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Ultrathin Lead Bromide Perovskite Platelets Spotted with Europium(II) Bromide Nanodots

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Ultrathin Lead Bromide Perovskite Platelets Spotted with Europium(II) Bromide Nanodots Ultrathin lead bromide perovskite platelets spotted with europium(II) bromide nanodots Ignacio Rosa-Pardo,a Salvador Pocoví,a Raul Arenal,b,c,d Raquel E. Galian,*a and Julia Pérez- Prieto*a We describe here the preparation of a novel nanohybrid comprising a two-layer cesium lead bromide nanoplatelet, [CsPbBr3]PbBr4 NPL, containing europium(II) bromide (EuBr2) nanodots, by ultrasound/heating treatment of toluene dispersions of CsPbBr3 nanomaterial in the presence of EuBr2 nanodots. The hybrid nanoplatelet exhibits the strong excitonic and narrow emission peaks characteristic of ultrathin NPLs at 430 and 436 nm, respectively, and remains mainly non-stacked after prolonged standing in solution. Lead halide perovskites are relevant semiconductor materials with the APbX3 formula, where A is a small-sized monocation (such as methylammonium, formamidinium, or cesium), and X is a halide (Cl-, Br- and/or I-). These materials present a three- dimensional (3D) inorganic framework consisting of corner- sharing PbX6 octahedra and the small-sized cations in the voids between them. They can easily be prepared with 3D morphology (bulk material) by simply mixing AX and PbX2, and also with other morphologies1: nanoparticles (0D material) and low-dimensional materials (such as nanowires and nanoplatelets, 1D and 2D materials, respectively). Recently the preparation of colloidal nanoparticles has been reported with photoluminescence quantum yields (ΦPL) of up to 100%, by using coordinating ligands which confine the material to the nanoscale and provide dispersibility; such nanoparticles are suitable for preparing thick films with a ΦPL close to that of the colloid.2-10 Their exceptional electronic and optical properties make them of great interest in light-emitting devices, photodetectors and photovoltaics.9, 11, 12 Figure 1: Transformation of CsPbBr3 nanoparticle nanowires (NPNWs) into Currently, there is an increasing interest focused on perovskites ultrathin nanoplatelets (NPLs) under ultrasound/heating treatment in the presence of a EuBr2 solid. Top: conventional TEM image of the NPNWs (scale with 2D morphology, in particular, nanoplatelets (NPLs) with a bar 50 nm), absorption and emission spectra of the NPNWs; inset: TEM image few lead halide layers and the L2[APbX3]n-1PbX4 formula, where at scale bar of 2 µm. Bottom: conventional TEM image of the NPLs (scale bar “L” represents the ligand and “n” stands for the number of 200 nm), absorption and emission spectra of the NPLs. layers.13, 14 As long as the NPL thickness is homogeneous, they In particular, we report here that ultrasound/heating treatment exhibit the same emission peak, independently of their lateral of a toluene colloid of CsPbBr nanoparticles capped with dimensions, as well as exceptionally narrow absorption and 3 dodecylamine (DDA) in the presence of europium(II) bromide emission (full width at half maximum (FWHM) ca. 10 nm) and nanodots (EuBr NDs) lead to the formation of blue, highly small Stokes shift (<10 meV). They have been prepared as 2 stable two-layer [CsPbBr ]PbBr NPLs spotted with EuBr colloids following different strategies: i) exfoliation of the bulk 3 4 2 nanodots. material by sonication in the presence of coordinating First, CsPbBr nanoparticles were prepared by the re- solvents15; ii) hot-injection crystallization13; and iii) non-solvent 3 precipitation technique with some modifications.17, 18 Briefly, crystallization16. we prepared a solution containing an equimolar concentration We devised that the ultrasound treatment of a mixture of two of cesium bromide (CsBr) and lead bromide (PbBr ) in a 9:1 different materials could be used not only for the exfoliation of 2 dimethylformamide/dimethylsulfoxide mixture. Then, 200 µL of one of the materials, which might lead to a novel nanohybrid, this solution were mixed with DDA (0.053 mmol) to obtain the but also for avoiding the stacking of the exfoliated material. precursor solution, which was added dropwise to a toluene solution of myristic acid (MA, 0.709 mmol); therefore, the DDA:MA molar ratio used in this preparation was 7:94 (see experimental section for further details). Finally, the dispersion nm and 510 nm; the first can be ascribed to the formation of was centrifuged at 5500 rpm for 5 min and the precipitate was two-layer caesium lead bromide nanoplatelets . Similar results redispersed in 2 mL of toluene for further use and the were obtained when the treatment was performed for 7 h supernatant was discarded. This combination of ligands led to without sampling. Table S1 resumes the PL quantum yield of the the formation of micrometer-sized wires with a width of ca. 100 reaction along the time. nm, together with square-shaped nanoparticles of ca. 7 nm The subsequent experiments were performed using 7 h of deposited at the edges of the wires; see Figure 1(top). heating/ultrasonic treatment. Then, the synthesis was carried This material presented an exciton peak at 500 nm, an emission out using different amounts of: i) EuBr2 (0.6 mg, 1.6 mg), ii) maximum at 510 nm with a FWHM of 20 nm (Figure 1(top)), a CsPbBr3 colloid volume (125 µ L, 250 µL, 500 µL), and iii) total ΦPL of 31% and an average PL lifetime (τav) of 34.4 ns (the PL volume of the mixture (500 µL). The best results, in terms of decay fitted to 3 exponential decays, see details in the dispersibility and emissive properties, were obtained using 0.6 experimental section); for further characterization data see mg of EuBr2, 125 µL of CsPbBr3 NPNWs and 500 µL of the total thermogravimetry analysis (TGA), proton nuclear magnetic volume. Figure 1(bottom) shows the absorption and emission resonance (H-NMR), transmission electron microscopy (TEM), spectra that correspond to the colloid obtained after X-ray photoelectron spectroscopy (XPS), and X-ray powder ultrasound/heating treatment of the CsPbBr3 NPNWs in the diffraction (PXRD) (Figure S1-S4). presence of EuBr2 for 7 h. The PL (λex= 365 nm) spectrum of the In the TGA spectrum, the weight loss of 76% in the 100-200 0C optimal sample exhibited an emission at 436 nm and 510 nm range, assigned to the DDA ligand, was followed by a small loss with a total ΦPL of 41 %. The PL decays fitted to three 0 (4%) ascribed to MA, and then a loss of 20% in the 500-600 C components and the PL τav was 16 ns and 8 ns for the emissions range attributed to the inorganic components (PbBr2 and CsBr) at 436 nm and 510 nm, respectively. Table S2 contains the (Figure S1). The 1H-NMR spectrum corroborated that DDA was luminescence lifetime of the colloid obtained after practically the only capping ligand on the CsPbBr3 NPNW´s ultrasound/heating treatment of CsPbBr3 NPNWs in the surface (Figure S2). presence EuBr2 for 7 h, recorded at λex 510 nm and 436 nm. The The XPS analysis of Pb 4f showed two symmetrical peaks at 138 and 143 eV attributed to Pb 4f7/2 and Pb 4f5/2, respectively (Figure S3). The presence of two additional symmetrical bands at a lower energy, specifically at 137.7 and 142 eV, cannot be attributed to metallic lead or lead oxide19 and therefore, they could be indicative of perovskite Pb in a different environment. The peaks at 68.8 and 67.7 eV were assigned to the Br 3d present in the perovskite and are similar to those observed by other authors.20 The N 1s spectrum showed two peaks at 401.5 and 399.8 eV that corresponded to DDA as ammonium and amine, respectively.21 The O1s spectra showed three peaks at 533.7, 532.4 and 531.3 eV attributed to the equivalent O atoms of the carboxylate, non-equivalent O of carboxylic acid, and to the O-O bond. The C 1s spectra exhibited an intense peak at 284.6 eV assigned to the C-C aliphatic chain, which was used as a reference. Two small contributions at 288.3 and 286.7 eV were ascribed to the carbonyl group and C-O bond of the MA and the peak at 285.4 eV corresponded to the C-N signal.22 Finally, the typical peaks at 737 and 723 eV were attributed to the Cs 3d.9 The powder XRD spectrum showed the presence of peaks at 0 0 0 0 15.08 (002), 15.22 (110), 21.50 (112), 30.38 (004), 30.71 0 (220) and 34.37 (222); which are characteristic of the 23, 24 orthorhombic phase of CsPbBr3 (Figure S4). Secondly, the first attempt to prepare a hybrid material consisted of mixing a small amount of the freshly prepared CsPbBr3 colloid (0.5 mL) with the EuBr2 salt (1.2 mg) in a vial and submitting the mixture to ultrasound/heating treatment. Small Figure 2: HAADF-HRSTEM images and EDS spectra recorded on different µ aliquots (50 L) were extracted after 1, 3, 5 and 7h and their nanostructures present in the samples. (a) HAADF-STEM micrographs of: UV-visible and PL spectra were systematically recorded (Figure (i) a cesium lead bromide platelet, (ii) two EuBr2 nanodots, (iii) an EuBr2 S5). The absorption spectrum of the material after 7 h of nanoparticle, (iv) a perovskite NP, (v) an amorphous agglomerate treatment showed the appearance of a peak at 430 nm together containing europium and (vi) PbBr2 NP, respectively. (b) EDS spectra recorded rastering the electron beam on the highlighted red areas of with that of the excitonic peak of the CsPbBr3 perovskite at 500 each of the previous images. nm (Figure SX). The PL spectrum showed two main peaks at 436 luminescence kinetics decays are shown in Figure S6. temperature during the ultrasound treatment is required. In Furthermore, the relative intensity between the emission peaks addition, in the absence of EuBr2, the CsPbBr3 NPNWs did not change when exciting at 280 nm, where EuBr2 does not transformed into micro-sized perovskite particles after 7 h of absorb, thus ruling out the contribution of EuBr2 to the emission ultrasound/heating treatment.
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