scholarly journals Out-of-equilibrium processes in crystallization of organic-inorganic perovskites during spin coating

2021 ◽  
Vol 12 (1) ◽  
Author(s):  
Shambhavi Pratap ◽  
Finn Babbe ◽  
Nicola S. Barchi ◽  
Zhenghao Yuan ◽  
Tina Luong ◽  
...  
Keyword(s):  
Spin Coating ◽  
Grazing Incidence ◽  
Lead Iodide ◽  
In Situ Data ◽  
X Ray Scattering ◽  
Equilibrium Processes ◽  
Complex Phenomena ◽  
Methylammonium Lead Iodide ◽  
Solvent Complex

AbstractComplex phenomena are prevalent during the formation of materials, which affect their processing-structure-function relationships. Thin films of methylammonium lead iodide (CH3NH3PbI3, MAPI) are processed by spin coating, antisolvent drop, and annealing of colloidal precursors. The structure and properties of transient and stable phases formed during the process are reported, and the mechanistic insights of the underlying transitions are revealed by combining in situ data from grazing-incidence wide-angle X-ray scattering and photoluminescence spectroscopy. Here, we report the detailed insights on the embryonic stages of organic-inorganic perovskite formation. The physicochemical evolution during the conversion proceeds in four steps: i) An instant nucleation of polydisperse MAPI nanocrystals on antisolvent drop, ii) the instantaneous partial conversion of metastable nanocrystals into orthorhombic solvent-complex by cluster coalescence, iii) the thermal decomposition (dissolution) of the stable solvent-complex into plumboiodide fragments upon evaporation of solvent from the complex and iv) the formation (recrystallization) of cubic MAPI crystals in thin film.

scholarly journals Temperature-Dependent Crystallization Mechanisms of Methylammonium Lead Iodide Perovskite From Different Solvents

2021 ◽  
Vol 9 ◽  
Author(s):  
Oleksandra Shargaieva ◽  
Hampus Näsström ◽  
Jinzhao Li ◽  
Daniel M. Többens ◽  
Eva L. Unger
Keyword(s):  
Perovskite Phase ◽  
Grazing Incidence ◽  
Lead Iodide ◽  
Solution Processed ◽  
X Ray Scattering ◽  
Intermediate Phases ◽  
Different Temperatures ◽  
Solvent Molecules ◽  
Methylammonium Lead Iodide ◽  
Precursor Molecules

Hybrid perovskites are a novel type of semiconductors that show great potential for solution-processed optoelectronic devices. For all applications, the device performance is determined by the quality of the solution-processed perovskite thin films. During solution processing, the interaction of solvent with precursor molecules often leads to the formation of solvate intermediate phases that may diverge the crystallization pathway from simple solvent evaporation to a multi-step formation process. We here investigate the crystallization of methylammonium lead iodide (MAPbI3) from a range of commonly utilized solvents, namely dimethyl sulfoxide (DMSO), N,N-dimethylformamide (DMF), N-methylpyrrolidone (NMP), and gamma-butyrolactone (GBL) at different temperatures ranging from 40°C to >100°C by in-situ grazing-incidence wide-angle X-ray scattering (GIWAXS) measurements. For all solvents but GBL, we clearly observe the formation of solvate-intermediate phases at moderate processing temperatures. With increasing temperatures, an increasing fraction of the MAPbI3 perovskite phase is observed to form directly. From the temperature-dependence of the phase-formation and phase-decomposition rates, the activation energy to form the MAPbI3 perovskite phase from the solvate-phases are determined as a quantitative metric for the binding strength of the solvent within the solvate-intermediate phases and we observe a trend of DMSO > DMF > NMP > GBL. These results enable prediction of processing temperatures at which solvent molecules can be effectively removed.

scholarly journals Micellar‐Mediated Block Copolymer Ordering Dynamics Revealed by In Situ Grazing Incidence Small‐Angle X‐Ray Scattering during Spin Coating

2019 ◽  
Vol 29 (10) ◽  
pp. 1806741 ◽  
Author(s):  
Guillaume Fleury ◽  
Daniel Hermida‐Merino ◽  
Dong Jingjin ◽  
Karim Aissou ◽  
Aleksei Bytchkov ◽  
...  
Keyword(s):  
Block Copolymer ◽  
Small Angle ◽  
Spin Coating ◽  
Grazing Incidence ◽  
X Ray ◽  
X Ray Scattering ◽  
Ray Scattering

scholarly journals In situ investigation of degradation at organometal halide perovskite surfaces by X-ray photoelectron spectroscopy at realistic water vapour pressure

2017 ◽  
Vol 53 (37) ◽  
pp. 5231-5234 ◽  
Author(s):  
Jack Chun-Ren Ke ◽  
Alex S. Walton ◽  
David J. Lewis ◽  
Aleksander Tedstone ◽  
Paul O'Brien ◽  
...  
Keyword(s):  
Water Vapour ◽  
Photoelectron Spectroscopy ◽  
Ambient Pressure ◽  
Water Vapour Pressure ◽  
Lead Iodide ◽  
X Ray ◽  
In Situ Investigation ◽  
Organometal Halide Perovskite ◽  
Methylammonium Lead Iodide

Near-ambient-pressure X-ray photoelectron spectroscopy enables the study of the reaction of in situ-prepared methylammonium lead iodide (MAPI) perovskite at realistic water vapour pressures for the first time.

scholarly journals In Situ Investigation of the Early-Stage Growth of Nanoporous Alumina

2018 ◽  
Vol 2018 ◽  
pp. 1-9
Author(s):  
Thérèse Gorisse ◽  
Ludovic Dupré ◽  
Marc Zelsmann ◽  
Alina Vlad ◽  
Alessandro Coati ◽  
...  
Keyword(s):  
Early Stage ◽  
Grazing Incidence ◽  
Alumina Layer ◽  
Nanoporous Alumina ◽  
X Ray ◽  
X Ray Scattering ◽  
In Situ Investigation ◽  
Low X ◽  
X Ray Absorption

We report the successful use of in situ grazing incidence small-angle X-ray scattering to follow the anodization of aluminum. A dedicated electrochemical cell was designed and developed for this purpose with low X-ray absorption, with the possibility to access all azimuthal angles (360°) and to remotely control the temperature of the electrolyte. Three well-known fabrication techniques of nanoporous alumina, i.e., single, double, and pretextured, were investigated. The differences in the evolution of the scattering images are described and explained. From these measurements, we could determine at which moment the pores start growing even for very short anodization times. Furthermore, we could follow the thickness of the alumina layer as a function of the anodization time by monitoring the period of the Kiessig fringes. This work is aimed at helping to understand the different steps taking place during the anodization of aluminum at the very early stages of nanoporous alumina formation.

Atomic scale characterization of organometallic vapor phase epitaxial growth using in-situ grazing incidence X-ray scattering

1992 ◽  
Vol 124 (1-4) ◽  
pp. 1-9 ◽  
Author(s):  
D.W. Kisker ◽  
G.B. Stephenson ◽  
P.H. Fuoss ◽  
F.J. Lamelas ◽  
S. Brennan ◽  
...  
Keyword(s):  
Epitaxial Growth ◽  
Vapor Phase ◽  
Grazing Incidence ◽  
Atomic Scale ◽  
X Ray ◽  
X Ray Scattering ◽  
Scale Characterization ◽  
Ray Scattering
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