Optimizing CsPbBr₃ nanowires for high-performance optoelectronics: focusing on blue shift and superfast kinetics through amine-rich synthesis

Abstract

In this study, we successfully synthesized high-purity CsPbBr₃ perovskite nanocrystals (NCs) and nanowires (NWs) using a hot-injection method within an amine-rich environment, followed by a detailed analysis of their structural and optical properties. By carefully tuning the ratios of oleylamine (OAm) and octylamine (OctAm), as well as optimizing reaction temperature and time, we achieved enhanced morphology and photoluminescence characteristics of the products. The results indicate that increasing the amine content reduces the nanowire thickness and improves crystallinity, yielding NWs with an approximate diameter of 3 nm and NCs with a uniform size distribution of 9.7 ± 0.2 nm. X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM) confirmed that the CsPbBr₃ nanostructures exhibit a pure orthorhombic phase. Photoluminescence (PL) and UV-vis absorption analyses revealed narrow emission peaks at 520 nm and 465 nm for NCs and NWs, respectively, with the NWs showing a pronounced blue shift and a primary exciton absorption peak at 450 nm, indicating a strong quantum confinement effect. Time-resolved photoluminescence spectroscopy (TRPL) measurements showed an average exciton lifetime of 15.29 ns for NWs, which is notably longer than the 10.55 ns observed for NCs. Femtosecond transient absorption spectroscopy (fs-TA) further demonstrated significant differences in ground-state bleach (GSB) dynamics between the nanostructures, with NWs reaching peak bleach at 9.32 ps compared to 6.16 ps for NCs. These findings highlight the slower carrier recombination rate in NWs, which enhances quantum confinement effects. This work provides both theoretical and experimental insights into the potential application of one-dimensional perovskite nanostructures in high-efficiency optoelectronic devices.

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1. lntroduction

Lead halide perovskite materials have attracted widespread attention in the optoelectronic field.^1,2 Their superior luminous efficiency,³ high quantum yield,⁴ and unique ability to control size and morphology⁵ make them important candidate materials for applications in optoelectronic emission,^3,6 photovoltaics,⁷ and lasers,⁸ among others. Perovskite nanocrystals (NCs), owing to their defect tolerance within the crystal lattice structure,⁹ can dynamically tune their bandgap through the chemical regulation of halide anions,¹⁰ making them a versatile optoelectronic material. These materials can be synthesized at relatively low cost and temperature,¹¹ and their absorption and emission spectra can be modulated by adjusting the quantum dot size, allowing for enhanced quantum confinement effects.^12,13 However, the conventional synthesis and application of perovskite NCs face challenges in stability and morphology control. For NCs with strong quantum confinement, maintaining optical uniformity and enhancing stability through effective size control remain critical issues.¹⁴

In perovskite NCs, the quantum confinement effect is a key factor influencing their optical property. By confining electron and hole wave functions at the nanoscale, quantum confinement substantially alters the bandgap and optical absorption characteristics of the NCs.¹⁵ Recently, researchers have succeeded in synthesizing highly size-controlled CsPbBr₃ NCs using an equilibrium approach,¹⁶ achieving spectral narrowing and manipulation of bright and dark exciton states.^17,18 However, despite these advancements granting perovskite NCs broad application potential in optoelectronic devices, most existing studies have focused on two-dimensional nanosheets^19–23 and three-dimensional NCs,^24–30 with only a limited number of systematic studies on the synthesis of one-dimensional nanowires (NWs) and nanorods.^31–36 For example, in 2023, Shin et al. proposed a biphasic passivation strategy that successfully synthesized all-inorganic perovskite NWs with minimal surface defects, significantly enhancing their photoluminescence quantum yield (PLQY), carrier lifetime, and water stability.³³ In the same year, Liang et al. introduced a universal platform based on cylindrical single-molecule nanoreactors, enabling precise control over the size, composition, and stability of one-dimensional perovskite nanorods.³⁴

One-dimensional CsPbBr₃ nanostructures, such as NWs and nanorods, exhibit unique anisotropy and stronger quantum confinement effects, making them promising candidates for applications in lasers, single-photon emitters, and quantum computing.³⁷ However, their synthesis remains challenging, with key issues including: (1) how to precisely control the diameter and morphology of NWs, (2) how to enhance their optical stability, and (3) how to optimize synthesis conditions to improve their luminescence properties.³⁸ Given the significant uncertainties surrounding the size-dependent optical properties of perovskite NWs, further investigations into their structure–property relationships are crucial for achieving commercial applications.

To address these challenges, this study employs a hot-injection synthesis strategy in an amine-rich system, optimizing the ratio of oleylamine (OAm) to octylamine (OctAm), reaction temperature, and reaction time to achieve precise control over the morphology of CsPbBr₃ NCs and NWs. Experimental results demonstrate that this method not only significantly enhances the crystallinity of NWs but also improves their photoluminescence properties, exhibiting longer exciton lifetimes and slower carrier recombination rates compared to NCs. The findings of this study provide new theoretical and experimental insights for the application of one-dimensional perovskite NWs in high-performance optoelectronic devices.

2. Results and discussion

To explore the synthesis of CsPbBr₃ nanowires (NWs) and investigate the photoluminescence properties of the resulting products, this study employs a hot-injection synthesis strategy in an amine-rich system, using different ratios of oleylamine (OAm) and octylamine (OctAm) as organic ligands. The synthesis protocol was based on the method described by Di Stasio et al.,³⁹ with specific modifications introduced to enhance luminescent performance. For a comparative analysis of the optical properties, CsPbBr₃ nanocrystals (NCs) were also synthesized under amine-rich conditions. The synthesis process, outlined in Fig. 1, involved initially mixing the PbBr₂ precursor with the non-coordinating solvent octadecene (ODE) in a flask. After degassing for a period, ligand reagents in varying proportions were added. Different nanostructures were obtained by carefully controlling the reaction temperature and time (details of the synthesis steps are provided in the ESI†).

Fig. 1 Schematic illustration of the synthesis of CsPbBr₃ NCs and CsPbBr₃ NWs.

To explore nanowire synthesis, we initially considered strategies for reducing kinetic rates in an amine-rich system. At an initial reaction temperature of 120 °C, a series of CsPbBr₃ perovskite nanosheet structures were synthesized using varying amounts of amines. As shown in Fig. S1(a–c) (ESI†), with an increasing amount of oleylamine, the thickness of the nanosheets decreases, while their lateral size increases. In contrast, in the control group Fig. S1(d) (ESI†), the addition of extra octylamine does not significantly affect the thickness of the nanosheets compared to S1(c) (ESI†), but it notably increases their lateral size and improves their crystallinity. Next, we examined the effect of temperature on the synthesized nanostructures. As depicted in Fig. 2(a) and Fig. S2 (ESI†), lowering the synthesis temperature led to a progression from NCs to nanosheets, ultimately resulting in amorphous nanoclusters. Finally, we studied the impact of reaction time on nanowire morphology (Fig. S3) (ESI†). With extended reaction time, the NWs evolved from low crystallinity to higher crystallinity and eventually became more disordered, with additional small CsPbBr₃ NCs appearing. We also investigated the volatility of OctAm under low vacuum conditions. When an equal volume of OAm and OctAm was pre-added before degassing, the resulting NWs exhibited poor crystallinity, numerous defects, and a broad size distribution. The products obtained in a pure OAm system are amorphous nanoclusters (Fig. S2(c), ESI†). Subsequently, by adding OctAm and adjusting the molar ratio of OAm to OctAm (1 : 1, 1 : 1.5, 1 : 2), products with different ratios were obtained, and the TEM images are shown in Fig. S4 (ESI†). When the molar ratio of OAm to OctAm is 1 : 1, the reaction kinetics are relatively slow, and it is difficult to form crystals with distinct edges. When the molar ratio of OAm to OctAm is adjusted to 1 : 1.5 (Fig. 3(a)), well-formed nanowire structures can be produced. As the OctAm content increases, and the molar ratio of OAm to OctAm reaches 1 : 2, the reaction kinetics accelerate. Although nanowire structures can form, the faster reaction rate makes it challenging to fully control the uniformity of the products, with some forming large impurity phases. Therefore, OctAm plays a crucial role in the synthesis of NWs.³³

Fig. 2 TEM (a) and HRTEM (b) images of CsPbBr₃ NCs, with the magnified image in the upper right corner of (b) corresponding to the red boxed area. (c) Size distribution histogram of CsPbBr₃ NCs. (d) XRD pattern of CsPbBr₃ NCs. (e) STEM image of CsPbBr₃ NCs and the corresponding elemental mapping for Cs (yellow), Pb (purple), and Br (red). Scale bars are 20 nm.

Fig. 3 TEM (a) and HRTEM (b) images of CsPbBr₃ NWs, with the magnified image in the upper right corner of (b) corresponding to the red boxed area. (c) Size distribution histogram of CsPbBr₃ NWs. (d) XRD pattern of CsPbBr₃ NWs. (e) STEM image of CsPbBr₃ NWs and the corresponding elemental mapping for Cs (yellow), Pb (purple), and Br (red). Scale bars are 50 nm.

To investigate the structure of the synthesized CsPbBr₃ NCs, we conducted high-resolution transmission electron microscopy (HRTEM) analysis. As shown in Fig. 2(a), CsPbBr₃ NCs synthesized by direct hot injection exhibit a uniformly distributed state, with no significant aggregation or uneven dispersion. The size distribution of the NCs is very uniform, with regular shapes, no obvious defects, and no other impurity phases (such as nanosheets). These results indicate that the CsPbBr₃ synthesized using our modified method has a very high purity. The local HRTEM image (Fig. 2(b)) reveals lattice spacings of 0.58 nm and 0.41 nm, corresponding to the (11̄0) and (200) planes of CsPbBr₃. The fast Fourier transform (FFT) shown in Fig. S5(b) (ESI†) reveals two distinct diffraction spots when observed along the [0,0,1] direction. The two clearest diffraction spots are A (OA = 3.41 nm⁻¹, corresponding to the (2,2̄,0) plane) and B (OB = 2.41 nm⁻¹, corresponding to the (2,0,0) plane). The angle between A and B (∠AOB) is 45°, respectively. Fig. 2(c) shows a size distribution of 9.7 ± 0.2 nm for the NCs, highlighting their uniform emission wavelength and electronic structure.¹⁷ For further structural analysis, X-ray diffraction (XRD) was employed. The primary distinction between the orthorhombic and cubic phases of CsPbBr₃ lies in the presence of a double peak around 30°, which is clearly observed in Fig. 2(d), confirming that the synthesized CsPbBr₃ NCs are indeed in the orthorhombic phase. The diffraction peaks at 21.4°, 30.3°, and 30.6° correspond to the (112), (004), and (220) planes of orthorhombic γ-CsPbBr₃ NCs, consistent with the reference JCPDS #97-009-7851.³¹ High-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) was used to perform elemental mapping, confirming the presence and uniform distribution of Cs, Pb, and Br within the CsPbBr₃ NCs (Fig. 2(e)).

We also examined the crystal structure of the CsPbBr₃ NWs. Fig. 3(a) shows the directly synthesized NWs, which tend to adhere to one another and are distributed in a crossed arrangement. No impurities, such as NCs, were observed, indicating high purity and uniform morphology of the product. A local HRTEM image of the NWs (Fig. 3(b)) reveals lattice spacings of 0.59 nm and 0.41 nm, corresponding to the (002) and (11̄2) planes of CsPbBr₃, respectively, and indicating that the NWs grow along the [001] crystallographic direction. The fast Fourier transform (FFT) shown in Fig. S5(d) (ESI†) reveals two distinct diffraction spots when observed along the [1,1,0] direction. The two clearest diffraction spots are A (OA = 3.36 nm⁻¹, corresponding to the (0,0,2) plane) and B (OB = 2.45 nm⁻¹, corresponding to the (1,1̄,0) plane). The angle between A and B (∠AOB) is 45°. Fig. 3(c) shows that the nanowire diameters are approximately 3 nm. XRD analysis was conducted to provide additional structural information for the NWs. In Fig. 3(d), the diffraction peaks of the directly synthesized CsPbBr₃ NWs align with those observed for the NCs, confirming that the NWs also possess the orthorhombic γ-CsPbBr₃ crystal structure. HAADF-STEM elemental mapping analysis further verified the presence and uniform distribution of Cs, Pb, and Br within the NWs (Fig. 3(e)).

Fig. 4 explains the growth principles of NCs and NWs. Fig. 4(a) describes the growth strategy of the NCs as anisotropic growth, where the growth rate on each crystal face differs. Combined with high-resolution images (such as Fig. 2(b)) and other information, it can be inferred that CsPbBr₃ NCs are primarily terminated with {110} and {002} crystal planes.

Fig. 4 Schematic illustration of the microscopic formation mechanism of (a) CsPbBr₃ NCs and (b) CsPbBr₃ NWs.

Due to the relatively low reaction temperature and the amine-rich environment with OAm and OctAm, CsPbBr₃ monomers form gradually only at the onset of the reaction. The reduced reaction kinetics allow for the maintenance of a high monomer concentration throughout the process, providing sufficient monomeric units to support the slow axial growth of the NWs.⁴⁰ As shown in Fig. 4(b) and the high-resolution image in Fig. 3(b), the NWs grow slowly along the [001] crystallographic direction. Meanwhile, there is minimal change in the radial direction perpendicular to the growth axis, indicating stable and controlled axial growth.

To analyze the optical properties of the synthesized NCs and NWs, we conducted steady-state photoluminescence (PL) spectroscopy, UV-visible absorption spectroscopy (UV-vis), and time-resolved photoluminescence (TRPL) spectroscopy measurements. The steady-state PL spectrum and UV-vis absorption spectrum of the NCs (Fig. 5(a)) show a prominent first exciton absorption peak at 505 nm and a narrow PL emission peak at 520 nm. The UV-vis absorption spectrum and steady-state photoluminescence spectrum of the NWs (Fig. 5(b)) exhibit a strong first exciton absorption peak at 450 nm, a broader photoluminescence emission peak at 465 nm, and a shoulder peak at 480 nm. In the PL spectrum, the shoulder peak has two possible origins: one is a redshift caused by the exciton delocalization due to the aggregation and entanglement of the NWs,⁴¹ and the other is the combined contribution of subpopulations of NWs with different diameters.⁴² To explore the origin of the shoulder peak, the UV-vis absorption and steady-state PL spectra of the sample diluted 20 times were tested (Fig. S6, ESI†), and a noticeable decrease in the shoulder peak was observed. These results indicate that the shoulder peak is closely related to the entanglement and aggregation state of the NWs.³⁹ The NCs and NWs synthesized under varying conditions exhibit distinct exciton absorption and emission characteristics. As the synthesis temperature decreases, synthesis products show a blue shift in their absorption and emission peaks. This blue shift is attributed to the strong quantum confinement effect, which arises from reduced particle sizes due to decreased thermodynamic equilibrium and slowed reaction kinetics at lower temperatures, leading to a wider bandgap.⁴³

Fig. 5 (a) Normalized absorption and photoluminescence spectra of CsPbBr₃ NCs and (b) thin CsPbBr₃ NWs. Inset: Optical photographs of the corresponding samples under ambient light (AL) and UV light illumination. (c) Time-resolved photoluminescence decay curves of CsPbBr₃ NCs (green dots) and CsPbBr₃ NWs (blue dots). (d) Schematic illustration of the luminescence mechanism of CsPbBr₃ NCs and NWs.

Fig. 5(c) presents the TRPL decay curves for CsPbBr₃ NWs and CsPbBr₃ NCs. The photoluminescence lifetimes, derived from fitting the decay curves using an exponential decay model (eqn (1) and (2)), are listed in Table S1 (ESI†). These fitted values provide insights into the exciton dynamics and recombination processes in the CsPbBr₃ nanostructures:⁴⁴

I(t) = A₁e^−t/τ₁ + A₂e^−t/τ₂ (1)

τ_ave = (A₁τ²₁ + A₂τ²₂ +)/(A₁τ₁ + A₂τ₂) (2)

The time-resolved photoluminescence spectra (Fig. 5(c)) reveal distinct exciton lifetimes and varying contributions of each exciton lifetime component. In CsPbBr₃ materials, photo-luminescence decay is primarily due to the recombination of photogenerated carriers, with exciton recombination being the main contributor. In Table S1 (ESI†), τ₁ represents the short-lived nonradiative recombination lifetime, while τ₂ corresponds to the exciton recombination lifetime within the carrier recombination process.⁴⁵ The NWs tested exhibit an enhanced exciton lifetime (A₂%) that is 6% higher than that of the NCs. We also conducted PLQY tests on the samples, as shown in Fig. S7 (ESI†). In Fig. S7 (ESI†), the PLQY of the NCs (76%) is higher than that of the NWs (42%). This is because NWs, in constrained structures, are more prone to bending, leading to more surface defects compared to NCs. The higher PLQY of NCs does not necessarily imply that their fluorescence lifetime is superior to that of NWs. Due to the defect effects, NWs have a lower surface-to-volume ratio compared to NCs, which results in a smaller impact of surface defect states on exciton recombination. As a result, the fluorescence lifetime of NWs is longer than that of NCs. In addition, NWs and NCs exhibit significant differences in size and dimensional effects. NWs, with their one-dimensional structure, provide a longer drift path for excitons. The smaller diameter of the NWs induces a stronger quantum confinement effect, which significantly enhances the exciton binding energy and suppresses non-radiative recombination, thereby prolonging the exciton lifetime.⁴⁵ In contrast, NCs, with their larger particle size in a three-dimensional structure, exhibit weaker quantum confinement effects and shorter exciton drift paths, leading to shorter exciton lifetimes.⁴⁶Fig. 5(d) reveals differentiated fluorescence emission characteristics under a 365 nm excitation light source: the fluorescence emission wavelength of the NCs is 520 nm, while that of the NWs is 465 nm.

To investigate the fine structure of the energy bands in the synthesized nanostructures, we utilized femtosecond transient absorption (fs-TA) spectroscopy to explore the ultrafast dynamics of carrier recombination. Excitation was performed at a pump wavelength of 355 nm with a power density of 6.4 μJ cm⁻², detecting changes in absorbance across a wavelength range of 350 nm to 650 nm, with the results presented in Fig. 6. From Fig. 6(a–c) and (c–f), it can be observed that all samples exhibit three distinct features in their transient absorption spectra under the same pump intensity. The NWs display a positive photogain absorption (PA) band between 400 nm and 420 nm, while the NCs show this feature in the 450 nm to 480 nm range (denoted as PA₁). Additionally, both the NWs and NCs exhibit ground state bleaching (GSB) peaks, with the NWs peaking at approximately 455 nm and the NCs at around 505 nm. A second positive photogain absorption band, denoted as PA₂, emerges for the NWs within the range of 480 nm to 510 nm, and for the NCs within the range of 550 nm to 570 nm. The PA₁ signal has been reported in other literature on transient absorption spectra and is attributed to the activation of forbidden transitions within the NCs under laser excitation. Specifically, the photogenerated electron–hole pairs break the spatial symmetry, thereby violating the optical selection rules for transitions. This allows the originally forbidden optical transitions—from the valence band edge to the second conduction band level, and from the second valence band level to the conduction band minimum—to become optically allowed. This explains why the PA₁ signal is situated between the first and second exciton absorption peaks in the absorption spectrum.⁴⁷ The ground state bleaching observed at PB is caused by the filling of low-energy states at the band edge, corresponding to the first exciton absorption peak in the steady-state absorption spectra shown in Fig. 5(a and b).⁴⁸ The red shift of the signal at PA₂ can be attributed to the transient Stark effect caused by the Coulomb interaction between hot excitons and band-edge excitons.⁴⁹ It is currently known that ΔA is proportional to the exciton density in the lowest excited state. By analyzing the data differences in Fig. S8 (ESI†) and Table S2 (ESI†), it can be observed that the exciton annihilation rate is faster in the NCs. Over the delay time range from 2 ps to 1000 ps, we observe that the signal intensity of the two characteristic peaks, PA₂ and PB, decreases synchronously as the delay time increases, because the absorbance essentially returns to the initial steady state when the electrons relax back to the ground state. The NWs reach the peak absorption of PA₁ at 9.32 ps, while the NCs reach their peak much faster, at 6.16 ps. The fs-TA results indicate that the decay time of the GSB and positive PA signals in the NWs is significantly longer than in the NCs. This is attributed to the slower exciton capture and recombination rates in the NWs, as well as their lower defect density and higher defect tolerance.⁵⁰

Fig. 6 (a) and (b) Time-resolved transient absorption spectra of perovskite nanowires at different delay times. (c) 2D contour plot of the transient absorption spectra for perovskite nanowires. (d) and (e) Time-resolved transient absorption spectra of perovskite nanocrystals at different delay times. (f) 2D contour plot of the transient absorption spectra for perovskite nanocrystals.

3. Conclusions

In this study, we successfully synthesized high-purity, highly crystalline CsPbBr₃ nanocrystals (NCs) and nanowires (NWs) using an optimized hot-injection method. These nanostructures exhibited marked differences in their optical properties. CsPbBr₃ NWs demonstrated an average exciton lifetime of 15.29 ns, significantly longer than the 10.55 ns observed in NCs, indicating a lower density of defect states and higher luminescence efficiency. The emission peak for NWs at 465 nm shows a notable blue shift compared to the 520 nm emission of NCs, underscoring a stronger quantum confinement effect resulting from controlled size. Transient absorption analysis revealed that the ground-state bleach recovery time for NWs was 9.32 ps, compared to 6.16 ps for NCs, suggesting a longer photoluminescence lifetime and superior defect tolerance in NWs. These properties highlight the potential advantages of CsPbBr₃ NWs for optoelectronic applications, confirming the critical role of an amine-rich synthesis environment in tuning the structure and performance of perovskite NCs. This work establishes a solid foundation for developing efficient and stable perovskite materials for next-generation optoelectronic devices.

Author contributions

Junwei Zhou: data curation, formal analysis, investigation, visualization, writing – original draft. Xiaohu Zhao: visualization. Yanchen Jiang: visualization. Qingyuan Zhou: visualization. Yusheng He: visualization. Jiaxin Rui: visualization. Jianhui Sun: visualization. Kai Pan: conceptualization, methodology, funding acquisition, project administration, resources, supervision, writing – review & editing.

Data availability

The data supporting this article have been included as part of the ESI.†

Conflicts of interest

There are no conflicts to declare.

Acknowledgements

This work was financially supported by the National Natural Science Foundation of China (21473051), and the Start-up Fund of Changzhou University.

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Footnote

† Electronic supplementary information (ESI) available. See DOI: https://doi.org/10.1039/d4tc05078a

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