Fabrication of CsPb1−xMnxBr3−2xCl2x (x = 0–0.5) quantum dots for near UV photodetector application

Ba-Duc Tran; Phuong-Nam Tran; Xuan-Thanh Bui; Duy-Hung Nguyen; Thanh-Tung Duong

doi:10.1515/gps-2022-0047

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Fabrication of CsPb_1−xMn_xBr_3−2xCl_2x (x = 0–0.5) quantum dots for near UV photodetector application

Ba-Duc Tran , Phuong-Nam Tran , Xuan-Thanh Bui , Duy-Hung Nguyen and Thanh-Tung Duong

Published/Copyright: May 23, 2022

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From the journal Green Processing and Synthesis Volume 11 Issue 1

Abstract

In this study, CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5) nanoparticles were synthesized directly in toluene solvents at high temperature. This approach results in small-size nanoparticles, which can be used in photoelectric components without adding a filtration process to eliminate high-temperature solvents such as octadecene. The high content Mn²⁺-incorporated CsPb(Cl/Br)₃ host is observed by strongly wideband emission at 592 nm of manganese d-states spin and orbital forbidden transition. After infiltration into mesoporous TiO₂, the Mn²⁺ ion receives energy from the CsPb(Cl/Br)₃ host (irradiated 405 nm light-emitting diode source) and effectively transfers to the TiO₂ scaffold layer. As a result, a metal/semiconductor/metal planar structure photodetector with m-TiO₂/CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5) composite showed several figures of merit compared to bare m-TiO₂ and m-TiO₂/CsPbBr₃ such as on/off ratio of 10⁴ times, responsivity of 1.67 A·W⁻¹, and detectivity of 4.42 × 10⁹ Jones. The key factors contributing to the growth of the on/off ratio include the decreasing dark current and enhancing exciton energy and transportation due to the infiltration of CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5) perovskite quantum dots into mesopores of the m-TiO₂ scaffold layer.

Keywords: photodetector; CsPb1–x Mn x Br3–2x Cl2x (x = 0–0.5); metal/semiconductor/metal structure

1 Introduction

All inorganic perovskite semiconductor materials recently have attracted much attention as active materials for optoelectronic devices such as solar cells [1–3], light-emitting diode (LED) [4,5], photodetector [6–9], etc. Typically, the bulk perovskite crystals exhibit poor phase stability due to the weak ion bonding nature easily leading to phase separation [10–12]. By reducing the size of crystals, the performance of nanosize semiconductor was largely improved due to reduced crystal strain resulting in their good phase stability, narrow photoluminescence (PL) emission, tunable light absorption spectrum, and high PL quantum yield in comparison with bulk counterparts. As a consequence, nanosemiconductors have shown great potential for applications not only in optoelectronic fields but also not restricted in spectral decoy for protecting space assets, photocatalyst, sensor, biosensor, etc. [13–16].

Besides reducing the particle size, replacing Pb²⁺ ions such as Mn²⁺ not only minimizes toxic lead elements but also improves optoelectronic performance. Xu et al. have shown that the doping of manganese in CsPbCl₃ improves the perovskite UV photodetector performance due to fast exciton to manganese energy transfer, long charge carrier lifetime, and the excited electrons effectively transfer to the TiO₂ scaffold layer. As a result, the self-powered UV photodetector of carbon/CsPbCl₃:Mn/FTO with photocurrent density has enhancement from 0.08 to 0.14 mA·cm⁻² and responsivity of 7.3 mA·cm⁻² at 340 nm excitation light source [17]. It requires a dissolve and recrystallization process to ensure that the nanocrystal penetrates into the bottom of the devices. He et al. also fabricated an FTO/TiO₂/CsPbBr₃:Mn/Spiro/Au, which showed a remarkable improvement in the photocurrent density of components compared to the non-doped CsPbBr₃ counterpart [18].

In this study, we introduced a one-step heating process directly in iso-octane solvent for fabrication of CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5) nanoparticles (NCs) with a small size. These particles can easily infiltrate into the mesopores of the TiO₂ scaffold layer. A metal–semiconductor–metal planar structure of UV photodetector based on TiO₂/perovskite composite presented several significant figure-of-merit parameters for evaluating, such as on–off ratio, responsivity (R), and detectivity (D*). Although the primary parameter to be considered may be different depending on the application, this result shows the potential for the UV photodetector application.

2 Experimental section

2.1 Materials

Cesium carbonate (Cs₂CO₃, Macklin, 99.9%), lead bromide (PbBr₂, Macklin, 99.9%), 1-octadecene (ODE, Macklin, >90%), oleic acid (OA, 90%), oleylamine (OAm, 80–90%), iso-octane, ethanol, toluene, and ethyl acetate (EA, >99%) were purchased from Fisher, and TiO₂ paste (Dyesol 18NR-T). All chemicals were used without any further purification. Manganese chloride tetrahydrate (MnCl₂·4H₂O, Aladdin, 99%) was dried by heating in a vacuum at 100°C.

2.2 Fabrication of CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5) quantum dots (QDs)

CsPbBr₃ and CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5) perovskite nanocrystals were fabricated via a one-pot strategy by directly heating perovskite precursors in toluene in air. First, Cs precursors were obtained by mixing 0.6 mmol of Cs₂CO₃ powder, 30 mL of octane, and 1.5 mL of OA together in a 100 mL stand-up flask and heating the mixture to 90°C in a heating agitator until all the Cs₂CO₃ powder was dissolved. The MnCl₂/PbBr₂ with different mol feed ratios were mixed with 30 mL iso-octane, 1.5 mL OA, and 3 mL OAm together in a 100 mL stand-up flask. The mixture was then heated to 110°C in a heating agitator until all the powder was dissolved. The initial solution was centrifuged at 6,000 rpm for 5 min to precipitate the large particles, and the supernatant was retained for subsequent use.

2.3 Photodetector device fabrication

The planar integrated Ti/Pt (50/200 nm) electrode is fabricated using standard photolithography to pattern the photoresist for subsequent metallization and lift-off. The electrode included 40 fingers with the channel width and length of 20 μm and 1.60 mm, respectively. The total active area was 0.128 mm².

To obtain the 2 μm-thick mesoporous-TiO₂ layers on the Ti/Pt electrode, the substrate is deep-coated with TiO₂ paste diluted in an ethanol solvent with a mass ratio of 1:3. Then, the layer was sintered under an air atmosphere at 500°C for 30 min. Finally, 1 μL of 1 mg·mL⁻¹ CsPbBr₃ or CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5) QDs solution was drop-cast directly on the m-TiO₂ layer with pre-patterned Pt electrodes and annealed at 80°C for 30 min in a vacuum tube for the solvent evaporation.

2.4 Characterization techniques

The surface morphology and chemical composition of obtained samples were characterized by transmission electron microscopy (TEM, JEOL-JEM 1010, Japan), field emission scanning electron microscopy (FE-SEM) coupled with Energy-dispersive X-ray spectroscopy (EDS), (JSM-7600F, Jeol), respectively. The crystalline structure of samples was analyzed by powder X-ray diffraction (XRD, Rigaku D/MAX-2500/PC) using CuKα radiation (λ = 0.154 nm) operated at 40 mA tube current. PL properties of all samples were investigated by using a PL spectrophotometer (Nanolog, Horiba Jobin Yvon) equipped with a 450 W xenon discharge lamp as the excitation source. The photoresponse was detected by Keithley 4200-SCS, America, coupled with a 405 nm UV LED source.

3 Results and discussion

CsPbBr₃ and CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5) perovskite nanocrystals have been fabricated simply by mixing the precursors Cs₂CO₃, PbBr₂, MnCl₂, and OLA, OA in iso-octane solvents and heating. Although there is no direct evidence of the replacement of Mn²⁺ with Pb²⁺ ions in crystals, PL, X-ray, EDS, and PL spectral measurements show their presence in the crystal structure. As shown in Figure 1a, by increasing the MnCl₂ to PbBr₂ mol feed ratio from 0:1 to 1:1, the narrow emission of CsPb(Cl, Br)₃ host crystals was strongly blue-shifted from 520 to 440 nm due to the replacement of Cl^– to Br^– ions in the host crystals. Besides, a broadband emission centered at 592 nm is assigned to the Mn²⁺ ions doped in the CsPb(Cl/Br)₃ host NCs, which can be attributed to the transition from ⁴T₁ to ⁶A₁ energy levels of the Mn²⁺ 3d states [17]. With the decrease of CsPb(Cl, Br)₃ emission, the strong 592 nm emission at high Mn content indicated that Mn²⁺ can act as an effective energy acceptor of the excited CsPb(Cl/Br)₃ host. Figure 1b and c shows the optical absorption and PL of CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5) with 0.6:1 and 1:1 MnCl₂/PbBr₂ mol feed ratios of precursors, respectively. The optical absorption curve revealed that CsPb(Cl/Br)₃:Mn²⁺ had a large absorbance in the UV, and visible spectral region with band edges started at the first narrow emission band of CsPb(Cl/Br)₃ host.

Figure 1

(a) The PL spectra of CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5) nanocrystals synthesized directly in iso-octane solvent at 110°C with different MnCl₂ to PbBr₂ mol feed ratios. (b and c) The optical absorption and PL of CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5) with 0.6:1 and 1:1 MnCl₂/PbBr₂ mol feed ratios of precursors, respectively.

The XRD patterns of CsPbBr₃ and CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5) NCs are shown in Figure 2. It can be seen that the as-synthesized CsPbBr₃ NCs have a cubic structure (JCPDS No. 54-0752) with the 2θ peaks at 21.1, 30.2, 34.2, 36.1, and 44.9°, corresponding to (110), (200), (211), (210), and (202) planes, respectively. A detailed view of the (211) and (220) peak position showed that a peak shifted toward the larger theta angle as MnCl₂ content increases. The difference in ion radius between [Pb²⁺ (1.19 A°), Br⁻ (0.196 A°)] and [Mn²⁺ (0.8 A°), Cl⁻ (0.175 A°)] is the original of the peak shift. Consequently, the shift indicated the incorporation of MnCl₂ in the CsPbBr₃ host. However, the main perovskite peaks disappear, and several unknown peaks exist with the further increased MnCl₂ content (MnCl₂/PbBr₂ mol feed ratio up to 1.2).

Figure 2

The XRD pattern of CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5) NCs with different MnCl₂ to PbBr₂ mol feed ratios.

It is well known that temperature and reaction time are important parameters for controlling the size of nanoparticles [19]. Generally, low temperature and fast reaction time can make small size of nanocrystals. Figure 3 shows the TEM image of the CsPbBr₃ and CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5) nanocrystals after fabrication at 100°C and reaction time at 30 s. The nanocrystals are in the cubic shape with a size of about ∼7 and ∼5 nm, respectively (Figure 3a and c). It is much smaller than the mean size of the mesopores in the m-TiO₂ layer (Figure A1), ensuring them deep infiltration into the mesoporous layer. The insets of Figure 3a and c show the size distribution and photos of dried nanocrystal films with strongly bright green and orange-red color in ambient daylight. Samples analyzed by EDX measurements showed a Cs:Pb:Br ratio of 1:1:3 for CsPbBr₃ NCs and the Mn²⁺/Pb²⁺ ratio of CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5) ∼0.9:1 for the MnCl₂/PbBr₂ ∼1:1 mol feed ratio (Figure 3b and d). Further increasing MnCl₂ content sharply decreased the PL intensity (not shown here) due to the changing of the crystal structure as described in the above XRD results.

Figure 3

SEM images and EDX spectra of (a and b) CsPbBr₃ and (c and d) CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5) nanocrystals.

The temperature-dependent PL study provides information about the physical properties of the nanocrystals. Figure 4a and c shows the temperature-dependent PL spectra of CsPbBr₃ and CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5) NCs as prepared. Photos of two samples placed in a cooling chamber irradiated with a 405 nm laser source show a strong green light of CsPbBr₃ and a bright red light of CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5) nanocrystals, respectively. As expected, the peaks are blue shifted due to the thermal expansion of the crystal leading to the forbidden gap increase, which are consistent with the previous reported results [20]. For the CsPbBr₃ QDs, the PL spectrum separates into two peaks: a main peak (from 515 to 505 nm according to temperatures between 10 and 300 K) and a small peak at longer wavelengths due to heavy hole–electron and light hole–electron transitions [20]. The PL intensity quickly decreases with increasing temperature. For the CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5) QDs, the PL spectra show only one peak, and the peak shifted from 610 to 590 nm when the ambient temperature increased from 10 to 300 K. In particular, the optical intensity of the sample is maintained above 80% when the temperature rises to 300 K. The activation energy is extracted by plotting the relationship between the integral PL intensity and the measured temperature, as shown in Figure 4b and d. The activation energy of samples can be deduced with the following equation [21]:

(1) I ( T ) = I 0 / ( 1 + A e − E B / ( k B T ) )

where I ₀ and I(T) represent the intensity of the NCs at the 0 K temperature and the testing temperature, respectively. A is a constant and k is Boltzmann’s constant (8.62 × 10⁻⁵ eV·K⁻¹). According to the Arrhenius equation, the activated energy values reached 40 and 120 meV for the CsPbBr₃ and CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5), respectively. The high E _B value of CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5) ensures that the excited state of Mn²⁺ luminescent energy levels can be able to maintain above room temperature for their potential applications in optoelectronic applications.

Figure 4

Temperature-dependent PL spectra and PL intensity versus inverse temperature and Arrhenius fit of CsPbBr₃ NCs (a and b) and CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5) (c and d).

In order to demonstrate the carriers charge transfer between Mn²⁺ in perovskite NCs and mp-TiO₂ scaffold layer, the PL spectrum and decay curve of QDs on mp-TiO₂ and aluminum foil substrate were measured (Figure 5). As shown in Figure 5a, the PL intensity of CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5) QDs/mp-TiO₂ was reduced by a 3.5-time magnitude compared to that of the QDs on aluminum foil substrate. Moreover, the radiative lifetime decreases from 1.54 ms to 80 µs for the CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5) in m-TiO₂ (Figure 5b). It strongly indicates that mp-TiO₂ can extract charge carriers from the CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5) QDs.

Figure 5

(a) PLE/PL spectra and (b) PL decay curves of CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5) NCs.

For the UV photodetector measurement, three samples of m-TiO₂, m-TiO₂/CsPbBr₃, and m-TiO₂/CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5) on the pre-patterned Pt electrodes were tested as shown in Figure A2. Two probes I–V were measured in the dark and under illumination by using a 405 nm UV-LED chip (3 mW·cm⁻²). Figure 6a and b shows the I–V curves of three samples under dark and near UV irradiation. For the m-TiO₂ sample, the dark current was high with hysteresis due to H₂O, O₂ absorption, and catalyst activity of TiO₂ or Pt electrode materials for water-splitter reaction, as well as a different work function between TiO₂ semiconductor and Pt metal electrode [22]. By introducing UV light to their layer, the excited electron of the TiO₂ semiconductor was dominant leading to the increase of the current and the hysteresis disappeared. In particular, by infiltration of perovskite QDs into the mesopore of m-TiO₂, dark currents have plummeted, while photocurrents have increased markedly. Figure 6c shows the corresponding current on/off ratios of three devices at 1.5 V bias voltage, and it is stable at values of ∼3.5, 10², and 10⁴ times for m-TiO₂, m-TiO₂/CsPbBr₃, and m-TiO₂/CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5), respectively. Two important parameters of the device, the sensitivity I and detection index (D*), can be obtained from the following equations [23]:

(2) R = I ph / P l ight

(3) D ∗ = R / 2 q I dark

where I _ph is the photocurrent, P _light is the light power intensity (3 mW·cm⁻²), I _dark is the dark current, and q is the elementary charge (Coulomb). The highest values of R and D* are 1.67 A·W⁻¹ and 4.42 × 10⁹ Jones, respectively, for the m-TiO₂/CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5) sample. This result shows the potential for the UV photodetector application.

Figure 6

Logarithmic I–V curves of planar structure photodetector based on (a) m-TiO₂, (b) m-TiO₂/CsPbBr₃ and m-TiO₂/CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5) composite films in the dark and NUV light irradiation. (c) Photocurrent–time response measured in the dark and under illumination under 1.5 V bias.

4 Conclusions

In conclusion, CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5) nanocrystals have been fabricated by the one-pot heating directly in toluene solvent method. The small crystals were directly infiltrated into m-TiO₂ scaffold layer without further washing process. The Mn²⁺ effectively received energy from CsPb(Cl/Br)₃ host and transferred to m-TiO₂ scaffold layer resulting in enhancement of UV photodetector performance. As a consequence, a metal/semiconductor/metal planar structure photodetector with m-TiO₂/CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5) composite showed several figures of merit compared to bare m-TiO₂ and m-TiO₂/CsPbBr₃ such as on/off ratio of 10⁴ times, responsivity of 1.67 A·W⁻¹, and detectivity of 4.42 × 10⁹ Jones. This result shows the potential for the UV photodetector application.

Funding information: This research is funded by the Hanoi University of Science and Technology (HUST) under project number T2020-SAHEP-037.
Author contributions: Ba-Duc Tran: methodology, investigation; Phuong-Nam Tran: writing – original draft; Xuan-Thanh Bui: methodology; Duy-Hung Nguyen: writing – review and editing; Thanh-Tung Duong: conceptualization, writing – editing.
Conflict of interest: Authors state no conflict of interest.

Appendix

Figure A1

(a–c) The SEM images of patterned Pt electrode-coated mp-TiO₂.

Figure A2

(a and b) The SEM cross-section images of mp-TiO₂ before and after perovskite QD infiltration. (c) EDS spectrum of CsPb_1–xMn_xBr_3–2xCl_2x (x = 0.5)-coated m-TiO₂ sample.

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Received: 2022-02-07

Revised: 2022-03-19

Accepted: 2022-03-30

Published Online: 2022-05-23

This work is licensed under the Creative Commons Attribution 4.0 International License.

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https://doi.org/10.1515/gps-2022-0047

Keywords for this article

photodetector; CsPb1–x Mn x Br3–2x Cl2x (x = 0–0.5); metal/semiconductor/metal structure

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Fabrication of CsPb1−xMnxBr3−2xCl2x (x = 0–0.5) quantum dots for near UV photodetector application

Article

Abstract

1 Introduction

2 Experimental section

2.1 Materials

2.2 Fabrication of CsPb1–x Mn x Br3–2x Cl2x (x = 0–0.5) quantum dots (QDs)

2.3 Photodetector device fabrication

2.4 Characterization techniques

3 Results and discussion

4 Conclusions

Appendix

References

Articles in the same Issue

Articles in the same Issue

Articles in the same Issue

Fabrication of CsPb_1−xMn_xBr_3−2xCl_2x (x = 0–0.5) quantum dots for near UV photodetector application

2.2 Fabrication of CsPb_1–xMn_xBr_3–2xCl_2x (x = 0–0.5) quantum dots (QDs)