High Detectivity and Rapid Response in Perovskite CsPbBr3 Single

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High Detectivity and Rapid Response in Perovskite CsPbBr Single Crystal Photo-Detector 3

Jianxu Ding, Songjie Du, Zhiyuan Zuo, Ying Zhao, Hongzhi Cui, and Xiaoyuan Zhan J. Phys. Chem. C, Just Accepted Manuscript • DOI: 10.1021/acs.jpcc.7b01171 • Publication Date (Web): 23 Feb 2017 Downloaded from http://pubs.acs.org on February 25, 2017

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The Journal of Physical Chemistry

High Detectivity and Rapid Response in Perovskite CsPbBr3 Single Crystal Photo-detector Jianxu Ding 1,*, Songjie Du 1, Zhiyuan Zuo 2, *, Ying Zhao 1, Hongzhi Cui 1, *, Xiaoyuan Zhan 1 (1. College of Materials Science and Engineering, Shandong University of Science and Technology, Qingdao 266590, China; (2. Advanced Research Center for Optics, Shandong University, Jinan 250100, China.

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ABSTRACT: Band gap tunable hybrid organic- inorganic lead halide perovskites (APbX3, A= CH3NH3+ and NH2CH=NH2+, and X=Cl, Br or I) have attracted significant attentions in optoelectronic and photovoltaic related fields on account of their outstanding optoelectronic properties. Single crystals of hybrid perovskites, such as CH3NH3PbI3 and CH3NH3PbBr3, were certified to be advantageous over thin films as photodetectors. However, their resistance towards heat and moisture hinders their future development. Fully inorganic perovskite CsPbBr3 stands a chance to fill the gap as a novel photodetector with perovskite structure. In this paper, we revealed the growth of CsPbBr3 single crystal was of a 2D nucleation mechanism. Similarities of d values and octahedra arrangements along [101] and [020] orientations restricted single crystal growth. Under optimized conditions, orthorhombic CsPbBr3 single crystals with (101) crystallographic facets were grown by using methyl alcohol as anti- solvent from saturated DMSO solution. The optoelectronic properties of the single crystal were explored through a metal- semiconductor- metal (MSM) photodetector device. Meanwhile, their steady and transient performances were also investigated. A highest responsivity of 0.028 A/W and a response time of less than 100 ms were achieved.

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1. INTRODUCTION Because of their outstanding optoelectronic characteristics, hybrid organic- inorganic lead halide perovskites (ABX3, A= CH3NH3+ and NH2CH=NH2+, and X=Cl, Br or I) have recently shown great potential applications in laser,1 light emitting diodes,2 photo-detector,3 and especially in solar cells.4-5 Many approaches have been proposed to enhance conversion efficiencies, such as tuning band gap, improving crystallinity and decreasing grain boundaries in thin films in photovoltaic related areas.6-8 As for photodetectors, both polycrystalline films and single crystal are adopted to fabricate them. The optoelectronic properties associated with carrier mobilities,

lifetimes

and

defect

tolerance

of

single

crystals

exhibit

more advantages than that of polycrystalline,9-10 evoking worldwide attentions upon hybrid lead halide perovskite based single crystal photodetectors. However, the instabilities of hybrid lead halide perovskites under moisture, heat or light,11-13 severely limited their applications as long-term devices. To lift the instability barrier for their applications, various strategies are proposed. Among them, replacing organic compound by inorganic one is the most promising one. For example, cesium lead halides (CsPbX3), fully inorganic perovskites, demonstrate much long term stability without sacrificing any photovoltaic and optoelectronic properties.14-15 As an important member in cesium lead halides family, CsPbBr3 possess many interesting properties, like direct optical band gap, narrow emission line-width, large optical absorption across the visible spectra band, high quantum yields, and highly luminescent. Such properties render them huge potential applications in the fields of 3



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LED and photoluminescence,16 laser,17-18 optoelectronic devices,19 and γ-ray detection.20 Most these research utilizes CsPbBr3 nanocrystals, nanowires, and thin films, where both cubic and orthorhombic phases CsPbBr3 present. Using polycrystalline, the photoelectric of orthorhombic CsPbBr3 was recently reported.21 However, to the best of our knowledge, only few optoelectronic devices based on CsPbBr3 single crystal has been reported, and their optoelectronic properties have not been thoroughly revealed.22-23 To deeply understand the intrinsic optoelectronic properties and bridge the discrepancy between single crystal and polycrystalline counterpart, large scale monocrystalline wafer suitable for optoelectronic devices are highly demanded. Kanatzidis et al synthesized orthorhombic CsPbBr3 single crystals by reacting equimolar amounts of CsBr and PbBr2 at 600 °C by vertical Bridgman method.20 Cahen and coworkers successfully grew CsPbBr3 single crystals from solutions at low temperature. The pioneer work provides a novel and facile method to grow single crystals.24 In the work, CsPbBr3 single crystal exposing (101) crystallographic planes were successfully grown by controlling anti- solvent vapor diffusion velocity and growth temperature. To harvest optoelectronic performance based on single crystal, gold interdigitated electrodes were adopted to fabricate MSM devices. The optoelectronic performances, such as photo-current, responsivity and time response were investigated, respectively.

2. EXPERIMENTAL SECTION 4


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Chemicals and reagents. High-purity CsBr (≥99.5 %), PbBr2 (≥99.5 %), methyl alcohol (≥99.5%), ethanol (≥99.7%) and dimethyl sulfoxide (DMSO, ≥99.5 %) were purchased from Aldrich. All raw materials and solvents were purchased without any further purification. CsPbBr3 single crystal growth. CsPbBr3 single crystal were grown from saturated solutions by dissolving CsBr and PbBr2 with 1:1 molar ratio in 5 ml DMSO solution with continuous stirring at room temperature. After all the raw materials dissolved, a transparent solution was obtained. The saturated solution was controlled by titrating methyl alcohol into the solution until light yellow- white undissolved reserved (Figure S1a). The solution was then heated to 40 °C and stood for more than 24 hours by continuous stirring. The precipitation transferred to yellow- green (Figure S1b). The saturated transparent solution was filtered and transferred to another container. CsPbBr3 single crystals were grown using methyl alcohol and ethanol as anti solvent. By controlling diffusion of the anti- solvent vapor and growth temperature, the crystal growth process would differ. Device fabrication. Planar photo-detector was fabricated on (101) facet of CsPbBr3 single crystal. The surface was well polished and dust cleared under nitrogen flow before device fabrication. Through conventional lithography (MABA6, SUSS) and wet etching, hollow aluminium contact pattern mask was fabricated, and laid flat on the smooth (101) surface of CsPbBr3 single crystal. Au interdigitated electrodes were formed on the blank area of the hollowed mask during sputtering process (Discovery-550, Denton). The aluminium mask area was the corresponding light 5



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absorption area of the photo-detector. Characterizations and measurements. Both powder and planar of CsPbBr3 single crystal X-ray diffraction patterns of were collected in the range of 10-50° on X-ray diffract meters (D/Max2500PC), with Cu KαI irradiation using tube voltage at 40 kV and 40 mA. The UV-vis spectra of CsPbBr3 powders were carried out on a UV-2550 spectrometer with an integrating sphere over the spectral range of 400-700 nm. A FLS-920 fluorescence spectroscopy had been used to collect photoluminescence spectrum (PL), and the excitation wavelength is 405 nm. The time-resolved measurement was carried out on an Edinburgh Instruments FLS980 with a nanosecond fluorescence spectrometer under 445 nm excitation wavelength. To depict the growth mechanism of CsPbBr3 single crystal through surface evolution, atomic force microscopy (AFM, Veeco Dimension Icon) in a tapping mode in an ambient atmosphere at room temperature was chosen to observe the surface structure. After the single crystal finished growth, the residual solutions on surfaces were cleared using filter papers at constant temperature. The optoelectronic properties of the planar photo-detector were investigated inside of a copper shielding box in air at room temperature using an electrical properties measurement system (B1500A with preamplifier, Agilent) and a probe station (PM5, SUSS). Semiconductor laser diodes (LD, 450nm, 20 mW, InGaN based) were chosen as the excitation light sources to collect photocurrents, and a high frequency InGaN based light emitting diode (LED) were employed in the time-depended on-off circle measurement. All the light sources used in this study 6


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had been carefully calibrated by a standard Si CCD (DSI200, Zolix) before measurement.

3. RESULTS AND DISCUSSION Hybrid organic- inorganic perovskites are aware of being resolved in a variety of organic solvents with temperature reverse solubility, enabling them to be grown from organic solvents by temperature rising25-26 and anti-solvent method,27 etc. Compared with hybrid perovskites, fully inorganic perovskite CsPbBr3 behaves a similar temperature reverse solubility in DMSO. It noted that the concentration could reach to 0.5 M in DMSO by dissolving equivalent CsBr and PbBr2 simultaneously at room temperature. However, a too high concentration solution caused fast growth process, resulting in simultaneous crystals. On the other hand, in the Cs-Pb-Br system, Cs4PbBr6 and CsPb2Br5 are unexpected compounds, which are prone to emerging with slight element deviation of 1:1 ratio of PbBr: CsBr.24 The titrating of methyl alcohol process, as well as increasing temperature (to 40 °C, for example) was effective to eliminate the appearance of Cs4PbBr6, an unexpected yellow-green material with strong fluorescence under UV light (Figure S1c). Figure 1a illustrates the growth process of CsPbBr3 single crystal using methyl alcohol as anti- solution. The growth of CsPbBr3 single crystal was divided into two stages: nucleation and facet evolution, both of which were affected by diffusion velocity of methyl alcohol and growth temperature. For example, at a growth temperature of 60 °C, plenty of single crystals appeared separately and can hardly grow beyond 2 mm in length. 7



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While tiny single crystals tend to be aggregate together and form opaque bulk polycrystalline at room temperature, as shown in Figure 1b, suggesting nuclei velocity was too high. Accordingly, by controlling the diffusion velocity of methyl alcohol vapor into the growth solution (adjusting the pore number), and holding temperature at 40 °C as well, CsPbBr3 single crystals with various shapes were successfully grown (Figure 1c). The powder XRD patterns, as displayed in Figure 1d. Based on the XRD pattern, the crystal structure is assigned to orthorhombic perovskite structure, and the space group is assigned to Pnma with unit cell parameters a= 8.24 Å, b= 11.75 Å, c= 8.20 Å. The XRD analysis shows that the crystal parameters are in agreement with the previous reported data.28 The planar XRD pattern was collected by scanning the exposed facet of CsPbBr3 single crystal, in which both (101) and (020) diffraction peaks appeared. The synchronized appearance of (101) and (020) is attributed to their close d values (5.81 Å for (101) and 5.86 Å for (020)), and common X-ray diffraction could not distinguish such difference. According to the detail analysis in Ref,24 the facet was determined and assigned to (101) facet. The stoichiometric ratio of the elements was characterized by means of EDS (Figure S2).

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Figure 1. Descriptions of CsPbBr3 single crystal. (a) Schematic representation of the single crystal growth process via anti-solvent method; (b, c) Photos of CsPbBr3 crystals grown at room temperature (polycrystalline) and 40 °C (single crystal), respectively; (d) Powder and planar XRD patterns of orthogonal CsPbBr3 grown at room temperature and 40 °C, respectively.

The growth of CsPbBr3 single crystal depends on facet evolution, which is associated with the incorporation of growth units onto crystal surface. Therefore, to deeply understand the growth mechanism of CsPbBr3 single crystal, the surface structure should be resolved. The macroscopic surfaces structures of polycrystalline CsPbBr3 crystals grown at room temperature were observed under optical 9



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microscope, as shown in Figure 2a. Such polycrystalline was constructed by various tiny single crystals, each of which presented respective growth orientations. For example, the tiny single crystals marked with red rectangles exhibited layer by layer growth model with two vertical growth directions, which coincided the crystal morphologies displayed in Figure 1b. On the other hand, from the Figure 2b, each single crystal performed layer by layer growth, whereas the connection of the individual single crystals seemed like grain boundaries. We believe that besides of grain boundaries were [101] and [020] orientations. Two reasons could account for the claim, one is that the d values along [101] and [020] orientations were close enough to form coherent boundaries. The other is that the connection between anionic polyhedra [PbBr6]- along both [101] and [020] orientations were similar, both were connected with alternating [PbBr6]- and Cs+ arrays, as illustrated in Figure 2c-d. Once growths of both (101) and (020) become entangled, bulk polycrystalline were easily occurred and therefore the growth of a single crystal became more difficult. As for (101) facet of CsPbBr3 single crystal, the surface structures were identified through AFM, as displayed in Figure 2e. Apparently, the growth of (101) facet of CsPbBr3 single crystal was controlled by the 2D nucleation mechanism and the motion of their derivative steps. By measuring the step heights in the white rectangle marked section, as shown in Figure 2f, the elementary step heights were determined to be 0.56-0.73 nm, equivalent to the d value of (101) facet of CsPbBr3. The results suggest that the minimum growth layer was one interplanar space. The 1.21 nm step height indicated that two elementary step could bunch together. The coexistence of 10


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elementary and bunched steps could incorporate with volume varied growth units, which was beneficial to single crystal growth.

Figure 2. Growth mechanism analysis of CsPbBr3 crystal. (a-b) Surface morphologies of the bulk polycrystalline of CsPbBr3 observed via optical microscopy; (c-d) Comparison of [PbBr6]- and Cs+ arrays along [101] and [020] orientations; (e) AFM topologies of 2D nucleation on (101) facet of CsPbBr3 single crystal; (f) Height files of the 2D nucleation and the derivative steps. 11



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Figure 3a present the optical absorption and PL spectra of CsPbBr3 single crystal. The absorption edge was located around 560 nm. By fitting the Tauc plot, the energy band gap (Eg) was calculated to be 2.16±0.02 eV, lower than ~2.32 eV of thin film29 or ~2.25 eV of high temperature grown single crystal.20 Our lower Eg value suggests that CsPbBr3 single crystal is more suitable in application as photodetector than polycrystalline film. Figure S3 displays the calculated band structure. The magnitude of the band gap is estimated to be 2.23 eV, which fits well with the experiment result. In addition, it shows a direct band-gap with the highest point in valence band and the lowest point in conduction bands both occurring at the G point. From the PL spectrum with a 405 nm excitation, the PL peak centered at 540 nm was detected, a red shift relative to nanowires (519 nm)19 and nanocrystals (511 nm),30 which also provide evidence that such CsPbBr3 single crystal could hold great promise for applications in photodetector. Moreover, the broad PL emission width was from 510 to 570 nm, imply that near-edge defects levels related to surface states played roles in emission process.31 Figure 3b depicts the time-resolved PL decay, which is fit to biexponential decay. The faster decay time (τ1) and slower decay time (τ2) are corresponded to trap- assisted recombination on surface and free carrier recombination in bulk, respectively. Both faster and slower decay times were shorter than other reported results of CsPbBr3 (τ1=4.4 ns and τ2=30 ns).24

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Figure 3. Descriptions optical properties of CsPbBr3 single crystal. (a) The absorption and photoluminescence spectra of CsPbBr3 single crystal; (b) Time-resolved PL (λexc = 445 nm) for CsPbBr3 single crystal.

Figure 4. Photocurrents, responsivities, EQEs and detectivities of the devices of CsPbBr3 single crystal. (a) The photo responses (b) Responsivities and EQEs (c) Detectivities of the devices, respectively.

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Figure 4 shows the photocurrent, responsivity, external quantum efficiency (EQE) and detectivities of the CsPbBr3 single crystal photodetector. The dark and photocurrents (Figure 4a) were obtained by using a 450 nm laser diode (LD). At an applied voltage of 5 V, the dark current is as low as 7.98×10-8 A. Positive correlation can be found between photocurrents and applied voltages as well as illumination intensities. The tendency of dark current shows mainly linear feature and is in accordance with the ohmic phenomenon. The responsivities R and EQEs can be calculated by using:

=

∙

(1)

and:

=

∙

(2)

Where IPC and Idark are currents measured with and without illumination respectively.

Pirra is the irradiation power density, S is the effective area of the detector, c is the speed of light and λ stands for the wavelength of light source.32 Responsivity reveals the ratio of photon excited current to irradiation power, and in order to evaluate the photocurrent conversion ability of the device, the EQEs had been obtained from responsivity by changing the ratio of current/incident light power to electron quantity/photon quantity. As the wavelength were fixed at 450 nm during all the measurements in this study, responsivities and EQEs can be expressed in one group of curves(Figure 4b). Responsivities and EQEs depend on the applied voltage and incident light power density, and both responsivities and EQEs increase when applied voltages grow larger. With an irradiation power of 1mW and an 5.00 V bias , the 14


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highest responsivity and EQE under 450 nm illumination is 0.028 A/W and 7.00 % respectively. The detectivity of CsPbBr3 single crystal photodetector was calculated according to formula and is displayed in Figure 4c: ∗ =

∗ /

(3)

Where R and Idark are responsivities and dark current respectively.33

Figure 5. Time-dependent photocurrents and the swiching times. (a) shows five continues on-off circles under various applied voltages of the devices; (b) detail response times under various applied voltages of the devices.

Transient measurements were performed to obtain switching characteristics of the device at different applied voltages (Figure 5a). The switch features of the devices were measured by employing a high fequency light emitting diode (LED) with a dominant wavelength of 462 nm. A highest on/ off ratio of ~100 was achieved under 5.00 V bias. Significant overshoot can be seen while the illustration is on due to the sudden excited and departed carriers.21 Similar current values of subsequent cycles under different bias voltages reveal a weak built-in potential34 induced by ions and charged vacancies.35 Figure 5b shows the rise and decay properties of the device. With increasing times, a positive correlation with applied voltages could be observed 15



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and no similar phenonmenon was found during the decay processes. Compared to previous reports on the rise and decay time of polycrystalline CsPbBr3 film,21 the time scales less than 100 ms for both of rise and decay processes obtained on (101) lattice plane from single crystal are much faster. The short response time could benefit from the low defects density, less grain boundries and unified lattice orientation. This superiority may lead the CsPbBr3 devices to a higher band width.

4. CONCLUSION In summary, by optimizing growth conditions to overcome the restrictions caused by similarities of d values and octahedra arrangements along [101] and [020] orientations, orthorhombic CsPbBr3 single crystals were successfully grown. The optoelectronic properties based on CsPbBr3 single crystal photodetector device were proved to be superior to that of polycrystalline CsPbBr3 film.

ASSOCIATED CONTENT Supporting Information The supporting information is available free of charge via http://pubs.acs.org.

Pretreatment of the growth solution, element distribution of CsPbBr3, calculated band structure, and the description of the photo-detector device.

AUTHOR INFORMATION Corresponding Authors 16


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*

E-mail: [email protected] (J. X. Ding), Tel +86(532) 80691739

E-mail: [email protected] (Z. Y. Zuo), Tel +86 (532) 80691739 E-mail: [email protected] (H. Z. Cui), Tel +86(532) 80691739 Notes The authors declare no competing financial interest.

ACKNOWLEDGEMENTS This work was financially supported by the National Science Foundation of Shandong Province (ZR2016EMQ10), the National Natural Science Foundation of China (No. 51202131), Scientific Research Foundation of Shandong University of Science and Technology for Recruited Talent (No. 2014RCJJ001), SDUST Research Fund and Joint Innovative Center for Safe and Effective Mining Technology and Equipment of Coal Resources, Shandong Province (No. 2014JQJH102), National Key Research Project (2016YFB0401802), and Fund of State Key Laboratory of Crystal Materials in Shandong University (No. KF1504).

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Organic-inorganic Perovskites: Low-Cost Semiconductors with Intriguing Charge-Transport Properties. Nat. Mater. Rev. 2016, 1, 15007.

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High Detectivity and Rapid Response in Perovskite CsPbBr3 Single

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