
Citation: | Shuoshuo Zang, Yan Yu, Lan Zhang, Hewen Liu. Perovskite Phase Transformation Products for Repeatable Fluorescence Response to Solvents[J]. Chinese Journal of Chemical Physics . DOI: 10.1063/1674-0068/cjcp2409126 |
Based on the transformation between different phase structures, lead halide perovskite materials can achieve interesting fluorescence response to water, heat, and pressure. Here, we achieve a novel fluorescence response to solvents on a three-dimensional perovskite (3D, CsPbBr3) that is transformed from zero-dimensional perovskite (0D, Cs4PbBr6). The phase transformation process is realized by extracting excess CsBr from Cs4PbBr6 by tungstosilicic acid (TSA). The phase transformation product (U-CsPbBr3) with more surface defects shows weak photoluminescence (PL) emission, but shows bright green PL emission immediately when it is wetted with some solvents such as methyl acetate, acetone, tetrahydrofuran, and acetonitrile. Repeatable and time-controlled fluorescence response can be achieved by adjusting solvents with different volatility. This unique property can be possibly used in anti-counterfeiting or electrowetting display, etc.
As an outstanding photoelectric material, three-dimensional (3D) cesium lead halide (CsPbX3, X = Cl, Br, and I) perovskites nanocrystals (NCs) have been studied widely in recent years and already made significant progress in many fields [1, 2]. Besides 3D perovskites, there are a wide range of perovskites [3]. Zero-dimensional (0D) perovskites (Cs4PbX6) with special structure and mysterious photoluminescence (PL) properties have attracted attention recently [4]. 3D perovskite CsPbX3 is usually composed of a framework of corner-sharing [PbX6]4− octahedra extending in all three dimensions, while Cs cations fill the voids. In stark contrast, the 0D perovskite Cs4PbX6 features a series of isolated [PbX6]4− octahedra, which are separated by Cs cations [5]. Due to the isolation of [PbBr6]4– octahedra in Cs4PbBr6, orbital coupling between the valence band (Pb-6s and Br-4p) and conduction band (Pb-6p and Br-4p) is weak, resulting in both flattened bands and a wide bandgap (~3.9 eV) which is much larger than that of CsPbBr3 (~2.4 eV) [6].
Cs4PbBr6 with wide-band gap is generally considered to be a kind of nonluminescent perovskite [7, 8]. However, as Cs4PbBr6 with abnormal green PL emission [9, 10] has been reported, the mysterious origin of PL emission has been debated [6, 11−14]. There are mainly two views on the origin of green emission for Cs4PbBr6, i.e., intrinsic emission (due to the presence of defects) [15−17] and CsPbBr3 inclusion/impurity emission [11, 18]. Although the origin of green photoluminescence for Cs4PbBr6 is still under debate so far, however, one thing for sure, there exists mutual transformation between Cs4PbBr6 and CsPbBr3 under certain conditions due to their highly ionic nature [19]. Cs4PbBr6 NCs were regarded as a PbBr2-deficient material, and Cs4PbBr6 NCs could be converted into CsPbBr3 NCs by treating presynthesized Cs4PbBr6 NCs with excess PbBr2 [20]. Subsequently, Cs4PbBr6 could also be converted into CsPbBr3 by thermal annealing and chemical reaction with Prussian Blue [21]. Meanwhile, Cs4PbBr6 NCs were also regarded as a CsBr-rich structure with high ion-diffusion property, and CsPbBr3 NCs could be converted from nonluminescent Cs4PbBr6 NCs by stripping CsBr through an interfacial reaction with water [22, 23]. In addition, the type and content of organic ligands were crucial for the stability and structure of perovskites [24, 25]. Ligand mediated transformation of presynthesized CsPbBr3 NCs to Cs4PbBr6 NCs was initiated by the addition of amines [26−28]. Reversible structural transformation between CsPbX3 and Cs4PbX6 could be realized by the addition of an excess of oleylamine (OAm) or oleicacid (OA) [29]. The participation of inorganic ligand NOBF4 also enabled the chemical transformation from Cs4PbBr6 NCs to CsPbBr3 nanoplates [30]. The changes in structure and composition for perovskites usually cause obvious changes in PL properties, which has important application value in the fields of anti-counterfeiting and information encryption [31−34]. In addition to structural transformation, changes in PL properties caused by external stimuli are also the mainstream direction of responsive materials. For example, wetting display materials control surface wettability through external electric fields to manipulate oil inks and display desired images, which can be utilized for the fields of electronic devices, smart homes, and information communication [35, 36].
In this work, we demonstrated a facile method for the phase transformation from Cs4PbBr6 NCs to CsPbBr3. And the obtained phase transformation product (CsPbBr3) with more surface defects had the characteristic of repeatable fluorescence response to some solvents.
Lead bromide (PbBr2, 99.0%), cesium carbonate (Cs2CO3, 99.9%), 1-octadecene (ODE, 90%), oleic acid (OA, 85%), oleylamine (OAm, 80%–90%), tungstosilicic acid hydrate (TSA, AR) and copper sulfate pentahydrate (CuSO4·5H2O, 99%) were purchased from Aladdin. Sodium dihydrogen phosphate dehydrate (NaH2PO4·2H2O, AR), zinc acetate dihydrate ((CH3COO)2Zn·2H2O, AR) and sodium tetraborate decahydrate (Na2B4O7·10H2O, AR) were purchased from Sinopharm Chemical Reagent Co., Ltd. The above chemicals except TSA were used directly without further purification. TSA powder was dried in a vacuum drying oven (60 °C for 2 h and 90 °C for 2 h).
Cs4PbBr6 NCs were synthesized as reported in the literature with a slight change [20]. All syntheses were performed in air and without any pre-dried chemicals or solvents. 0.4 g Cs2CO3 was dissolved in 8 mL OA at 150 °C to form CsOA for later use. In a typical synthesis, PbBr2 (0.4 mmol) was dissolved in ODE (20 mL), OA (0.8 mL) and OAm (6 mL) in a flask at 150 °C. After the PbBr2 was completely dissolved, the flask was allowed to cool down to 80 °C. And then, 3 mL of CsOA was swiftly injected. After about 30 s the reaction turned turbid white and was quickly cooled down to room temperature with a cold water bath. The NCs were directly washed via centrifugation (4500 r/min, 10 min), followed by redispersion in 24 mL n-hexane.
TSA powder (25 mg) was added into Cs4PbBr6 NCs colloidal solution (4 mL), and the mixture was subjected to ultrasonic treatment for 10 min. Unreacted TSA powder was removed with dropper. Yellow colloids were obtained and precipitated. The precipitates were washed three times with n-hexane and then tetrahydrofuran. The product was stored in n-hexane. The product obtained under ultrasonic treatment was named U-CsPbBr3. As a control, CsPbBr3 was also obtained by leaving the reaction mixture standing for dozens of hours without agitation, according to the above-mention process. The product obtained by standing treatment was named S-CsPbBr3.
The dispersion of U-CsPbBr3 was coated on filter paper and dried under ambient condition. And dry U-CsPbBr3 showed very weak PL emission under the excitation of 365 nm UV light. A cotton swab filled with a solvent wetted U-CsPbBr3 gently. And the wetted U-CsPbBr3 showed bright green PL emission. After the solvent volatilized, U-CsPbBr3 returned to the pristine weak PL emission state.
UV-visible absorbance spectra were recorded on a Shimadzu UV-2600i spectrophotometer (Japan). The PL spectra were collected by a GANGDONG F-380 fluorescence spectrophotometer (Tianjin, China) equipped with a xenon lamp. The absolute PL quantum yields (PLQYs) were measured using a calibrated integrating sphere in an Edinburgh FLS1000 photoluminescence spectrometer (England). Time-resolved PL decay spectra were obtained by a JY Fluorolog-3-Tou spectrometer (Horiba Jobin Yvon, France) coupled with a 375 nm ps pulsed diode laser. X-ray powder diffraction (XRD) patterns were obtained on a Rigaku Smartlab X-ray diffractometer (Japan) equipped with a Cu Kα radiation source (λ = 1.5418 Å). The samples were scanned from 5° to 50° with a step of 0.02°. Fourier transform infrared (FTIR) spectra were obtained on a BRUKER TENSOR Ⅱ (Germany) in the range from 4000 cm−1 to 400 cm−1. X-ray photoelectron spectroscopy (XPS) were carried out by a ESCALAB 250Xi (Thermo Fisher, UK) with monochromatic Al Kα source (1486.6 eV), and the binding energy of the C 1s peak at 284.8 eV was taken as an internal pristine. Raman spectroscopy measurements were carried out with a LabRAM HR Evolution spectrometer (Horiba Jobin Yvon, France) using a 633 nm laser source. Transmission electron microscopy (TEM) images were obtained on a HT-7650 transmission electron microscope (Hitachi, Japan). High-resolution transmission electron microscopy (HRTEM) images were obtained on a JEOL JEM-2100F field transmission electron microscope (Japan) with an acceleration voltage of 200 kV.
According to our previous work [37], the PL property of CsPbX3 NCs could be improved by adding TSA. Synthesis of Cs4PbBr6 NCs was performed under ambient condition according to published literature [20]. A TEM image (FIG. 1(a)) shows that the obtained Cs4PbBr6 NCs had monodispersed quasi-spherical morphology with an average edge length around 19.8 nm (FIG. 1(b)). And the measured d-spacing of 0.41 nm from HRTEM agreed well with the (104) plane of hexagonal Cs4PbBr6. The obtained Cs4PbBr6 NCs matched exactly the diffraction pattern of the hexagonal Cs4PbBr6 phase (PDF card No. 73-2478) in XRD patterns (FIG. 1(c)). This result indicated that the synthesized product was the target product and there was no impurity phase in it. As shown in FIG. 1(d), the Cs4PbBr6 NCs colloidal solution was colorless and had a strong and narrow optical absorption band at 314 nm, which was the characteristic UV absorption peak of Cs4PbBr6 NCs. In addition, no PL emission was observed from the Cs4PbBr6 NCs colloidal solution under 365 nm UV light. It should be noted that the issue of whether 0D perovskites have the property of PL emission is still in the controversial stage. We focused on the relevant process about phase transformation from 0D to 3D perovskites in this paper.
To explore the effect of TSA on 0D perovskite, different amounts of TSA powder was mixed with Cs4PbBr6 NCs colloidal solution with agitation at first. TSA powder was hard to dissolve in most organic solvents. UV absorption spectra of the upper liquid were used to monitor whether Cs4PbBr6 NCs was reduced in the reaction system. As shown in FIG. 2(a–e), the intensity of characteristic UV absorption peak (314 nm) for Cs4PbBr6 NCs decreased with time in the presence of TSA. The amount of TSA had obvious influence on Cs4PbBr6 NCs in the mixture system, which ruled out the factor of settlement (FIG. 2(f)). When adding 125 mg TSA and the mixture stood for 48 h, the intensity of characteristic UV absorption of Cs4PbBr6 remained only 19% of the original. Yellow precipitate with green PL emission appeared near TSA powder in the bottom, which was the PL characteristic of 3D perovskite (CsPbBr3). Therefore, we speculated that the reduced Cs4PbBr6 NCs should be converted to fluorescent CsPbBr3 because of the interaction between TSA powder and Cs4PbBr6 NCs in organic phase.
We analyzed the obtained yellow precipitates with green PL emission. The XRD patterns (FIG. 3(a)) shows that 3D perovskite CsPbBr3 was indeed presented in the yellow precipitate. And it was named S-CsPbBr3. In addition, there was also a large amount of TSA mixed with it. In the FTIR spectra (FIG. 3(b)), the yellow precipitate had the same characteristic peak (700–1100 cm−1) of Keggin structure as TSA, which was precisely attributed to TSA derivative. Moreover, the C-H stretching vibration (2851, 2925 and 2960 cm−1) and bending vibration (1460 and 1380 cm−1) indicated the presence of organic ligand (OA and OAm), which was derived from Cs4PbBr6 NCs. The PL peak (516 nm) and UV absorption edge (about 510 nm) of S-CsPbBr3 (FIG. 3(c)) were consistent with the optical properties of conventional 3D perovskite, further demonstrating the formation of CsPbBr3. TEM image (FIG. 3(d)) also shows cubic S-CsPbBr3 surrounding TSA particles in the yellow precipitate. And the spacing of crystal plane (0.29 nm) was consistent with the lattice plane (002) for CsPbBr3 in HRTEM. These results confirmed that the reduced Cs4PbBr6 NCs were transformed to CsPbBr3 in the yellow precipitate. This perovskite phase transformation was caused by the TSA, which was quite different from the reported phase transformation pathways [20−22].
Although the mixture of TSA and Cs4PbBr6 NCs could enable the phase transformation from Cs4PbBr6 NCs to S-CsPbBr3 by standing for dozens of hours, this process was too slow and difficult to realize completely. In order to speed up this phase transformation process, ultrasonic treatment was performed on the mixture system. In the absence of TSA, ultrasonic treatment alone had no impact on Cs4PbBr6 NCs (FIG. 4(a, e)). When TSA powder was added, ultrasonic treatment could significantly accelerate the phase transformation process (FIG. 4(b)). Yellow precipitate began to appear (FIG. 4(f)) in the bottom after 3 min, while the absorbance at 314 nm for Cs4PbBr6 decreased, reaching a phase transformation yield of 91% (FIG. 4(c)) in only 8 min. UV absorption and PL emission (FIG. 4(d)) showed the characteristic optical properties of CsPbBr3. The above results indicated that ultrasonic treatment could accelerate the phase transformation process.
The phase transformation product obtained under ultrasonic treatment was further analyzed. The XRD result (FIG. 5(a)) shows that the obtained precipitate with green PL emission was the mixture of TSA and CsPbBr3. The diffraction peak of Cs4PbBr6 has completely disappeared. Differing from the case of S-CsPbBr3, a small amount of TSA (25 mg) was needed to complete phase transformation of Cs4PbBr6 under ultrasonic. Raman spectra (FIG. 5(b)) could provide the vibrational modes of the metal halide sublattice [38]. Raman spectra about Cs4PbBr6 exhibited three characteristic peaks at 69.6, 83.8 and 123.8 cm−1, which can be assigned to the vibrational mode of the [PbBr6]4− octahedron [38−40]. After TSA and ultrasonic treatment, the Raman signals of Cs4PbBr6 disappeared. For U-CsPbBr3, two Raman-active modes with a strong peak at 72.6 cm−1 and a weak peak at 127.4 cm−1 were observed. According to a previous report [41] about CsPbCl3 crystal, peaks at 72.6 and 127.4 cm−1 were assigned to the vibrational mode of [PbBr6]4− octahedron and motion of Cs+ cations [38, 39]. Since the product (U-CsPbBr3) obtained by ultrasonic treatment was composed of TSA and CsPbBr3, the FTIR spectra (FIG. 5(c)) contained not only the characteristic peak of Keggin structure (TSA), but also the organic ligands (OA and OAm). TEM image (FIG. 5(d)) shows cubic U-CsPbBr3 surrounded by the derivatives related to TSA.
The XPS results reflected the surface information of phase transformation product. The change of the connection mode of [PbBr6]4− octahedron will cause the distinction between inside and outside for Br in perovskite. The Br 3d peaks could be fitted into two peaks with binding energies of 68.1 and 69.1 eV for Cs4PbBr6, S-CsPbBr3 and U-CsPbBr3 (FIG. 5(e)). According to the previous reports [42, 43], the peaks of Br 3d at low binding energy (68.1 eV) and high binding energy (69.1 eV) corresponded to the inner Br ions and the surface Br ions in 3D perovskite, respectively. Since the [PbBr6]4− octahedron in Cs4PbBr6 was in a completely decoupled state, Br cations did not differ as described above. The surface to inner Br peak ratios of S-CsPbBr3 and U-CsPbBr3 were 0.97 and 0.76, respectively. Obviously, the surface of S-CsPbBr3 had more abundant Br than that of U-CsPbBr3. The Br-rich surface [44] was conductive to self-passivate defects and facilitated radiative recombination. Therefore, the PLQY of S-CsPbBr3 (9.89%) was higher than that of U-CsPbBr3 (0.93%). As shown in FIG. 5(f), the W 4f binding energy of U-CsPbBr3 and S-CsPbBr3 (38.0 eV and 35.9 eV) was different from that of TSA (38.4 eV and 36.3 eV) because the phase transformation products include TSA and the derivatives related to TSA. It was further confirmed that TSA was involved in the phase transformation process.
Cs4PbBr6 NCs were regarded as a CsBr-rich perovskite material [22]. The perovskite phase transformation from 0D to 3D could be realized by extracting excess CsBr in Cs4PbBr6 NCs with water [22]. According to our previous work [37], TSA could etch the surface of CsPbBr3 by reacting with Cs+. TSA could extract the excess Cs+ in Cs4PbBr6, and the phase transformation from Cs4PbBr6 to CsPbBr3 was realized. Comparing the size of Cs4PbBr6 NCs (19.8±1.3 nm, FIG. 1(b)), the size of CsPbBr3 NCs obtained under ultrasonic were smaller than that obtained for standing (17.9±3.4 nm for standing and 18.0±3.0 nm under ultrasonic) (FIG. 6). The shrinkage in size of the NCs supported the hypothesis that CsBr was extracted from the Cs4PbBr6 NCs [21].
Interestingly, although the obtained phase transformation product (U-CsPbBr3) exhibited very weak PL emission in the dry solid state, as shown in FIG. 7(a), the PL emission intensity was significantly increased once U-CsPbBr3 was wetted with tetrahydrofuran. Moreover, repeated operation (wetting and drying) was measured for U-CsPbBr3 with tetrahydrofuran, the fluorescence response was repeatable (FIG. 7(b)). For this peculiar phenomenon, the exciton recombination dynamics of U-CsPbBr3 under dry and wet states was investigated. As shown in FIG. 7(c) and Table I, the PL decay profiles of U-CsPbBr3 were significantly different in dry and wet states. The dry U-CsPbBr3 presented a biexponential decay curve that can be fitted on the basis of Eq.(1). Two extremely short PL lifetime components (0.23 ns and 1.15 ns) were usually caused by the trap states arising from the surface defects [45]. In other words, U-CsPbBr3 had more surface defects in the dry state, which was consistent with weak PL emission and ultra-low PLQY (0.93%). Therefore, the average PL lifetime that can be calculated according to Eq.(2) was only 0.6 ns. The wetted U-CsPbBr3 exhibited a triexponential decay curve. Obviously, the proportion of the above PL lifetime components associated with surface defects decreases significantly, and a longer PL lifetime component appeared. The wetting effect led to the temporary reduction of perovskite surface defects, so the PL emission intensity of U-CsPbBr3 was significantly increased (PLQY≈5.86%) and the average PL lifetime was also increased to 3.6 ns.
State | E1/% | τ1/ns | E2/% | τ2/ns | E3/% | τ3/ns | τavg/ns |
Dry | 54.4 | 0.23 | 45.6 | 1.15 | − | − | 0.6 |
Wet | 4.4 | 0.37 | 37.2 | 1.49 | 58.4 | 5.14 | 3.6 |
I(t)=A1e−t/τ1+A2e−t/τ2+A3e−t/τ3 |
(1) |
τavg=A1τ12+A2τ22+A3τ32A1τ1+A2τ2+A3τ3=E1τ1+E2τ2+E3τ3 |
(2) |
where τ1, τ2, τ3 are the lifetimes, A1, A2, A3 and E1, E2, E3 are constants. In addition to tetrahydrofuran, some solvents such as cyclohexanone, acetone, acetonitrile and methyl acetate (FIG. 8(a, b)) could also enable the significant fluorescence response for U-CsPbBr3, while n-hexane and isopropanol (FIG. 8(c)) could not. This may be related to the groups contained in the solvent molecule. Besides conventional acid-base ligands, the ester, carbonyl and cyanide groups were common groups for surface ligands [46, 47] of perovskite, which could passivate surface defects to some extent. When these solvents were used to moisten U-CsPbBr3, the temporary passivation of surface defects could make U-CsPbBr3 emit bright green PL. U-CsPbBr3 would return to the original PL state after the solvent volatilization. By contrast, the hydroxyl group contained in isopropanol molecule was unfriendly to perovskites and usually belonged to the category of destructive factors [48, 49]. As a general perovskite dispersion solvent, n-hexane itself did not have groups that can passivate perovskite surface defects.
The above experiments showed that U-CsPbBr3 coated on filter paper had excellent fluorescence response to some specific solvents. In order to further broaden its application range, other kinds of substrates were tested. As shown in FIG. 8(d–f), U-CsPbBr3 was coated on glass, silicon wafer and polymethyl methacrylate (PMMA), respectively. And U-CsPbBr3 could also show the same fluorescence response after being wetted by tetrahydrofuran.
After clarifying the mechanism for fluorescence response of U-CsPbBr3 to some solvents, the fluorescence response time can be controlled by the solvents with different volatility. For this purpose, we chose two solvents (tetrahydrofuran and cyclohexanone) with great difference in volatility. As a low volatile solvent, cyclohexanone was used to wet U-CsPbBr3 and the fluorescence response time lasted for up to 6 min (FIG. 8(g)). By contrast, U-CsPbBr3 returned to original PL state in about 12 s (FIG. 8(h)), if being wetted by tetrahydrofuran with high volatility. This characteristic of controlling fluorescence response time with volatility difference can not only be used to determine the type of solvents, but also for the development of molecular recognition, anti-counterfeiting materials, information encryption and decryption [32, 50].
In conclusion, we used TSA powder to successfully convert the non-fluorescent Cs4PbBr6 into 3D perovskite phase, achieving a 91% conversion yield in 8 min with the help of ultrasonic treatment. The obtained phase transformation product (U-CsPbBr3) exhibited very poor PL properties (PLQY~0.93%) due to more surface defects. Interestingly, U-CsPbBr3 was wetted by some solvents with passivation defects such as acetone, methyl acetate, tetrahydrofuran and acetonitrile, the PL properties can be temporarily improved and have bright green PL emission. The fluorescence response to solvents was repeatable, and the length of time for the fluorescence appearance can be controlled by taking advantage of differences in solvent volatility. The unique fluorescence response not related to structural changes was rare in perovskite materials, which had great application potential in anti-counterfeiting materials.
This work was supported by the National Natural Science Foundation of China (Nos. 21871243 and 51673181).
The authors declare no competing financial interest.
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State | E1/% | τ1/ns | E2/% | τ2/ns | E3/% | τ3/ns | τavg/ns |
Dry | 54.4 | 0.23 | 45.6 | 1.15 | − | − | 0.6 |
Wet | 4.4 | 0.37 | 37.2 | 1.49 | 58.4 | 5.14 | 3.6 |