whereas questions related to the crystallography of cyclic twins and reasons for their formation remained open

  • We found that the microstructure of SnO2-based ceramics sintered with small additions of Co- and Nb-oxides consists of untwinned grains, contact twins and a small fraction of multiple, mostly cyclic twins with coplanar and alternating morphology

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Summary

Introduction

The sintering of SnO2 (cassiterite) with small amounts of Coand Nb-oxides results in the development of a polycrystalline ceramic microstructure composed of randomly oriented cassiterite grains with a fairly large fraction of grains containing {101} twin boundaries (TBs) (Tominc et al, 2018). This type of multiple twin forms by self-assembly during unconstrained growth in three dimensions, e.g. by exsolution from saturated hydrothermal solutions. Another configuration of multiple twins are 2D intergrowths, where all domains intersect at $60 and are oriented along a common crystallographic axis. In rutile, such reticulated (or geniculated) intergrowths are known as sagenite, their formation is related to epitaxial growth on a structurally related substrate (epitaxial twinning) or oriented recrystallization of a structurally related precursor (topotaxial twinning) like ilmenite (FeTiO3) (Armbruster, 1981; Force et al, 1996; Recnik et al, 2015). The mechanisms leading to the formation of cyclic twins are not yet fully understood

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