Phase Identification
and Structure Solution by Three-Dimensional
Electron Diffraction Tomography: Gd–Phosphate Nanorods
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Abstract
Hydrothermal synthesis of GdPO<sub>4</sub> in the presence of poly(methacrylic acid) yields nanorods
with a diameter of 15 nm and an aspect ratio of 20. Powder X-ray diffraction
patterns showed that the GdPO<sub>4</sub> nanorods display peaks characteristics
for both monoclinic and hexagonal structures. Three-dimensional electron
diffraction tomography (3D EDT) was used to determine the structures <i>ab initio</i> on the basis of reciprocal volume reconstruction
of electron diffraction data sets collected from single nanorods.
The crystal structure of the monoclinic form was shown to be <i>P</i>2<sub>1</sub>/<i>n</i>, corroborating previous
work. We were able to solve the 3D structure of the hexagonal <i>P</i>6<sub>2</sub>22 form, which has not been reported previously.
Our work shows that 3D EDT is a powerful method that can be used for
solving structures of single nanocrystals