X pert pro super diffractometer

The phase detection of
products was performed by powder XRD (Philips X’Pert Pro Super
diffractometer, Cu Kα radiation, λ = 1.54178 Å).
TEM and FESEM images were recorded with a transmission electron microscope
(JEOL, JEM-1011) and a field emission scanning electron microscope
(JEOL, JSM-6700F), respectively. HRTEM images were recorded using
an electron microscope (JEM-2100F, accelerating voltage: 200 kV) coupled
with an X-ray energy-dispersive spectroscopy (EDX) instrument. TGA
(PerkinElmer Diamond TG/DTA apparatus) was conducted at a heating
rate of 10 °C/min in flowing air. FTIR spectra were recorded
on a Bruker EQUINOX55 spectrometer with a potassium bromide pellet
as a control.

NMR spectra were
recorded on a Bruker AV300 NMR spectrometer (resonance frequency of
300 MHz for 1 h) operated in the Fourier transform mode. CDCl₃ was used as the solvent. FTIR spectra were measured on a
NICOLET FT-IR spectrometer, using pressed KBr tablets. UV–vis
spectra were recorded on a Solid Spec-3700 spectrophotometer at room
temperature. Fluorescence measurements were recorded on the Fluorolog-3-Tau
(Jobin Yvon, France) fluorescence spectrometer. The excitation wavelength
for the fluorescence spectra was 290 nm, which was produced by a xenon
lamp equipped with a grating monochromator. Low temperatures were
achieved by the CCS-355 (Janis, America) low-temperature equipment.
The field emission scanning electron microscopy images were taken
on a FEI Sirion-200 scanning electron microscope. TEM images were
obtained by a Hitachi model H-800 instrument with a tungsten filament,
using an accelerating voltage of 200 kV. The XRD patterns were recorded
using a Philips X’Pert Pro Super diffractometer with Cu Kα
radiation (λ = 1.54178 Å). The magnetic data were acquired
using a magnetic property measurement system (MPMS) 5XL Quantum design
SQUID magnetometer at room temperature. DSC measurements were taken
on a Mettler-toledo DSC823e instrument (temperature range: 300–650
K; aluminum crucible with pierced lid; sample mass: 3.5 mg; air atmosphere;
and heating/cooling rate: 5/5 K min^–1).