Efficient and Stable Perovskite Photodetectors Based on Thiocyanate

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Letter

Efficient and Stable Perovskite Photodetectors Based on Thiocyanate Assisted Film Formation Yingli Chu, Yantao Chen, Jiachen Zhou, Bilei Zhou, and Jia Huang ACS Appl. Mater. Interfaces, Just Accepted Manuscript • DOI: 10.1021/acsami.9b01715 • Publication Date (Web): 08 Apr 2019 Downloaded from http://pubs.acs.org on April 8, 2019

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ACS Applied Materials & Interfaces

Efficient and Stable Perovskite Photodetectors Based on Thiocyanate Assisted Film Formation Yingli Chu†, Yantao Chen†, Jiachen Zhou†, Bilei Zhou† and Jia Huang*,†,‡

†Interdisciplinary Materials Research Center, School of Materials Science and Engineering, Tongji

University, Shanghai, 201804, P. R. China

‡Putuo

District People's Hospital, Tongji University, Shanghai, 200060, P. R. China

KEYWORDS: organometal halide perovskite, lead thiocyanate, photodetector, long-term stability

ABSTRACT: Thiocyanate-based perovskite (SCN-PVSK) photodetectors have been fabricated by introducing lead thiocyanate precursor. Incorporating SCN groups into CH3NH3PbI3 can significantly improve the device stability in air. Compared with pure CH3NH3PbI3 films, SCNPVSK films have larger grain size and reduced trap states. The perovskite layers can be prepared by a simple solution method in air. Solvent effects on the crystallization of SCN-PVSK films have also been investigated. It is found that highly uniform, pinhole-free perovskite films can be obtained utilizing the N,N-dimethylformamide (DMF) solution of Pb(SCN)2. The SCN-PVSK based photodetectors performed a high responsivity of 12.3 A/W and a decent detectivity over 1.3×1013 Jones. More important, the SCN-PVSK based two-terminal photodetectors, without

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encapsulation, have shown great stability with 92% of the initial photocurrent being retained after storage in air (relative humidity > 50%) for 10 days, while the value is only 10% for pure CH3NH3PbI3 devices tested under the same conditions.

Offering advantages of excellent light absorption property and high carrier transport performance, organometal halide perovskites (OHPs) have received enormous scientific attention for promising applications in solar cells, photodetectors and light emitting diodes , and many research achievements have been made in this field.1-4 Taking solar cell based on these perovskites as an example, the power conversion efficiency (PCE) of which has been raised from 3.8% to 22.7% in only ten years,.5-6 Besides this, photodetectors, the fundamental elements for many optoelectronic applications, , have been further developed with these perovskites, targeting higher performance, such as higher responsivity, detectivity and photoelectric transformation efficiency.79

The OHP-based photodetectors with high optoelectronic performance, such as a broad

photoresponse range and fast response speed, have been carried out.10-13 However, the structure of -PbX3 easily decomposes with moisture due to its low formation energy, which becomes one of the biggest obstacles for OHP-based devices toward commercial viability.14, 15 To improve the stability of OHP materials, one of the feasible methods is to introduce mixed cations or halides into the neat perovskite, which assists the film formation and results in less trap density in the perovskite materials.11, 16-18 Michael et al. introduced a small amount cesium (Cs) into organic perovskite to form a triple Cs/MA/FA cation perovskite, thus perovskite seeds were


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added at room temperature, which in turn became nucleation sites and uniform grains were obtained.19 The solar cells based on the triple cation perovskite achieved a decent PCE of 21.1% and 18% after 250 h of storage in the glove box. Xu et al. used two thiocyanate ions (SCN¯) to replace two iodides in CH3NH3PbI3, which improved the moisture tolerance of the perovskite film and little degradation was observed after storage in wet air for over four hours.18 Meanwhile, the solar cell based on the CH3NH3Pb(SCN)2I exhibited a decent PCE comparable to that of solar cell based on the CH3NH3PbI3. However, in most of the related literatures, those halides perovskites need to be prepared and operated under inert atmosphere to eliminate the effect of water. When the fabrication is processed under ambient environment, the resulted unsealed perovskite devices usually would not exhibit high performance.20, 21 Almost all these works focused on the stability of mixed cations and/or halides perovskite solar cells, works on photodetectors with similar materials are rare studied. Herein, we have fabricated photodetectors based on thiocyanate mixed hybrid perovskites (SCNPVSK) by a two-step sequential solution method in air. A small amount of SCN groups were incorporated into CH3NH3PbI3 through lead thiocyanate additive, which remarkably improved the crystalline quality of perovskite film with fewer defects, less grain boundaries and better stability against moisture compared with the pure CH3NH3PbI3 film. The photodetectors based on thiocyanate mixed hybrid perovskite (referred as CH3NH3Pb(SCN)xI3-x) have performed a high responsivity of 12.3 A/W at 550 nm, and a decent detectivity of 1.3 × 1013 Jones. More importantly, the devices have shown greatly improved long-term stability even without encapsulation,


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maintaining approximate 90% of the initial photocurrent over 10 days’ storage in high relative humidity air (>50%), while the photocurrent of photodetectors based on pure CH3NH3PbI3 decreased to 10% of the original value under the same storage and test conditions. This approach is simple but effective, and the solution processing method used here can be easily applied to largescale fabrication. This work provides an exciting opportunity of employing perovskite for highperformance, low-cost, and long-term air stable optoelectronic devices. As shown in Figure 1a, CH3NH3Pb(SCN)xI3-x films were fabricated in ambient air by a two-step sequential solution method (see supporting information). In the first step, Pb(SCN)2 layers were dip-coated on the substrates from the solution of Pb(SCN)2. The uniform morphology of pure Pb(SCN)2 film is shown in Figure S1a. Subsequently, the isopropyl alcohol (IPA) solution of CH3NH3I was dropped and then spin-coated on top of the Pb(SCN)2 film. Thiocyanate mixed hybrid perovskite films have a continuous morphology consisting of perovskite crystals. The Xray diffraction (XRD) patterns of SCN-PVSK is shown in Figure 1b, and the XRD peaks at 2θ = 13.97°, 19.93°, 23.44°, 24.20°, 28.22°, 31.48°, 40.42° and 43.01° are assigned to the (110), (112), (211), (202), (220), (220), (310), (224) and (314) planes of cubic system perovskite crystals, respectively. The XRD patterns of SCN-PVSK and CH3NH3PbI3 films have no significant difference, which may be attributed to the similar ionic radii of thiocyanate (0.215-0.22 nm) and iodide (0.22 nm) and SCN replacing I during the perovskite formation leads little change in crystal structure of the perovskite film.11, 15 The Raman spectroscopy (Figure S1b) of SCN-PVSK films shows no peak of Pb(SCN)2 , indicating a complete reaction between Pb(SCN)2 and CH3NH3I.


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During reacting with CH3NH3I, the Pb(SCN)2 films changed strikingly in color (from white to dark) when forming CH3NH3Pb(SCN)xI3-x film, as shown in insertion of Figure 1c. Figure 1c shows the wavelength-dependent absorbance of SCN-PVSK and CH3NH3PbI3. The light absorption of the SCN-PVSK films were substantially enhanced in the long-wavelength region as compared to the reference CH3NH3PbI3 films, which could be contributed to the larger grains and better crystallization in the former film. The improvement of light absorption of the active layer is beneficial in improving the photosensitivity and detectivity of the photodetectors based on the SCN-PVSK films. In order to obtain the accurate atomic ratio of SCN and I remaining in the SCN-PVSK films, the element analysis by X-ray photoelectron spectra (XPS) was carried out. Figure S2 shows the XPS analysis and element core level spectra, in which both of the signals of S 2p at 163 eV and I 3d at 620 eV are observed, and the signal from S 2p energy level is much weak. The atomic ratio of S/(S+I) is 1.51%, which was calculated through the integral signal area under I 3d and S 2p, manifesting that during the perovskite films formation, most of the SCN¯ had evaporated and only a handful of SCN groups remained in SCN-PVSK films. The minor SCN groups left corresponds to Raman spectra of the perovskite films. Since the volatilization rate of solvents is one of the main affect factors for the crystallization of perovskite film, we have also screened the kinds of solvents used for perovskite film preparation.14,

22

Dimethyl sulfonate (DMSO) and N, N-

dimethylformamide (DMF) are among the most common polar solvents for perovskite preparation, we selected them and their mixed solvent (1:1, volume ratio) to dissolve Pb(SCN)2. Regardless of


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the types of solvents, the number and location of the XRD peaks of SCN-PVSK films are the same, indicating that there is no difference in their crystal structure, as shown in Figure S3a. However, the relative strength of the main diffraction peak (13.97°) in the XRD spectra increases gradually in the order of DMSO, DMF/DMSO and DMF, suggesting SCN-PVSK films prepared with DMF have better crystallinity, which is further confirmed by the full width at half maximum (FWHM) of aforementioned main diffraction peak (Figure S3b). Figure 2a, b and c are the scanning electron microscope (SEM) images of SCN-PVSK films prepared with DMSO, DMSO/DMF and DMF, respectively. In Figure 2a, the SCN-PVSK film exhibits poor crystallization with a large number of ravine-like grain boundaries, while Figure 2b shows densely packed grain crystals but still with lots of grain boundaries. In Figure 2c, the SCN-PVSK film have larger grain size and fewer grain boundaries, which could attribute to lower boiling point, lower viscosity and higher saturated vapor pressure of DMF than that of DMSO and thus favoring the crystallization of Pb(SCN)2. Meanwhile, the chunky morphology is also observed in the CH3NH3PbI3 films surface (Figure 2d), which has many defects and grain boundaries, and water and oxygen molecules could easily diffuse into the films, significantly reducing the stability of perovskites.6, 14, 21 We fabricated the photodetectors based on SCN-PVSK and measured their photosensing performance. After SCN-PVSK layers were deposited onto the pre-cleaned substrates, gold electrodes of 50 nm were thermally evaporated to complete the device fabrication. The channel length is 50 μm, and the channel width is 1 mm. Figure S4a shows the current-voltage (I-V) curves measured under illumination with the same intensity (0.5 mW/cm2) but varied wavelengths (365


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to 850 nm). The photodetectors irradiated by the visible and ultraviolet light exhibited higher photocurrents, compared with those illuminated by near-infrared light (wavelengths of 800 nm and 850 nm), which is consistent with the absorption spectra of SCN-PVSK films in Figure 1c. Figure S4b plots the photocurrent and photoresponsivity (R = Iphoto/PS, where P is the illumination intensity, and S is the effective area under illumination) change with illumination wavelength, which exhibits an obvious cutoff at the wavelength around 750 nm, further indicating the wavelength selectivity of SCN-PVSK based photodetectors to visible and ultraviolet light. Figure 3a depicts the I-V curves of the SCN-PVSK based photodetectors under dark and 550 nm light of various intensities (0.005-1.78 mW/cm2), respectively. The dark current (Idark) of the device was only 2.7×10-10 A at 10 V bias, which is in favor of the high performance of photodetectors, and the photocurrent (Iphoto = Ilight - Idark) increased more than ten times compared to the dark current even when the illumination was very weak (0.005 mW/cm2). The photocurrents have been plotted as a function of the light intensity in Figure 3b. To evaluate the photoresponse of the SCN-PVSK based photodetectors, the light intensity-dependent photocurrents were fitted using a power law (Iphoto ∝ Pα) and a sublinear relationship was observed.. Regardless of the value of bias voltage, the index α equals to 0.52. This sublinear relationship is a reflection of the complex photoelectric processes within the active layer, which determined by the charge transport properties and dynamics of the material.23, 24 The light intensity, as well as the bias voltage, can modulate the photocurrents. The dependence of the photocurrent to dark current ratio (Iphoto/Idark) and the photoresponsivity on the light intensity are shown in Figure 3c. The Iphoto/Idark increased


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with increasing light intensity, and the maximum Iphoto/Idark of our photodetectors was up to 400, indicating an effective light switching characteristic. The Iphoto/Idark can be further improved under higher incident light intensity. The maximum R measured is approximately 12 A/W under 550 nm light with applied bias voltage of 10 V. To further evaluate the photosensitivity performance of the SCN-PVSK based photodetectors, another two key figures-of-merit, detectivity (D* = R(S/2eIdark)1/2, where e represents the elementary charge) and external quantum efficiency (EQE = Rhc/λe, where hc/λe represents the photo energy) were calculated. The illumination power density-dependent D* and EQE at different biases are shown in Figure 3d, and D* and EQE increased greatly as the incident light intensity decreased. When the applied voltage is 10 V and the light intensity is 0.005 mW/cm2, the photodetectors delivered a high D* of 1.3 × 1013 Jones and a high EQE of 3000%. Significantly, the R value and D* value of SCN-PVSK based photodetector are comparable or even higher than that of most of CH3NH3PbI3 nanostructure/thin film devices as far as we know.2, 8, 25-27 The R, D* and EQE decrease linearly as the light intensity increased on a logarithmic scale, thus making our photodetectors promising for practical applications in photoelectric detection field. Fast and reproducible response to incident light is also of great importance to high-performance photodetectors. Here, the excellent photoresponse characteristic of our device is demonstrated by the fast response to illumination with a stepwise increasing light intensity, which is shown in Figure 4a. The response was measured at a voltage of 10 V with light intensities varying from 0.005 to 1.78 mW/cm2. The periodic monochromatic light was controlled by an ultrafast shutter


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and the shutter time was set as 10 s in each cycle. The current increased with light intensity also in a stepwise way, indicating the sensitive response of the SCN-PVSK based photodetector to illumination. Figure S5 displays the optical on-off switching cycles of the SCN-PVSK based photodetector, which was recorded at a fixed light intensity of 1.78 mW/cm2. The photodetector possesses stable and reproducible response. The response and recovery speed of the photodetector can be extract from the switching cycles between on and off states .28, 29 The short photoresponse time is shown in Figure 4b, and the rise (from dark to light) and decay (from light to dark) time for the devices are 7.5 ms and 11.1 ms, respectively. The poor stability in air is the major disadvantage for perovskite-based electrical devices towards practical applications.15, 16, 19 The perovskite materials are easily decomposed once moisture is introduced. The long-term stability of SCN-PVSK films stored in air, where the mean temperature and relative humidity were 20 °C and over 50 %, respectively, has been investigated. It showed that the photodetectors based on SCN-PVSK presented a substantial enhancement in stability compared to the devices based on CH3NH3PbI3 films. As shown in Figure 5a and b, the dark currents and light currents of the devices were recorded for 10 days, the SCN-PVSK devices still maintained approximate 90% of the initial photocurrent in 10th day. In contrast with SCN-PVSK based photodetectors, the CH3NH3PbI3 based photodetectors experienced continued reduction in light current, which decreased to only 10% of the original value after 10 days (Figure 5c and d). These results confirm that devices constructed from SCN-PVSK film have much stronger resistance to the degradation induced by ambient condition than the CH3NH3PbI3 film. Though a


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fraction of SCN¯ had evaporated during the formation of SCN-PVSK film, they induced large crystalline particles in the film, which attributed to the air stability of our photodetectors.11, 15, 30 In summary, we fabricated OHPs-based photodetectors in air with high photosensing performance and long-term stability. It was observed that a small amount of SCN groups incorporated into CH3NH3PbI3 by lead thiocyanate additive can efficiently increase grain sizes in perovskite film and a much uniform morphology can be obtained. The photodetectors illuminated by 550 nm of light exhibited outstanding photoresponse performance with a high R of 12 A/W, a decent detectivity of 1.3 × 1013 Jones and a response time of 7.5 ms. Furthermore, the devices possessed excellent long-term stability when stored in humid air for 10 days. As discussed above, Pb(SCN)2 can be preferred than PbI2 as the precursor for the fabrication of high performance, low cost and long-term stable perovskite photo devices.


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FIGURES

Figure 1. (a) Schematic diagram of the fabrication process of the SCN-PCSK films. (b) The XRD patterns of CH3NH3PbI3 and CH3NH3Pb(SCN)xI3-x films. (c) Absorption spectra of Pb(SCN)2, CH3NH3PbI3 and CH3NH3Pb(SCN)xI3-x films. Inset is the optical images of Pb(SCN)2 (left) and CH3NH3Pb(SCN)xI3-x films (right).


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Figure 2. The SEM images of CH3NH3Pb(SCN)xI3-x film prepared by using (a) DMSO, (b) DMF/DMSO and (c) DMF as the solvent of Pb(SCN)2, (d) SEM image of CH3NH3PbI3 film.


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Figure 3. (a) I-V curves of SCN-PVSK based photodetectors in dark and under varied light intensities from 0.005 to 1.78 mW/cm2. (b) The light intensity- dependent photocurrent of SCNPVSK based photodetectors at different bias voltages. (c) Iphoto/Idark ratio and R values, and (d) D* and EQE values of SCN-PVSK based photodetectors change with light intensity at a fixed voltage of 10 V.


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Figure 4. (a) Time-dependent photoresponse of SCN-PVSK based photodetectors at a fixed voltage of 10 V. (b) The response and recovery time of SCN-PVSK based photodetectors.


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Figure 5. (a) The output characteristics of SCN-PVSK based photodetectors in dark and under light (0.5 mW/cm2) with different exposure time in air. (b) Variation of dark current and light current with days of SCN-PVSK based photodetectors stored in ambient air. (c) The output characteristics of CH3NH3PbI3 based photodetectors in dark and under light (0.5 mW/cm2) with different exposure time in air. (d) Photocurrents of CH3NH3PbI3 based and SCN-PVSK based photodetectors change with time in ambient air.


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ASSOCIATED CONTENT

Supporting Information.

The following files are available free of charge.

Materials and Methods; the SEM image of Pb(SCN)2 film and Raman spectra of perovskite film (Figure S1); the XPS spectra of SCN-PVSK film (Figure S2); the XRD information of SCN-PVSK film (Figure S3); the electrical characteristic of SCN-PVSK based photodetector (Figure S4); the periodic photoresponse of SCN-PVSK based photodetector (Figure S5). AUTHOR INFORMATION Corresponding Author *Email: [email protected] (J.H.)

Author Contributions J.H. designed the concept, Y. Chen, Y. Chu, J.Z. and B.Z. carried out the experiment. Y. Chu and Y. Chen wrote the paper. J.H supervised the project.

Notes The authors declare no competing ﬁnancial interest.


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ACKNOWLEDGMENT

This work was supported by the Science & Technology Foundation of Shanghai (17JC1404600), National Nature Science Foundation of China (61822405), Shuguang Program supported by Shanghai Education Development Foundation and Shanghai Municipal Education Commission (18SG20), National Key Research and Development Program of China (2017YFA0103904), the Fundamental Research Funds for the Central Universities, and the support of College of Transportation Engineering, Tongji University’s Shanghai “Gaofeng” subject.

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Efficient and Stable Perovskite Photodetectors Based on Thiocyanate

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