Chirality Transfer from Chiral Mesoporous Silica to Perovskite CsPbBr 3 Nanocrystals - The Role of Chiral Confinement

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Metadata	Details
Publication Date	2022-02-12
Journal	CCS Chemistry
Authors	Zhen Li, Yan Yan, Wenyan Ma, Jiaqi Zhao, Yong Fan
Institutions	Jilin University, State Key Laboratory of Inorganic Synthesis and Preparative Chemistry
Citations	13

Abstract

Open AccessCCS ChemistryCOMMUNICATION7 Nov 2022Chirality Transfer from Chiral Mesoporous Silica to Perovskite CsPbBr3 Nanocrystals: The Role of Chiral Confinement Zhen Li, Yan Yan, Wenyan Ma, Jiaqi Zhao, Yong Fan and Yu Wang Zhen Li State Key Laboratory of Inorganic Synthesis and Preparative Chemistry, College of Chemistry, Jilin University, Changchun 130012 , Yan Yan State Key Laboratory of Inorganic Synthesis and Preparative Chemistry, College of Chemistry, Jilin University, Changchun 130012 , Wenyan Ma State Key Laboratory of Inorganic Synthesis and Preparative Chemistry, College of Chemistry, Jilin University, Changchun 130012 , Jiaqi Zhao State Key Laboratory of Inorganic Synthesis and Preparative Chemistry, College of Chemistry, Jilin University, Changchun 130012 , Yong Fan *Corresponding authors: E-mail Address: [email protected] E-mail Address: [email protected] College of Chemistry, Jilin University, Changchun 130012 and Yu Wang *Corresponding authors: E-mail Address: [email protected] E-mail Address: [email protected] State Key Laboratory of Inorganic Synthesis and Preparative Chemistry, College of Chemistry, Jilin University, Changchun 130012 https://doi.org/10.31635/ccschem.022.202101596 SectionsSupplemental MaterialAboutAbstractPDF ToolsAdd to favoritesDownload CitationsTrack Citations ShareFacebookTwitterLinked InEmail A convenient and universal in situ growth strategy has been employed for constructing CsPbBr3/chiral mesoporous silica (CsPbBr3@CMS) composite. The circular dichroism spectra show that the CsPbBr3@CMS composite has the same left-handed chirality with chiral mesophorous silica (CMS), which confirms that the chirality can be transferred from CMS to the CsPbBr3 perovskite nanocrystals (NCs) by confining the CsPbBr3 NCs in the helix channels of CMS. The spiral arrangement of CsPbBr3 NCs results in a circularly polarized luminescence response with a dissymmetry factor |glum| up to 5.4 × 10−3. The quantum confinement effect provided by CMS causes the shift of the band edge toward higher energies with photoluminescence (PL) emission of 474 nm. Furthermore, the CMS matrix immensely improves the stability of the CsPbBr3 NCs, which enables the PL intensity of this composite to remain constant under the condition of continuous UV light irradiation for 48 h and exposure to the air for more than 6 months. Based on these merits, the CsPbBr3@CMS composite can be used to prepare high-performance blue light-emitting diodes. Download figure Download PowerPoint Introduction Chiral perovskites have attracted considerable attention due to their particular optical and optoelectronic properties as well as their tremendous potential in circularly polarized light detection,1-3 circularly polarized luminescence (CPL),4-7 nonlinear optics,8-10 ferroelectrics,11-14 spintronics, and so on.15-17 Generally, there have been four strategies employed to obtain chiral perovskites: (1) The chirality of perovskite crystals can be induced by the chiral organic molecules. For example, the chiral perovskite crystal structure can be obtained by introducing the chiral amine molecules, which enables the perovskites to crystallize in the chiral space group and present inherent chiral characteristics.18-22 (2) The chiral molecules can cause chiral distortion on the surface of perovskite nanocrystals (NCs). (3) The electronic coupling can take place between the chiral ligand molecules and achiral perovskite.4,10,23,24 (4) The chirality of perovskite can be realized by the screw dislocation of the assembly of perovskite NCs.25 The first to third approaches have a common characteristic, which is that the chirality of perovskite can be induced by chiral ligands, resulting in a weaker circular dichroism (CD) response, lower photoluminescence quantum yield (PLQY), and CPL intensity due to the strong phonon energy of chiral ligands. For the fourth strategy, the CD response can be achieved based on the screw dislocation of CsPbBr3 NC aggregates. However, the CD response is only one-tenth of the chiral hybrid perovskite crystal structures, even though there is no chiral molecule to be introduced.25 Therefore, it is difficult to prepare chiral perovskites with strong chiroptical response when no chiral molecules are used as inductive agents. The chiroptical property is very important for the chiral perovskites. In general, the chirality of chiral perovskites originates from the ground state and the excited state, respectively. The chirality of the ground state can be measured by the CD spectrum, and the chirality of the excited state is confirmed by the CPL spectrum. Compared with the chiral perovskites with a CD response, there are few reports on chiral perovskites with a CPL response. For example, a chiral perovskite NC can be obtained by modifying it with chiral α-octylamine, which exhibits a CPL response and a |glum| of 1.0 × 10−3.10 In addition to the chiral organic amine, the perovskite NCs can be endowed with CPL characteristics by assembling the CsPbX3 NCs with organic gel soft templates.4 The CPL response can also be realized by coupling the CsPbBr3 NCs on the surface of the inorganic silica nanohelixes.6 Although the chiral perovskite composites show obvious chiroptical properties, the presence of organic gel and the exposure of perovskites to air immensely reduce their stability. Recently, however, the stability of perovskites has been improved via coating silica shell on the surface of the perovskite NCs and filling the pores of the mesoporous silica with perovskites.26,27 It is undoubtedly advisable to synthesize chiral perovskites through filling the channels of chiral mesoporous silica (CMS) with them. The helical channels of CMS not only guide the spiral arrangement of perovskite NCs but also protect them from air to improve their stability. Herein, we prepare a novel chiral CsPbBr3/CMS composite by growing all-inorganic perovskite CsPbBr3 NCs inside a CMS template without using any chiral ligands. To the best of our knowledge, no example of combining CMS and perovskites to construct CPL-active materials has been reported yet. The helical channels of CMS not only transfer its chirality to CsPbBr3 NCs, but also confine the size of CsPbBr3 NCs, which results in the shift of the band edge toward high energy and 13.7% PLQY. In-depth chiroptical analysis demonstrates that the CsPbBr3@CMS composite has an obvious CD and CPL response with a CPL dissymmetry factor that reaches 5.4 × 10−3. In addition, the stability of CsPbBr3 NCs has been significantly improved due to the protection of the CMS matrix, which is useful for high-performance blue light-emitting diodes (LEDs). This work provides guidance for the synthesis of chiral perovskites with a strong CPL response and further provides insight into the structure-property relationship. Results and Discussion The CMS template was synthesized by heating a mixture of hexadecyl trimethyl ammonium bromide (CTAB) and tetraethyl orthosilicate (TEOS) in ammonia solution (NH3·H2O) according to a previous report with some modifications.28 Subsequently, the as-prepared CMS was calcined to remove CTAB for the next step of perovskite precursor soaking. The transmission electron microscopy (TEM) and scanning electron microscopy (SEM) images of the CMS nanorods are shown in Supporting Information Figure S1. The as-prepared CMS nanorods have rod-like helical morphologies with an average diameter (D), length (L), and aspect ratio (L/D) of 80-200 nm, 0.5-1 μm, and 2.5-12.5, respectively. The high-resolution TEM (HRTEM) image shows the intermittent lattice fingers (the red arrow corresponds to the (10) planes of the CMS) with a constant period ( Supporting Information Figure S1b, inset), confirming the one-dimensional (1D) helical channel structure and the chirality of the CMS.28,29 The chiral direction can be determined to be left-handed according to the previous report.28,30 The X-ray diffraction (XRD) pattern of calcined CMS is shown in Supporting Information Figure S2, the well-resolved peaks at 2.15°, 3.71°, 4.26°, and 5.58° can be indexed to (10), (11), (20), and (21) reflections of two-dimensional (2D) hexagonal p6mm unit cells, respectively, corresponding to the results of TEM. The specific surface areas and pore size distributions of the CMS nanorods were calculated on the basis of the nitrogen adsorption-desorption data ( Supporting Information Figure S3). The nitrogen adsorption-desorption isotherm of the calcined CMS nanorods exhibit a type IV isotherm with an H1 hysteresis loop, suggesting the presence of uniform channel-like mesopores with a pore diameter of 2.8 nm. The Brunauer-Emmett-Teller (BET) surface area is calculated to be 1138 m2/g. The pore volume result obtained from the N2 adsorption volumes at the specific point (P/P0 = 0.99) is 0.99 cm2/g, which implies that the CMS nanorods can be filled with perovskite guests. The schematic diagram of in situ fabrication of CsPbBr3@CMS composite is shown in Scheme 1. When the concentration of the perovskite precursor solution was in the range of 0.1 to 0.25 M, and the immersion temperature was in the range from room temperature to 100 °C, the solutions of perovskite precursor infiltrated into the pores of CMS via capillary action. Then the excess solution of the perovskite precursor was removed by centrifugation and finally annealed at 140 °C for 12 h to obtain the CsPbBr3@CMS composite (see Supporting Information). Scheme 1 | Illustration of the in situ template-assisted synthesis of CsPbBr3@CMS composite. Download figure Download PowerPoint The SEM image of the CsPbBr3@CMS composite shows that their morphology is the same as the CMS nanorods (Figure 1a), confirming that the filling of perovskite NCs cannot change the morphology of the CMS matrix. Figure 1b shows that the CsPbBr3 NCs can homogeneously crystallize and arrange along the 1D helical channel of the CMS nanorods to form a “1D” helical line (right inset). The HRTEM image of CsPbBr3@CMS shows the presence of rod-shaped CsPbBr3 NCs extending along the channels (Figure 1c). The CsPbBr3 NC size distribution histograms (Figure 1d) measured on HRTEM, closely match pore size distribution of the 2.8 nm channels of CMS. Energy-dispersive X-ray spectrometry (EDX) mapping analysis reveals that the CsPbBr3@CMS composites contain Cs, Pb, Br, and Si elements, and the distributions of these elements are homogeneous (as shown in Figure 1e). The content of Si is dominant, and the ratio of Cs:Pb:Br is 1:0.95:2.72 is close to the stoichiometric ratio of CsPbBr3 perovskites ( Supporting Information Figure S4). Furthermore, the sharp decrease in the BET surface area (from 1138 to 380 m2/g) and pore volume (from 0.99 to 0.27 cm3/g) of CsPbBr3@CMS composite once again proves that the CsPbBr3 NCs successfully filled into the CMS ( Supporting Information Figure S5). The nitrogen adsorption data show that the pore structure of the CMS matrix cannot be completely crammed with CsPbBr3 nanocrystals (NCs), even though the BET surface area and pore volume have obviously decreased ( Supporting Information Figure S5). The above-mentioned results clearly confirm that CsPbBr3 NCs are filled inside of the CMS channels and arrange themselves along the helical channel of the CMS nanorods. Figure 1 | (a) SEM and (b) TEM images of CsPbBr3@CMS, inset: the image of obvious spiral arrangement of CsPbBr3 perovskites with scale bar of 50 nm; the white arrow corresponds to the (10) fringes of CMS. (c) HRTEM image of CsPbBr3@CMS, some NCs have been marked with red lines. (d) The CsPbBr3 NCs size distribution histograms with Gaussian fitting. (e) The elemental mapping by EDX of CsPbBr3@CMS. Download figure Download PowerPoint The XRD patterns of CsPbBr3@CMS are presented in Figure 2a. The peaks at 21.50°, 30.38°, and 37.60° can be indexed to the (110), (002), and (121) reflections of the monoclinic phase of the CsPbBr3 structure (JCPDS No. 18-0364), respectively. The narrow full width at half maxima of the reflection peaks demonstrates the good crystallinity of the CsPbBr3 NCs. The X-ray photoelectron survey spectra (XPS) show the characteristic peaks of Cs 1s, Pb 4f, Br 3d, Si 2p, and O 1s, which are consistent with CsPbBr3 and CMS (Figure 2b). The Pb and Br XPS spectra each exhibit prominent doublets, in agreement with previous studies of perovskites: the Pb 4f5/2 and 4f7/2 doublet is at 143.8 and 138.9 eV (Figure 2c), and the Br 3d5/2 and 3d3/2 doublets are at 68.7 and 69.7 eV ( Supporting Information Figure S6b). The doublets at 739.5 and 725.5 eV correspond to the Cs 3d3/2 and 3d5/2 electron energy levels ( Supporting Information Figure S6a), which confirm that only Pb-Br exists in the octahedron, and the crystal structure of CsPbBr3 cannot be destroyed.24 In addition, the peaks of 103.9 and 533.2 eV correspond to the Si 2p and O 1s binding energies for SiO2 in CMS ( Supporting Information Figures S6c and S6d). The elemental ratio of Pb:Br is 1:2.63 surveyed by XPS, which is probably caused by loss of halogen.31 This evidence demonstrates that the CsPbBr3 NCs are distributed tightly within the CMS template. Figure 2 | (a) XRD patterns and (b) XPS survey spectra of CsPbBr3@CMS. (c) The high-resolution XPS spectra of CsPbBr3@CMS for Pb 4f spectra. Download figure Download PowerPoint To better understand the photophysical process of CsPbBr3@CMS, we fabricated CsPbBr3 polycrystalline film to compare it with the CsPbBr3@CMS composite. The CsPbBr3 film exhibited yellow color and weaker green emission under visible and 365 nm light illumination (Figure 3a). Impressively, the obtained CsPbBr3@CMS composite exhibited a yellow color under visible light, but the bright blue emission was observed in the 365 nm UV lamp illumination (Figure 3b). This result suggests that the strong blue emission of CsPbBr3@CMS originates from the size decrease of CsPbBr3 NCs due to the limitation of the CMS template.27 To further prove this point, we conducted the UV-vis absorption spectrum and PL spectrum. Supporting Information Figure S7 shows that the CsPbBr3 film exhibited a band-edge exciton peak around 512 nm, with a long adsorption edge around 536 nm and a PL emission centering around 525 nm. However, the UV-vis absorption spectra of CsPbBr3@CMS showed two absorption peaks: a peak of confining CsPbBr3 NCs at 458 nm and another peak at 525 nm corresponding to the absorption of CsPbBr3 adsorbed on the CMS surface. However, the NCs filling in CMS channels still occupied the vast majority of the channels (Figure 3c). The CsPbBr3@CMS composite showed a PL emission peak at 474 and 52 nm blue-shift in contrast to the CsPbBr3 film, which can be attributed to the strong quantum confinement effect of the CsPbBr3 NCs within the 2.8 nm pore of CMS template (Figure 3d). Due to the 2.8 nm pore size of the CMS less than the exciton Bohr radius of the CsPbBr3 perovskite (rB = 7 nm),32 the quantum confinement effect occurred, which was also observed in the perovskite coated with mesoporous silica.33-35 Figure 3 | Photographs of (a) CsPbBr3 polycrystalline film and (b) CsPbBr3@CMS composite under visible illumination and UV 365 nm illumination. (c) UV-vis absorption spectra and (d) PL emission spectra of CsPbBr3@CMS. Download figure Download PowerPoint The optical activity of the CsPbBr3@CMS composite was further investigated by CD spectra. For CsPbBr3 polycrystalline film ( Supporting Information Figure S8), no CD signal was found in the wavelength range of 300-700 nm due to the absence of the chiral factor. However, the obvious CD signal was observed for the CsPbBr3@CMS composite. Figure 4a exhibits a positive CD peak at 488 nm, which is attributed to the CsPbBr3 NCs confined in the CMS channels and corresponds to the maximum absorption wavelength position of the CsPbBr3@CMS composite (Figure 3c). In addition, another CD peak at 537 nm was also found, which was caused by the spirally distributed CsPbBr3 on the surface of the CMS. This result clearly demonstrates that the chirality can be transferred from the CMS template to CsPbBr3 perovskites. Figure 4 | The chiral characterization of CsPbBr3@CMS. (a) CD spectra, (b) CPL spectra, and (c) luminescence dissymmetry factor (glum) of CsPbBr3@CMS. Download figure Download PowerPoint Additionally, we conducted the CPL test to verify the chirality of the excited state. As expected, the CsPbBr3@CMS composite showed obvious circularly polarized emission, and the right-handed CPL signal around 470 nm is shown in Figure 4b. These results clearly explain that the confinement effect of the spiral channels of the CMS template forces the CsPbBr3 NCs to helically arrange themselves, and the chirality of the CMS template is transferred to the achiral perovskite NCs, so the CsPbBr3@CMS composite is endowed with CD and CPL activity. To further develop CPL materials, a key issue is obtaining a high luminescence dissymmetry factor (glum), which is used to quantify the level of CPL. The luminescence dissymmetry factor is defined as glum = 2(IL − IR)/(IL + IR), where IL and IR refer to the intensity of left- and right-handed CPL, respectively.36 The maximum |glum| value of CsPbBr3@CMS was up to 5.4 × 10−3 (Figure 4c), which is a comparable value to other perovskite composites such as chiral gel-capped CsPbX3 NCs (7.3 × 10−3) and CsPbBr3 NCs grafted on the silica nanohelical surfaces (6.9 × 10−3), in which the preparation method of the composite and the instability of the NCs exposed on the surface greatly limits its application.4,6 These results clearly indicate that coassembly between perovskite NCs and CMS plays a vital role in the chirality transfer. Well-ordered organization of perovskite NCs along the chiral pores is the key point for the achievement of induced CPL of perovskite NCs. Thus, this method is a general approach to fabricating CPL-active perovskite NCs. To gain more insights into the carrier recombination dynamics of perovskite NCs, time-resolved PL (TRPL) measurements were carried out. Supporting Information Figure S9 shows the TRPL spectra of CsPbBr3 film and CsPbBr3@CMS, the decay curves of CsPbBr3 film and CsPbBr3@CMS sample can be well fitted into multiexponential and triexponential equations. Slow decay and fast decay are related to excitonic recombination and the high trap density at the crystal surface, respectively ( Supporting Information Table S1).31 The average lifetime (τave) of CsPbBr3 NCs lengthened from 12.28 to 19.16 ns after confinement growth in CMS. These kinetics test results indicate that a much lower quantity of defects and vacancies were created by the Pb-Br antisite and undercoordinated Pb atoms for the CsPbBr3 NCs within the CMS matrix and significantly suppressed the nonradiative decay of the CsPbBr3 NCs. These results are similar to previously reports about [email protected] and perovskite-gel composite materials.4,31 To better characterize the luminous properties of the composite, we conducted a PLQY test on the CsPbBr3@CMS. The 13.7% PLQY was more than twice the reported CH3NH3PbBr3 nanoparticles grown in mesoporous silica (< 5.5 %),33 which confirms the excellent emission performance of the CsPbBr3@CMS composite. As we all know, lead halide perovskite samples are sensitive to UV light. We exposed the CsPbBr3 film and CsPbBr3@CMS samples to UV 365 nm light to verify their stability. The CsPbBr3 film was strongly affected by UV light. After 48 h UV irradiation, the PL intensity of the CsPbBr3 film was only 40% retained ( Supporting Information Figure S10a), which confirmed its poor UV light stability. In contrasst, the CsPbBr3@CMS composite samples have strong resistance to UV irradiation. The PL intensity of the CsPbBr3@CMS sample hardly decreased after 48 h of continuous UV illumination ( Supporting Information Figure S10a). In addition, CsPbBr3@CMS composite was placed in the air for over 6 months without undergoing any decomposition, and the PL intensity remained basically unchanged ( Supporting Information Figure S10b). These results support the idea that confining the perovskite NCs can avoid degradation within the rigid CMS template, which provides spatial confinement and limits ion migration. The CMS coating reduces the contact of NCs with air, providing the CsPbBr3@CMS composite with excellent stability. The emergence of perovskite provides new opportunities for large-area, low-cost, and color-saturated LEDs, which are very suitable for display and solid-state lighting applications. Therefore, the production of high-quality blue-emitting LEDs is of great significance to the development of the LED field in the future.37 In view of the excellent luminescence properties of the CsPbBr3@CMS composite, we used it as a phosphor to prepare a blue LEDs. Supporting Information Figure S11a shows the schematic diagram of the LEDs, when the power is turned on, the LEDs emit saturated and pure bright blue color ( Supporting Information Figure S11b). The device exhibits a strong PL centering at 477 nm. The relevant Commission Internationale de L’Eclairage chromaticity diagram is (0.11, 0.22), giving blue emission with high colour purity, as shown in Supporting Information Figure S11d. Notably, PL intensity gradually increases as the current is enhanced from 20 to 100 mΑ, and the shape does not change ( Supporting Information Figure S11c), indicating the improved color stability of our LEDs. Conclusion We have successfully designed and synthesized CsPbBr3@CMS via in situ growth. The CsPbBr3 NCs were crystallized into a “1D” spiral shape according to the channel of the CMS, thereby endowing chiroptical activity to the CsPbBr3 NCs. The CPL test confirmed that the CsPbBr3@CMS has a clear right-handed CPL response, and the dissymmetry factor |glum| reaches 5.4 × 10−3. Due to the quantum confinement effect of the CMS rigid template, ion migration is greatly suppressed, and its luminescence performance and stability have been greatly improved. Compared with bulk materials, the confined CsPbBr3 NCs have a blue shift of 52 nm, and their PLQY has reached 13.7%. This work enriches the scope of research on chiral perovskite materials and provides a new direction for the research of CPL functional materials. Such novel chiral inorganic luminescence material will bring new opportunities in nonlinear optics, biosensors, and chiral recognition. Supporting Information Supporting Information is available and includes detailed experimental procedures and characterization data. Conflict of Interest There is no conflict of interest to report. Funding Information This work was financially supported by the National Natural Science Foundation of China (no. 21771083). References 1. Chen C.; Gao L.; Gao W.; Ge C.; Du X.; Li Z.; Yang Y.; Niu G.; Tang J.Circularly Polarized Light Detection Using Chiral Hybrid Perovskite.Nat. Commun.2019, 10, 1927. Google Scholar 2. 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DOI: https://doi.org/10.31635/ccschem.022.202101596