Controlling Solvate Intermediate Growth for Phase-Pure Organic Lead Iodide Ruddlesden–Popper (C4H9NH3)2(CH3NH3)n-1PbnI3n+1 Perovskite Thin Films
Abstract
The growth of Ruddlesden-Popper perovskite thin films is complicated by the existence of multiple crystallization pathways available to precursors in solution. During conventional thin film growth processes, such as spin-coating or blade-coating, solvents can evaporate too quickly to clearly resolve different reaction intermediates and products that form during crystallization. Here, we resolve multiple reaction products and intermediates that form during Ruddlesden-Popper phase growth by studying drop-cast precursor solutions in situ through the evolution of X-ray diffraction, photoluminescence, and optical micrographs over long timescales in a thin film geometry. We found that methylammonium-rich solvate intermediates play a crucial role in directing the bulk optical properties of the films, and form simultaneously with smaller regions of Ruddlesden-Popper phases during growth. The microstructure and optical properties of these sub-phases were characterized during growth and after annealing, revealing that discrepancies between thin film and single-crystal optical properties originate from solvate intermediates. These lower band-gap solvate-mediated minority phases dominate the optical emission spectrum by means of rapid energy migration, and contribute to sub-band-gap electronic states in photovoltaic devices. Processing routes to yield thin films with optical properties similar to single crystals of Ruddlesden-Popper phases were developed by tuning the precursor stoichiometry and deposition kinetics.
- Authors:
-
[1];
[1];
[1];
[1];
[1]
- Univ. of California, Santa Barbara, CA (United States)
- Westmont College, Santa Barbara, CA (United States)
- Publication Date:
- Research Org.:
- Energy Frontier Research Centers (EFRC) (United States). Quantum Materials for Energy Efficient Neuromorphic Computing (Q-MEEN-C); Univ. of California, Santa Barbara, CA (United States)
- Sponsoring Org.:
- USDOE Office of Science (SC), Basic Energy Sciences (BES)
- OSTI Identifier:
- 1594806
- Grant/Contract Number:
- SC0012541; SC0019273; AC02-76SF00515; AC0205CH11231
- Resource Type:
- Accepted Manuscript
- Journal Name:
- Chemistry of Materials
- Additional Journal Information:
- Journal Volume: 31; Journal Issue: 15; Journal ID: ISSN 0897-4756
- Publisher:
- American Chemical Society (ACS)
- Country of Publication:
- United States
- Language:
- English
- Subject:
- 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; Thin films; Crystallization; Precursors; Solvates; Deposition
Citation Formats
Dahlman, Clayton J., DeCrescent, Ryan A., Venkatesan, Naveen R., Kennard, Rhys M., Wu, Guang, Everest, Michael A., Schuller, Jon A., and Chabinyc, Michael L. Controlling Solvate Intermediate Growth for Phase-Pure Organic Lead Iodide Ruddlesden–Popper (C4H9NH3)2(CH3NH3)n-1PbnI3n+1 Perovskite Thin Films. United States: N. p., 2019.
Web. doi:10.1021/acs.chemmater.9b01952.
Dahlman, Clayton J., DeCrescent, Ryan A., Venkatesan, Naveen R., Kennard, Rhys M., Wu, Guang, Everest, Michael A., Schuller, Jon A., & Chabinyc, Michael L. Controlling Solvate Intermediate Growth for Phase-Pure Organic Lead Iodide Ruddlesden–Popper (C4H9NH3)2(CH3NH3)n-1PbnI3n+1 Perovskite Thin Films. United States. https://doi.org/10.1021/acs.chemmater.9b01952
Dahlman, Clayton J., DeCrescent, Ryan A., Venkatesan, Naveen R., Kennard, Rhys M., Wu, Guang, Everest, Michael A., Schuller, Jon A., and Chabinyc, Michael L. Tue .
"Controlling Solvate Intermediate Growth for Phase-Pure Organic Lead Iodide Ruddlesden–Popper (C4H9NH3)2(CH3NH3)n-1PbnI3n+1 Perovskite Thin Films". United States. https://doi.org/10.1021/acs.chemmater.9b01952. https://www.osti.gov/servlets/purl/1594806.
@article{osti_1594806,
title = {Controlling Solvate Intermediate Growth for Phase-Pure Organic Lead Iodide Ruddlesden–Popper (C4H9NH3)2(CH3NH3)n-1PbnI3n+1 Perovskite Thin Films},
author = {Dahlman, Clayton J. and DeCrescent, Ryan A. and Venkatesan, Naveen R. and Kennard, Rhys M. and Wu, Guang and Everest, Michael A. and Schuller, Jon A. and Chabinyc, Michael L.},
abstractNote = {The growth of Ruddlesden-Popper perovskite thin films is complicated by the existence of multiple crystallization pathways available to precursors in solution. During conventional thin film growth processes, such as spin-coating or blade-coating, solvents can evaporate too quickly to clearly resolve different reaction intermediates and products that form during crystallization. Here, we resolve multiple reaction products and intermediates that form during Ruddlesden-Popper phase growth by studying drop-cast precursor solutions in situ through the evolution of X-ray diffraction, photoluminescence, and optical micrographs over long timescales in a thin film geometry. We found that methylammonium-rich solvate intermediates play a crucial role in directing the bulk optical properties of the films, and form simultaneously with smaller regions of Ruddlesden-Popper phases during growth. The microstructure and optical properties of these sub-phases were characterized during growth and after annealing, revealing that discrepancies between thin film and single-crystal optical properties originate from solvate intermediates. These lower band-gap solvate-mediated minority phases dominate the optical emission spectrum by means of rapid energy migration, and contribute to sub-band-gap electronic states in photovoltaic devices. Processing routes to yield thin films with optical properties similar to single crystals of Ruddlesden-Popper phases were developed by tuning the precursor stoichiometry and deposition kinetics.},
doi = {10.1021/acs.chemmater.9b01952},
journal = {Chemistry of Materials},
number = 15,
volume = 31,
place = {United States},
year = {2019},
month = {7}
}
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Figure 1.: a) Crystal structures of Ruddlesden-Popper phases of (C4H9NH3)2(CH3NH3)n-1PbnI3n+1 for n = 1 – 4 shown along the (101) plane. b) Optical microscopy of the growth of crystals in ambient from drop-cast RP precursor solutions in DMF for
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