Starting materials: PbO (99.9%), dimethylammonium chloride (99%), hydroiodic acid (HI, 57 wt % in H2O, distilled, stabilized, 99.95%), butylamine, hypophosphorous acid solution (H3PO2, 50 wt % in H2O)
Product: red plate-shaped crystals
Description: First, PbO (223 mg, 1 mmol) and DMA chloride acetate (40.8 mg, 0.5 mmol) were added to 1.75 mL of concentrated HI solution. These substances were dissolved under constant stirring and heating. Then, BA (49.6.1 μL, 0.5 mmol) was added to 0.25 mL of concentrated aqueous H3PO2 in a separate vial. This solution was stirred and was soon added to the initial solution. The temperature was lowered to 125º C until crystals began to form. The temperature was lowered again to 80ºC, the hot plate was turned off after 60 minutes, and after 30 minutes thereafter, the crystals were collected.
Method: UV-vis absorption
Description: A Shimadzu UV-3600 UV-vis NIR spectrometer (at 200-2500 nm region at 293 K) was used. BaSO4 was used as a reference of 100% reflectance for all measurements.
Crystal system: orthorhombic
| Photoluminescence peak position, eV |
|---|
Starting materials: PbO (99.9%), dimethylammonium chloride (99%), hydroiodic acid (HI, 57 wt % in H2O, distilled, stabilized, 99.95%), butylamine, hypophosphorous acid solution (H3PO2, 50 wt % in H2O)
Product: red plate-shaped crystals
Description: First, PbO (223 mg, 1 mmol) and DMA chloride acetate (40.8 mg, 0.5 mmol) were added to 1.75 mL of concentrated HI solution. These substances were dissolved under constant stirring and heating. Then, BA (49.6.1 μL, 0.5 mmol) was added to 0.25 mL of concentrated aqueous H3PO2 in a separate vial. This solution was stirred and was soon added to the initial solution. The temperature was lowered to 125º C until crystals began to form. The temperature was lowered again to 80ºC, the hot plate was turned off after 60 minutes, and after 30 minutes thereafter, the crystals were collected.
Method: Photoluminescence
Description: A Horiba LabRAM HR Evolution confocal Raman microscope was used with a 473 nm laser to excite samples at 50x magnification.
Starting materials: PbO (99.9%), dimethylammonium chloride (99%), hydroiodic acid (HI, 57 wt % in H2O, distilled, stabilized, 99.95%), butylamine, hypophosphorous acid solution (H3PO2, 50 wt % in H2O)
Product: red plate-shaped crystals
Description: First, PbO (223 mg, 1 mmol) and DMA chloride acetate (40.8 mg, 0.5 mmol) were added to 1.75 mL of concentrated HI solution. These substances were dissolved under constant stirring and heating. Then, BA (49.6.1 μL, 0.5 mmol) was added to 0.25 mL of concentrated aqueous H3PO2 in a separate vial. This solution was stirred and was soon added to the initial solution. The temperature was lowered to 125º C until crystals began to form. The temperature was lowered again to 80ºC, the hot plate was turned off after 60 minutes, and after 30 minutes thereafter, the crystals were collected.
Method: Photoluminescence
Description: A Horiba LabRAM HR Evolution confocal Raman microscope was used with a 473 nm laser to excite samples at 50x magnification.