Robust, Cationic Lead Halide Layered Materials with Efficient

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Robust, Cationic Lead Halide Layered Materials with Efficient Broadband White-Light Emission Jinlin Yin, Huimin Yang, and Honghan Fei Chem. Mater., Just Accepted Manuscript • DOI: 10.1021/acs.chemmater.8b05345 • Publication Date (Web): 07 May 2019 Downloaded from http://pubs.acs.org on May 7, 2019

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Chemistry of Materials

Robust, Cationic Lead Halide Layered Materials with Efficient Broadband White-Light Emission Jinlin Yin, Huimin Yang, and Honghan Fei* Shanghai Key Laboratory of Chemical Assessment and Sustainability, School of Chemical Science and Engineering, Tongji University, 1239 Siping Rd., Shanghai 200092, P. R. China. ABSTRACT: Only a selected class of corrugated 2D hybrid lead halide perovskites exhibit broadband white-light emission from self-trapped excitons. Recently, we have discovered ultrastable layered lead halide photoemitters overcoming the stability problems of perovskites, despite in need of deep-UV irradiation to achieve photoluminescence quantum efficiency (PLQE) of over 10%. Herein, we have employed a robust, non-conjugated dicarboxylate ligand to pillar the cationic 1D [PbBr]+ chains. The unique corrugated stacking of [PbBr]+ chains facilitates the structural deformation to form self-trapped excitons, thus enabling an 8-fold enhancement of PLQE over our previous reported bilayer bromoplumbate structures. The PLQE of 17.2% is not only among the highest in all of the layered lead halide white-light emitters, but overcoming the problem of our previous photoemitters requiring the deep-UV LED excitation. In addition, by tuning the stacking mode of the pillaring molecules, the chloride analog successfully incorporates a second photoluminescence center to the broadband emission from self-trapped excitons. The two-component emission strategy in [Pb2Cl2][O2C(C6H10)CO2] offers the intrinsic photoemitter to exhibit tunable cold-to-warm white light upon different excitation lights. The materials demonstrate high chemical robustness over a wide pH range (3~9) and undiminished photoluminescence in air upon UV irradiation for 30 days. Density functional theory calculations indicate that the broadband emission of both materials are induced by the structural deformation of [Pb2X2]2+ (X=Cl/Br) inorganic connectivity, which offers self-trapped electrons from Pb–Pb dimerization and self-trapped holes from Cl–Cl pairing in the excited states.

INTRODUCTION Solid-state lighting, comprising light-emitting diodes (LEDs) coated with phosphors, is an emerging class of light sources with high-energy efficiency and longterm stability.1,2 However, the commercial YAG:Ce3+based white LEDs have poor color-rendering indexes (CRIs) and low color stability due to limited coverage of the visible spectrum and the “halo” effect.3-7 Moreover, solid-state lighting systems that emit warm or cold white light must be installed as needed (e.g., warm white-light for domestic lighting and cold white-light for surgery uses).8 Thus, developing a single-phase, broadband white-light phosphor with a high CRI and tunable color temperature is a fundamental objective in the development of SSL technologies.8,9 Hybrid inorganic–organic metal halide perovskites occupying (110)-oriented corrugated layers or distorted (100)-oriented sheets are a rare class of intrinsic broadband white-light emitters, which are distinguished by their formation of self-trapped excitons from strong electron-phonon coupling.10-15 Although these single-source white light emitters are a class of promising phosphors, most of layered perovskites suffer from two drawbacks: low

photoluminescence quantum yields (PLQEs, 50% was observed upon 1 h irradiation at atmospheric condition.18,21 Recently, we have employed flexible α,ωalkanedicarboxylates as structure-directing agents to template a class of cationic lead halide white-light emitters with high chemical/photo-stability.22-24 These long-sought ultrastable lead halide materials exhibit undiminished broadband photoluminescence under continuous UV-irradiation in air. However, only TJU-4 ([Pb2Cl2][O2C(CH2)4CO2]) reached a PLQE of >10% when exposed to middle-UV irradiation (327 nm). Indeed, the emitted power and efficiencies of group III-nitride-based near-UV LED sources (>350 nm) are at least one order of magnitude higher

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compared with deep/middleUV sources.25 Despite the bromide analog is suitable for near-UV excitation due to the suitable bandgap, the thick [Pb2Br2]2+ bilayer motif with low corrugation limit the structural deformation and achieved a low PLQE of only ~2%.22 Moreover, this class of cationic lead halide materials often has low CRI values (i.e., CRI of 68 for TJU-4), which is not acceptable for normal lighting applications.26,27 This Figure 1. Crystallographic view of TJU-10 (a) and TJU-11 (b). Insets show the is largely due to the asymmetric Pb-X coordination environments. Green, blue, yellow, red, and gray deficiency in blue and/or red spheres represents Pb, Cl, Br, O, and C atoms, respectively. H atoms are omitted for emissions, which are located clarity. The insets highlight the coordination between PbII centers and halogen atoms. at both ends of the visible structure. Perchloric acid is necessary for successful spectrum. An ultrastable, single-component whitesynthesis, performing as an acid to tune pH and as a light phosphor with a high CRI (>80) and high stabilizer as for hydrofluoric acid in zeolite synthesis. stability is necessary for the development of eye27,28 Single-crystal X-ray crystallography reveals the friendly lighting applications. Thus, it is structure of TJU-10 comprises slightly corrugated imperative to advance this class of ultrastable lead + layers, which are coordinatively bridged by [PbCl] halide materials toward near-UV-excited broadband the anionic trans-1,4-chdc ligands residing in the photoemitters with high PLQE. interlamellar region (Figure 1a). In each [PbCl]+ plane, Herein, two new members of ultrastable lead halide the adjacent 1D [PbCl]+ zigzag chains that hybrid emitters are identified; then, they are templated propagating along c-axis weakly interact with each using a robust and non-conjugated trans-1,4cyclohexanedicarboxylate (trans-1,4-chdc, other by forming [Pb2Cl2]2+ square units. The −O C(C H )CO −). The robust pillaring ligand templates interchain Pb-Cl atmoic distances are 3.119(3) Å, 2 6 10 2 1D cationic bromoplumbate chains that are stacked with slightly longer than the wideply accepted Pb-Cl bond strong corrugation, achieving enhanced structural lengths (~2.84 Å, CSD) (Figure S2). All 1,4-chdc deformation than the previously reported bilayered ligands are in e,e-trans conformation, and are linked counterpart. The resultant PLQE of 17.2% is among the to the adjacent [PbCl]+ layers in a tilted direction highest in all of the layered lead halide white-light (Figure 1a). Both carboxylate ends of the 1,4-chdc emitters.10,14 In addition, the chloride analog is the first molecules have one oxygen perpendicularly pointing ultrastable photoemitter to incorporate a second towards the conjugated plane of the carboxylate photoluminescence center to the broadband emission group from the adjacent 1,4-chdc molecule (Figure from self-trapped excitons. The resultant S3a). The oxygens are in close proximity towards the [Pb2Cl22+][−O2C(C6H10)CO2−] is capable of producing carbon from the nearest carboxylate with the -OCO… tunable cold-to-warm broadband white-light COO- distance of 3.238(5) Å, contributing to the πphotoluminescence via variations in excitation lights. orbital interactions of the carboxylate groups. The hybrid photemitter exhibits a tunable white-light [Pb2Br22+][−O2C(C6H10)CO2−] (TJU-11) form under color temperature that ranges from 3748 to 11034 K under hydrothermal condition between PbBr2, trans-1,4different excitation wavelengths (e.g., 304–344 nm), and a cyclohexanedicarboxylic acid disodium salt (transCRI as high as 92 upon excitation at 322 nm. 1,4-chdcNa2), and hydrobromic acid (HBr). The addition of HBr provides a second Br source to form lead bromide layers, while also performing as an acid RESULTS AND DISCUSSION to tune the pH. In contrast to the zigzag chains in TJU-10, the 1D [PbBr]+ chains in TJU-11 are nearly The solvothermal reaction of PbCl2, trans-1,4straight with intrachain Pb-Br-Pb bond angles of chdc, and perchloric acid in DMF/EtOH produced o. In addition, the 1D bromoplumbate linear 169.09(4) colorless plate-like crystals of 2+ − − chains are more discrete, occupying the nearest [Pb2Cl2 ][ O2C(C6H10)CO2 ](TJU-10, TJU=Tongji o interchain Pb-Br distances of 3.37~3.50 Å that University) (Figure S1). Slow cooling at a rate of 15 C -1 significantly exceed the accepted Pb-Br bond lengths h is necessary to facilitate the high-yielding (2.97 Å) (Figure S2). The [PbBr]+ chains are weakly synthesis, resulting in a high-purity crystalline stacked into loosely packed and corrugated [PbBr]+


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Table 1. Photophysical properties of TJU-10 and TJU-11 crystals. Materials λex (nm) λem (nm) CCT(K) φ (%) CRI 304 433 11034 20.0 n.d. TJU-10 324 550 n.d. 2.7 91 344 550 3748 2.4 79 TJU-11 354 500 7644 17.2 81 λexis the excitation wavelength; λem is the wavelength at the emission maxima; φ is the external photoluminescence quantum efficiency; CRI is color-rendering index. n.d.=not determined.

gap (3.62 eV) is rather close to the experimentally slabs, which are pillared by trans-1,4-chdc ligands observed value (3.37 eV) (Table 2). (Figure 1b). PbII centers are coordinated with four intralayer Br and three O atoms from trans-1,4-chda Importantly, the excitation spectrum of TJU-10 molecules. Unlike TJU-10, the trans-1,4-chda ligands demonstrates two maximum at 304 and 344 nm, are well aligned in the same direction, leading to no owing to the presence of two photoluminescence close interaction between oxygens and carbons from components (Figure S6). Upon excitation at 344 nm, the adjacent ligand moieties (Figure S3c). TJU-10 exhibits a broadband photoluminescence with Both TJU-10 and TJU-11 are synthesized with high a maximum at 550 nm with the presence of the lowyields (>75 %) and phase purity, which is evidenced intensity blue emission (400–450 nm) (Figure 2 and via experimental powder X-ray diffraction (PXRD) S7). Interestingly, lowering the excitation wavelength patterns. These patterns match the simulated results in an obvious enhancement in the blue patterns from single-crystal data (Figure S3). photoluminescence centered at 433 nm and a Thermogravimetric analysis and ex-situ concomitant reduction in the intensity of the thermodiffraction indicate that TJU-10 and TJU-11 are yellowish broadband photoluminescence (maximum thermally stable up to 260 oC and 330 oC, respectively, at 550 nm) (Figure 2c). Upon excitation at 324 nm, in air (Figure S3-S4). Moreover, both TJU-10 and the hybrid emitter displays nearly identical maximum TJU-11 demonstrate high robustness over a wide pH range (3~9), which also applies to organic solvents that were examined by incubation of the solids into a diluted HCl or NaOH solution or organic solvents for 24 h. No significant loss of diffraction peaks was observed in the PXRD, and a 4.00 Å. By contrast, no significant change was observed in the stacking mode of the interlamellar trans-1,4-chdc ligands, excluding their contribution to the broadband emission at 550 nm (Figure S13). The calculated excitation and emission energies (at the PBE level) are 3.92 and 2.38 eV, respectively (Table 2). These values correspond well with the experimental optical transition energies (3.60 eV for excitation energy and 2.25 eV for emission energy). These results suggest that the lattice deformation in TJU-10 introduces self-trapped electrons from Pb–Pb dimerization and self-trapped holes from Cl–Cl pairing with short-range bonding distances between the nearest neighboring ions.32,39 After confirming the origin of the broadband emissive component centered at 550 nm for TJU-10, the contribution of high-energy blue emission is further investigated. The emission spectrum of trans1,4-chdNa2 is measured at room temperature (Figure S14), which well match with the high-energy emissive



profile of TJU-10. This is owing to the π-orbital interactions of the adjacent carboxylates, which are quite parellel and close to each other in VBM of TJU10 (Figure S15).40 The interaction mode that having one oxygen perpendicularly pointing towards the conjugated plane of the other carboxylate has also been observed in trans-1,4-chdK2 (Figure S16), which has nearly identical emissive behavior with TJU-10 upon 304 nm excitation (Figure S14). Moreover, the lifetimes of TJU-10 excited upon 304 nm and 344 nm are 215 μs and 3.6 ns, respectively (Figure 3e and S17). The long lifetime (215 μs) is attributed to the transition of the intraligand π* → n from the free trans-1,4-chdNa2 ligand, while the decay lifetime of 3.6 ns is consistent with our initial assumptions regarding self-trapped excitons.41-43 Overall, it is clear that the extremely high CRI of TJU-10 upon excitation at 324 nm is achieved by a combination of two independent emission bands [Pb2Cl2]2+ and trans1,4-chdc, respectively. In contrast to that of TJU-10, the excitation spectrum of TJU-11 exhibits a prominent peak at 354 nm from [PbBr]+ layers with a rather weak and broad ligand-based contribution at 304 nm (Figure S6). Adjusting the excitation light from 304 to 354 nm, TJU-11 shows a single, broadband emissive component with negligible blue emission from the free trans-1,4-chda ligands (Figure S18). This phenomenon confirms that the emission from the free trans-1,4-chda ligand strongly depends on the stacking mode in the interlamellar region. Almost no ligand-based emission in TJU-11 is attributed to the lack of π-orbital interactions from the carboxylate groups in trans-1,4-chdc molecules (Figure S15). Upon 354 nm excitation, TJU-11 displays a cold broadband white-light emission with a maximum at 500 nm, a FWHM of 178 nm (0.86 eV), and a high external PLQE of 17.2 % (Figure 4a, Table 1). The PLQE is significantly higher than most of the previously reported layered lead halide materials (up to 9-11 %). More importantly, the near-UV excitation for TJU-11 is a substantial advance over TJU-4 (PLQE of 11.8%) requiring a middle-UV light (327 nm) excitation, due to the much higher efficiencies of group III-nitride-based near-UV LED sources.22 Importantly, post-thermal or chemical treatment TJU-11 exhibits the identical broadband emission, demonstrating its “inert” nature as the ultrastable photoemitter (Figure S10).44 The broadband emission from TJU-11 has a significantly higher PLQE (17.2%) than TJU-10 (2.4~2.7%), which is probably due to two structural features. Firstly, in contrast to the adjacent zigzag [PbCl]+ chains in TJU-10 having interactions to form [Pb2Cl2]2+ square units, the 1D haloplumbate chains in TJU-11 are more straight and separated. Indeed, the low-dimensional haloplumbate connectivity will enhance the electron-phonon coupling and lower the

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potential barrier of self-trapped excited states.33 Thus, the more discrete [PbBr]+ chains will facilitate the exciton self-trapping and enhance the efficiency of broadband emission. Secondly, each 2D [PbBr]+ layer in TJU-11 have two flat haloplumbate sheets consisting of every other [PbBr]+ chains (Figure S2d). Each given [PbBr]+ chain is located out-of-plane between two adjacent chains, forming the highly corrugated layers, which are similar to the (110)oriented layered perovskites. Indeed, the highly corrugated lead halide layer with acute Pb-(μ-Br)-Pb angles allow for greater lattice distortion in the excited state (Figure 4d and 4e). Overall, the rather discrete [PbBr]+ chains as well as the corrugated lead bromide layers contribute to the high PLQE of broadband emission from TJU-11. Owing to the high PLQE of TJU-11, the mechanism of its broadband emission was examined using DFT calculations. The total DOS demonstrate a calculated band gap of 3.11 eV, which is close to the measured band gap (3.22 eV) using absorption spectroscopy (Figure 4f and S5). The VBM and CBM of TJU-11 are primarily attributed to the full Br-4p orbitals and empty Pb-6p orbitals, respectively. In addition, the dicarboyxlate ligands partially contribute to the VBM, which is most likely caused by the oxygen atoms of the carboxylates gaining electrons from Pb-O bonding. In contrast to TJU-10 having separated ligand-based bandgap and [PbX]+-based bandgap (based on absorption spectra, Figure 2a and S5), these two very mixed gaps in TJU-11 indicate a higher degree of covalency in Pb-carboxylate bonding. To note, the broadband emission energy of TJU-11 is slightly higher than that of TJU-10, despite the VBM (Br-4p) for TJU-11 occupying higher energy than the VBM (Cl-3p) for TJU-10. This is likely due to that the broadband emission from TJU-11 is primarily contributed by low-energy self-trapped electrons (Pb23+), while the self-trapped holes (X2- and/or Pb3+) play a more important role in the emisson from TJU10. Each [Pb2Br2]2+ monolayer in the ground state TJU-11 exhibits obvious corrugation from the regular 2D squaregrid-type architecture, and demonstrates a higher tendency to induce structural distortion than the inorganic slabs in TJU-10 as well as our previously reported TJU-5 (Figure S2c).22 Accordingly, DFT calculations indicate larger structural deformation in the excited state of TJU-11. Both Br–Br pairing (3.38 Å) and Pb–Pb dimerization (3.20~3.21 Å) are observed in the calculated excited state (Figure 4e). The atomic distances of TJU-11 in its excited state are not only significantly lower than the ground state (Pb–Pb of >4.47 Å and Br–Br of > 4.34 Å) (Figure 4d and 4e), but smaller than the dimerized units of TJU-10 in its excited state as well. The shorter Pb–Pb distance in excited state TJU-11 also agrees with our earlier speculation that the broadband emission is largely contributed by self-trapped electrons (Pb23+). In


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addition, based on the PLQEs and lifetimes (Figure 3e and 4c), the radiative decay rates was calculated to be approximately 0.67 ×107 S-1 for TJU-10 and 0.15 ×107 S-1 for TJU-11, while the nonradiative decay rates of approximately 27.3×107 S-1 for TJU-10 and 0.72×107 S-1 for TJU-11, respectively. The lower nonradiative decay rates of TJU-11 along with atomic distances values from DFT calculations indicate that the excited state TJU-11 is more likely to form self-trapped excitons such as Pb23+ and Br2–.18,40 More importantly, no obvious movement of the interlamellar dicarboxylate ligands were observed from ground state to excited state, confirming the origin of the broadband emissions is exclusively associated with the structural deformation of [Pb2Br2]2+ layers (Figure S20).

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CONCLUSIONS Two new members of ultrastable lead halide structures have been templated using photoactive rigid organic ligand, which exhibit intrinsic broadband white-light emission. Among them, the two-component emission strategy in TJU-10 enables an ultrahigh CRI of up to 92, which is among the highest in intrinsic white-light emitters. TJU-11 achieves the first ultrastable near-UV-excited broadband white-light emitter with a moderately high PLQE of 17.2%, owing to its unique cationic bromoplumbate chains stacked with high corrugation. DFT calculations indicate the broadband emissions originate from the Pb–Pb dimerization and Cl–Cl pairing in [Pb2X2]2+ (X=Cl/Br) layers. We believe that crystal engineering of these intrinsic, ultrastable lead halide photoemitters offers promising possibilities in the development of high-performance singlecomponent white-light phosphors.

ASSOCIATED CONTENT Supporting Information. Experimental details and addition characterization as well as crystallographic data. The Supporting Information is free of charge on the ACS Publication website

AUTHOR INFORMATION

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Corresponding Author *E-mail: [email protected]

ACKNOWLEDGMENT This work was supported by grants from the National Natural Science Foundation of China (51772217), the Recruitment of Global Youth Experts by China, the Fundemental Research Funds for the Central Universities, and Science & Technology Commission of Shanghai Municipality (14DZ2261100).

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Robust, Cationic Lead Halide Layered Materials with Efficient

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