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In Situ Observation of Electron Beam-Induced Phase Transformation of CaCO3 to CaO via ELNES at Low Electron Beam Energies

Published online by Cambridge University Press:  08 April 2014

Ute Golla-Schindler ,
Gerd Benner ,
Alexander Orchowski  and
Ute Kaiser
Ute Golla-Schindler*
Affiliation:
Group of Electron Microscopy of Material Science, University Ulm, Albert-Einstein-Allee 11, 89081 Ulm, Germany
Gerd Benner
Affiliation:
Materials Division, Carl Zeiss Microscopy GmbH, Carl-Zeiss Str. 22, 73447 Oberkochen, Germany
Alexander Orchowski
Affiliation:
Materials Division, Carl Zeiss Microscopy GmbH, Carl-Zeiss Str. 22, 73447 Oberkochen, Germany
Ute Kaiser
Affiliation:
Group of Electron Microscopy of Material Science, University Ulm, Albert-Einstein-Allee 11, 89081 Ulm, Germany
*
*Corresponding author. [email protected]
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Abstract

It is demonstrated that energy-filtered transmission electron microscope enables following of in situ changes of the Ca-L2,3 edge which can originate from variations in both local symmetry and bond lengths. Low accelerating voltages of 20 and 40 kV slow down radiation damage effects and enable study of the start and finish of phase transformations. We observed electron beam-induced phase transformation of single crystalline calcite (CaCO3) to polycrystalline calcium oxide (CaO) which occurs in different stages. The coordination of Ca in calcite is close to an octahedral one streched along the <111> direction. Changes during phase transformation to an octahedral coordination of Ca in CaO go along with a bond length increase by 5 pm, where oxygen is preserved as a binding partner. Electron loss near-edge structure of the Ca-L2,3 edge show four separated peaks, which all shift toward lower energies during phase transformation at the same time the energy level splitting increases. We suggest that these changes can be mainly addressed to the change of the bond length on the order of picometers. An important pre-condition for such studies is stability of the energy drift in the range of meV over at least 1 h, which is achieved with the sub-Ångström low-voltage transmission electron microscope I prototype microscope.

Keywords

ELNESlow kV TEMSALVECaCO3 (calcite)radiation damage
Type
EDGE Special Issue
Information
Microscopy and Microanalysis , Volume 20 , Issue 3 , June 2014 , pp. 715 - 722
Copyright
© Microscopy Society of America 2014 

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