Crystal system: orthorhombic
| a: | 8.856 Å |
| b: | 8.576 Å |
| c: | 12.472 Å |
| α: | 90° |
| β: | 90° |
| γ: | 90° |
Starting materials: CsI (Alfa Aesar, 99.9%), PbI2 (TCI)
Product: Black-phase CsPbI3 powder
Description: Stoichiometric quantities of CsI (Alfa Aesar, 99.999%) and PbI2 (Sigma Aldrich, 99.999%) were ground in a mortar and pestle in nitrogen atmosphere for 30 minutes, transferred to a quartz ampoule, and sealed under vacuum. The 2 ampoule was heated to 525 °C for over 72 hours and cooled at 50 °C/hour, to form a solid mass of CsPbI3. This mass was ground into a powder and reheated at 400 °C in batches, each for approximately 20 s (until black to the eye), before being transferred to a piece of room temperature aluminium foil to cool quickly.
Comment: While the paper also describes a synthesis method for CsPbI₃ films, those details are not included here.
Method: X-ray diffraction
Description: A Panalytical X'pert powder diffractometer with Cu anode X-ray source (Cu kα1, 1.54060 Å) was used for XRD characterisation measurements of both powders and films. All measurements were made at 293 K. Anton Paar Domed Sample Holders were used for measurements under nitrogen of black powders and films of CsPbI3. The scratched powders were dropped onto greased quartz discs, and powder from solid state synthesis was prepared as packed powder samples.