To prepare the CH
3NH
3PbI
3 specimens, equimolar CH
3NH
3I and PbI
2 (98%, Sinopharm) were mixed in γ-butyrolactone (97%, Sinopharm) at 60 °C overnight whilst being stirred. Then, the aqueous precursor was deposited on FTO glass by spin-coating at 2000 rpm for 40s. Finally, the specimens were annealed at 100 °C for 15 min on a preheated hot plate, and the obtained CH
3NH
3PbI
3/FTO films were brown black27 .
In situ synchrotron radiation XRD was performed at the BL14B station of Shanghai Synchrotron Radiation Facility (SSRF), and the experimental setup is schematically shown in
Fig. 1. The diffractive patterns were recorded by a two-dimension x-ray detector (charge coupled device, CCD) with 3072 × 3072 pixels. To monitor the reaction at real-time, the diffraction patterns were continuously recorded with 10 seconds per frame and 1 second between adjacent frames.
To investigate the CH
3NH
3PbI
3 film morphology before/after the reaction, microscopy analysis was performed by using optical microscope (OLYMPUS, BX51) and scanning electron microscope (SEM,
JSM-6700F).
Zhao J., Cai B., Luo Z., Dong Y., Zhang Y., Xu H., Hong B., Yang Y., Li L., Zhang W, & Gao C. (2016). Investigation of the Hydrolysis of Perovskite Organometallic Halide CH3NH3PbI3 in Humidity Environment. Scientific Reports, 6, 21976.