Bis(ethanolammonium) lead iodide

Chemical Formula: C4H16N2O2PbI4
IUPAC: bis(2-hydroxyethanaminium) lead(II) iodide
Alternate Names: EOA2PbI4, bis(ethanolammonium) lead iodide, (C2H8ON)2PbI4
Organic: OC2NH8
Inorganic: PbI4, Lead iodide
Dimensionality: 2D n:
Formal Stoichiometry: C : 4 , H : 16 , N : 2 , O : 2 , Pb : 1 , I : 4
Atomic structure
Origin: experimental (T = 173.0 K)
Lattice parameters

Crystal system: monoclinic

a:10.167 (±0.003) Å
b:9.038 (±0.003) Å
c:8.93 (±0.003) Å
α:90°
β:100.572 (±0.005)°
γ:90°
Fixed parameters:
  • temperature = 173.0 K
A. Lemmerer and D. G. Billing, Effect of heteroatoms in the inorganic–organic layered perovskite-type hybrids [(ZCnH2nNH3)2PbI4], n = 2, 3, 4, 5, 6; Z = OH, Br and I; and [(H3NC2H4S2C2H4NH3)PbI4], CrystEngComm 12, 1290‑1301 (2010). doi: 10.1039/B917824D.
System description
Dimensionality: 2D n:
Sample type: single crystal

Starting materials: PbI2, HI, EOA, diethyl ether

Product: Red single crystals (EOA2PbI4)

Description: PbI2 (0.16 g, 0.35 mmol) is dissolved in HI solution (1 mL). Then, EOA (80 μL, 1.3 mmol) is added. This solution is sonicated at room temperature for five minutes. It is then kept at 3 °C in a fridge. Later, red single crystals can be filtered and washed with diethyl ether. They are vacuum dried overnight.

Method: Single-crystal X-ray diffraction

Description: Single crystal X-ray diffraction data was collected at 173 K using a Bruker SMART 1K CCD detectordiffractometer with graphite monochromated Mo Kα radiation (λ = 0.71073 Å). Software used in this process was Bruker SAINT+ and SHELXS-97. Further data was gathered using PLATON, WinGx, ORTEP, and DIAMOND.

A. Lemmerer and D. G. Billing, Effect of heteroatoms in the inorganic–organic layered perovskite-type hybrids [(ZCnH2nNH3)2PbI4], n = 2, 3, 4, 5, 6; Z = OH, Br and I; and [(H3NC2H4S2C2H4NH3)PbI4], CrystEngComm 12, 1290‑1301 (2010). doi: 10.1039/B917824D.

Extraction method: manual
Entry added on: Nov. 22, 2022, 10:46 a.m.
Entry added by: Harrison York Duke University
Last updated on: Nov. 29, 2022, 9:43 a.m.
Last updated by: Harrison York Duke University

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Data set ID: 2148 Did you find any mistakes or inconsistencies about this data? Send us a note and we'll have a look at it and send you a reply. Thanks!

 

Atomic coordinates


Absorption (Kubelka−Munk)
Exciton binding energy, Eb ≈ 46 meV
Origin: experimental (T = 298.0 K)
X. Chen, H. Lu, K. Wang, Y. Zhai, V. Lunin, P. Sercel, and M. Beard, Tuning Spin-Polarized Lifetime in Two-Dimensional Metal−Halide Perovskite through Exciton Binding Energy, Journal of the American Chemical Society 143, 19438‑19445 (2021). doi: doi.org/10.1021/jacs.1c08514.
System description
Dimensionality: 2D n:
Sample type: powder
Related data
This data set is directly linked to other data sets: See all related data

Starting materials: lead iodide (PbI2), hydroiodic acid (HI, 57% w/w aqueous, stabilized with H3PO2), ethanolamine (EOA), diethyl ether

Product: Red single crystals (EOA2PbI4)

Description: PbI2 (0.16 g, 0.35 mmol) is dissolved in HI solution (1 mL). Then, EOA (80 μL, 1.3 mmol) is added. This solution is sonicated at room temperature for five minutes. It is then kept at 3 °C in a fridge. Later, red single crystals can be filtered and washed with diethyl ether. They are vacuum dried overnight.

Method: Diffuse reflectance spectroscopy

Description: Powder samples of EOA2PbI4 were used to measure absorption. Linear absorptions can be determined from measurements of UV-vis reflection.

Comment: A 2D Elliot formula was used to create a fit for the data. This formula can be found in the supporting information of the referenced publication and the files attached to this dataset. The formula can extract the exciton binding energy of this material. The analysis yields an exciton binding energy of ≈ 46 meV.

X. Chen, H. Lu, K. Wang, Y. Zhai, V. Lunin, P. Sercel, and M. Beard, Tuning Spin-Polarized Lifetime in Two-Dimensional Metal−Halide Perovskite through Exciton Binding Energy, Journal of the American Chemical Society 143, 19438‑19445 (2021). doi: doi.org/10.1021/jacs.1c08514.

Extraction method: manual
Entry added on: Nov. 10, 2022, 11:08 a.m.
Entry added by: Harrison York Duke University
Last updated on: Nov. 22, 2022, 9:52 a.m.
Last updated by: Harrison York Duke University

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Data set ID: 2142 Did you find any mistakes or inconsistencies about this data? Send us a note and we'll have a look at it and send you a reply. Thanks!

Transient reflectance Verified
5 picosecond pump-probe delay
Origin: experimental (T = 298.0 K)
Space group: P 2₁/c
X. Chen, H. Lu, K. Wang, Y. Zhai, V. Lunin, P. Sercel, and M. Beard, Tuning Spin-Polarized Lifetime in Two-Dimensional Metal−Halide Perovskite through Exciton Binding Energy, Journal of the American Chemical Society 143, 19438‑19445 (2021). doi: doi.org/10.1021/jacs.1c08514.
System description
Dimensionality: 2D n:
Sample type: single crystal

Starting materials: lead iodide (PbI2), hydroiodic acid (HI, 57% w/w aqueous, stabilized with H3PO2), ethanolamine (EOA), diethyl ether

Product: Red single crystals (EOA2PbI4)

Description: PbI2 (0.16 g, 0.35 mmol) is dissolved in HI solution (1 mL). Then, EOA (80 μL, 1.3 mmol) is added. This solution is sonicated at room temperature for five minutes. It is then kept at 3 °C in a fridge. Later, red single crystals can be filtered and washed with diethyl ether. They are vacuum dried overnight.

Method: Pump-probe spectroscopy

Description: Pump-probe delay spectroscopy was used with single crystals of EOA2PbI4 to measure transient reflectance spectra. A Ti:sapphire laser amplifier (Coherent Astrella, 800 nm, pulse duration ∼60 fs, ∼5 mJ/pulse, and 1 kHz repetition rate) was used for this measurement, and a Helios Ultrafast System was used as the transient reflection spectrometer. A fundamental beam of 800 nm was split into two beams, one being sent to generate the pump pulse and the other focused to create the white light probe (1.6---2.8 eV). The pump beam size was ∼590 μm and the probe size was ∼200 μm. The pump beam was sent directly toward the crystal from 90°, and the probe beam hit the crystal at 45°.

X. Chen, H. Lu, K. Wang, Y. Zhai, V. Lunin, P. Sercel, and M. Beard, Tuning Spin-Polarized Lifetime in Two-Dimensional Metal−Halide Perovskite through Exciton Binding Energy, Journal of the American Chemical Society 143, 19438‑19445 (2021). doi: doi.org/10.1021/jacs.1c08514.

Extraction method: manual
Entry added on: Nov. 15, 2022, 11:45 a.m.
Entry added by: Harrison York Duke University
Last updated on: Nov. 21, 2022, 6:42 p.m.
Last updated by: Rayan C Duke University
Data correctness verified by:
  • Rayan C Duke University

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Data set ID: 2143 Did you find any mistakes or inconsistencies about this data? Send us a note and we'll have a look at it and send you a reply. Thanks!

Transient absorption Verified
Origin: experimental (T = 298.0 K)
Space group: P 2₁/c
X. Chen, H. Lu, K. Wang, Y. Zhai, V. Lunin, P. Sercel, and M. Beard, Tuning Spin-Polarized Lifetime in Two-Dimensional Metal−Halide Perovskite through Exciton Binding Energy, Journal of the American Chemical Society 143, 19438‑19445 (2021). doi: doi.org/10.1021/jacs.1c08514.
System description
Dimensionality: 2D n:
Sample type: single crystal

Starting materials: lead iodide (PbI2), hydroiodic acid (HI, 57% w/w aqueous, stabilized with H3PO2), ethanolamine (EOA), diethyl ether

Product: Red single crystals (EOA2PbI4)

Description: PbI2 (0.16 g, 0.35 mmol) is dissolved in HI solution (1 mL). Then, EOA (80 μL, 1.3 mmol) is added. This solution is sonicated at room temperature for five minutes. It is then kept at 3 °C in a fridge. Later, red single crystals can be filtered and washed with diethyl ether. They are vacuum dried overnight.

Method: Pump-probe spectroscopy

Description: Pump-probe delay spectroscopy was used with single crystals of EOA2PbI4 to measure transient reflectance spectra. A Ti:sapphire laser amplifier (Coherent Astrella, 800 nm, pulse duration ∼60 fs, ∼5 mJ/pulse, and 1 kHz repetition rate) was used for this measurement, and a Helios Ultrafast System was used as the transient reflection spectrometer. A fundamental beam of 800 nm was split into two beams, one being sent to generate the pump pulse and the other focused to create the white light probe (1.6---2.8 eV). The pump beam size was ∼590 μm and the probe size was ∼200 μm. The pump beam was sent directly toward the crystal from 90°, and the probe beam hit the crystal at 45°. A Kramers---Kronig transformation was used to obtain the change in absorbance of the reflected light.

X. Chen, H. Lu, K. Wang, Y. Zhai, V. Lunin, P. Sercel, and M. Beard, Tuning Spin-Polarized Lifetime in Two-Dimensional Metal−Halide Perovskite through Exciton Binding Energy, Journal of the American Chemical Society 143, 19438‑19445 (2021). doi: doi.org/10.1021/jacs.1c08514.

Extraction method: manual
Entry added on: Nov. 15, 2022, 2:57 p.m.
Entry added by: Harrison York Duke University
Last updated on: Nov. 21, 2022, 6:51 p.m.
Last updated by: Rayan C Duke University
Data correctness verified by:
  • Rayan C Duke University

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Data set ID: 2144 Did you find any mistakes or inconsistencies about this data? Send us a note and we'll have a look at it and send you a reply. Thanks!

Exciton binding energy

See all entries for this property (2 total)

Origin: experimental
Exciton binding energy

Crystal system: monoclinic

Exciton binding energy, meV
X. Chen, H. Lu, K. Wang, Y. Zhai, V. Lunin, P. Sercel, and M. Beard, Tuning Spin-Polarized Lifetime in Two-Dimensional Metal−Halide Perovskite through Exciton Binding Energy, Journal of the American Chemical Society 143, 19438‑19445 (2021). doi: doi.org/10.1021/jacs.1c08514.
System description
Dimensionality: 2D n:
Sample type: powder
Related data
This data set is directly linked to other data sets: See all related data

Starting materials: lead iodide (PbI2), hydroiodic acid (HI, 57% w/w aqueous, stabilized with H3PO2), ethanolamine (EOA), diethyl ether

Product: Red single crystals (EOA2PbI4)

Description: PbI2 (0.16 g, 0.35 mmol) is dissolved in HI solution (1 mL). Then, EOA (80 μL, 1.3 mmol) is added. This solution is sonicated at room temperature for five minutes. It is then kept at 3 °C in a fridge. Later, red single crystals can be filtered and washed with diethyl ether. They are vacuum dried overnight.

Method: Diffuse reflectance spectroscopy

Description: Powder samples of EOA2PbI4 were used to measure absorption. Linear absorptions can be determined from measurements of UV-vis reflection, and a 2D Elliot formula was used to create a fit for the data. This formula can be found in the supporting information of the referenced publication and the files attached to this dataset. The formula can extract the exciton binding energy of this material. The analysis yields an exciton binding energy of ≈ 46 meV.

X. Chen, H. Lu, K. Wang, Y. Zhai, V. Lunin, P. Sercel, and M. Beard, Tuning Spin-Polarized Lifetime in Two-Dimensional Metal−Halide Perovskite through Exciton Binding Energy, Journal of the American Chemical Society 143, 19438‑19445 (2021). doi: doi.org/10.1021/jacs.1c08514.

Extraction method: manual
Entry added on: Nov. 22, 2022, 10:38 a.m.
Entry added by: Harrison York Duke University
Last updated on: Nov. 22, 2022, 10:38 a.m.
Last updated by: Harrison York Duke University

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Data set ID: 2147 Did you find any mistakes or inconsistencies about this data? Send us a note and we'll have a look at it and send you a reply. Thanks!

Band gap (fundamental) Verified
Method: Electroabsorption
Origin: experimental (T = 15.0 K)
Band gap (fundamental)

Crystal system: unknown

Band gap (fundamental), eV
Fixed parameters:
  • temperature = 15.0 K
K. Hansen, C. Wong, C. E. McClure, B. Romrell, L. Flannery, D. Powell, K. Garden, A. Berzansky, M. Eggleston, D. King, C. Shirley, M. Beard, W. Nie, A. Schleife, J. Colton, and L. Whittaker-Brooks, Uncovering Unique Screening Effects in 2D Perovskites: Implications for Exciton and Band Gap Engineering, ResearchSquare Preprint, 1‑22 (2023). doi: https://doi.org/10.21203/rs.3.rs-2667143/v1.
System description
Dimensionality: 2D n:
Sample type: film

Starting materials: PbO, HI, H3PO2, ethanolamine

Product: spin-coated thin film, high crystallinity and strong exciton absorption

Description: First step: EOA2PbI4 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. 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.

K. Hansen, C. Wong, C. E. McClure, B. Romrell, L. Flannery, D. Powell, K. Garden, A. Berzansky, M. Eggleston, D. King, C. Shirley, M. Beard, W. Nie, A. Schleife, J. Colton, and L. Whittaker-Brooks, Uncovering Unique Screening Effects in 2D Perovskites: Implications for Exciton and Band Gap Engineering, ResearchSquare Preprint, 1‑22 (2023). doi: https://doi.org/10.21203/rs.3.rs-2667143/v1.

Extraction method: Manual from article (Table S1)
Entry added on: June 8, 2023, 8:22 p.m.
Entry added by: Kelly Ma
Last updated on: June 9, 2023, 1:23 p.m.
Last updated by: Volker Blum Duke University
Data correctness verified by:
  • Volker Blum Duke University

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Data set ID: 2313 Did you find any mistakes or inconsistencies about this data? Send us a note and we'll have a look at it and send you a reply. Thanks!

Exciton energy
Method: Electroabsorption
Origin: experimental (T = 15.0 K)
Exciton energy

Crystal system: unknown

Exciton energy, eV
Fixed parameters:
  • temperature = 15.0 K
K. Hansen, C. Wong, C. E. McClure, B. Romrell, L. Flannery, D. Powell, K. Garden, A. Berzansky, M. Eggleston, D. King, C. Shirley, M. Beard, W. Nie, A. Schleife, J. Colton, and L. Whittaker-Brooks, Uncovering Unique Screening Effects in 2D Perovskites: Implications for Exciton and Band Gap Engineering, ResearchSquare Preprint, 1‑22 (2023). doi: https://doi.org/10.21203/rs.3.rs-2667143/v1.
System description
Dimensionality: 2D n:
Sample type: film

Starting materials: PbO, HI, H3PO2, ethanolamine

Product: spin-coated thin film, high crystallinity and strong exciton absorption

Description: First step: EOA2PbI4 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. 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.

K. Hansen, C. Wong, C. E. McClure, B. Romrell, L. Flannery, D. Powell, K. Garden, A. Berzansky, M. Eggleston, D. King, C. Shirley, M. Beard, W. Nie, A. Schleife, J. Colton, and L. Whittaker-Brooks, Uncovering Unique Screening Effects in 2D Perovskites: Implications for Exciton and Band Gap Engineering, ResearchSquare Preprint, 1‑22 (2023). doi: https://doi.org/10.21203/rs.3.rs-2667143/v1.

Extraction method: Manual from article (Table S1)
Entry added on: June 8, 2023, 8:37 p.m.
Entry added by: Kelly Ma
Last updated on: June 14, 2023, 4:10 p.m.
Last updated by: Kelly Ma

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Data set ID: 2315 Did you find any mistakes or inconsistencies about this data? Send us a note and we'll have a look at it and send you a reply. Thanks!


License

All data is available under the Creative Commons license with attribution clause, described here and, in its full text, here.