Solvent-Assisted Thermal-Pressure Strategy for Constructing High

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Solvent-Assisted Thermal-Pressure Strategy for Constructing High-Quality CH3NH3PbI3-xClx Films as High-Performance Perovskite Photodetectors Ning Dong, Xianwei Fu, Gang Lian, Song Lv, Qilong Wang, Deliang Cui, and Ching-Ping Wong ACS Appl. Mater. Interfaces, Just Accepted Manuscript • DOI: 10.1021/acsami.8b00425 • Publication Date (Web): 28 Feb 2018 Downloaded from http://pubs.acs.org on February 28, 2018

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ACS Applied Materials & Interfaces

Solvent-Assisted Thermal-Pressure Strategy for Constructing High-Quality CH3NH3PbI3-xClx Films as High-Performance Perovskite Photodetectors Ning Dong,† Xianwei Fu,† Gang Lian,*,†,§ Song Lv,† Qilong Wang,‡ Deliang Cui,*,† and ChingPing Wong§ †

State Key Lab of Crystal Materials, Shandong University, Jinan 250100, P.R. China

‡

Key Laboratory for Special Functional Aggregated Materials of Education Ministry, School of

Chemistry & Chemical Engineering, Shandong University, Jinan 250100, P.R. China §

School of Materials Science and Engineering, Georgia Institute of Technology, Atlanta, Georgia

30332, United States KEYWORDS: CH3NH3PbI3-xClx, large-sized grains, solvent engineering, thermal pressure, photodetectors ABSTRACT: High-quality CH3NH3PbI3−xClx films have attracted research interests in photoelectric devices because of their improved carrier diffusion length and charge mobility. Herein, a solvent-assisted thermal-pressure strategy is developed to promote the secondary growth of perovskite grains in the films. Then highly oriented perovskite films are obtained with large-sized grains (5-10 µm). As a consequence, the photodetectors based on the high-quality CH3NH3PbI3−xClx films exhibit enhanced ophtoelectrical performance, including high on/off

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ratio (>2.1×104), fast response time (54/63 µs), and high detectivity (~1.3 ×1012). This work suggests an effective approach for high-quality perovskite films, which will be promising candidates for other high-efficiency photoelectric devices. Rapid advances in organic-inorganic hybrid perovskite materials have enabled highly efficient solar cells,1 highly sensitive photodetectors,2 tunable light-emitting diodes,3 and solid-state lasers,4 due to their high absorption coefficient,5 broad spectral absorption,6 weak exciton binding energy,7

long

carrier diffusion

length,8

high

carrier

mobility,9

and

high

photoluminescence quantum yield.10 Notably, the certified power conversion efficiency of perovskite-based solar cell has exceeded 22.1%.11 Through control over the compound stoichiometry, tunable optical absorption and emission of perovskite materials with remarkable electro-optical properties have also pioneered some studies on photodetectors, which can be widely applied in imaging, optical communication, biomedical sensing devices.12,13 In spite of these stunning developments in performance, the electronic properties of perovskites have not yet met the requirement possibly due to defect-assisted trapping from disordered polycrystalline thin films composed of small-sized grains.14 Highly oriented and crystalline perovskite films consisting of large crystal grains have been identified as a crucial role for high-performance photodetectors. These structural features can vastly reduce defect densities, decrease carrier recombination, and improve the electrical and optical qualities of the films when grain boundaries are removed.15 Therefore, recent efforts have focused on improving the size and crystallinity of the grains in the perovskite films via many strategies, such as traditional or modified thermal annealing,16 gasflow assisted spin coating,17 dual-source co-evaporation deposition,18 “solvent engineering”


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methods,19 thermal nanoimprint technology,20–22 and so on. Although the grain size and crystallinity of these films have been improved in some extent,23,24 ensuring a high-quality perovskite film, including high crystallinity, high orientation, large grain size, high smoothness and surface coverage, is still one of main concerns and key scientific challenges for highperformance photodetector devices. Understanding the crystal growth mechanism of perovskite films, undoubtedly, will benefit us to tailor the quality of them. By analyzing these methods, it is easily believed that controlling over the solubility of precursors and evaporation rate of solvents is favorable for crystal growth of the films. Based on the analysis, a secondary crystal growth strategy can be expected to transform a poor-quality film to a high-quality one. To suppress growth of the grains along the direction perpendicular to the substrate, a space-confined treatment is essential in the secondary crystal-growth process. Herein, a solvent-assisted thermal-pressure (ST) strategy is proposed to obtain high-quality CH3NH3PbI3-xClx films. It involves the deposition of CH3NH3PbI3-xClx precursor films via onestep spin-coating method, followed by adsorbing poor solvent (cyclohexane) in the films and controlled thermal-pressure annealing in a relatively sealed circumstance. The resultant perovskite films are highly covered by large-sized crystal grains with high crystallinity and orientation. All of the single-crystal grains vertically span the entire film thickness. The highquality films with long carrier lifetime present predominantly enhanced optoelectrical performance as photodetector devices. The device exhibits orders-of-magnitude improvement in the on/off ratio, compared with the conventionally annealed (CA) perovskite film, as well as high stability, fast response and high detectivity.


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Figure 1. Schematic illustration of preparing the high-quality film via solvent-assisted thermalpressure approach. Solvent-engineering process is an effective strategy to prepare perovskite film, but direct removal of these solvents via evaporation in an open circumstance degrades the growth of largesized grains in the films. In addition, high pressure can improve the crystallinity and decrease the concentration of defects in the process of crystal growth.25 Therefore, a ST treatment in a relatively sealed circumstance was designed to dominate the secondary growth of perovskite grains in the films, which is schematically illustrated in Figure 1. This approach is composed of three steps: fabrication of perovskite precursor films; adsorption of cyclohexane in the films; secondary growth of grains by thermal-pressure treatment in a relatively sealed circumstance. It should be mentioned that the poor solvent of cyclohexane can no damage the precursor films at room temperature. The whole process was conducted in a N2-filled glove box. Firstly, the crystal structure of ST CH3NH3PbI3-xClx film was measured by X-ray diffraction (XRD, Figure 2a). The diffraction peaks can be indexed to (110), (220), (310) and (330) planes of CH3NH3PbI3-xClx with tetragonal I4/mcm structure.26 Peak intensity ratio of (110) to (310) planes is ~534, which is much higher than that of CA film (~51, Figure S1), indicating high (110) orientation of the ST film.27 The ST film was further observed by optical and SEM images (Figure 2b-c). The top-view images show that the film presents high surface coverage and is


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constructed of large-sized crystal grains (5-10 µm), which is one order larger than that of CA film (Figure S2). High crystallinity and large-sized grains absolutely determine that a large number of defects and grains boundaries are removed. Then these grains with smooth surfaces and good boundary interconnection are packed to form a relatively flat and dense film (Figure 2d and S6). The corresponding EDS result shows that the Cl element was successfully doped into CH3NH3PbI3 (Figure 2e). The XPS-determined molar ratio of Cl element in the film is 3.45 % (Figure S3). Roughness and surface topography of the film were detected by atomic force microscopy (AFM, Figure 2f). Clear crystal grains can be easily observed, which is consisted with the SEM result. Uniform contrast of bright and dark indicates high flatness of the film. The calculated root-mean square value of the entire region (17.5 µm× 17.5 µm) is as low as 15.4 nm (Figure S4), which is much smaller than that of reported results.28 Actually, the space-confined effect obviously suppressed growth of the grains along the vertical direction in the process of solvent-assisted secondary crystal growth, greatly decreasing the surface roughness of the film. The cross-section SEM image shows that the single-crystal grains fully span the film thickness with larger lateral dimension (Figure 2g). The thickness of the film is ~500 nm. In contrast, the small-sized polycrystalline grains are randomly stacked across the thickness of the CA film (Figure S5). Actually, although the adsorbed cyclohexane could not damage the film at room temperature, partial small-sized perovskite domains with poor crystallinity could be dissolved at high temperature and pressure. In the relatively sealed circumstance, the quick evaporation of cyclohexane was suppressed, which allowed for prolonged growth of these undissolved grains, as the seed crystals, to yield large-sized domains. The quasi-liquid condition also benefited effective diffusion of dissolved precursors and Ostwald ripening of crystal grains. Then the highquality CH3NH3PbI3-xClx films, including large-sized grains, good boundary interconnection,


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single-crystal feature across the thickness of the film, high surface coverage, high orientation, and high smoothness, are prepared by our designed ST approach.

Figure 2. Structural analysis of the obtained ST CH3NH3PbI3-xClx film. (a) XRD pattern, (b) optical image, (c) top-view SEM image, (d) high-magnified SEM image, (e) the corresponding EDS result, (f) AFM image and (g) cross-section SEM image of the ST perovskite film. Furthermore, the optical and transport properties of the ST films were investigated. The ultraviolet-visible (UV-vis) absorption spectra present a clear band edge cutoff (Figure 3a). An onset at ~780 nm is the typical absorption characteristic of the CH3NH3PbI3−xClx.6 The stronger absorption of ST film in the range of 400-780 nm indicates a low concentration of in-gap defect.14 The steady photoluminescence (PL) peak of the ST film is located at ~773 nm (Figure 3b), which is blue-shifted compared to that of CA film (785 nm), implying lower trap density of the ST film around the band-edge.1–4 Time-resolved PL spectra were further utilized to illustrate the recombination dynamics of photo-generated carriers in the CA and ST films (Figure 3c), which is a stronger indicator of good crystalline quality. Two time components, including a fast decay (τ1) and a slower component (τ2), were fitted with a bi-exponential decay function. They correspond to the interfacial charge transfer (τ1) and carrier recombination in the bulk of


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CH3NH3PbI3-xClx grains (τ2), respectively.30 The CA film exhibits a fast-decay component (τ1: 396 ns) and a slow-decay compoment (τ2: 1365 ns) with 53% and 47% contributions, respectively. As a contrast, not only the slow-decay component process becomes the major process with 80 % contribution for the ST film, but also its characteristic time (τ2) is up to 2352 ns, which is much longer than reported values of CH3NH3PbI3-xClx films.1–4

Figure 3. Optical and transport properties of the perovskite films prepared by CA and ST strategies. (a) The UV-vis absorption and (b) normalized time-resolved PL spectra of the CA and ST perovskite films. (c) Time-resolved PL spectra for the CA and ST films. They are fitted with a bi-exponential decay function. The high-quality CH3NH3PbI3-xClx film with long carrier lifetime is a promising candidate for photodetector device, as designed in Figure 4a. Each pair of interdigitated gold (Au) wire electrodes is 4 mm in length, 400 µm in width and 125 nm in thickness. The current-voltage (I-V) curves in dark and under illumination of different lasers with a power density of 8 mW/cm2 were shown in Figure 4b. Compared to the dark current as low as 4 nA at 10 bias voltage (Figure S7), the photocurrents presented remarkable increase. The improvement of current should be derived from the generation of electron-hole pairs because the energy of incident photons is larger than the band gap. In the high absorption range of 405 to 671 nm (Figure 3a), every photon is expected to generate one electron-hole pair. Therefore, the photocurrent under 671 nm is pronouncedly higher than these under 405, 465 and 532 nm, which also depends on the light


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power density. The dynamic response curves of the device under 671 nm laser with different power density were presented in Figure 4c. The corresponding bias voltage is 10 V. The photocurrent is as high as 12 µA when the device was exposed to a light as low as 0.9 mW/cm2, which is improved to ~83 µA under higher illumination intensity (20.6 mW/cm2). There is not obvious variation for the photocurrent in the signal amplitude during the on/off cycles, indicating a good reversibility and stability of the ST film device (Figure 4d). What’s more, the photocurrent is linearly proportional to the incident irradiation intensity range from 2×10-6 to 1.0×10-1 W/cm2 (Figure 4e). Linear dynamic range is given by the formula (LDR=20logIlight/Idark) and a linear dynamic range exceeding 70 dB is achieved under 10 V bias. Furthermore, the photoelectrical performance of ST and CA film devices is compared in Figure 4f. The wavelength and power density of illuminated laser is 671 nm and 20.6 mW/cm2. Although the dark current of ST film device was slightly improved in comparison with that of CA film device (Figure S7), more remarkable enhancement of photocurrent from 6.4 to 83 µA was achieved for the ST film device. The remarkable improvement of photocurrent naturally results in ultrahigh on/off ratio of the ST film device. As shown in Figure 4g, the on/off ratio under 20.6 mW/cm2 is as high as 2.1×104 at 10 V bias voltage, which is much higher than that of CA film photodetector (2.5×103). In spite of the power density as low as 0.9 mW/cm2, the on/off ratio of ST-based photodetector is also over 2.5×103. Response time is an another important parameter to evaluate the performance of the photodetector. Herein, rise and decay times are defined as the time necessary to increase the photoresponse from 10 to 90 % and reduce that from 90 to 10 %, respectively. As shown in Figure 4h, the rise and decay times are as low as 54 and 63 µs, respectively. The fast response actually indicates low defect concentration and superior electronic quality of the ST film device. Furthermore, detectivity of the ST film photodetector as


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a function of power density was analyzed, shown in Figure 4i. The detectivity is ~1.3×1012 Jones at a power density of 0.9 mW/cm2, which is obviously higher than that of CA film device (Figure S8). Furthermore, the optoelectronic performance of ST-based photodetector devices has been compared with these of reported similar perovskite devices (Table S1). In terms of these features including high photocurrent, high on/off ratio, good stability, fast response and high detectivity, a sensitive and fast-response perovskite photodetector device is simultaneously realized, based on the high-quality CH3NH3PbI3-xClx film.

Figure 4. Photoelectrical performance of the CH3NH3PbI3-xClx films obtained by CA and ST strategies. (a) Schematic diagram of the perovskite-based photodetector device. (b) I−V curves of the ST film based photodetectors in dark and irradiated by lasers with different wavelength under


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8 mW/cm2. (c) Transient photoresponse properties of the photodetectors based ST film for 671 nm laser with bias voltage of 10 V under different illumination power density. (d) Reproducible on/off switching of the device illuminated by 671 nm laser with a power density of 20.6 mW/cm2. (e) Linear dynamic range of the CH3NH3PbI3-xClx photodetector, photocurrent vs incident light intensity under 671 nm at 10 V bias. (f) I–V curves of photodetectors with CA and ST films for 671 nm laser under 20.6 mW/cm2, respectively. (g) The Ilight/Idark ratio of the photodetectors based on CA and ST films under different illumination power densities for 671 nm laser. (h) Transient photocurrent (current-time curve) of the ST film photodetector. (i) Detectivity of the ST film photodetector as a function of light intensity at 671 nm laser. In summary, we demonstrate a solvent-assisted thermal-pressure strategy to achieve secondary growth of crystal grains and obtain high-quality CH3NH3PbI3-xClx films. Such films are composed of large-sized grains with excellent crystallinity and high orientation perpendicular to the substrate, which vertically span the entire film thickness. The synergetic effects of poor solvent, pressure and space confine determine the formation of high-quality perovskite films. The corresponding photodetector devices exhibit dramatically improved optoelectrical performance, such as high photocurrent response, high on/off ratio, excellent stability, fast response time, and high detectivity. Such high-performance features can be mainly attributed to reduced carrier recombination sites due to removal of defects and grain boundaries in the films. This work represents a significant development for realizing high-quality perovskite films and high-efficiency optoelectronic devices. ASSOCIATED CONTENT Supporting Information


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The Supporting Information is available free of charge on the ACS Publications website. Experimental section, XRD patterns of the CA and ST CH3NH3PbI3-xClx films, top-view and cross-section SEM images of the film, XPS spectra of ST CH3NH3PbI3-xClx film, threedimensional topographic image of the film, I–V curve of photodetector in dark, and detectivity of the CA film photodetector. AUTHOR INFORMATION Corresponding Authors * E-mail: [email protected] * E-mail: [email protected] Author Contributions The manuscript was written through contributions of all authors. All authors have given approval to the final version of the manuscript. Notes The authors declare no competing financial interest. ACKNOWLEDGMENTS This work was supported by the National Natural Science Foundation of China (NSFC, No. 51372143, 51102151). ABBREVIATIONS CA, the conventional annealing; ST, solvent-assisted thermal-pressure; XRD, X-ray diffraction; SEM, scanning electron microscope; AFM, Atomic force microscopy; XPS, X-ray photoelectron spectroscopy. REFERENCES


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Solvent-Assisted Thermal-Pressure Strategy for Constructing High

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