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Rapid sampling during synthesis of lead halide perovskite nanocrystals for spectroscopic measurement

Published online by Cambridge University Press:  13 June 2019

James C. Sadighian Open the ORCID record for James C. Sadighian [Opens in a new window] ,
Michael L. Crawford  and
Cathy Y. Wong Open the ORCID record for Cathy Y. Wong [Opens in a new window]
James C. Sadighian
Affiliation:
Department of Chemistry and Biochemistry, University of Oregon, Eugene, Oregon97403, USA
Michael L. Crawford
Affiliation:
Department of Chemistry and Biochemistry, University of Oregon, Eugene, Oregon97403, USA
Cathy Y. Wong*
Affiliation:
Department of Chemistry and Biochemistry, University of Oregon, Eugene, Oregon97403, USA Oregon Center for Optical, Molecular, and Quantum Science, University of Oregon, Eugene, Oregon97403, USA Materials Science Institute, University of Oregon, Eugene, Oregon97403, USA
*
*(Email: cwong3@uoregon.edu)
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Abstract

The photophysical properties of lead halide perovskite nanocrystals (NCs) are critical to their potential application in light emitting devices and other optoelectronics, and are typically characterized using optical spectroscopies. Measurements of nuclei and nascent NC photophysics during synthesis provide insight into how the reaction can be changed to control the properties of the resulting NCs. However, these measurements are typically only performed ex situ after growth is halted by centrifuging the reaction mixture for several minutes. Here, a method is reported to rapidly sample the reaction mixture during a solvation-limited synthesis to enable multiple spectroscopic measurements during nucleation and NC growth. Absorbance and fluorescence measurements of a reaction mixture during the formation of methylammonium lead triiodide perovskite NCs are reported. The changing positions of spectral features as a function of reaction time show the expected weakening of exciton confinement during NC growth. The evolving fluorescence spectra demonstrate that the capping and surface passivation of nascent NCs changes during the reaction. The species in the reaction mixture, particularly during the early stages of the synthesis, are shown to be unstable. This indicates that, even for a relatively slow solvation-limited reaction, the photophysics of the reaction mixture can only be accurately captured if spectroscopic measurements are completed within seconds of sampling. The common use of centrifugation to quench NC syntheses prior to spectroscopic measurement biases the NC population towards more stable, well-capped NCs and does not accurately report on the full NC population in a reaction mixture.

Keywords

perovskitesnanoscalenanostructurein situspectroscopy
Type
Articles
Information
MRS Advances , Volume 4 , Issue 36: Energy and Sustainability , 2019 , pp. 1957 - 1964
Copyright
Copyright © Materials Research Society 2019 

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References

REFERENCES

Schmidt, L. C., Pertegás, A., González-Carrero, S., Malinkiewicz, O., Agouram, S., Mínguez Espallargas, G., Bolink, H. J., Galian, R. E., and Pérez-Prieto, J., "Nontemplate Synthesis of CH3NH3PbBr3 Perovskite Nanoparticles," J. Am. Chem. Soc. 136, 850–853 (2014).CrossRefGoogle ScholarPubMed
Li, G., Rivarola, F. W. R., Davis, N. J. L. K., Bai, S., Jellicoe, T. C., de la Peña, F., Hou, S., Ducati, C., Gao, F., Friend, R. H., Greenham, N. C., and Tan, Z.-K., "Highly Efficient Perovskite Nanocrystal Light-Emitting Diodes Enabled by a Universal Crosslinking Method," Advanced Materials 28, 3528–3534 (2016).CrossRefGoogle ScholarPubMed
Luo, B., Pu, Y.-C., Lindley, S. A., Yang, Y., Lu, L., Li, Y., Li, X., and Zhang, J. Z., "Organolead Halide Perovskite Nanocrystals: Branched Capping Ligands Control Crystal Size and Stability," Angewandte Chemie International Edition 55, 8864–8868 (2016).CrossRefGoogle ScholarPubMed
Boles, M. A., Ling, D., Hyeon, T., and Talapin, D. V., "The surface science of nanocrystals," Nature Materials 15, 141 (2016).CrossRefGoogle ScholarPubMed
Peterson, M. D., Cass, L. C., Harris, R. D., Edme, K., Sung, K., and Weiss, E. A., "The Role of Ligands in Determining the Exciton Relaxation Dynamics in Semiconductor Quantum Dots," Annual Review of Physical Chemistry 65, 317–339 (2014).CrossRefGoogle ScholarPubMed
Qu, L., Yu, W. W., and Peng, X., "In Situ Observation of the Nucleation and Growth of CdSe Nanocrystals," Nano Lett. 4, 465–469 (2004).CrossRefGoogle Scholar
Abécassis, B., Testard, F., Spalla, O., and Barboux, P., "Probing in situ the Nucleation and Growth of Gold Nanoparticles by Small-Angle X-ray Scattering," Nano Lett. 7, 1723–1727 (2007).CrossRefGoogle ScholarPubMed
Yoon, S. J., Draguta, S., Manser, J. S., Sharia, O., Schneider, W. F., Kuno, M., and Kamat, P. V., "Tracking Iodide and Bromide Ion Segregation in Mixed Halide Lead Perovskites during Photoirradiation," ACS Energy Lett. 1, 290–296 (2016).CrossRefGoogle Scholar
Dang, Z., Shamsi, J., Palazon, F., Imran, M., Akkerman, Q. A., Park, S., Bertoni, G., Prato, M., Brescia, R., and Manna, L., "In Situ Transmission Electron Microscopy Study of Electron Beam-Induced Transformations in Colloidal Cesium Lead Halide Perovskite Nanocrystals," ACS Nano 11, 2124–2132 (2017).CrossRefGoogle ScholarPubMed
Yoon, S. J., Kuno, M., and Kamat, P. V., "Shift Happens. How Halide Ion Defects Influence Photoinduced Segregation in Mixed Halide Perovskites," ACS Energy Lett. 2, 1507–1514 (2017).CrossRefGoogle Scholar
Samu, G. F., Janáky, C., and Kamat, P. V., "A Victim of Halide Ion Segregation. How Light Soaking Affects Solar Cell Performance of Mixed Halide Lead Perovskites," ACS Energy Lett. 2, 1860–1861 (2017).CrossRefGoogle Scholar
Murray, C. B., Norris, D. J., and Bawendi, M. G., "Synthesis and characterization of nearly monodisperse CdE (E = sulfur, selenium, tellurium) semiconductor nanocrystallites," Journal of the American Chemical Society 115, 8706–8715 (1993).CrossRefGoogle Scholar
Protesescu, L., Yakunin, S., Bodnarchuk, M. I., Krieg, F., Caputo, R., Hendon, C. H., Yang, R. X., Walsh, A., and Kovalenko, M. V., "Nanocrystals of Cesium Lead Halide Perovskites (CsPbX3, X = Cl, Br, and I): Novel Optoelectronic Materials Showing Bright Emission with Wide Color Gamut," Nano Lett. 15, 3692–3696 (2015).CrossRefGoogle ScholarPubMed
Hassan, Y., Ashton, O. J., Park, J. H., Li, G., Sakai, N., Wenger, B., Haghighirad, A.-A., Noel, N. K., Song, M. H., Lee, B. R., Friend, R. H., and Snaith, H. J., "Facile Synthesis of Stable and Highly Luminescent Methylammonium Lead Halide Nanocrystals for Efficient Light Emitting Devices," J. Am. Chem. Soc. 141, 1269–1279 (2019).CrossRefGoogle ScholarPubMed
Protesescu, L., Yakunin, S., Bodnarchuk, M. I., Krieg, F., Caputo, R., Hendon, C. H., Yang, R. X., Walsh, A., and Kovalenko, M. V., "Nanocrystals of Cesium Lead Halide Perovskites (CsPbX3, X = Cl, Br, and I): Novel Optoelectronic Materials Showing Bright Emission with Wide Color Gamut," Nano Lett. 15, 3692–3696 (2015).CrossRefGoogle ScholarPubMed
Hassan, Y., Song, Y., Pensack, R. D., Abdelrahman, A. I., Kobayashi, Y., Winnik, M. A., and Scholes, G. D., "Structure-Tuned Lead Halide Perovskite Nanocrystals," Advanced Materials 28, 566–573 (2016).CrossRefGoogle ScholarPubMed
Wang, L., Williams, N. E., Malachosky, E. W., Otto, J. P., Hayes, D., Wood, R. E., Guyot-Sionnest, P., and Engel, G. S., "Scalable Ligand-Mediated Transport Synthesis of Organic–Inorganic Hybrid Perovskite Nanocrystals with Resolved Electronic Structure and Ultrafast Dynamics," ACS Nano 11, 2689–2696 (2017).CrossRefGoogle ScholarPubMed
Stamplecoskie, K. G., Manser, J. S., and Kamat, P. V., "Dual nature of the excited state in organic–inorganic lead halide perovskites," Energy Environ. Sci. 8, 208–215 (2014).CrossRefGoogle Scholar
Thanh, N. T. K., Maclean, N., and Mahiddine, S., "Mechanisms of Nucleation and Growth of Nanoparticles in Solution," Chem. Rev. 114, 7610–7630 (2014).CrossRefGoogle ScholarPubMed
Peng, X., Wickham, J., and Alivisatos, A. P., "Kinetics of II-VI and III-V Colloidal Semiconductor Nanocrystal Growth: “Focusing” of Size Distributions," J. Am. Chem. Soc. 120, 5343–5344 (1998).CrossRefGoogle Scholar