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Submicrometer-scale spatial heterogeneity in silicate glasses using aberration-corrected scanning transmission electron microscopy

  • Katherine D. Burgess EMAIL logo , Rhonda M. Stroud , M. Darby Dyar and Molly C. McCanta
Published/Copyright: November 30, 2016
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American Mineralogist
From the journal American Mineralogist Volume 101 Issue 12

Abstract

Experimental silicate glasses are often used as analog and calibration material for terrestrial and planetary materials. Measurements of Fe oxidation state using electron energy loss spectroscopy (EELS) in an aberration-corrected scanning transmission electron microscope (ac-STEM) show that a suite of experimental silicate (e.g., basaltic, andesitic, rhyolitic) glasses have spatially heterogeneous oxidation states at scales of tens of nanometers. Nano-crystals are observed in several of the glasses, indicating nucleation and incipient crystallization not seen at the scale of electron microprobe analysis (EMPA). Glasses prepared in air are uniformly oxidized while glasses prepared at the iron-wustite (IW) or quartz-fayalite-magnetite (QFM) buffers range from reduced to highly oxidized. EELS spectral shapes indicate that oxidized glasses have tetrahedral Fe3+. The nanoscale compositional and structural heterogeneities present in the experimental glasses mean that the suitability of such glasses as analogs for natural materials and calibration standards depends strongly on the scale of the measurements being done. The electron beam quickly damages silicate glass, but data showing changes in oxidation state among and within samples can be obtained with careful control of the beam current and dwell time. Determination of oxidation state in silicate glasses via STEM-EELS is very challenging, and accurate and reliable measurements of Fe3+/ΣFe require careful sample preparation and control of microscope conditions and benefit from comparison to complementary techniques.

Key words: Iron oxidation; silicate glass; transmission electron microscopy (TEM); electron energy loss spectroscopy (EELS); beam damage

Acknowledgments

This work was supported by the RIS4E node of NASA’s Solar System Exploration Research Virtual Institute. It is SSERVI publication number SSERVI-2016-031. We thank A. Brearly, F. Langenhorst, and B. Mysen for thorough and constructive reviews.

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Received: 2016-1-28
Accepted: 2016-7-6
Published Online: 2016-11-30
Published in Print: 2016-12-1

© 2016 by Walter de Gruyter Berlin/Boston

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https://doi.org/10.2138/am-2016-5696
Keywords for this article
Iron oxidation; silicate glass; transmission electron microscopy (TEM); electron energy loss spectroscopy (EELS); beam damage

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  38. Statistical petrology reveals a link between supercontinents cycle and mantle global climate
  39. Letter
  40. An improved clinopyroxene-based hygrometer for Etnean magmas and implications for eruption triggering mechanisms
  41. Research Article
  42. New Mineral Names
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