Subgrain boundary analyses in deformed orthopyroxene by TEM/STEM with EBSD-FIB sample preparation technique

Toshihiro Kogure,Akihito Kumamoto,Yuichi Ikuhara,Eiko Fujii,Hugues Raimbourg

doi:10.1186/1880-5981-66-84

Abstract

High-resolution structure analyses using electron beam techniques have been performed for the investigation of subgrain boundaries (SGBs) in deformed orthopyroxene (Opx) in mylonite from Hidaka Metamorphic Belt, Hokkaido, Japan, to understand ductile deformation mechanism of silicate minerals in shear zones. Scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD) analysis of Opx porphyroclasts in the mylonitic rock indicated that the crystal orientation inside the Opx crystals gradually changes by rotation about the b-axis by SGBs and crystal folding. In order to observe the SGBs along the b-axis by transmission electron microscopy (TEM) or scanning TEM (STEM), the following sample preparation protocol was adopted. First, petrographic thin sections were slightly etched with hydrofluoric acid to identify SGBs in SEM. The Opx crystals whose b-axes were oriented close to the normal of the surface were identified by EBSD, and the areas containing SGBs were picked and thinned for (S) TEM analysis with a focused ion beam instrument with micro-sampling system. High-resolution TEM imaging of the SGBs in Opx revealed various boundary structures from a periodic array of dissociated (100) [001] edge dislocations to partially or completely incoherent crystals, depending on the misorientation angle. Atomic-resolution STEM imaging clearly confirmed the formation of clinopyroxene (Cpx) structure between the dissociated partial dislocations. Moreover, X-ray microanalysis in STEM revealed that the Cpx contains a considerable amount of calcium replacing iron. Such chemical inhomogeneity may limit glide motion of the dislocation and eventually the plastic deformation of the Opx porphyroclasts at a low temperature. Chemical profiles across the high-angle incoherent SGB also showed an enrichment of the latter in calcium at the boundary, suggesting that SGBs are an efficient diffusion pathway of calcium out of host Opx grain during cooling.

Highlights

The interplay between deformation, grain size decrease, and mechanical weakening is considered as a major process to account for the localization of the ductile deformation of rocks in the shear zones (e.g., Boullier and Gueguen 1975; Rice 1976; Poirier 1980; Braun et al 1999; Furusho and Kanagawa 1999; Precigout et al 2007; Raimbourg et al 2008)
transmission electron microscopy (TEM) works on dislocations and subgrain boundaries (SGBs) are plenty (e.g., Kohlstedt and Vander Sande 1973; McLaren and Etheridge 1976, 1980), there is no systematic investigation of the transition from SGBs to true grain boundary (GB) which is the objective of the present work
The present study describes the result of scanning TEM (STEM) microanalysis to show the local chemical segregation at the SGBs, as well as the description of the sample preparation procedure

Summary

Introduction

The interplay between deformation, grain size decrease, and mechanical weakening is considered as a major process to account for the localization of the ductile deformation of rocks in the shear zones (e.g., Boullier and Gueguen 1975; Rice 1976; Poirier 1980; Braun et al 1999; Furusho and Kanagawa 1999; Precigout et al 2007; Raimbourg et al 2008). We reported and discussed the SGB structures in naturally deformed orthopyroxene ((Mg, Fe)SiO3, hereafter abbreviated as Opx) porphyroclasts in sheared metamorphic rock, by preparing TEM specimens from petrographic thin sections using FIB and EBSD (Raimbourg et al 2011). Following this previous work, the present study describes the result of scanning TEM (STEM) microanalysis to show the local chemical segregation at the SGBs, as well as the description of the sample preparation procedure. We discuss the implication of such chemical heterogeneities for the process of exsolution and the mobility of dislocations, using observations of microstructures in deformed Opx porphyroclasts

Methods

Results

Conclusion