Paper-based Broadband Flexible Photodetectors with van der Waals materials

doi:10.21203/rs.3.rs-1494690/v1

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Paper-based Broadband Flexible Photodetectors with van der Waals materials

https://doi.org/10.21203/rs.3.rs-1494690/v1

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Layered metal chalcogenide materials are exceptionally appealing in optoelectronic devices thanks to their extraordinary optical properties. Recently, their application as flexible and wearable photodetectors (PDs) have received a lot of attention. Herein, broadband and high-performance paper-based PDs were established in a very facile and inexpensive method by rubbing molybdenum disulfide (MoS₂) and titanium trisulfide (TiS₃) crystals on papers. Transferred layers were characterized by SEM, EDX mapping, and Raman analyses, and their optoelectronic properties were evaluated in a wavelength range of 405-810 nm. Although the highest and lowest photoresponsivities were respectively measured for TiS₃ (1.50 mA/W) and MoS₂ (1.13 μA/W) PDs, the TiS₃-MoS₂ heterostructure not only had a significant photoresponsivity but also showed the highest on/off ratio (1.82) and fast response time (0.96 s) compared with two other PDs. This advantage is due to the band offset formation at the heterojunction, which efficiently separates the photogenerated electron-hole pairs within the heterostructure. Numerical simulation of the introduced PDs also confirmed the superiority of TiS₃-MoS₂ heterostructure over the other two PDs and exhibited a good agreement with the experimental results. Finally, MoS₂ PD demonstrated very high flexibility under applied strain, but TiS₃ based PDs suffered from its fragility and experience a remarkable drain current reduction at strain larger than ± 0.33%. However, at lower strains, all PDs displayed acceptable performances.

Flexible

Paper

Photodetectors

MoS2

TiS3

Heterostructure

Strain

With the development of smart and Internet of Things (IoT) based technologies, great efforts have been made on wearable and flexible electronic devices which are mostly implemented on Polyethylene terephthalate (PET) and Polydimethylsiloxane (PDMS) substrates¹. However, in addition to high manufacturing costs and lack of biodegradability, their fabrication processes require advanced laboratory equipment, which obstruct their possible practical applications². Flexible paper-based electronic devices are a new class of high-performance devices that offer admirable properties with facile and low-cost fabrication processes, ending in lightweight and environmentally friendly devices that are very promising for the future of smart electronics^3–5. Flexible photodetectors (PDs), as a member of this family, have received a great deal of attention, suitable for optoelectronic systems such as optical communications, environmental monitoring, and imaging⁶.

Two-dimensional (2D) materials, especially the chalcogenides family, have been increasingly used in optoelectronic devices in recent years due to their adjustable band gap, high electrical conductivity, and effective light-matter interactions⁷. Metal chalcogenide based PDs have shown high photoresponsivity, fast response time, and high quantum efficiency⁸. Interestingly, their paper-based PDs also demonstrates such a high performance^9–11. Sahatiya et al. fabricated a MoS₂-Carbon Quantum dot (CQDs) based PD on cellulose paper using a hydrothermal growth of MoS₂ and casting of CQDs¹². Their reported device showed a photoresponsivity of 18 mA/W in the visible region with a response time of ~ 0.57 s. Selamneni et al. hydrothermally grown MoS₂ on cellulose paper followed by decorating with various metal nanoparticles (Au, Pt, and Pd)¹¹. The photoresponsivities and response times of the PDs were measured to be around 45–100 mA/W and 0.9–1.2 s in the visible range, respectively. Cordeiro et al. introduced near-infrared PDs by growing MoS₂ on cellulose paper using a hydrothermal technique. Their PD showed a photoresponsivity of about 200 mA/W and a response time of 3.7 s ¹³. However, majority of methods used for the fabrication of paper-based PDs are time-consuming, complex, and consisting wet procedures. In contrast, rubbing of bulk crystal on ordinary paper can be a potential alternative to facile realization of paper-based PDs through a simple, fast and completely dry process. As an example, Mazaheri et al. transferred MoS₂ flakes by rubbing the corresponding crystal on paper and reported a paper based PD with a photoresponsivity of 1.5 µA/W in a wavelength range of 365 to 940 nm¹⁴.

In this work, MoS₂ and TiS₃ flakes were transferred on papers by rubbing their corresponding bulk crystals. Three types of MoS₂, TiS₃, and TiS₃-MoS₂ PDs were fabricated and their optoelectronic properties were carefully evaluated in the wavelength range of 405 to 810 nm. Based on the results, the highest photoresponsivity were measured for TiS₃ PDs and the lowest for MoS₂ PDs. In the case of TiS₃-MoS₂ (MoS₂ film was placed on top of the TiS₃ film and exposed to light), it exhibited a faster response time, and higher on-off ratio thanks to formation of band offset at semiconductor heterojunctions. Numerical simulations also confirmed the superiority of TiS₃-MoS₂ PDs over MoS₂ PDs. Moreover, to evaluate the flexible performance of the PDs, the introduced devices were bent on both positive and negative curvatures and their I_ds-V_ds and photocurrent characteristics were measured under strain range of ± 0.27% to ± 0.54%. The results showed that MoS₂ PDs had high flexibility, but TiS₃ based PDs were associated with the decline of drain current and photodetection responsivity at applied strains larger than ± 0.33%.

SEM image and XRD analysis of the grown TiS₃ microcrystals are presented in Figure S1. Before transferring the flakes, the surface of paper was investigated by SEM and EDX measurements. As can be seen in Figure S2a, the paper is formed by stacked cellulose fibers and it presents deep gaps/voids between fibers. EDX analysis also confirms the presence of carbon (C), oxygen (O), calcium (Ca), silicon (Si), aluminum (Al), iron (Fe), sodium (Na), and manganese (Mg) in the raw paper where their atomic percentages are listed in the inset of Figure S2b.

Figure 1 shows the characterization of the deposited flakes on paper substrates. The schematic illustration of the TiS₃-MoS₂ heterostructure and its corresponding photograph are also presented in panels (a) and (b) of Fig. 1, respectively. Figure 1c exhibits the SEM image of the MoS₂ flakes on the paper. According to the figure, MoS₂ flakes cover the fibers and gaps between fibers of the paper. The deposited TiS₃ flakes are also presented in Fig. 1d in which the thickness of the film is measured to be ~ 10 µm. Moreover, the SEM image of the TiS₃-MoS₂ heterostructure is observed in Fig. 1e. Due to softness and flexibility of MoS₂, it forms a smoother film than TiS₃ on paper, which is visible in Fig. 1e. The EDX analysis of MoS₂, TiS₃, and TiS₃-MoS₂ samples on papers is presented in Figs. 1f-g. By rubbing MoS₂ on the paper, the Mo and S elements becomes significant (Fig. 1f). The EDX analysis of TiS₃ sample also proves the presence of S and Ti elements according to Fig. 1g. SEM-EDX analysis of transferred TiS₃ flakes is also presented in Figure S3. In the case of TiS₃-MoS₂ film, dominant elements are S, Mo, and Ti (Fig. 1h). The C, O and Ca elements come from raw paper. Table S1 summarizes the element contents of all samples with their weight and atomic percentages.

Figure 2a exhibits the magnified SEM image of the TiS₃-MoS₂ film where the MoS₂ film is deposited on the TiS₃ film. However, some TiS₃ microcrystals may also appear on top of the film due to the rubbing process. The Raman spectra of MoS₂, TiS₃, and TiS₃-MoS₂ samples are also presented in Fig. 2b. For MoS₂, E¹_2g and A_1g peaks are found at 379 and 403 cm^− 1, respectively¹⁵. In the case of TiS₃, the 193, 385 and 627 cm^− 1 peaks refer to A_g and E_g modes, respectively¹⁶. There is also one additional peak located at 507 cm^− 1, which refers to B_1g peak of TiO₂¹⁷. This oxide peak may have appeared during the growth of TiS₃ microcrystals in the ampoule process. The Raman spectrum of TiS₃-MoS₂ sample contains all peaks of both structures. Figure 2c shows the mapping analysis of the TiS₃-MoS₂ sample where the dominant elements are separately shown in Fig. 2d. Accordingly, O, C, and Ca elements are due to the raw paper, and elements of Ti, Mo, and S originate from the TiS₃ and MoS₂ films. It can be seen that all elements are uniformly distributed on the paper.

To investigate the optoelectronic properties of the films, MoS₂, TiS₃, and TiS₃-MoS₂ PDs were fabricated. Details of their fabrication are provided in the experimental section. The fabrication steps of MoS₂ and TiS₃ PDs are shown in Figures S4 and S5, respectively. In the case of TiS₃-MoS₂ PD, the fabrication steps are presented in Fig. 3.

Panels (a) to (c) of Fig. 4 display I-V characteristics of the MoS₂, TiS₃, and TiS₃-MoS₂ PDs at a bias range of -10 to + 10 V in dark and under 532 nm laser illumination at different power intensities. In all three PDs, significant photocurrents were generated compared to the dark state. The incident power is normalized in terms of laser spot and PD’s channel areas. Accordingly, the effective incident power is calculated as:

P_eff = P_laser×A_device/A_laser (1)

Where P_laser is the power of the laser, A_device is the area of the PD’s channel, and A_laser is the area of the laser spot. The diameter of the 532 nm laser spot was 2.81 mm and its area (A_laser) was measured to be 6.22 mm². As the laser intensity increases, the photocurrent also increases for all three PDs. In detail, the drain currents were measured in the range of ~ 0–4 nA, ~ 0–8 µA and ~ 0-450 nA for MoS₂, TiS₃, and TiS₃-MoS₂ PDs at a biasing voltage of 0–10 V, respectively. Interestingly, the I_ds in TiS₃-MoS₂ is significantly higher than that of individual MoS₂, which indicates the effective role of the band offset formation in increasing the photocurrent. The I-V curves of the all PDs in response to 405, 655, and 810 nm laser illuminations are also shown in Figure S6 where all PDs respond to the laser irradiation by an increase in current. Figure 4d-i compare the photocurrent and photoresponsivity of all three PDs at different power intensities of 532 nm at an applied voltage of 10 V. According to Fig. 4d-f, with increasing effective incident power (from zero to a few mW), increase in the photocurrents are occurred. In the MoS₂ PD, the photocurrent increases to about 1.6 nA. For TiS₃, this value is more noticeable and a 1.0 µA increase of photocurrent is observed. In the case of TiS₃-MoS₂ PD, photocurrent increases up to 300 nA. The photoresponsivity of the PDs are calculated based on the following Eq. 1⁸:

R = I_ph/P_eff (2)

Where I_ph is the photocurrent of the PDs. In the MoS₂ PD, increasing the effective power associates with decrease of the photoresponsivity. The same trends are also observed for TiS₃, and TiS₃-MoS₂ PDs. As the incident power increases, more photocarriers are generated, which increases the recombination rate of photogenerated carriers or the possibility of being captured by the traps, leading to a decrease in R ^19,20. In general, the photoresponsivities are measured in the range of 0.4–1.2 µA/W, 0.4–1.6 mA/W, and 90–170 µA/W for MoS₂, TiS₃, and TiS₃-MoS₂ PDs, respectively. Accordingly, the photoresponsivity of the last two PDs is three and two orders of magnitude greater than that of MoS₂ PD.

Figure 5a-c show the measured photocurrent in terms of the different effective powers of the 532 nm laser. Accordingly, an increase in the optical powers leads to an increase in photocurrent in all PDs. Panels (d) to (f) of Fig. 5 display the time trace response of the PDs to 532 nm laser illumination at a drain voltage of 10 V at an incident power of 10 mW. Rise time (τ_on) is defined as the time taken to increase the current from 10–90% of its baseline under laser illumination²¹. The fall time (τ_off) is the time required to reduce the current from 90–10% of its baseline²². For MoS₂, the rise and fall times are measured to be 2.17 and 9.99 s, respectively. In the TiS₃ PD, the τ_on and τ_off of 2.4 and 17.44 s are measured and in the TiS₃-MoS₂ PD, τ_on and τ_off of about 0.96 and 8.42 s are calculated that it shows faster switching performance compared with two other PDs.

Figure 6a compares the photoresponsivity of several fabricated PDs at an applied voltage of 10 V under a laser wavelength of 532 nm. It is observed that all three TiS₃ PDs have the highest photoresponsivity, followed by TiS₃-MoS₂ and MoS₂ samples, respectively. In general, the R are measured in the range of 0.67–1.56 mA/W for TiS₃ PDs and 0.20–1.93 µA/W in the case of MoS₂ PDs. For TiS₃-MoS₂ PDs, these values are measured in the range of 0.08 to 0.19 mA/W. Accordingly, MoS₂ has the lowest photoresponsivity and TiS₃ possess the highest photoresponsivity. However, both photoresponsivity and photocurrent of TiS₃-MoS₂ PDs are considerable compared to the MoS₂ PD. Moreover, a similar trend is observed in the order of magnitude of all calculated R in these PDs. Figure 6b shows the photoresponsivity of all three devices in terms of different laser wavelengths at the same power of 15 mW and supply voltage of 10 V. All three PDs have a broad response within the range of 400 to 800 nm. The photoresponsivity of the TiS₃ PDs are one order of magnitude greater than that of the TiS₃-MoS₂ PDs and two orders greater than that of the MoS₂ PDs. Figure 6c compares the measured I_on/I_off ratio and dark current of all three PDs under 532 nm laser irradiation. The error line shows the deviation of the values obtained for the same PDs. The on-off ratio (I_on/I_off) is usually used to describe the signal-to-noise ratio²³. According to Fig. 6c, the values of 1.35, 0.17, and 1.82 are obtained for MoS₂, TiS₃, and TiS₃-MoS₂ PDs, respectively. Based on them, the highest signal-to-noise ratio is related to the TiS₃-MoS₂ PDs. Interestingly, the dark currents are lowest in MoS₂ (~ 1.2 nA) and highest in TiS₃ (~ 6.0 µA). Since the light detection mechanism is based on the change of drain current in these PDs, less dark current provides better performance in light detection as will be discussed below²⁴. Another important parameters are the rise and fall times which are presented in Fig. 6d. Accordingly, the TiS₃-MoS₂ PD has the fastest response time to laser radiation than the other two PDs. Figure 6e shows the energy band diagram of the TiS₃-MoS₂ heterostructure and its corresponding photodetection mechanism. TiS₃ is an n-type semiconductor with an energy band gap of 1.1 eV and MoS₂ is also an n-type semiconductor with an energy band gap in the range of 1.2–1.8 eV ^25,26. Here, the energy band gap of bulk MoS₂ is considered because most layers are thick, although the deposited film can contain single and few layers of MoS₂. The electron affinities of MoS₂ and TiS₃ are around 4 and 4.7 eV, respectively, and hence the conduction band of TiS₃ is located of MoS₂, forming an n-n⁺ heterostructure^27,28. In the MoS₂ film under laser irradiation, electron-hole pairs are generated and the photogenerated electrons enter into the TiS₃ due to its lower conduction band which prevents electrons from recombination with the holes. Moreover, the valence band of MoS₂ is located higher than that of TiS₃ resulting in transferring of minority holes from TiS₃ into MoS₂. Hence, the recombination rate of the carriers is decreased in the heterostructure. Such charge separation in the heterostructure is responsible for faster response time, and improved photoresponsivity of the heterostructure compared with individual MoS₂ PDs.

Since the substrate is made of paper, the performance of the introduced PDs was thoroughly investigated under applied strain. For this purpose, a homemade setup was fabricated to apply strain to the substrates as shown in Figure S7. This setup includes a cage covered with aluminum foil to act as a Faraday cage. The sample is fixed to a motor shaft through a hook to provide upward and downward strains by moving in a clockwise or counter-clockwise direction. The strain applied to the PDs was calculated according to ε = t/2R equation, where t is the thickness of the substrate and r is the radius of bending curvature²⁹. Figure S8 presents the applied strains in the PDs, which are performed in the range of -0.54% to + 0.54%˚. As can be seen, at strains larger than ± 0.33%, a significant bending is occurred in the substrates.

Figures 7a and 7b show the schematic of applying the upward and downward strain in the PDs under exposing to 532 nm laser illuminations, respectively. Panels (c), (d), and (e) of Fig. 7 compare the I_ds-V curves of the MoS₂, TiS₃, and TiS₃-MoS₂ PDs in the flat state and under negative and positive strains, respectively. For the MoS₂ sample, it is observed that the drain current in the flat state almost remains the same as under different applied strains without any significant change. The flexible and soft structure of MoS₂ is the main reason for this behavior³⁰. For TiS₃, it is found that the I_ds decreases after applying downward strains, but a more significant decrease is observed in the upward strains. Moreover, after upward strain, by returning the TiS₃ to its flat position, current does not return to its original value of before any strain. The structure of TiS₃ is more fragile than that of MoS₂, and bending can break the contact between TiS₃ and Ag paste, affecting the conductivity³¹. As a result, even after the sample has returned to the flat state, the current dramatically suffers from decline. A similar trend is observed in the TiS₃-MoS₂ PD, but with a more noticeable decrease after positive strains, which could be due to the separation of the two films at the interface and the reduction of the electric field in the channel. Figures 7f-h show the photocurrent characteristics of all PDs under 532 nm laser irradiation at a drain voltage of 10 V and an incident power of 15 mW. For MoS₂ PD, the photocurrent is well switched under negative and positive strains of 0.33% similar to the flat state. In the case of TiS₃, the photocurrent decreases in both applied strains of -0.33% and + 0.33%, but TiS₃-MoS₂ shows a more noticeable decrease compared to its flat state. As discussed, the brittle structure of TiS₃ as well as the separation of the two films at the junction, especially at a strain of + 0.33%, play important roles in this performance deterioration of the TiS₃ based PDs.

Numerical simulation is employed to present further insight about the physics of light-induced generation-recombination processes for charged carriers in these devices. We used the model to calculate the photocurrent of the devices in response to the incident light under various biasing conditions. Details of the simulation can be found in the supporting information section. Panels (a) to (c) of Fig. 8 depict the schematic of the devices consisting MoS₂, TiS₃ and heterostructure with stacked layers of both materials. Overlapped part in the heterostructure device was exposed to the incident light with the wavelength of 532 nm. Stray electromagnetic field due to unintentional exposure is also took into the account. Corresponding light-induced electric field can be seen in Fig. 8d for all devices due to laser exposure. Vertical electric field was established by applying a voltage difference between the two terminals at both ends, where contacts are located. Figure 8e-f show the electron and hole concentrations under this biasing condition in a logarithmic scale, respectively. As can be seen, the distribution of electrons and holes in the two structures of MoS₂ and TiS₃ is almost uniform, but in the TiS₃-MoS₂ device, the band offset accelerates the separation of electrons and holes and causes a non-uniform distribution of carriers at the two-layer boundary. These results indicate that the formed n-n + heterostructure can more efficiently separate the charge and confirms its superior optoelectronic performance compared with the individual MoS₂ case.

At various light intensities, I-V characteristic curves has been simulated for MoS₂, TiS₃, and TiS₃-MoS₂ photodetectors. The obtained curves for drain currents are consistent with the measurements as illustrated in Figure S9a-c. Relative differences between the amplitude of photocurrent is in all devices is in total agreement with the experiments where TiS₃ and MoS₂ PDs have higher and lower photocurrents, respect to the hybrid structure under identical biasing and light exposure conditions.

Table 1 compares the performance of the introduced PDs with some other reported paper-based PDs. According to it, most of them have a photoresponsivity in the range of a few µA/W. In the case of MoS₂, it is observed that our introduced PD has a slightly higher photoresponsivity than the others. The TiS₃ PD shows a much higher photoresponsivity (in the range of mA/W), which has a significant improvement in performance compared to other reported PDs. However, it shows a larger dark current and a smaller on/off ratio than MoS₂ PDs which can limit its optical detection performance. Finally, the photoresponsivity of the TiS₃-MoS₂ heterostructure shows a significant improvement, which indicates its superiority over other works.

Table 1

Comparison of the performance of introduced paper-based PDs with other PDs based on different 2D materials.
Paper-based PDs	V_ds	λ	R	ref
Te—TiO₂	0 V	400 nm	30 µA/W	³²
ZnS-MoS₂	1 V	554 nm	18 µA/W	³³
MoTe₂	1 V	532 nm	1.1 µA/W	³⁴
MoSe₂	1 V	532 nm	0.2 µA/W
WS₂	1 V	532 nm	0.06 µA/W
MoS₂	1 V	532 nm	0.02 µA/W
MoS₂	20 V	532 nm	1.1 µA/W	14
MoS₂	10 V	532 nm	1.2 µA/w	This work
TiS₃	10 V	532 nm	1600 µA/W
TiS₃-MoS₂	10 V	532 nm	170 µA/W

The two-dimensional (2D) layered family of transition metals chalcogenides shows high potential as photodetectors because they not only interact effectively with light but also provide high carrier transport properties. In this report, a very simple, fast and promising clean method is introduced to fabricate the paper-based photodetectors using MoS₂, TiS₃ and their integration. The all introduced photodetectors show remarkable photoresponsivities in the range of 405 to 810 nm. In the case of TiS₃-MoS₂ heterostructure, it associates with fast response time and large on-off ratio compared to individual MoS₂ and TiS₃ photodetectors. The numerical simulation results are consistent with the experimental results and confirm the superiority of the hybrid structure over the two other PDs. Moreover, the bending results of the photodetectors indicate that in applied strains smaller than ± 0.33%, these devices still show acceptable performance.

Material: Naturally occurring molybdenite crystal, from Wolfram Camp Mine, Queensland, Australia, were used. Silver paste was purchased from Dycotec Materials, UK DM-SIP-3060S. Ordinary papers (CopiMax, Thailand) were used as substrates.

TiS₃ preparation: TiS₃ microcrystals were synthesized by a solid-gas reaction of titanium powder through direct sulfurization. In detail, titanium powder (Goodfellow, > 99% purity) and sulfur powder (Merck, > 99.9% purity) were vacuum sealed in an ampule and heated up to 500 ˚C for 20 hours. Then, the ampule was cooled down to room temperature and grown microcrystals were collected.

Fabrication of MoS₂ (TiS₃) paper-based photodetector: First, a piece of paper with 2×6 cm² dimensions was cut and attached on a slide glass using adhesive tape. A shadow mask (a 1×6 mm² rectangular window) was then opened in the center of the paper with adhesive tape. A piece of bulk MoS₂ (or TiS₃) was rubbed several times along the length and width of the open-window reign. After deposition of a homogeneous layer of MoS₂ (TiS₃), the mask was removed from the paper. Silver paste was then placed on the both sides of the deposited film, and two pieces of soft copper wire were mounted on the paste and kept at room temperature for 24 hours for improving the adhesion. Then, the dried silver paste was covered with epoxy glue for strengthening and achieving higher mechanical stability. The photograph of the fabrication steps of MoS₂ and TiS₃ PDs are presented in the supporting file.

Fabrication of TiS₃-MoS₂ paper-based photodetector: First, a piece of paper with a dimension of 2×6 cm² was cut and attached to a slide glass. A rectangular shadow mask (mask 1) was opened by the adhesive tape in the center of the paper. With the use of another mask (mask 2), this part was divided into two sections with dimensions of 1×4 mm² (for TiS₃ deposition) and 1×2 mm² (for MoS₂ deposition). A piece of bulk TiS₃ was rubbed several times in the open-window region. Then, mask 2 was removed from the paper and MoS₂ crystal was finger-rubbed several times on the 1×2 mm² part of the bare paper and 1×1 mm² part of the deposited TiS₃. Thus, the center of the sample (device) with dimensions of 1×1 mm² was a film composed of TiS₃ and MoS₂, in which TiS₃ was placed beneath the MoS₂ film. After removing mask 1 from the paper, a homogeneous film composed of TiS₃, MoS₂ and, TiS₃-MoS₂ with dimensions of 1×3, 1×1, and 1×1 mm² can be achieved, respectively. Similar to previous PDs, copper wires were added to both sides of the film. The TiS₃-MoS₂ PD is ready for testing.

Characterizations: SEM images and EDX analyses were taken by TESCAN MIRA 3 and EDX (Energy-dispersive X-ray) systems. Crystalline structure was identified by using a Panalytical X`Pert Pro X-ray diffractometer at glancing angle configuration (incident angle of 1.7º) with CuKα radiation. Raman spectra of the transferred flakes were measured by Avantes (AVASPEC-ULS3648-RS) system under 532 nm laser illumination. Electrical measurements were carried out by a Keithley 2450 source meter. Optical measurements were done under different laser excitations including 405, 532, 655, and 810 nm at room temperature in air ambient. Bending tests were performed with a homemade setup capable of applying both upward and strains.

Acknowledgments

This work was supported by the Iran National Science Foundation: INSF (grant number 98016920). MIRE Group authors acknowledge the financial support of the Spanish MICINN (RTI2018-099794-B-I00 project).

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No competing interests reported.

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Paper-based Broadband Flexible Photodetectors with van der Waals materials

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