Acsphotonics 8b01675

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Article
In-situ fabrication of 2D WS/Si type-II heterojunction for self-
2
powered broadband photodetector with response up to mid-infrared

Enping Wu, Di Wu, Cheng Jia, Yuange Wang, Huiyu Yuan, Longhui
Zeng, Tingting Xu, Zhifeng Shi, Yongtao Tian, and Xin Jian Li
ACS Photonics, Just Accepted Manuscript • DOI: 10.1021/acsphotonics.8b01675 • Publication Date (Web): 09 Jan 2019
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Page 1 of 31 ACS Photonics
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1 In-situ fabrication of 2D WS2/Si type-II
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2 heterojunction for self-powered broadband
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3 photodetector with response up to mid-infrared
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4 Enping Wu,a Di Wu,*, a Cheng Jia,a Yuange Wang,a Huiyu Yuan,b Longhui Zeng,*,c Tingting Xu,a
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23 5 Zhifeng Shi,a Yongtao Tiana and Xinjian Lia
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26 6 aSchool of Physics and Engineering, and Key Laboratory of Material Physics of Ministry of
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7 Education, Zhengzhou University, Zhengzhou, Henan, 450052, China
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8 bHigh Temperature Ceramic Institute, School of Materials Science and Engineering, Zhengzhou
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33 9 University, Zhengzhou, Henan, 450052, China
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35 10 cDepartment of Applied Physics, The Hong Kong Polytechnic University, Hung Hom, Kowloon,
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38 11 Hong Kong, China
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40 12 KEYWORDS: WS2, 2D materials, heterojunction, mid-infrared, photodetector, polarization
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42 13
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46 14 ABSTRACT: The high-performance broadband photodetectors have attracted intensive scientific
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48 15 interests due to their potential applications in optoelectronic devices. Despite great achievements
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51 16 have been achieved in two-dimensional (2D) materials based photodetectors such as graphene and
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53 17 black phosphorus, obvious disadvantages such as low optical absorbance and instability preclude
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55 18 their usage for the broadband photodetectors with the desired performance. An alternative
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60 ACS Paragon Plus Environment
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3 1 approach is to find promising 2D materials and fabricate heterojunction structures for
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6 2 multifunctional hybrid photodetectors. In this work, 2D WS2/Si heterojunction with a type-II band
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8 3 alignment is formed in-situ. This heterojunction device produced a high Ion/Ioff ratio over 106,
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10 4 responsivity of 224 mA/W, specific detectivity of 1.5×1012 Jones, high polarization sensitivity and
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5 broadband response up to 3043 nm. Furthermore, a 4×4 device array of WS2/Si heterojunction
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15 6 device is demonstrated with high stability and reproducibility. These results suggest that the
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17 7 WS2/Si type-II heterojunction is an ideal photodetector in broadband detection and integrated
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8 optoelectronic system.
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10 Photodetectors, converting incident light into electric signals, are of tremendous interests due to
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28 11 their applications in industry and military, such as biochemical analysis, industrial automatic
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30 12 control, missile warning and so on.1-5 Photodetectors can be categorized into the broadband and
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13 the selective photodetectors, corresponding to wide-spectrum and spectrally-distinctive
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35 14 photoresponse.6-7 Compared to the photodetectors with the relatively narrow response, the
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37 15 broadband photodetectors have great potential applications for ultraviolet-visible-infrared (UV-
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39 16 Vis-IR) light communication, memory storage and wide spectral switch in a single optoelectronic
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42 17 device system.8 At present, a number of commercial photodetectors are generally based on
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44 18 crystalline GaN, Si, InGaAs with very mature fabrication technologies, which are used for 250-
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46 19 400 nm (UV), 400-800 nm (visible) and 900-1700 nm (near-infrared, NIR) detection,
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20 respectively.9 In addition, long wavelength infrared detectors are mostly based on semiconductors
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51 21 with narrow band-gaps, such as HgCdTe, InSb, and quantum-well structure.10-13 It is a challenge
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53 22 to realize high-performance detectors based on as-mentioned materials due to existing bottlenecks
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23 such as toxicity, sophisticated fabrication processes and low operating temperature.14-15 Thereby,
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3 1 identifying new materials to fabricate multifunctional hybrid photodetectors for multiband
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6 2 response ranging from deep ultraviolet to mid-infrared is highly desirable.16-19
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9 3 Recently, two-dimensional (2D) materials have emerged as an ideal platform for realizing a
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11 4 variety of optoelectronic devices due to their unique properties.20-25 Among these 2D materials,
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5 WS2 has been intensively studied in photodetection applications. For example, Yao et al. first
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16 6 demonstrated a multilayer WS2 film based photodetector, which exhibits good photoresponse
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18 7 properties in terms of a high responsivity of 0.51 A/W, high carrier mobility of 31 cm2 V-1 s-1 and
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8 broadband response.26 Kim et al. designed a WS2/Si heterojunction photodetector, which is
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23 9 sensitive to light illumination ranging from UV to NIR with an ultrafast response speed of 1.1 μs.27
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25 10 Considering the good above achievements, the 2D WS2 film has exhibited its excellent
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27 11 optoelectronic properties in photodetection applications. However, limited by its inherent band-
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30 12 gap, WS2 based photodetectors are mainly operated in visible regime, leading to the restriction in
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32 13 the infrared region, especially in mid-infrared applications.28 To address this issue, it is advisable
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34 14 to create multifunctional hybrid heterostructures with well-designed type-II band alignment for the
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15 interlayer optical excitation.18 Such hybrid heterostructures can provide more powerful and extra
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39 16 functions compared with the individual component based devices.29-31 For photodetectors, the
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41 17 heterostructures with type-II band alignment can extend the range of the spectral response by
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18 breaking the limitation of the intrinsic band-gaps of the component materials. This is quite
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46 19 fascinating for the design of broadband photodetectors, especially for that operating in long
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48 20 wavelength.32-34
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51 21 Herein, we reported the high-performance broadband photodetectors using in-situ fabrication
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54 22 of 2D WS2/Si heterostructures with type-II band alignment. It is revealed that the as-assembled
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56 23 device is capable of capturing deep UV-Vis-IR light at zero bias. The device presented a high
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3 1 current On/Off ratio (Ion/Ioff) over 106, a high responsivity of 224 mA/W and a specific detectivity
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6 2 over 1012 Jones, as well as a fast response speed of 16/29 μs under 980 nm light illumination at 0
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8 3 V. In particular, the creation of type-II band alignment allows device to response to a mid-infrared
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10 4 light up to 3043 nm. Our results suggest that the high-performance WS2/Si heterojunction
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5 photodetector would have great potential for broadband infrared detection.
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16 6 Experimental Section
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19 7 The large-area 2D WS2 thin films were synthesized by a two-step thermal decomposition method
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8 according to our previous studies.35 In detail, the SiO2/Si substrates were continuously cleaned by
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24 9 using acetone, alcohol and deionized water in an ultrasonic bath. Ar-plasma was then used for
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26 10 hydrophilic treatment of the substrates. The precursor solution prepared by mixing (NH4)2WS4
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28 11 (0.25 g, Sigma-Aldrich, purity of 99.99%) and dimethylformamide (DMF, 20 ml) was spin-coated
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31 12 on SiO2/Si substrates and baked at 100 °C to form (NH4)2WS4 film. Afterwards, the (NH4)2WS4
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33 13 film was annealed at 550 °C for one hour under Ar/H2 atmosphere with a pressure of 1 Torr in a
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35 14 horizontal tube furnace, followed by a second annealing process at 850 °C for 30 min under Ar/S
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15 atmosphere with a pressure of 500 Torr. The thickness of WS2 film was controlled by changing
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40 16 the spin-coating speed. The as-prepared 2D WS2 films were identified by X-ray diffraction (XRD),
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42 17 Raman spectrometer, atomic force microscope (AFM) and X-ray photoelectron spectroscopy
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18 (XPS).
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48 19 To in-situ fabricate WS2/Si heterojunction devices, a 4 × 4 Si window array was defined by a
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50 20 photolithography process combined with wet etching using buffered oxide etch (BOE) solution.
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52 21 Then, the WS2 film was in-situ grown on the patterned SiO2/Si substrate. Au electrodes were
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55 22 fabricated on WS2 film by photolithography and e-beam evaporation. A Cu foil was connected to
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3 1 Si via In/Ga and high-purity silver conducting paint. After that, a 4×4 device array of the WS2/Si
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6 2 heterojunction (sixteen independent devices) was obtained. The schematic diagram of the device
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8 3 fabrication process is shown in Figure 2.
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11 4 The performance of WS2/Si heterojunction devices was evaluated by a measurement system
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5 including a semiconductor characterization system (Keithley 4200-SCS, Keithley), a spectrometer
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16 6 (Omni-λ300, Zolix), an oscilloscope (DPO2012B, Tektronix), light sources and a waveform
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18 7 generator (SDG1032X, Siglent).
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8 Results and Discussions
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25 9 The XRD patterns of as-obtained WS2 sample are shown in Figure 1a. The strong peaks verified
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27 10 the high-quality WS2 layers stacked along the (002) direction. The two Raman modes E2g and A1g
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29 11 at 354.6 and 422.8 cm-1 were clearly observed as shown in Figure 1b, indicating a high-quality
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32 12 film obtained as well. The wavenumber difference between the two modes is 65.7 cm-1, revealing
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34 13 a multilayered structure of the as-obtained WS2.36 The multilayered structure was further
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36 14 confirmed by the AFM measurement (∼5.6 nm), as depicted in Figure 1c. Furthermore, the
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39 15 chemical composition of WS2 film was investigated by XPS, as shown in Figure 1d and e. One
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41 16 can clearly see that the well-defined peaks can be acquired by fitting XPS spectra of W4+ and S2-
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43 17 regions, respectively, precluding the presence of any impurities.
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18 To explore optoelectronic properties of the as-synthesized WS2 samples, 4×4 arrayed WS2/Si
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49 19 heterojunction devices were integrated on the SiO2/Si substrates, and the fabrication procedures
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51 20 were shown in Figure 2. (More details are referred to the experiment section). Figure 3a shows a
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53 21 digital photograph of 16 photodiode arrays. Typical dark current-voltage (I-V) curve of the as-
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56 22 assembled device is shown in Figure 3b. The rectification behavior suggests the p-n diode was
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3 1 formed across the interface of WS2/Si, because the formation of good Ohmic-contacts were
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6 2 revealed for Au-WS2 and In/Ga alloy-Si (Inset of Figure 3b). A rectification ratio over 102 under
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8 3 ± 5 V operating conditions was obtained. When the device was illuminated by different laser
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10 4 diodes with wavelengths of 265, 650, 780, 980, 1310 and 1550 nm, the current at reverse bias of
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5 the heterojunction device increased sharply, as shown in Figure 3c. Notably, the remarkable
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15 6 photovoltaic effects of WS2/Si heterojunction can be observed (Inset of Figure 3c). The current at
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17 7 zero bias greatly increased from 2.5×10-12 A under a dark condition to 4×10-7 A at 265 nm (2.1
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8 mW/cm2), 1.3×10-6 A at 650 nm (42.6 mW/cm2), 1.5×10-6 A at 780 nm (54.2 mW/cm2) and 5×10-6
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22 9 A at 980 nm (57.2 mW/cm2), respectively, leading to high Ion/Ioff ratios. Therefore, we can easily
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24 10 conclude that WS2/Si heterojunction device can function as a self-powered photodetector.
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26 11 Subsequently, in Figure 3d, real-time photoresponse characteristics of the WS2/Si heterojunction
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29 12 photodetector to light illumination with different wavelengths at 0 V were recorded. The results
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31 13 suggest that the as-assembled heterojunctions exhibited high and broadband photosensitivity to
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33 14 different light wavelengths in range from deep UV (200 nm) to mid-infrared (MIR, 3043 nm) with
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15 stable, fast, repeatable photoresponse, and a high Ion/Ioff over 106 under light illumination of 980
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38 16 nm (57.2 mW/cm2). Importantly, the pronounced responses at 1310 and 1550 nm indicate its
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40 17 potential applications for optical communication and fiber optic cable testing in O-band and C-
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18 band.37 Furthermore, the device can be operated in mid-infrared regime (3043 nm, 35.9 mW/cm2)
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45 19 by forming type-II band alignments, which will be discussed later. Such special spectral selectivity
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47 20 can be further revealed by a spectral response at a constant intensity, as revealed in Figure 3e.
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49 21 Apparently, the heterojunction photodetector exhibits broadband photoresponse with the highest
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52 22 sensitivity around 900 nm, being well consistent with the absorption of Si.38 Moreover, the
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54 23 absorption spectrum of WS2/Si heterojunction was investigated, which is in accordance with the
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3 1 response spectrum. The longer wavelength photoresponse (>1200 nm) of WS2/Si heterojunction
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6 2 photodetector is far beyond the corresponding bandgaps of WS2 and Si, which is correlated to the
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8 3 type-II heterostructure band alignment.18 In Figure 3f, a type-II heterojunction band alignment was
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10 4 formed between n-WS2 and p-Si, which is capable of generating interlayer excitation due to the
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5 small gap between valence band maximum of Si and conduction band minimum of WS2.
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15 6 Therefore, this special band alignment allows a direct transition from the valence band of Si to the
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17 7 conduction band of WS2 under infrared light with a wavelength below the band-gaps of WS2 and
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8 Si. Such excitation is also observed in other heterojunction photodetectors made of MoTe2-MoS2
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25 10 Light intensity plays an important role in performance evaluation of photodetectors. Hence,
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27 11 light intensity-dependent photoresponse properties of WS2/Si heterojunction photodetector were
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30 12 investigated, as demonstrated in Figure 4. Figure 4a shows the I-V characteristics of WS2/Si
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32 13 heterojunction photodetector under 980 nm illuminations with light intensities varying from dark
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34 14 to 57.2 mW/cm2. The photocurrents of the device at reverse bias heavily reliant on light intensity,
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15 and increase from 2.5×10-12 A in dark to 5×10-6 A at 57.2 mW/cm2 under zero bias. The real-time
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39 16 photoresponses to 980 nm light with varying light intensity were plotted in Figure 4b. The Ion/Ioff
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41 17 of the photodetector can be adjusted from 102 (0.39 μW/cm2) to 106 (57.2 mW/cm2) by changing
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18 the power intensity of incident light. It is worth noting that a high Ion/Ioff of ~102 was achieved
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46 19 under a weak light intensity of 0.39 μW/cm2, revealing its ability to detect ultra- weak optical
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48 20 signals. The dependence of the photocurrent on the light intensity was depicted in Figure 4c, which
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50 21 exhibited a good linear relationship of photocurrent and light intensity in double logarithmic
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53 22 coordinates with a power exponent of 0.72 by fitting power law of I∝Pθ.16, 40 The obtained value
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3 1 is less than 1 due to the existence of trap states between the Fermi level and the conduction band
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9 3 Another two important figure of merits for photodetector, the responsivity (R) and specific
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11 4 detectivity (D*) of WS2/Si heterojunction photodetector can be calculated by the following
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5 formulas:43
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Popt  S
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(2)
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8 where Iph, Popt, S, A, e and ID are photocurrent, light intensity, irradiation area, device area, unit
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31 9 charge and dark current, respectively. The R and D* with varying light intensities (980 nm) were
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33 10 plotted in Figure 4d. Both R and D* increased with decreasing light intensity, and reached 224
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11 mA/W and 1.5×1012 Jones (1 Jones = 1 cm Hz1/2 W-1) under a light intensity of 0.03 μW/cm2 at 0
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38 12 V, respectively, which is associated with increased carrier recombination dynamics under higher
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40 13 light intensity. Moreover, a high R of 8.3 A/W and D* of 4.6×1014 Jones can be obtained under a
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42 14 bias voltage of -5 V. Such results are much superior to previous reported results.27, 36, 44-45 In a
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45 15 near-future study, it is expected that the responsivity can be further enhanced by optimizing the
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47 16 device configuration to facilitate carrier separation/transport effectively and appropriate surface
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49 17 passivation to lower the surface recombination.46 In addition, the improvement of the crystallinity
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18 of 2D layered WS2 film and the introduction of plasmonic nanostructures resonated in the NIR
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54 19 region are also effective methods for enhancing photocurrent and then resulting in higher
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3 1 To evaluate the response speed of this WS2/Si heterojunction photodetector, the frequency
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6 2 responses of the photodetector were investigated. The responses to the pulsed laser of 980 nm with
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8 3 different frequencies were monitored by an oscilloscope, as shown in Figure 5a. The response to
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10 4 light signals of 1 and 8 kHz were exhibited in Figure 5b and c, which demonstrated stable and fast
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5 response to pulsed optical signals of 980 nm. From the relative balance [(Imax-Imin)/Imax] versus the
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15 6 frequency as shown in Figure 5d, a wide frequency response range over 80 kHz and a high 3dB
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17 7 frequency (f3dB) of 8 kHz were observed for the WS2/Si heterojunction photodetector, suggesting
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8 that such photodetector has the ability to monitor ultrafast varying optical signals. The response
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22 9 speeds were investigated by calculating the rising and falling time of single response cycle at
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24 10 different frequencies. A fast response speed of 16.2/29.4 μs was obtained at a frequency of 8 kHz
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29 12 reveals that the response speeds of rising and falling decreased with the increasing frequency, and
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31 13 reached 3.8/11μs at 30 kHz. Table 1 summarized the performance of the WS2/Si heterojunction
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33 14 photodetector and some reported WS2-based photodetectors for comparison. Notably, the
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15 performances of WS2/Si heterojunction photodetector in our work are better than the reported
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41 17 For accurate detection of infrared signals in a complex environment, the polarization information
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18 of incident light should be provided.48 The anisotropic crystal structure of WS2 makes it sensitive
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46 19 to polarized light.49 Hence, the photoresponse properties of the WS2/Si heterojunction device to
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48 20 polarized light were investigated, and the results are shown in Figure 6. A polarizer, which can
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50 21 turn natural light into polarized light, was put between the laser diode of 980 nm and the WS2/Si
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53 22 heterojunction device. The photocurrent versus the polarization angle of incident light was plotted
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55 23 in Figure 6b. The results demonstrated that the photocurrent was highly dependent on the
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3 1 polarization angle. The measured photocurrent reached peak values at polarization angles of 0°
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6 2 and 180°, and valley values at polarization angles of 90° and 270°, which is well consistent with a
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8 3 sine function. And a high peak-to-valley ratio of 2.8 can be obtained. The high polarization
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10 4 sensitive property of the WS2/Si heterojunction device is attributed to the strongly anisotropic
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5 absorption of 2D WS2 film.48
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16 6 Furthermore, the stability and repeatability of the WS2/Si heterojunction devices were
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18 7 investigated, as shown in Figure 7. A consecutive response of 2000 cycles of the WS2/Si
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23 9 of the device with no degradation even after 2000 consecutive response. In this work, a 4×4 device
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25 10 array including sixteen independent heterojunction devices was fabricated. The spatially resolved
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27 11 photocurrent mapping under light illumination of 980 nm with a light intensity of 57.2 mW/cm-2
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30 12 at zero bias was shown in Figure 7b. The as-obtained photocurrent from different device arrays is
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32 13 approaching to each other. The uniform distribution of photocurrent indicates the good
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34 14 repeatability of the WS2/Si heterojunction photodetectors, suggesting that it has great potential for
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40 16 Conclusion
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43 17 In summary, the large-area 2D layered WS2 films were synthesized by a two-step thermal
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18 decomposition method. The as-synthesized 2D layered WS2 films were further demonstrated to be
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48 19 a good candidate to integrate with Si, resulting in high-performance photodetector. The superior
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50 20 properties of a high polarization sensitivity, a high Ion/Ioff over 106, a responsivity of 224 mA/W, a
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52 21 specific detectivity of 1.5×1012 Jones, as well as a fast response speed of 16/29 μs at 0 V were
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55 22 achieved. Remarkably, the as-assembled device exhibited broadband response up to 3043 nm by
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3 1 benefiting from special advantages of type-II band alignments. Therefore, as-fabricated WS2/Si
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29 3 Figure 1. (a) XRD patterns and (b) Raman spectrum of the synthesized WS2 film. (c) AFM image
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31 4 and corresponding height profile. The XPS spectra show the binding energies of (d) W and (e) S
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42 2 Figure 3. (a) A photograph of the WS2/Si heterojunction device. (b) I-V curves of heterojunction
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3 device in linear and logarithmic coordinates in dark. The inset shows I-V curves of WS2 and Si
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47 4 with Ohmic contacts. (c) I-V curves of the device under light illumination with different
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51 6 photoresponse properties under light illumination with different wavelengths. (e) Wavelength-
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54 7 dependent responsivity and absorption spectrum of the WS2/Si heterojunction device. (f) Energy
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56 8 band diagram of the n-WS2/p-Si heterojunction under light illumination.
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30 2 Figure 4. (a) I-V curves and (b) time-dependent photoresponse of the WS2∕Si heterojunction under
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32 3 varied light intensities (980 nm, Vbias =0 V). (c) Logarithmic plot of the photocurrent versus light
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4 intensity. The curve is fitted well by the power law. (d) Responsivity and specific detectivity of
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37 5 the WS2/Si heterojunction photodetector as a function of light intensity.
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44 2 Figure 5. (a) A schematic diagram of the measurement configuration for frequency response.
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46 3 Photoresponse characteristics of the WS2/Si heterojunction to a pulsed light with frequencies of
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49 4 (b) 1 kHz and (c) 8 kHz, respectively. (d) The relative balance [(Imax-Imin)/Imax] vs. switching
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51 5 frequency. (e) Rising and falling edges for estimating rise time and the fall time at 5 kHz. (f) The
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20 2 Figure 6. (a) A schematic diagram of the polarization sensitivity measurement. (b) Normalized
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22 3 photocurrent of the WS2/Si heterojunction as a function of the polarization angle.
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2 Figure 7. (a) The stability of the WS2/Si heterojunction with 2000 photoresponse cycles. (b)
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20 3 Spatial resolved photocurrent mapping of a 4×4 heterojunction device array.
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3 1 Table 1. Comparison of the performances of WS2-based photodetectors.
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R D* Rise/fall
Device λ (nm) Self-powered Ion/Ioff Ref.
8 (mA/W) (Jones) time
9 Yes (0V) 106 224 1.5×1012 This
10 WS2/Si 200-3043 16/29 μs
No (-5 V) 103 8309 4.6×1014 work
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12
13 WS2/Si 365-1000 Yes (0V) 104 4 1.5×1010 39/48 μs 27
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15
WS2/MoS2 532 Yes (0V) 102 4.36 4.4×1013 4/4 ms 44
16 WS2/Si 340-1100 No (-5 V) ~102 5700 / 670/998 μs 36

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18 WS2/Si 400-1100 No (-2 V) / 1100 5×1011 42/76 ms 45
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20 WS2/Bi2Te3 370-1550 No (3 V) / 30400 2.3×1011 20/20 ms 50
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22 WS2 370-1064 No (9 V) / 510 2.7×109 4.1/4.4 s 26
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24 2
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26
27 3 AUTHOR INFORMATION
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30 4 Corresponding Author
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5 *Di Wu, E-mail: wudi1205@zzu.edu.cn
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36 6 *Longhui Zeng, E-mail: lhzeng.hfut@gmail.com
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39 7 Notes
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41 8 The authors declare no competing financial interest.
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43
44
9 ACKNOWLEDGMENT
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47 10 Thanks for the financially support from the National Natural Science Foundation of China (Nos.
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49 11 61605174 and 11604302), the Key Projects of Higher Education in Henan Province (No.
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51 12 17A140012) and Young top-notch talent of Zhengzhou University (No. 32310142).
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55 13
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6 2 In-situ fabrication of 2D WS2/Si type-II heterojunction for self-powered broadband
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4 Enping Wu,a Di Wu,*, a Cheng Jia,a Yuange Wang,a Huiyu Yuan,b Longhui Zeng,*,c Tingting
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powered broadband photodetector with response up to mid-infrared

is published by the American Chemical Society. 1155 Sixteenth Street N.W.,

16 WS2/Si 340-1100 No (-5 V) ~102 5700 / 670/998 μs 36

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