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May 15, 2018 September 9, 2026

Single Crystal Growth of Hybrid Lead Bromide Perovskites Using a Spin-Coating Method - Notes

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ACS Omega · Journal article · 15 May 2018

R. García-Aboal, R. Fenollosa, F. Ramiro-Manzano, I. Rodríguez, F. Meseguer and P. Atienzar

ACS Omega

Volume 3

Pages 5229-5236

2018

Published abstract

Synthesis and studies of single crystals of hybrid perovskite are important for achieving a better understanding of the optoelectronic phenomena occurring in this material and for improving ongoing applications. Here, we report on the growth of micrometer-size single crystals of methylammonium lead bromide (MAPbBr3) using the spin coating deposition method on a quartz substrate. We studied the influence of the rotation speed and the use of three different additives N-cyclohexyl-2-pyrrolidone, dimethyl sulfoxide, and 4-tert-butylpyridine on the crystal size and shape. The introduction of an additive in the precursor solution is revealed to be very useful for obtaining crystals with well-defined geometries and for decreasing the amount of defects. In this way, high-quality single crystals that sustain optical resonating modes were obtained and characterized by transmittance and photoluminescence measurements.

Figures

Figure 1 from the ACS Omega article
Figure 1. Summary. Average crystal size (dots) as a function of the spin coater rotation speed for a precursor solution without additive (A) and with (B) CHP, (C) DMSO, and (D) TBP as additive. The error bars correspond to the standard deviation.

From R. García-Aboal et al., ACS Omega 3, 5229-5236 (2018), DOI 10.1021/acsomega.8b00447. © 2018 American Chemical Society. Reproduced for non-commercial research communication under the ACS AuthorChoice usage agreement.

Figure 2 from the ACS Omega article
Figure 2. Summary. Scanning electron microscopy (SEM) images of MAPbBr3 crystals grown on quartz substrates by spin coating at 1000 rpm, corresponding to samples NA (a), CHP (b), DMSO (c), and TBP (d).

From R. García-Aboal et al., ACS Omega 3, 5229-5236 (2018), DOI 10.1021/acsomega.8b00447. © 2018 American Chemical Society. Reproduced for non-commercial research communication under the ACS AuthorChoice usage agreement.

Figure 3 from the ACS Omega article
Figure 3. Summary. XRD pattern of a layer of crystals of (a) NA, (b) CHP, (c) DMSO, and (d) TBP samples.

From R. García-Aboal et al., ACS Omega 3, 5229-5236 (2018), DOI 10.1021/acsomega.8b00447. © 2018 American Chemical Society. Reproduced for non-commercial research communication under the ACS AuthorChoice usage agreement.

Figure 4 from the ACS Omega article
Figure 4. Summary. (a)-(d) Optical microscopy images at 40× magnification of samples NA, CHP, DMSO, and TBP, respectively, for a rotation speed of 1000 rpm. (e)-(h) The corresponding photoluminescence images.

From R. García-Aboal et al., ACS Omega 3, 5229-5236 (2018), DOI 10.1021/acsomega.8b00447. © 2018 American Chemical Society. Reproduced for non-commercial research communication under the ACS AuthorChoice usage agreement.

Figure 5 from the ACS Omega article
Figure 5. Summary. (A) UV-vis absorption spectra and (B) photoluminescence spectra of the sample areas of Figure 4, corresponding to samples NA, CHP, DMSO, and TBP.

From R. García-Aboal et al., ACS Omega 3, 5229-5236 (2018), DOI 10.1021/acsomega.8b00447. © 2018 American Chemical Society. Reproduced for non-commercial research communication under the ACS AuthorChoice usage agreement.

Figure 6 from the ACS Omega article
Figure 6. Summary. Optical microscopy images of crystals synthesized by increasing concentrations of CHP additive: (a) 5, (b) 15, (c) 25, (d) 50, and (e) 60% v/v in DMF. The scale bars correspond to 200 µm.

From R. García-Aboal et al., ACS Omega 3, 5229-5236 (2018), DOI 10.1021/acsomega.8b00447. © 2018 American Chemical Society. Reproduced for non-commercial research communication under the ACS AuthorChoice usage agreement.

Figure 7 from the ACS Omega article
Figure 7. Summary. (A) Average crystal size versus spin coater rotation speed obtained using 5% CHP additive in DMF. The shaded areas indicate rod- and cuboid-like growth regimes.

From R. García-Aboal et al., ACS Omega 3, 5229-5236 (2018), DOI 10.1021/acsomega.8b00447. © 2018 American Chemical Society. Reproduced for non-commercial research communication under the ACS AuthorChoice usage agreement.

Figure 8 from the ACS Omega article
Figure 8. Summary. Photoluminescence (black curve) and transmittance (red curve) spectra of (a) a plate-shaped crystal and (c) a pyramid-shaped crystal. (b, d) The corresponding optical microscopy images.

From R. García-Aboal et al., ACS Omega 3, 5229-5236 (2018), DOI 10.1021/acsomega.8b00447. © 2018 American Chemical Society. Reproduced for non-commercial research communication under the ACS AuthorChoice usage agreement.

Figure 9. Optical setup for transmittance and photoluminescence
Figure 9. Summary. Diagram showing the setup used for measuring the optical transmittance and photoluminescence spectra, where the acronyms are lens (L), beam splitter (BS), spectrometer, and camera (CAM).

From R. García-Aboal et al., ACS Omega 3, 5229-5236 (2018), DOI 10.1021/acsomega.8b00447. © 2018 American Chemical Society. Reproduced for non-commercial research communication under the ACS AuthorChoice usage agreement.

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Article access and reuse

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Related publications

Connections within F. Ramiro-Manzano's publication record, selected from shared research topics and evidence reviewed in the source papers.

Figure 1. Schematic representation of the electric contact on the microcrystalline samples, showing the irradiation objective at the bottom part controlled with a piezoelectric stage.
Journal article
Nanomaterials 13, 2570 (2023)
Scanning Photocurrent Microscopy in Single Crystal Multidimensional Hybrid Lead Bromide Perovskites
E. Segura-Sanchis, R. García-Aboal, R. Fenollosa, F. Ramiro-Manzano and P. Atienzar

What the related paper adds

This later paper extends the research direction developed in Single Crystal Growth of Hybrid Lead Bromide Perovskites Using a Spin-Coating Method. This study moves from optical resonances to spatially resolved charge transport in individual lead-bromide perovskite crystals. Scanning photocurrent microscopy separates the two transport regimes found in three-dimensional crystals from the single dominant regime in multidimensional 2D-3D crystals and exposes crystal edges as important recombination regions.

What this paper adds to the related work

This paper provides an earlier basis for the later development reported in Scanning Photocurrent Microscopy in Single Crystal Multidimensional Hybrid Lead Bromide Perovskites. This study develops a fast spin-coating route to micrometre-sized MAPbBr3 single crystals and shows how rotation speed and coordinating additives control shape, orientation and defect density. The improved planar crystals are not only cleaner model specimens but also support optical resonances, providing the material platform used by later optical studies.

Figure 4: MAPbBr3 crystal optical properties
Article
Dalton Trans. 49(36), 12798-12804 (2020)
Optical Properties of Organic/Inorganic Perovskite Microcrystals through the Characterization of Fabry-Pérot Resonances
F. Ramiro-Manzano, R. García-Aboal, R. Fenollosa, S. Biasi, I. Rodriguez, P. Atienzar and F. Meseguer

What the related paper adds

This later paper extends the research direction developed in Single Crystal Growth of Hybrid Lead Bromide Perovskites Using a Spin-Coating Method. This work uses the Fabry-Perot fringes of individual MAPbBr3 microcrystals as a source of quantitative information. A simultaneous fit of transmittance and photoluminescence retrieves crystal thickness and the real and imaginary parts of the refractive index near the band edge, while defining when a planar microcrystal behaves as an optical cavity.

What this paper adds to the related work

This paper provides an earlier basis for the later development reported in Optical Properties of Organic/Inorganic Perovskite Microcrystals through the Characterization of Fabry-Pérot Resonances. This study develops a fast spin-coating route to micrometre-sized MAPbBr3 single crystals and shows how rotation speed and coordinating additives control shape, orientation and defect density. The improved planar crystals are not only cleaner model specimens but also support optical resonances, providing the material platform used by later optical studies.

Figure 3: CsPbBr3 nanowire characterization
Journal article
Materials Chemistry Frontiers 3(9), 1754-1760 (2019)
Groove-Assisted Solution Growth of Lead Bromide Perovskite Aligned Nanowires: A Simple Method towards Photoluminescent Materials with Guiding Light Properties
I. Rodriguez, R. Fenollosa, F. Ramiro-Manzano, R. García-Aboal, P. Atienzar and F. J. Meseguer

What the related paper adds

This later paper extends the research direction developed in Single Crystal Growth of Hybrid Lead Bromide Perovskites Using a Spin-Coating Method. This paper converts low-cost CD and DVD surface profiles into moulds for aligned CsPbBr3 and MAPbBr3 nanowires. The process controls wire width and alignment at room temperature, allows transfer to other substrates, and demonstrates bright photoluminescence together with guided light propagation over distances longer than twelve micrometres.

What this paper adds to the related work

This paper provides an earlier basis for the later development reported in Groove-Assisted Solution Growth of Lead Bromide Perovskite Aligned Nanowires: A Simple Method towards Photoluminescent Materials with Guiding Light Properties. This study develops a fast spin-coating route to micrometre-sized MAPbBr3 single crystals and shows how rotation speed and coordinating additives control shape, orientation and defect density. The improved planar crystals are not only cleaner model specimens but also support optical resonances, providing the material platform used by later optical studies.

Research fields

Bottom-up

MAPbBr₃ single microcrystals are grown directly on quartz by spin coating. Rotation speed and three solvent additives are varied systematically, showing how evaporation and precursor coordination control crystal size, coverage and morphology in a simple deposition process.

Characterization

Statistical optical microscopy is combined with SEM, X-ray diffraction, absorption and photoluminescence. The measurements connect each processing condition with crystal dimensions, phase purity and emission, rather than judging growth from surface appearance alone.

RESEARCH TOPICS

MaterialsSEM and optical microscopy in Figures 2 and 4 show how additive and rotation speed change the population from small grains to rods, cuboids and plates. This morphology control is important because fewer grain boundaries can reduce charge trapping and recombination.SetupsFigures 6 and 7 turn the microscopy observations into quantitative trends by tracking average crystal size and the rod-to-cuboid ratio against additive concentration. Optical characterization then selects individual crystals with a microscope, switches the collected signal between a CCD camera and an iHR320 spectrometer with a liquid-nitrogen-cooled silicon detector, and records photoluminescence and transmission from the same object rather than from an ensemble.ChemistryThree coordinating additives (N-cyclohexyl-2-pyrrolidone (CHP), DMSO and tert-butylpyridine) are compared because they alter nucleation and crystal growth during solvent evaporation. CHP provides particularly broad morphological control as its concentration is increased.
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