Starting materials: Lead Oxide (PbO), HI (57% w/w aqueous), H3PO2 (50% aqueous), butylammonium iodide (n-CH3(CH2)3NH3I) , solid CH3NH3Cl
Product: Dark red plate-like (BA)2(MA)2Pb3I10 crystals
Description: PbO powder (2232 mg, 10 mmol) was dissolved in a mixture of HI solution (10.0 mL, 76 mmol) and H3PO2 (1.7 mL, 15.5 mmol) by heating to boiling under constant magnetic stirring for about 5 min, which formed a bright yellow solution. Subsequent addition of solid CH3NH3Cl (450 mg, 6.67 mmol) to the hot yellow solution initially caused the precipitation of a black powder, which rapidly redissolved under stirring to afford a clear bright yellow solution. In a separate beaker, n-CH3(CH2)3NH2 (327 μL, 3.33 mmol) was neutralized with HI 57% w/w (5 mL, 38 mmol) in an ice bath resulting in a clear pale yellow solution. Addition of the n-CH3(CH2)3NH3I solution to the PbI2 solution initially produced a black precipitate, which was subsequently dissolved under heating the combined solution to boiling. The stirring was then discontinued, and the solution was left to cool to room temperature during which time deep-red/purple rectangular-shaped plates started to crystallize. The precipitation was deemed to be complete after ∼2 h. The crystals were isolated by suction filtration and thoroughly dried under reduced pressure.
Method: Single Crystal X-ray diffraction
Description: Single-crystal X-ray diffraction data were collected using an image plate STOE IPDS II diffractometer using Mo Kα radiation (λ = 0.71073 Å), operating at 50 kV and 40 mA. Data reduction and numerical absorption corrections were performed using the X-AREA suite
See all entries for this property (2 total)
Starting materials: Lead Oxide (PbO), HI (57% w/w aqueous), H3PO2 (50% aqueous), butylammonium iodide (n-CH3(CH2)3NH3I) , solid CH3NH3Cl
Product: Dark red plate-like (BA)2(MA)2Pb3I10 crystals
Description: PbO powder (2232 mg, 10 mmol) was dissolved in a mixture of HI solution (10.0 mL, 76 mmol) and H3PO2 (1.7 mL, 15.5 mmol) by heating to boiling under constant magnetic stirring for about 5 min, which formed a bright yellow solution. Subsequent addition of solid CH3NH3Cl (450 mg, 6.67 mmol) to the hot yellow solution initially caused the precipitation of a black powder, which rapidly redissolved under stirring to afford a clear bright yellow solution. In a separate beaker, n-CH3(CH2)3NH2 (327 μL, 3.33 mmol) was neutralized with HI 57% w/w (5 mL, 38 mmol) in an ice bath resulting in a clear pale yellow solution. Addition of the n-CH3(CH2)3NH3I solution to the PbI2 solution initially produced a black precipitate, which was subsequently dissolved under heating the combined solution to boiling. The stirring was then discontinued, and the solution was left to cool to room temperature during which time deep-red/purple rectangular-shaped plates started to crystallize. The precipitation was deemed to be complete after ∼2 h. The crystals were isolated by suction filtration and thoroughly dried under reduced pressure.
Method: Photoluminescence spectroscopy
Description: Oriented rectangular crystals were used in the collection of photoluminescence spectra. Crystals of type (BA)2(MA)2Pb3I10 provided data for the material with n=3. A Horiba LabRam Evolution Raman microscope spectrometer with a diode CW laser (600 g/mm diffraction grating; 473 m, 25 mW) and a Synapse CCD camera carried out measurements. The laser beam was focused at about 1 µm spot size was made parallel to the 010 orientation of the crystals. The power output of the laser source was limited to 0.1% of the maximum power output.
Crystal system: unknown
| Band gap (fundamental), eV |
|---|
Starting materials: PbO, HI, H3PO2, butylamine, MACl
Product: spin-coated thin film, high crystallinity
Description: First step: BA2MA2PbI4 single crystal flakes synthesized as follows: Slow-cooling in HI method: 2.232g (10 mmol) of PbO dissolved in glass vial containing 10 mL of HI and 1.7 mL of H3PO2. Brought to near-boiling temperature. 5 mmol of MACl added and dissolved. 10 mmol of the organic amine mixed with 5 mL HI, cooled in an ice bath. Solutions were mixed and heated, then cooled to room temperature, upon which single crystal flakes form. Crystals were then washed thrice with diethyl ether and dried under a vacuum. Second step (thin film formation): Flakes were dissolved in 4:1 DMF:DMSO solvent mixture, stirred for 30 minutes. Substrate: quartz substrate with 120 nm gold layer of interdigitated fingers. Precursor solution (0.05-0.1 molar) pipetted onto substrate and then spun at 4000 rpm for 30 seconds, targeting film thickness of 80-300nm. Film was solvent-annealed, then enclosed with 2mL dH2O.
Method: Electroabsorption
Description: Films were spin-coated onto interdigitated Au electrode array - 45 micron distance between opposing fingers. Samples mounted in cryostat with Cu wires soldered to opposing electrode stripes. Xe lamp light spectrally filtered, focused on sample and subsequently on UV-enhanced Si photodiode detector. Sample transmission, substrate transmission, and sample electrotransmission were collected in independent scans. Absorbance and electroabsorbance were then calculated from the respective transmissions. The fundamental gap is determined by the crossover point of absorption curves measured under different electric fields in the fundamental band gap region.
Comment: Significantly more detail in paper.
Crystal system: unknown
| Exciton binding energy, eV |
|---|
Starting materials: PbO, HI, H3PO2, butylamine, MACl
Product: spin-coated thin film, high crystallinity
Description: First step: BA2MA2PbI4 single crystal flakes synthesized as follows: Slow-cooling in HI method: 2.232g (10 mmol) of PbO dissolved in glass vial containing 10 mL of HI and 1.7 mL of H3PO2. Brought to near-boiling temperature. 5 mmol of MACl added and dissolved. 10 mmol of the organic amine mixed with 5 mL HI, cooled in an ice bath. Solutions were mixed and heated, then cooled to room temperature, upon which single crystal flakes form. Crystals were then washed thrice with diethyl ether and dried under a vacuum. Second step (thin film formation): Flakes were dissolved in 4:1 DMF:DMSO solvent mixture, stirred for 30 minutes. Substrate: quartz substrate with 120 nm gold layer of interdigitated fingers. Precursor solution (0.05-0.1 molar) pipetted onto substrate and then spun at 4000 rpm for 30 seconds, targeting film thickness of 80-300nm. Film was solvent-annealed, then enclosed with 2mL dH2O.
Method: Electroabsorption
Description: Films were spin-coated onto interdigitated Au electrode array - 45 micron distance between opposing fingers. Samples mounted in cryostat with Cu wires soldered to opposing electrode stripes. Xe lamp light spectrally filtered, focused on sample and subsequently on UV-enhanced Si photodiode detector. Sample transmission, substrate transmission, and sample electrotransmission were collected in independent scans.Absorbance and electroabsorbance were then calculated from the respective transmissions. The exciton binding energy arises as the difference of the 1s exciton peak energy observed in conventional absorption and the fundamental gap as determined by the crossover point of absorption curves measured under different electric fields in the fundamental band gap region.
Comment: Significantly more detail in paper.
Crystal system: unknown
| Exciton energy, eV |
|---|
Starting materials: PbO, HI, H3PO2, butylamine, MACl
Product: spin-coated thin film, high crystallinity
Description: First step: BA2MA2PbI4 single crystal flakes synthesized as follows: Slow-cooling in HI method: 2.232g (10 mmol) of PbO dissolved in glass vial containing 10 mL of HI and 1.7 mL of H3PO2. Brought to near-boiling temperature. 5 mmol of MACl added and dissolved. 10 mmol of the organic amine mixed with 5 mL HI, cooled in an ice bath. Solutions were mixed and heated, then cooled to room temperature, upon which single crystal flakes form. Crystals were then washed thrice with diethyl ether and dried under a vacuum. Second step (thin film formation): Flakes were dissolved in 4:1 DMF:DMSO solvent mixture, stirred for 30 minutes. Substrate: quartz substrate with 120 nm gold layer of interdigitated fingers. Precursor solution (0.05-0.1 molar) pipetted onto substrate and then spun at 4000 rpm for 30 seconds, targeting film thickness of 80-300nm. Film was solvent-annealed, then enclosed with 2mL dH2O.
Method: Electroabsorption
Description: Films were spin-coated onto interdigitated Au electrode array - 45 micron distance between opposing fingers. Samples mounted in cryostat with Cu wires soldered to opposing electrode stripes. Xe lamp light spectrally filtered, focused on sample and subsequently on UV-enhanced Si photodiode detector. Sample transmission, substrate transmission, and sample electrotransmission were collected in independent scans. Absorbance and electroabsorbance were then calculated from the respective transmissions.
Comment: Significantly more detail in paper.