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Title: Radiative Thermal Annealing/in Situ X-ray Diffraction Study of Methylammonium Lead Triiodide: Effect of Antisolvent, Humidity, Annealing Temperature Profile, and Film Substrates

Authors:
ORCiD logo [1];  [2]; ORCiD logo [2];  [3]
  1. National Renewable Energy Laboratory, Golden, Colorado 80401, United States; Department of Electrical, Computer, and Energy Engineering, University of Colorado Boulder, Boulder, Colorado 80309, United States
  2. Stanford Synchrotron Radiation Lightsource, SLAC National Accelerator Laboratory, Menlo Park, California 94025, United States
  3. National Renewable Energy Laboratory, Golden, Colorado 80401, United States
Publication Date:
Research Org.:
SLAC National Accelerator Lab., Menlo Park, CA (United States); National Renewable Energy Lab. (NREL), Golden, CO (United States)
Sponsoring Org.:
USDOE Office of Energy Efficiency and Renewable Energy (EERE), Solar Energy Technologies Office (EE-4S); USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22)
OSTI Identifier:
1393379
Alternate Identifier(s):
OSTI ID: 1390308
Report Number(s):
NREL/JA-5K00-68900
Journal ID: ISSN 0897-4756
Grant/Contract Number:
AC02-76SF00515; AC36-08G028308; EE0005951; AC36-08GO28308
Resource Type:
Journal Article: Accepted Manuscript
Journal Name:
Chemistry of Materials
Additional Journal Information:
Journal Volume: 29; Journal Issue: 14; Journal ID: ISSN 0897-4756
Publisher:
American Chemical Society (ACS)
Country of Publication:
United States
Language:
English
Subject:
14 SOLAR ENERGY; 36 MATERIALS SCIENCE; 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; XRD; perovskites; solar

Citation Formats

Dou, Benjia, Pool, Vanessa L., Toney, Michael F., and van Hest, Maikel F. A. M. Radiative Thermal Annealing/in Situ X-ray Diffraction Study of Methylammonium Lead Triiodide: Effect of Antisolvent, Humidity, Annealing Temperature Profile, and Film Substrates. United States: N. p., 2017. Web. doi:10.1021/acs.chemmater.7b01467.
Dou, Benjia, Pool, Vanessa L., Toney, Michael F., & van Hest, Maikel F. A. M. Radiative Thermal Annealing/in Situ X-ray Diffraction Study of Methylammonium Lead Triiodide: Effect of Antisolvent, Humidity, Annealing Temperature Profile, and Film Substrates. United States. doi:10.1021/acs.chemmater.7b01467.
Dou, Benjia, Pool, Vanessa L., Toney, Michael F., and van Hest, Maikel F. A. M. Thu . "Radiative Thermal Annealing/in Situ X-ray Diffraction Study of Methylammonium Lead Triiodide: Effect of Antisolvent, Humidity, Annealing Temperature Profile, and Film Substrates". United States. doi:10.1021/acs.chemmater.7b01467.
@article{osti_1393379,
title = {Radiative Thermal Annealing/in Situ X-ray Diffraction Study of Methylammonium Lead Triiodide: Effect of Antisolvent, Humidity, Annealing Temperature Profile, and Film Substrates},
author = {Dou, Benjia and Pool, Vanessa L. and Toney, Michael F. and van Hest, Maikel F. A. M.},
abstractNote = {},
doi = {10.1021/acs.chemmater.7b01467},
journal = {Chemistry of Materials},
number = 14,
volume = 29,
place = {United States},
year = {Thu Jul 06 00:00:00 EDT 2017},
month = {Thu Jul 06 00:00:00 EDT 2017}
}

Journal Article:
Free Publicly Available Full Text
This content will become publicly available on June 19, 2018
Publisher's Version of Record

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Cited by: 1work
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  • Perovskite-based solar cells are one of the emerging candidates for radically lower cost photovoltaics. Herein, we report on the synthesis and crystallization of organic-inorganic formamidinium lead triiodide perovskite films under controlled atmospheric and environmental conditions. Using in situ (scanning) transmission electron microscopy, we make observations of the crystallization process of these materials in nitrogen and oxygen gas with and without the presence of water vapor. Complementary planar samples were also fabricated in the presence of water vapor and characterized by in situ X-ray diffraction. Direct observations of the material structure and final morphology indicate that the exposure to water vapormore » results in a porous film that is metastable, regardless of the presence of argon, nitrogen, or oxygen. However, the optimal crystallization temperature of 175 degrees C is unperturbed across conditions. Rapid modulation about the annealing temperature of 175 degrees C in +/-25 degrees C steps (150-200 degrees C) promotes crystallization and significantly improves the film morphology by overcoming the presence of impregnated water trapped in the material. Following this processing protocol, we demonstrate substantial growth to micron-size grains via observation inside of an environmentally controlled transmission electron microscope. Adapting this insight from our in situ microscopy, we are able to provide an informed materials protocol to control the structure and morphology of these organic-inorganic semiconductors, which is readily applicable to benchtop device growth strategies.« less
  • Perovskite-based solar cells are one of the emerging candidates for radically lower cost photovoltaics. Herein, we report on the synthesis and crystallization of organic-inorganic formamidinium lead triiodide perovskite films under controlled atmospheric and environmental conditions. Using in situ (scanning) transmission electron microscopy, we make observations of the crystallization process of these materials in nitrogen and oxygen gas with and without the presence of water vapor. Complementary planar samples were also fabricated in the presence of water vapor and characterized by in situ X-ray diffraction. Direct observations of the material structure and final morphology indicate that the exposure to water vapormore » results in a porous film that is metastable, regardless of the presence of argon, nitrogen, or oxygen. However, the optimal crystallization temperature of 175 °C is unperturbed across conditions. Rapid modulation about the annealing temperature of 175 °C in ±25 °C steps (150-200 °C) promotes crystallization and significantly improves the film morphology by overcoming the presence of impregnated water trapped in the material. Following this processing protocol, we demonstrate substantial growth to micron-size grains via observation inside of an environmentally controlled transmission electron microscope. Adapting this insight from our in situ microscopy, we are able to provide an informed materials protocol to control the structure and morphology of these organic-inorganic semiconductors, which is readily applicable to benchtop device growth strategies.« less
  • We study the thermal stability of wurtzite (w) structure ZrAlN coatings by a combination of in situ high-energy x-ray scattering techniques during annealing and electron microscopy. Wurtzite structure Zr{sub 1−x}Al{sub x}N coatings with Al-contents from x = 0.46 to x = 0.71 were grown by cathodic arc evaporation. The stability of the w-ZrAlN phase depends on chemical composition where the higher Al-content coatings are more stable. The wurtzite ZrAlN phase was found to phase separate through spinodal decomposition, resulting in nanoscale compositional modulations, i.e., alternating Al-rich ZrAlN layers and Zr-rich ZrAlN layers, forming within the hexagonal lattice. The period of the compositional modulations variesmore » between 1.7 and 2.5 nm and depends on the chemical composition of the coating where smaller periods form in the more unstable, high Zr-content coatings. In addition, Zr leaves the w-ZrAlN lattice to form cubic ZrN precipitates in the column boundaries.« less
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