LaB6 filament operated at 100 kV. The NPs were dispersed
in hexane and then placed dropwise onto a holey carbon supported grid.
The particle size of the different samples and the standard deviation
were obtained by calculating the number average by manually measuring
the equivalent edge length of >200 octahedral particles from TEM
micrographs.
Ultrahigh-resolution TEM (UHRTEM) images were acquired at 200 kV on
a JEOL JEM-2200FS equipped with a Ω-filter (point resolution
0.19 nm). GPA was performed with the FRWRtools plugin for Digital
Micrograph (Gatan, Inc.) on
structure of the NPs was investigated by powder X-ray diffraction
(XRD) using a Bruker New D8 ADVANCE ECO diffractometer equipped with
Cu Kα radiation. The measurements were carried out in the range
of 20–90°, with a step size of 0.01° and a collection
time of 1 s. Quantitative analysis of the XRD data was undertaken
with a full pattern fitting procedure based on the Rietveld method
using the MAUD program.62 All the weighted
profile R-factors (RWP) obtained from Rietveld analysis are in the range between 0.082
and 0.091. The transition metal content (w/w) in NPs was assessed
by using an EDXRF spectrometer Shimadzu EDX-7000.