Metal halide perovskite nanocrystals offer a range of interesting properties and are being studied extensively for applications in solar cells, photodetectors and light-emitting devices. This perspective provides a number of best practices for the synthesis, purification, and characterization of metal halide perovskite nanocrystals, with detailed discussion of CsPbI3, CsPbBr3, CH3NH3PbI3 (MAPI), and Cs2AgBiBr6 as examples. The choice of reactants and ligands for hot-injection reactions are discussed, as well as how various reaction conditions, including temperature and time, affect yield, uniformity, and crystal phase. We extensively discuss the use of antisolvent precipitation methods for purification, since ligand coordination to most perovskite nanocrystals is weak and the nanocrystals are sensitive to degradation. Finally, we discuss some of the strategies for imaging these nanocrystals using transmission electron microscopy (TEM).
Capping ligand bonding and the thermal and colloidal stability of Cs 2 AgBiBr 6 nanocrystals were studied. Oleylamine and oleic acid bonding to Cs 2 AgBiBr 6 nanocrystals was studied with 1 H nuclear magnetic resonance and nuclear Overhauser effect spectroscopy. Both molecules are present in the ionic metathesis synthesis reaction, but only oleylamine remains bound to the nanocrystals after purification. Oleic acid is not a capping ligand; however, the synthesis requires it, and its concentration determines the yield of the reaction while oleylamine primarily affects the uniformity of the sample. Substitution of oleic acid in the reaction with diisooctylphosphinic acid still yielded nanocrystals with similar size, cuboidal shape, uniformity, cubic double-perovskite crystal structure, and optical properties. Nanocrystals were assembled into superlattices and heated in air. Grazing incidence smallangle and wide-angle X-ray scattering showed that the nanocrystals sinter at 250 °C, but the crystal structure and preferred crystal orientation on the substrate does not change. When nanocrystals were dispersed in hexane and exposed to light, they precipitated within 24 h. Scanning electron microscopy showed that the aggregated nanocrystals still retained their initial size and shape and had not coalesced.
Two-photon excitation in the near-infrared (NIR) of colloidal nanocrystalline silicon quantum dots (nc-SiQDs) with photoluminescence also in the NIR has potential opportunities in the field of deep biological imaging. Spectra of the degenerate two-photon absorption (2PA) cross section of colloidal nc-SiQDs are measured using two-photon excitation over a spectral range 1.46 < ℏω < 1.91 eV (wavelength 850 > λ > 650 nm) above the two-photon band gap E g (QD)/2, and at a representative photon energy ℏω = 0.99 eV (λ = 1250 nm) below this gap. Two-photon excited photoluminescence (2PE-PL) spectra of nc-SiQDs with diameters d = 1.8 ± 0.2 nm and d = 2.3 ± 0.3 nm, each passivated with 1-dodecene and dispersed in toluene, are calibrated in strength against 2PE-PL from a known concentration of Rhodamine B dye in methanol. The 2PA cross section is observed to be smaller for the smaller diameter nanocrystals, and the onset of 2PA is observed to be blue shifted from the two-photon indirect band gap of bulk Si, as expected for quantum confinement of excitons. The efficiencies of nc-SiQDs for bioimaging using 2PE-PL are simulated in various biological tissues and compared to efficiencies of other quantum dots and molecular fluorophores and found to be comparable or superior at greater depths.
Colloidal dodecene-passivated silicon (Si) nanocrystals were dispersed in hexane or chloroform and deposited onto substrates as face-centered cubic superlattices by slowly evaporating the solvent. The uniformity of the nanocrystals enables extended order; however, the solvent and the evaporation protocol significantly influence the self-assembly process, determining the morphology of the films, the extent of order, and the superlattice orientation on the substrate. Chloroform yielded superlattices with step-flow growth morphologies and (111), (100), and (110) orientations. Hexane led to mostly island morphologies when evaporated at room temperature with exclusively (111) orientations. Higher evaporation temperatures led to more extensive step-flow deposition. A model for the surface diffusion of nanocrystals adsorbed on the superlattice surface is developed.
Light-induced changes in photophysical and electronic properties in metal halide perovskites can affect their performance in photovoltaic devices, light-emitting diodes, and other applications. Here we reveal that light induces a slow, reversible enhancement in photoluminescence (PL) lifetime and intensity in films of perovskite-phase CsPbI3 nanocrystals. When films of CsPbI3 nanocrystals stored in air are photoexcited, their PL lifetime and intensity increase by as much as a factor of 5 over the course of 20–30 min. Several hours later, without additional light excitation, the initial PL lifetime and intensity return. Placing the films under vacuum or nitrogen for several minutes was also found to increase the PL lifetime and intensity. We propose a model of slow, humidity- and light-sensitive surface states in perovskite-phase CsPbI3 nanocrystals.
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