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Cite This: Inorg. Chem. XXXX, XXX, XXX−XXX
High Pressure Structural and Optical Properties of Two-Dimensional Hybrid Halide Perovskite (CH3NH3)3Bi2Br9 Qian Li,†,‡ Lixiao Yin,§ Zhongwei Chen,† Kerong Deng,† Shuiping Luo,† Bo Zou,*,¶ Zhongwu Wang,+ Jiang Tang,§ and Zewei Quan*,† †
Department of Chemistry, Southern University of Science and Technology (SUSTech), Shenzhen, Guangdong 518055, P. R. China SUSTech Academy for Advanced Interdisciplinary Studies, Southern University of Science and Technology, Shenzhen, Guangdong 518055, P. R. China § Wuhan National Laboratory for Optoelectronics (WNLO) and School of Optical and Electronic Information, Huazhong University of Science and Technology (HUST), Wuhan 430074, P. R. China ¶ State Key Laboratory of Superhard Materials, College of Physics, Jilin University, Changchun 130012, P. R. China + Cornell High Energy Synchrotron Source, Cornell University, Ithaca, New York 14853, United States
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‡
S Supporting Information *
ABSTRACT: Two-dimensional (2D) hybrid halide perovskite is emerging as the next generation of photoelectronic materials. Herein, a typical 2D halide perovskite of MA3Bi2Br9 (MA = CH3NH3) is chosen for high pressure research to explore the distinct structural and property characteristics of the inorganic and organic compositions therein. Upon compression above 4.3 GPa, the distortion and tilting of inorganic BiBr6 octahedra dominate the phase transition of MA3Bi2Br9 from trigonal to monoclinic. Meanwhile, exceptionally anisotropic compressibilities are observed between intra- and interlayer structures, which originate from the unique geometry of puckered layer. In addition, the presence of organic MA+ cations contributes to the flexible structural nature of MA3Bi2Br9. Meanwhile, the geometrical changes of inorganic components determine the relationships between structure and band gap under pressure. This work not only demonstrates the intriguing structure nature of MA3Bi2Br9 but also reveals the individual contributions on the structure−property diagram from inorganic (BiBr6 octahedra) and organic (MA cations) components.
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electronic structure of materials.6−8 High pressure studies on halide perovskites over the last three years have been intensively pursued, providing novel and valuable insights into their structures and optical/electronic properties.9−13 However, high pressure explorations are mostly focused on 3D hybrid halide perovskites, but little is known about high pressure structural and property responses of 2D hybrid halide perovskites.14−18 In particular, it still remains an open question how the two components (inorganic metal halide and organic cations) of 2D hybrid halide perovskites individually contribute to the pressure-induced structural transformations and property variations. In this work, 2D hybrid halide perovskite of MA3Bi2Br9 (MA = CH3NH3) is chosen for high pressure investigations. As one promising photovoltaic and optoelectronic material,19,20 MA3Bi2Br9 adopts a relatively simple but typical 2D perovskite structure. At ambient conditions, MA3Bi2Br9 crystallizes in a trigonal P3̅m1 symmetry with lattice parameters of a = b = 8.22(7) Å, c = 10.02(2) Å.21 The metallic halide layer contains
INTRODUCTION Two-dimensional (2D) hybrid halide perovskites are emerging as the promising candidates for next-generation photovoltaic and optoelectronic materials.1,2 The structural uniqueness of 2D hybrid halide perovskites make them excellent bulk quantum materials, in which the charge carriers are confined within inorganic sheets, exhibiting interesting photophysical phenomena at quantum levels.3 Meanwhile, the organic cations in 2D hybrid halide perovskites can also be applied to tune the durability and moisture tolerance of the system, which is crucial to increase the lifetime of perovskite-based device.4 For 2D hybrid halide perovskites, the inorganic and organic compositions adopt different structural and functional characteristics and are of great importance for their practical applications.5 An in-depth understanding of the individual structural nature of inorganic and organic components and their contributions to 2D hybrid halide perovskite property is highly desired and indispensable toward their future technological development and device fabrication. Physically compressing materials decreases interatomic distance continuously and dramatically, and thus, pressure has been often adopted to engineer the crystalline and © XXXX American Chemical Society
Received: November 14, 2018
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DOI: 10.1021/acs.inorgchem.8b03190 Inorg. Chem. XXXX, XXX, XXX−XXX
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Figure 1. (a) Representative ADXRD patterns of MA3Bi2Br9 from ambient conditions to the peak pressure of 10.1 GPa. The asterisks represent the newly emerged diffraction peaks at high pressure. (b and c) Rietveld refinement of the ADXRD pattern at 1 atm and corresponding crystal structure of ambient (trigonal) phase MA3Bi2Br9. (d and e) Rietveld refinement of the ADXRD pattern at 5.0 GPa and corresponding crystal structure of high pressure (monoclinic) phase MA3Bi2Br9. The dark yellow lines in (b) and (d) denote the differences between the observed and the simulated (red) profiles, and the purple verticals stand for the simulated peak positions. The different colors of the BiBr6 octahedral edge in (c) and (e) illustrate their different octahedra layers.
with space group of P21/a. Figures 1c and 1e reveal that the pressure-induced structural variations are dominated by the distortion of metal halide layers. Note that the MA+ can only be displayed as yellow spheres with average atomic positions of the cations, owing to their disordered and complex molecular conformations. As seen, over the course of this pressureinduced phase transition, the BiBr6 octahedra still adopt a corner-sharing way in six-membered ring, but an apparent tilting is noticeably observed between BiBr6 octahedra as shown by a decrease of the Bi−Br−Bi angle (Figure S1). In addition, the discontinuity of the Bi−Br bond length appears, indicative of a distortion of the BiBr6 octahedra (Figure S2). Both distortion and tilting jointly lead to the appearance of the two types of BiBr6 octahedra (Bi1 and Bi2, Figures 1e and S1) in this monoclinic structure. The observed discontinuities of axial parameters and cell volume (Figures S3 and S4) suggest the first-order nature of this trigonal-to-monoclinic phase transition.26 Upon continuous compression to 10.1 GPa, no additional and noticeable discontinuity is observed, indicating the structural stabilization of monoclinic MA3Bi2Br9 in this range. Compared with trigonal MA3Bi2Br9, the smaller average contraction rate of lattice axes (Figure S3) and the larger bulk modulus (Figure S4) of monoclinic MA3Bi2Br9 are indicative of its more rigid structural nature at high pressure. In addition, the obviously broadened and weakened diffraction peaks above 5.0 GPa illustrate the disorder and amorphization trends of monoclinic MA3Bi2Br9.27 To obtain the local structure information on both inorganic and organic components of MA3Bi2Br9, high pressure Raman experiments were conducted to 10.4 GPa. Upon increase of pressure to 4.1 GPa, all the Raman modes exhibit a blue-shift (Figures S5 and S6), owing to the continuous structural contraction of trigonal MA3Bi2Br9. As illustrated in Figure 2a, the two Raman peaks from 125 to 225 cm−1 are assigned to the Bi−Br stretching modes of MA3Bi2Br9 at 0.1 GPa.22,28 The
two sublayers, and the two corner-shared BiBr6 octahedra are linearly connected with Bi−Br−Bi bond angles of 180°, forming the intralayer six-membered rings. Meanwhile, the intralayer MA+ cations are filled into the central voids of the rings, i.e. one MA+ cation is surrounded by six BiBr6 octahedra. Between the layers, another MA+ cation is located between the adjacent BiBr6 octahedra to separate the metal halide sheets. The organic cations in MA3Bi2Br9 are disordered and possess almost a spherical symmetry dynamically.22
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EXPERIMENTAL SECTION
The crystals of MA3Bi2Br9 used in this work were synthesized according to a previous report.20 High pressure was generated using a diamond anvil cell (DAC), and a ruby fluorescence method was used to monitor the pressure value.23 Silicon oil served as a pressure transmitting medium (PTM) to maintain hydrostatic environment around the samples under pressure.24 The angle-dispersive synchrotron X-ray diffraction (ADXRD) measurements were performed at the B1 station of the Cornell High Energy Synchrotron Source (CHESS) using an monochromatic X-ray beam (λ = 0.4859 Å). ADXRD data analysis was performed using both Fit2D and Materials Studio software.25 High pressure Raman experiments were conducted using a customized system in which a 532 nm laser was used as an illumination source. Details of experiments are provided in the Supporting Information.
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RESULTS AND DISCUSSION Figure 1a presents the high pressure structural behavior of 2D hybrid halide perovskite MA3Bi2Br9. Upon increase of pressure to 3.5 GPa, the trigonal MA3Bi2Br9 exhibits a constant contraction, as evidenced by the continuous shift of the diffraction peaks to higher angles. Between 4.3 and 5.0 GPa, a new set of diffraction peaks gradually emerges, demonstrating the occurrence of a pressure-induced phase transition of MA3Bi2Br9. Rietveld refinement of diffraction pattern at 5.0 GPa offers the most possible high pressure structure of MA3Bi2Br9 (Figure 1d), which adopts a monoclinic structure B
DOI: 10.1021/acs.inorgchem.8b03190 Inorg. Chem. XXXX, XXX, XXX−XXX
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where l is the axial length of materials under pressure. This parameter is widely used to evaluate the pressure sensitivity and contraction ability of the structure along the specific direction.29 With increasing pressure, compressibilities of a axis are equal to that of b axis. As shown in Figure 3a, the axial
Figure 2. (a) Representative Raman spectra of lattice and Bi−Br stretching modes with increasing pressure to 10.4 GPa. (b and c) Evolutions of typical Raman modes from MA+ cations (CH3 bending, NH3 bending, and CH3 stretching) as a function of pressure to 7.7 GPa. The peak marked by the asterisks belongs to the signal of silicon oil PTM.
Figure 3. (a) High pressure compressibilities of lattice axes in trigonal MA3Bi2Br9. (b and c) Compressibility indicatrix in the ab plane of MA3Bi2Br9 and the corresponding crystal structure viewed in the same direction.
compressibilities gradually decrease, originating from the more compact structure at high pressure. As usual, the interlayer structure with relatively weak interactions should be more easily compressed, showing a larger compressibility.30 In contrast, MA3Bi2Br9 exhibits an unexpected interlayer contraction behavior. The compressibility of interlayer direction of c axis (Kc) is smaller than that of intralayer direction of b axis (Kb). This phenomenon is coincident with the smaller average contraction rate of c axis in trigonal MA3Bi2Br9 (Figure S3). From the structural viewpoint, such an exceptionally anisotropic phenomenon arises from the unique puckered layers of MA3Bi2Br9. In MA3Bi2Br9, one metal halide layer contains the two sublayers of BiBr6 octahedra. Within each sublayer, the BiBr6 octahedra are loosely arranged, improving the flexibility of the puckered structure (Figure S7). However, for the interlayer structures, the MA+ cations with short molecular length are not able to efficiently separate the metal halide layers. Meanwhile, interlayer space between one pair of BiBr6 octahedra is filled with MA+ cations, which are connected with BiBr6 octahedra through strong hydrogen bonds (Figure S7). Therefore, compared with the intralayer structure of puckered layers with numerous voids, the interlayer structure of MA3Bi2Br9 is more rigid, exhibiting a smaller Kc at high pressure. Furthermore, no obvious anisotropism is observed within the intralayer structure, evidenced by the rounded compressibility indicatrix in ab plane (Figures 3b and 3c). To confirm the contribution of MA+ cations on structure, another 2D bismuth halide perovskite of Cs3Bi2Br9, which possesses analogous structure with MA3Bi2Br9, was chosen for
Raman peaks marked by an arrow at 4.1 GPa are ascribed to the lattice modes, which gradually shift into the detection region. Between 4.4 and 5.4 GPa, the newly emergent Raman vibrations (Figures 2a, 2b, and S5) coincidently support the proposed phase transition from trigonal to monoclinic phase with a lower symmetry in MA3Bi2Br9. During the transition, the two Bi−Br stretching modes developed into three modes, implying a pressure-induced distortion of BiBr6 octahedra. Meanwhile, no obvious discontinuity is observed in the MA+ related Raman vibrations, including CH3 bending, NH3 bending, and CH3 stretching modes (Figures 2b, 2c, and S6). It is suggested that the organic component of MA+ cation negligibly contributes to this phase transition, consistent with the ADXRD observation. With additional compression, the CH3 stretching modes become too weak to be detected at pressures above 7.7 GPa, and all the Raman peaks display a continuous blue-shift and significant weakening and broadening. These observations indicate the gradual development of structural distortion and amorphization of monoclinic MA3Bi2Br9 in this pressure region.27 The ADXRD and Raman results coincidentally reveal the dominant contribution of inorganic component (i.e., in MA3Bi2Br9) to the pressureinduced trigonal-to-monoclinic phase transition. To explore the directional structural responses of trigonal MA3Bi2Br9, high pressure compressibilities were calculated following the equation below: ij ∂l yz Kl = −jjj zzz j ∂p z k {T
C
DOI: 10.1021/acs.inorgchem.8b03190 Inorg. Chem. XXXX, XXX, XXX−XXX
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Figure 4. (a and b) High pressure comparison between Cs3Bi2Br9 and MA3Bi2Br9 lattice parameters of (a) a or b axes and (b) c axis. The blue and red lines in (a) and (b) are only used for clarification. (c) High pressure compressibilities of b and c axes in Cs3Bi2Br9. (d) Compressibility indicatrix in the ab plane of Cs3Bi2Br9 and the corresponding crystal structure viewed in the same direction.
high pressure investigations. At ambient conditions, Cs3Bi2Br9 adopts the same atomic arrangement as that of MA3Bi2Br9 but has slightly decreased lattice parameters, due to a smaller size of Cs+ than MA+ (Figures S8 and S9).31 High pressure ADXRD experiments reveal that trigonal Cs3Bi2Br9 are stable below 4 GPa (Figure S10). Compared with MA3Bi2Br9, a larger bulk modulus (Figure S11), more rigid axial contraction, and smaller axial compressibility (Figures 4a−4d and S12) in Cs3Bi2Br9 are observed, demonstrating its enhanced rigid structure at high pressure. This is mainly attributed to less flexible cations of Cs+ and stronger covalent interactions between Cs+ and BiBr6. For the compressible anisotropy, the interlayer c axis in Cs 3 Bi 2 Br 9 also shows a smaller compressibility than that of intralayer a or b axes, owing to a puckered structural geometry similar to that in MA3Bi2Br9 (Figure 4c). This comparison reveals the structural contribution of organic MA+ cations at high pressure, i.e. promoting the flexibility of MA3Bi2Br9 structure. Based on the structural variations of MA3Bi2Br9, high pressure UV−vis absorption experiments were conducted to explore its structure−property relationships. At ambient conditions, MA3Bi2Br9 exhibits a light yellow color with a band gap of 2.65 eV, determined via the Tauc plot of the absorption signal (Figure S13). With increasing pressure to 4.1 GPa, the absorption edge of MA3Bi2Br9 displays a continuous red shift (Figure 5a), exhibiting a sustainable band gap narrowing of ∼0.2 eV (Figure 5c). Previous reports have demonstrated that the band gaps of Bi-based halide perovskites are insensitive to the organic cations but dominated by the metal and halide orbitals within the structure,9,32 and high pressure band gap evolution of metal halide perovskites usually relies on the contraction and tilting of octahedra.6−17 The band gap narrowing of trigonal MA3Bi2Br9 can be attributed to the promoted overlap of Bi and Br orbitals, which is introduced by the octahedra contraction and one-dimensional shrinkage of Bi−Br−Bi bonds in MA3Bi2Br9. In the transition range between 4.6 and 5.5 GPa, a blue shift is observed at the absorption edge with a slight ∼0.03 eV widening of the band gap. Such an abrupt discontinuity in band gap evolution is accompanied by the internal distortion and external tilting of
Figure 5. (a and b) High pressure absorption spectra of MA3Bi2Br9 from ambient conditions to 10.4 GPa. (c) Band gap evolution of MA3Bi2Br9 crystal as a function of pressure. The insets represent the optical micrographs within DAC at 1 atm and 10.4 GPa, showing the piezochromic process.
the BiBr6 octahedra. The off-aligned Bi−Br−Bi bonds bring about less coupling between Bi and Br orbitals and consequently lead to a band gap widening.9,17 With further compression to 10.4 GPa, the absorption edge of MA3Bi2Br9 exhibits a continuous red-shift with ∼0.1 eV band gap narrowing. Meanwhile, the crystal color gradually turns to orange yellow at 10.4 GPa, revealing the piezochromism phenomenon in MA3Bi2Br9 (Figures 5c and S14). In this pressure range, an observed decrease of Bi−Br−Bi bond angle in monoclinic MA3Bi2Br9 (Figure S1) may lead to band gap D
DOI: 10.1021/acs.inorgchem.8b03190 Inorg. Chem. XXXX, XXX, XXX−XXX
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up fund and Presidential fund from SUSTech. CHESS at Cornell University is supported by the NSF Award DMR1332208.
broadening. However, the contracted BiBr6 octahedra and the enlarged bond angle of Bi2−Br5−Bi1 (Figure S1) as well as the structural amorphization of MA3Bi2Br9 are all able to promote the coupling between Bi and Br orbitals, resulting in the band gap narrowing above 5.5 GPa.9 High pressure UV−vis absorption experiments clearly reveal the contribution of inorganic component to the property of MA3Bi2Br9, i.e. band gap variation.
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(1) Dou, L.; Wong, A. B.; Yu, Y.; Lai, M.; Kornienko, N.; Eaton, S. W.; Fu, A.; Bischak, C. G.; Ma, J.; Ding, T.; et al. Atomically Thin Two-Dimensional Organic-Inorganic Hybrid Perovskites. Science 2015, 349, 1518−1521. (2) Huo, C.; Cai, B.; Yuan, Z.; Ma, B.; Zeng, H. Two-Dimensional Metal Halide Perovskites: Theory, Synthesis, and Optoelectronics. Sma. Meth. 2017, 1, 1600018. (3) Saidaminov, M. I.; Mohammed, O. F.; Bakr, O. M. LowDimensional-Networked Metal Halide Perovskites: the Next Big Thing. ACS Energy Lett. 2017, 2, 889−896. (4) Cao, D. H.; Stoumpos, C. C.; Farha, O. K.; Hupp, J. T.; Kanatzidis, M. G. 2D Homologous Perovskites as Light-Absorbing Materials for Solar Cell Applications. J. Am. Chem. Soc. 2015, 137, 7843−7850. (5) Lin, H.; Zhou, C.; Tian, Y.; Siegrist, T.; Ma, B. Low-Dimensional Organometal Halide Perovskites. ACS Energy Lett. 2018, 3, 54−62. (6) Zhu, H.; Cai, T.; Que, M.; Song, J.-P.; Rubenstein, B. M.; Wang, Z.; Chen, O. Pressure-Induced Phase Transformation and Band-Gap Engineering of Formamidinium Lead Iodide Perovskite Nanocrystals. J. Phys. Chem. Lett. 2018, 9, 4199−4205. (7) Wu, H.; Bai, F.; Sun, Z.; Haddad, R. E.; Boye, D. M.; Wang, Z.; Huang, J. Y.; Fan, H. Nanostructured Gold Architectures Formed through High Pressure-Driven Sintering of Spherical Nanoparticle Arrays. J. Am. Chem. Soc. 2010, 132, 12826−12828. (8) Li, B.; Bian, K.; Zhou, X.; Lu, P.; Liu, S.; Brener, I.; Sinclair, M.; Luk, T.; Schunk, H.; Alarid, L.; et al. Pressure Compression of CdSe Nanoparticles into Luminescent Nanowires. Sci. Adv. 2017, 3, No. e1602916. (9) Wang, Y.; Lü, X.; Yang, W.; Wen, T.; Yang, L.; Ren, X.; Wang, L.; Lin, Z.; Zhao, Y. Pressure-Induced Phase Transformation, Reversible Amorphization, and Anomalous Visible Light Response in Organolead Bromide Perovskite. J. Am. Chem. Soc. 2015, 137, 11144−11149. (10) Jaffe, A.; Lin, Y.; Beavers, C. M.; Voss, J.; Mao, W. L.; Karunadasa, H. I. High-Pressure Single-Crystal Structures of 3D LeadHalide Hybrid Perovskites and Pressure Effects on their Electronic and Optical Properties. ACS Cent. Sci. 2016, 2, 201−209. (11) Szafrański, M.; Katrusiak, A. Mechanism of Pressure-Induced Phase Transitions, Amorphization, and Absorption-Edge Shift in Photovoltaic Methylammonium Lead Iodide. J. Phys. Chem. Lett. 2016, 7, 3458−3466. (12) Jiang, S.; Fang, Y.; Li, R.; Xiao, H.; Crowley, J.; Wang, C.; White, T. J.; Goddard, W. A., III; Wang, Z.; Baikie, T.; et al. PressureDependent Polymorphism and Band-Gap Tuning of Methylammonium Lead Iodide Perovskite. Angew. Chem., Int. Ed. 2016, 55, 6540− 6544. (13) Nagaoka, Y.; Hills-Kimball, K.; Tan, R.; Li, R.; Wang, Z.; Chen, O. Nanocube Superlattices of Cesium Lead Bromide Perovskites and Pressure-Induced Phase Transformations at Atomic and Mesoscale Levels. Adv. Mater. 2017, 29, 1606666. (14) Li, Q.; Wang, Y.; Pan, W.; Yang, W.; Zou, B.; Tang, J.; Quan, Z. High-Pressure Band-Gap Engineering in Lead-Free Cs2AgBiBr6 Double Perovskite. Angew. Chem., Int. Ed. 2017, 56, 15969−15973. (15) Lü, X.; Wang, Y.; Stoumpos, C. C.; Hu, Q.; Guo, X.; Chen, H.; Yang, L.; Smith, J. S.; Yang, W.; Zhao, Y.; et al. Enhanced Structural Stability and Photo Responsiveness of CH3NH3SnI3 Perovskite via Pressure-Induced Amorphization and Recrystallization. Adv. Mater. 2016, 28, 8663−8668. (16) Jaffe, A.; Lin, Y.; Mao, W. L.; Karunadasa, H. I. PressureInduced Metallization of the Halide Perovskite (CH3NH3)PbI3. J. Am. Chem. Soc. 2017, 139, 4330−4333. (17) Kong, L.; Liu, G.; Gong, J.; Hu, Q.; Schaller, R. D.; Dera, P.; Zhang, D.; Liu, Z.; Yang, W.; Zhu, K.; et al. Simultaneous Band-Gap
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CONCLUSIONS In summary, high pressure MA3Bi2Br9 study reveals different contributions of inorganic and organic components, respectively, to the structure and property of 2D hybrid halide perovskite. During compression, the inorganic component of BiBr6 octahedra dominates the phase transition of MA3Bi2Br9, which involves the distortion and tilting of octahedra in three dimensions. Meanwhile, the organic component of MA+ cations contributes to the flexible structural nature of MA3Bi2Br9. High pressure UV−vis absorption experiment provides the property function of inorganic composition, i.e. band gap determination. The tilting between BiBr6 octahedra gives rise to the broadening of band gap of MA3Bi2Br9. The contraction of BiBr6 octahedra and the structural amorphization are responsible for the narrowing of band gap. This work provides novel insights into the structure and property of 2D hybrid perovskites, which are expected to offer new strategies for further structure and band gap engineering of 2D hybrid halide perovskites.33,34
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ASSOCIATED CONTENT
S Supporting Information *
The Supporting Information is available free of charge on the ACS Publications website at DOI: 10.1021/acs.inorgchem.8b03190. Detailed experimental/structural description and data analysis (PDF)
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REFERENCES
AUTHOR INFORMATION
Corresponding Authors
*E-mail:
[email protected] (Z.Q.). *E-mail:
[email protected] (B.Z.). ORCID
Qian Li: 0000-0002-4847-4892 Bo Zou: 0000-0002-3215-1255 Zhongwu Wang: 0000-0001-9742-5213 Jiang Tang: 0000-0003-2574-2943 Zewei Quan: 0000-0003-1998-5527 Notes
The authors declare no competing financial interest.
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ACKNOWLEDGMENTS This work was supported by the National Natural Science Foundation of China (NSFC) (Grants 11604141, 51772142, and 21725304), Shenzhen Science and Technology Innovation Committee including fundamental research projects (Grants JCYJ20170412152528921, JCYJ20160530190717385, and JCYJ20160530190842589), Peacock Team (Grant KQTD2016053019134356), and Peacock Technology Innovation Project (Grant KQJSCX20170328085748757), Development and Reform Commission of Shenzhen Municipality (Novel Nanomaterial Discipline Construction Plan), and startE
DOI: 10.1021/acs.inorgchem.8b03190 Inorg. Chem. XXXX, XXX, XXX−XXX
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DOI: 10.1021/acs.inorgchem.8b03190 Inorg. Chem. XXXX, XXX, XXX−XXX
