X pert pro diffractometer

Powder diffraction studies were carried out using a PANalytical X'Pert Pro diffractometer equipped with an Anton Paar TCU 1000 N temperature control unit using Ni-filtered Cu Kα radiation (V = 40 kV, I = 30 mA). Transmission electron microscopy images were obtained using an FEI Tecnai G2 20 X-TWIN microscope equipped with a CCD FEI Eagle 2K camera with a HAADF detector and electron gun with a LaB₆ cathode. The pattern present on the left side of the TEM images is a microscope artifact.
An FLS1000 spectrometer from Edinburgh Instruments equipped with a R928P side window photomultiplier tube and a Hamamatsu detector was used to carry out measurements of photoluminescence decay curves and excitation spectra utilizing a micro-flash lamp and a halogen lamp, respectively. The emission spectra were measured using a Silver-Nova Super Range TEC spectrometer from Stellarnet of 1 nm spectral resolution and 808 nm excitation lines from a laser diode. The excitation pulse duration was modulated using a simple electronic PWM system. The temperature dependencies of both emission spectra and luminescence decay profiles were measured using a THMS 600 heating–cooling stage from Linkam (0.1 °C temperature stability and 0.1 °C set point resolution) to control the temperature.

Powder
X-ray diffraction patterns were recorded using a Bruker D8 Twin diffractometer
(Billerica, Massachusetts) with Cu Kα radiation λ = 1.54
Å at room temperature scanning between 2θ = 0 and 50°.
Variable-temperature powder X-ray diffraction data were collected
using a Panalytical X’Pert Pro diffractometer (Cu Kα_1,2, λ₁ = 1.540598 Å, λ₂ = 1.544426 Å) using a Bragg–Brentano geometry, equipped
with an Anton Paar XRK 900 high-temperature chamber.

Simultaneous thermal analysis (STA) measurements in the temperature range 30–900°C were performed with a ∼50 mg sample in a corundum crucible on a NETZSCH STA 449 C Jupiter system coupled with a Aeolos quadrupole mass analyzer. The quartz capillary was kept at 250°C. The measured mass signals were 2 (H₂), 12 (C), 14 (N), 15 (CH₃), 16 (CH₄, O), 17 (OH), 18 (H₂O), 28 (N₂, CO), 32 (O₂) and 44 (CO₂). All measurements were performed under a flowing argon atmosphere (20 ml min⁻¹) and heating rates of 10 K min⁻¹. Base line corrections of the TG curves were carried out by measuring the empty alumina crucible prior to each measurement. Temperature-dependent powder X-ray diffraction measurements (PXRD) were performed on a PANalytical X’Pert PRO diffractometer using a HTK1200 Anton-Paar high-temperature oven chamber mounted on the diffractometer. Prior to the measurement, the sample was finely ground and placed on a glass ceramic (Marcor) sample holder (depth 0.5 mm). The zero point was calibrated with a LaB₆ standard and automatically adjusted during the measurements with a PC-controllable alignment stage. The samples were heated under atmospheric conditions at 10 K min⁻¹ to the respective measurement temperature and kept for 5 min before measurement of each step to ensure temperature stability.