Grain rotation and lattice deformation during perovskite spray coating and annealing probed <i>in situ</i> by GI-WAXS

Lilliu, Samuele; Griffin, Jon; Barrows, Alexander T.; Alsari, Mejd; Curzadd, B.; Dane, Thomas G.; Bikondoa, Oier; MacDonald, John Emyr; Lidzey, David G.

doi:10.1039/c6ce00965d

Cited by 31 publications

(61 citation statements)

References 24 publications

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“…These peaks arise due to larger crystalline grains present with various orientations and reveal further information on the present process: Upon annealing, a shift of individual diffraction peaks in radial direction toward higher q values is observed that correspond to individually decreased lattice distances, as seen in Figure S4, Supporting Information. This finding can be attributed to lattice strain during the perovskite conversion from the precursor …”

Section: Resultsmentioning

confidence: 98%

Evolution of Perovskite Crystallization in Printed Mesoscopic Perovskite Solar Cells

et al. 2019

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Additives are frequently used to enhance material properties. The addition of the processing additive 5‐aminovaleric acid iodide (5‐AVAI) into printed mesoscopic perovskite solar cells is shown to have a strong impact on the device performance and stability. Although it is difficult to understand the impact of 5‐AVAI as a processing additive by examining only the final thin films, the evolution of morphology with and without 5‐AVAI reveals that 5‐AVAI influences the crystallization behavior of the perovskite. In situ grazing incidence wide angle X‐ray scattering (GIWAXS) is performed to follow the perovskite formation within the printable all‐porous TiO2/ZrO2/carbon architecture and investigate the influence of 5‐AVAI on the perovskite crystallization within the scaffold. Using such time‐resolved measurements, the suppression of large crystalline perovskite grains is identified early in the fabrication process when 5‐AVAI is present, resulting in improved material backfilling. These observations highlight the importance of 5‐AVAI in the precursor solution for reliable fabrication of printed perovskite solar cells relying on the infiltration of a scaffold structure.

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Section: Resultsmentioning

confidence: 98%

Evolution of Perovskite Crystallization in Printed Mesoscopic Perovskite Solar Cells

et al. 2019

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“…They reason that this is caused by nucleation sites at the grain boundaries, which leads to crystal growth at the expense of surrounding grains, leading to strain which causes rotation and lattice deformation. [50] By contemplating ex-situ SEM data they found further proof of grain fragmentation observed in earlier GISAXS studies. [13] Finally, many fabrication methods employ dimethylsulfoxide and other complex forming additives and solvents.…”

Section: Research Newsmentioning

confidence: 89%

“…As both fields are evolving, the future will most probably see even more sophisticated in-situ GIXS measurements looking into perovskite crystallization and degradation processes, along with the development of more complex analysis tools for treatment of large amounts of data as shown by recent studies. [30,32,50] Other possible applications of GIXS include the investigation of more industry-relevant film fabrication methods like roll-to-roll printing. [65] On the other hand, GIXS offers many experimental possibilities that can be exploited in static or quasi-static measurements, and thus are able to give more in-depth knowledge, e.g., by incident angle scans for depth-profiling of samples or making use of focused X-ray beams for mapping of sample homogeneity over larger scales.…”

Section: Resultsmentioning

confidence: 99%

“…[13,14] The mechanistic reorganization of the film morphology likely originates from the volume expansion by a factor of 1.7 during perovskite conversion. [14] However, a recent study by Lilliu et al suggests that this process is more complex than previously thought: [50] By placing tracks on individual reflexes on 2D GIWAXS data recorded in situ during a 1-step spray-deposition employing a MAI:PbCl 2 precursor, the authors monitored grain rotation and lattice deformation. Furthermore, with the help of self-organizing maps (SOM) in Matlab, the authors classified the structural evolution into four clusters.…”

Section: Research Newsmentioning

confidence: 99%

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Structure of Organometal Halide Perovskite Films as Determined with Grazing‐Incidence X‐Ray Scattering Methods

Schlipf

Müller‐Buschbaum

2017

Advanced Energy Materials

135

115

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Grazing‐incidence X‐ray scattering (GIXS) methods have proven to be a valuable asset for investigating the morphology of thin films at different length scales. Consequently, GIXS has been applied to the fast‐progressing field of organometal halide perovskites. This exciting class of materials has propelled research in the areas of cheap and sustainable photovoltaics, light emitting devices, and optoelectronics in general. Especially, perovskite solar cells (PSC) have seen a remarkable rise in power conversion efficiencies, crossing the 20% mark after only five years of research. This research news outlines GIXS studies focusing on the most challenging research topics in the perovskite field today: Current–voltage hysteresis, device reproducibility, and long‐term stability of PSC are inherently linked to perovskite film morphology. On the other hand, film formation depends on the choice of precursors and processing parameters; understanding their interdependence opens possibilities to tailor film morphologies. Owing to their tunability and moisture resistance, 2D perovskites have recently attracted attention. Examples of GIXS studies with different measurement and data analysis techniques are presented, highlighting especially in‐situ investigations on the many kinetic processes involved. Thus, an overview on the toolbox of GIXS techniques is linked to the specific needs of research into organometal halide perovskite optoelectronics.

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“…A nylon/metal-printed sample chamber filled with Helium was used to reduce background due to air scattering [33]. The X-ray energy was 10 keV and the beam size 100 µm × 260 µm (vert.…”

Section: Methodsmentioning

confidence: 99%

Structural stability of naphthyl end-capped oligothiophenes in organic field-effect transistors measured by grazing-incidence X-ray diffraction in operando

Huss-Hansen

Lauritzen

Bikondoa

et al. 2017

Organic Electronics

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. (2017) Structural stability of naphthyl end-capped oligothiophenes in organic field-effect transistors measured by grazingincidence X-ray diffraction in operando. Organic Electronics. Permanent WRAP URL:http://wrap.warwick.ac.uk/89989 Copyright and reuse:The Warwick Research Archive Portal (WRAP) makes this work by researchers of the University of Warwick available open access under the following conditions. Copyright © and all moral rights to the version of the paper presented here belong to the individual author(s) and/or other copyright owners. To the extent reasonable and practicable the material made available in WRAP has been checked for eligibility before being made available.Copies of full items can be used for personal research or study, educational, or not-for-profit purposes without prior permission or charge. Provided that the authors, title and full bibliographic details are credited, a hyperlink and/or URL is given for the original metadata page and the content is not changed in any way. A note on versions:The version presented here may differ from the published version or, version of record, if you wish to cite this item you are advised to consult the publisher's version. Please see the 'permanent WRAP URL' above for details on accessing the published version and note that access may require a subscription. AbstractWe report on microstructural durability of 5,5'-bis(naphth-2-yl)-2,2'-bithiophene (NaT2) in organic field effect transistors (OFETs) in operando monitored by grazing-incidence X-ray diffraction (GIXRD). NaT2 maintains its monoclinic bulk motif in operating OFETs with a = 20.31 ± 0.06Å, b = 6.00 ± 0.01Å, c = 8.17 ± 0.04Å and β = (96.64 ± 0.74)• . Crystallites appear as a mosaic of single crystals reaching through the whole 50 nm thick active layer. The lattice parameters variation (<1%) falls within the statistical error of structure refinement when the OFET gate voltage is varied from 0 V to -40 V; or when the OFET is continuously cycled within this voltage interval over more than 10 h period. Within the first few cycles, both the hole mobility and threshold voltage are changing but then reach stable levels with an average mobility of (3.25 ± 0.04) × 10 −4 cm 2 /Vs and an average threshold voltage of −13.6 ± 0.2 V, both varying less than 4% for the remainder of the 10 h period. This demonstrates crystalline stability of NaT2 in operating OFETs.

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Grain rotation and lattice deformation during perovskite spray coating and annealing probed in situ by GI-WAXS

Abstract: Synchrotron grazing incidence WAXS is used to track CH3NH3PbI3 precursor and perovskite crystallites rotation in situ during solution-deposition and thermal annealing.

Cited by 31 publications

References 24 publications

Evolution of Perovskite Crystallization in Printed Mesoscopic Perovskite Solar Cells

Evolution of Perovskite Crystallization in Printed Mesoscopic Perovskite Solar Cells

Structure of Organometal Halide Perovskite Films as Determined with Grazing‐Incidence X‐Ray Scattering Methods

Structural stability of naphthyl end-capped oligothiophenes in organic field-effect transistors measured by grazing-incidence X-ray diffraction in operando

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