Improved strain engineering of 2D materials by adamantane plasma polymer encapsulation

doi:10.21203/rs.3.rs-1942403/v1

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Improved strain engineering of 2D materials by adamantane plasma polymer encapsulation

https://doi.org/10.21203/rs.3.rs-1942403/v1

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published 30 Mar, 2023

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Two-dimensional materials present exceptional crystal elasticity and provide an ideal platform to tune electrical and optical properties through the application of strain. Here we extend recent research on strain engineering in monolayer molybdenum disulfide using an adamantane plasma polymer pinning layer to achieve unprecedented crystal strains of 2.8%. Using micro-reflectance spectroscopy, we report maximum strain gauge factors of -99.5 meV/% and − 63.5 meV/% for the A and B exciton of monolayer MoS₂, respectively, with a 50 nm adamantane capping layer. These results are corroborated with photoluminescence and Raman measurements on the same samples. Taken together, our results indicate that adamantane polymer is an exceptional capping layer to transfer substrate-induced strain to a 2D layer and achieve new heightened levels of crystal strain.

Strain engineering is a powerful technique to modify the optical and electronic properties of two-dimensional (2D) materials through the deformation of their crystal lattice. 2D materials present an outstanding resilience to mechanical deformations allowing for a broad range of tunability through strain engineering [1–8]. These strain properties have attracted great research interest but there are areas for further improvement and open challenges. In the vast majority of experiments relying on the deformation of a compliant flexible substrate, the strain transfer from substrate to crystal strongly depends on the Young’s modulus of the substrate itself [9, 10]: the higher the substrate’s Young’s modulus the higher the realizable strain transfer. This is particularly critical as some flexible polymer substrates may present very low Young’s modulus values, leading to an incomplete strain transfer from the deformed substrate to the 2D materials transferred on top. A second critical issue beyond this is that even when using substrates that ensure a good strain transfer, slippage of the flake typically limits the maximum strain that can be applied to roughly 0.8–1.4% [11]. These problems have motivated the scientific community to find viable solutions.

One investigated solution is trying to mitigate slippage by clamping the 2D material to the flexible substrate with metal contacts[12], so as to prevent the material from detaching from the substrate surface at high strain values. Nevertheless, this can lead to nonuniform strain that builds up at the contact locations and, unsurprisingly, relatively comparable uniaxial strain gauge factors have been obtained for MoS2 in metal clamped and unclamped samples [10, 11, 13–20]. Other works have tried to avoid slippage by covering the flake with a flexible polydimethylsiloxane (PDMS) layer [21–23] or with a polymethylmethacrylate (PMMA) film [24]; but a combination of large strain and gauge factor has not been obtained. An alternative and seemingly successful approach has been to use a spin coated polyvinyl alcohol (PVA) layer as a substrate [25]. The spin coated layer supposedly leads to better strain transfer through molecular bonding across the entire flake and at the edges. Using this technique, Li et al. found a large gauge factor of around − 136 meV/% for single-layer MoS2 but crystal strain was limited to 1.7%.

Here we implement a method to encapsulate 2D materials with nanometric films of adamantane (C10H16) plasma polymer to improve strain transfer and reduce slippage. Adamantane is the compound with the smallest cage structure of diamond crystal tand was isolated from petroleum in 1933 [26]. This material has been used in the field of medicine [27, 28], and for various applications in coatings for smart electronic displays [29] and as molecular building blocks for nanostructure self-assembly [30]. Adamantane plasma polymers were deposited at room temperature by solventless and scalable remote plasma-assisted vacuum deposition (RPAVD)[31, 32] using adamantane powder as precursor. These films present an extremely low roughness (RMS < 0.3 nm) and high transparency (bandgap 4.1 eV), thermal and chemical stability. Such properties together with the straightforward processing by dry etching and high conformality at the micro and nanoscale have prompted their applications in photonics[33, 34] and as protective layers for perovskite solar cells [35]. It is also worth stressing that the fabrication in downstream configuration, i.e. out of the glow discharge, provides high compatibility with the deposition on molecular materials as supported organic nanowires and graphene[36] without compromising their optical and electrical properties. In this work, we have deposited 50 nanometers of adamantane plasma polymer on top of several molybdenum disulfide (MoS2) monolayers that were previously transferred onto flexible polycarbonate substrates to test the improvement of the tunability of the bandgap of the material. We find a noticeable increase in the strain gauge factor for encapsulated flakes and reach unprecedented maximum crystal strains of 2.8%.

The adamantane polymer plasma encapsulation process consists of using remote plasma assisted vacuum deposition (RPAVD) to deposit a thin layer of adamantane polymer through the controlled sublimation of adamantane powder in the downstream region of an Ar microwave electron cyclotron resonance (ECR) plasma (Fig. 1(a)). We illustrate the utility of this encapsulation method by analyzing seven different single-layer MoS₂ samples. Figure 1(b) shows an optical image of a typical sample with a single-layer MoS₂ flake. We selected MoS₂ as it was one of the first isolated 2D semiconductors [37] and the modification of its properties through crystal deformation has been widely investigated [10–12, 14–23, 38–41]. This material consists of S-Mo-S layers that are held by weak van der Waal forces in a trigonal prismatic structure [42–45]. In its bulk form, MoS₂ presents an indirect bandgap around 1.2 eV; however, a monolayer of this material exhibits a direct bandgap of 1.8 eV and displays a considerable in-plane charge carrier mobility and high current ON/OFF ratio when employed in a transistor [46]. These properties make molybdenum disulfide an attractive semiconductor for use in optical, electronic and straintronic applications.

We have directly compared the effect of the adamantane encapsulation on the strain tunability of the optical properties of a single-layer MoS₂ flake. Figure 2 shows the micro-reflectance spectra of a single-layer MoS₂ flake by employing the three-points bending setup to bend the PC substrate to strain the 2D crystal (additional data sets for other flakes can be found in the Supporting Information, Figures S1-S8). Figure 2(a) presents the spectra acquired at different strain values before and after encapsulating the sample. The spectra exhibit two prominent peaks that correspond to the A and B excitons at around 1.9 eV and 2.0 eV and correspond to the direct bandgap transition at the K point of the Brillouin zone in monolayer MoS₂ [47–51]. It should be noted that the differential reflectance spectra obtained after encapsulating the sample are inverted due to the interference phenomena explained by a Fresnel-law-based model when one has a multilayer optical media with different refractive indexes [52]. Figure 2(b) shows the energy of the A and B peak positions as a function of the applied uniaxial strain before and after encapsulation. The slope of the linear trend followed by the experimental datapoints indicates the strain gauge factor (the change in exciton energy per % of uniaxial strain) for both excitons, being − 42.7 ± 1.9 meV /% and − 47.4 ± 5.5 meV/% for the A and B exciton, respectively, without encapsulation and − 76.6 ± 1.5 meV /% and − 59.1 ± 4.6 meV/% after depositing 50 nm of adamantane plasma polymer onto the sample. These values indicate that the gauge factor after the encapsulation process has increased by 24% and a 34% for the A and the B exciton, respectively.

Figure 3 shows the statistical information obtained after measuring seven different single-layer MoS₂ flakes (see the Supporting Information for data sets for other flakes, Figures S1-S8) for the gauge factors of the A and B excitons. Black dots show those samples that were measured before the encapsulation process, blue dots indicate the measured samples after encapsulating them with 50 nm of adamantane polymer film and the grey dots correspond to data collected from other 15 un-encapsulated single-layer MoS₂ samples reported in our previous work [11]. We can observe an overall improved strain tunability for the encapsulated samples, which is attributed to the fact that the strain is being transferred more effectively to the single-layer MoS₂ flakes. Note that the orange dots in Fig. 3 refer to the same sample that was tested in Fig. 2 after being subjected to several straining tests and forcing it to the failure limit (these results will be displayed in Fig. 4). These data demonstrate an increment in the gauge factor between a 24% and a 214% for the A exciton and between a 24% and a 253% for the B exciton, obtaining a maximum gauge factor of -99.5 meV/% for the A exciton and − 63.5 meV/% for the B exciton. We believe that this improved gauge factor could be due to the large Young’s modulus of 7.5 ± 0.3 GPa of the adamantane plasma polymer films (see the Supporting Information, Figure S9). Note that although Li et al. found larger gauge factors (around − 136 meV/%) for two MoS₂ samples using a PVA encapsulation and peeling-off method [25]; we attempted to improve the gauge factor of our samples by encapsulating MoS₂, deposited onto PC, with PVA on top without success (see the Supporting Information, Figure S10). This motivated our use of adamantane polymer films to improve the strain transfer in monolayer MoS₂ samples.

In Fig. 4, we subject a single-layer MoS₂ flake to very high strain values to determine the maximum strain before slippage. Panel (a) and (b) shows the A peak position and the B peak position as a function of the applied uniaxial strain, respectively. We can observe a clear linear behavior from 0–2.8% (blue dots), at which point the flake starts to slip and release strain as can be seen from the occurrence of sudden upward jumps in the exciton energy and the reduced slope (red dots). Another four adamantane plasma polymer coated samples, see the Supporting Information (Figures S11-S14), reached a maximum strain ranging between 1.7% and 2.4%. These maximum strain values with the adamantane polymer encapsulation are very promising given that un-encapsulated samples show signs of slippage for strains between 0.8% and 1.4% [11]. Our adamantane layer is ideal even when compared with the PVA encapsulation and peeling-off method given that the maximum reported strain value for a single MoS₂ sample was 1.7% [25].

We also tested the reproducibility of these measurements (see Fig. 5). We applied three straining/releasing cycles on a single-layer MoS₂ flake after being encapsulated with 50 nm of adamantane (optical picture in the inset). Panel (a) presents the spectra acquired during this cycling process and panel (b) summarizes the energy of the A and B peaks as a function of the applied uniaxial strain from 0–0.65%, showing a good agreement between the subsequent cycles.

To corroborate our micro-reflectance spectra data, we also acquired photoluminescence and Raman spectra of a single layer MoS₂ flake as a function of the applied strain. Figure 6(a) shows photoluminescence spectra before and after depositing 50 nm of adamantane, and the A peak position vs. the strain value can be observed in Fig. 6(b). Gauge factors of -37.1 ± 3.0 meV/% and − 70.2 ± 7.3 meV/% were obtained before and after the encapsulation, respectively. A remarkable increase in the gauge factor is appreciated, which agrees with the obtained micro-reflectance measurements. Notably, we observe a global offset in the A exciton energy position in the photoluminescence measurements in comparison to the micro-reflectance spectroscopy experiments. We associate this shift to the broad background signal in the photoluminescence measurements that is produced by the substrate and to the Stokes shift [53].

In Fig. 7 we present Raman spectra of a monolayer MoS₂ flake following the same methodology. Figure 7(a) shows the Raman spectra that were obtained before and after 50 nm adamantane film encapsulation as a function of different uniaxial strain values where E¹_2g and A_1g peaks for MoS₂ can be clearly observed. Figure 7(b) displays the peak position vs. the applied strain before and after encapsulation and a noticeable increase of the gauge factor for both peaks is detected. We note that a global shift in the Raman peaks at 0% strain is recorded in these measurements. This points to possible built-in crystal strain (compression) after the deposition of adamantane. This is supported by our micro-reflectance measurements as well which also display a shift in the exciton peak positions after adamantane deposition.

Figure 8 summarizes the maximum reported gauge factor and maximum achieved strain before slippage in uniaxial strain engineering experiments with single-layer MoS₂. By comparing with other experiments one can see how adamantane coating yields a good combination of large gauge factor and large maximum strain value. Black data points indicate data points acquired on bare (un-encapsulated or un-clamped) MoS₂ monolayers[18],[37],[54, 55]; blue data points correspond to those samples that were covered with a PDMS film to avoid the slippage [21, 23]; purple data point corresponds to the clamped sample [12]; the green data point indicates a single-layer MoS₂ flake that was encapsulated with a PMMA film [24]; and the yellow data point corresponds to the sample covered with a PVA coating [25]. As we can observe, the adamantane plasma polymer-coated samples have a good balance of high gauge factor and large maximum strain leading to a large band gap tunability. We further note that the adamantane-coated MoS₂ data were obtained after the samples were subjected to multiple straining tests, so the gauge factors and the maximum strain values could be lower than those that would have been obtained in a pristine sample.

In summary, we present a method to encapsulate two-dimensional materials with adamantane polymer layer that contributes to transfer the strain from the substrate to the flake more efficiently. The deposition process allows for the simultaneous conformal deposition of multiple devices in a solventless, room-temperature process. We demonstrate the performance of this technique by studying seven single-layer MoS₂ samples subjected to uniaxial strain before and after the adamantane polymer encapsulation. We find a higher gauge factor in all the studied samples after encapsulation. We have used differential reflectance spectroscopy, finding gauge factors ranging from − 58.9 meV/% to -99.5 meV/% for the A peak and − 49.4 meV/% to -63.5 meV/% for the B peak after encapsulation, which is considerably higher than those gauge factors that were obtained without any encapsulation, ranging from − 31.0 meV/% to -57.4 meV/% for the A exciton and − 18.0 meV/% to -47.4 meV/% for the B exciton. We have also found that, after depositing the adamantane film, a value of 2.8% of uniaxial strain can be achieved before slippage occurs. This value is approximately twice the maximum uniaxial strain values commonly found in un-encapsulated samples. We also tested the reproducibility of the measurements by subjecting a sample to various strain cycles, finding a good reproducibility between cycles. In addition, we have obtained photoluminescence and Raman spectra under strain to corroborate the measurements that were obtained with micro-reflectance spectroscopy. Finally, taken all together, our results show that adamantane plasma polymer encapsulation is an attractive method of encapsulation that gives rise to higher strain transfer and increases the maximum crystal strain that can be achieved in experiments. Our method advances development in strain engineering of materials and can be readily applied to other members of the interesting class of 2D materials.

We employ a three-point bending setup for applying uniaxial strain because we have found that a two point bending rig leads to sample repositioning and refocusing with application of strain [11, 14]. In addition, and as identified in our previous work, slippage is more common in uniaxial strain than in biaxial strain experiments [14]. It is therefore advantageous to develop an effective encapsulation process that mitigates slippage in uniaxial strain experiments. Accordingly, we carry out the same experiment before and after the adamantane deposition in order to test the efficiency of the encapsulation. All information about the calibration of this setup can be found in our previous work [11].

The fabrication of the MoS₂ samples consists of exfoliating bulk MoS₂ crystals (Molly Hill mine, Quebec, Canada) with Nitto tape (SPV224) and transferring the obtained flakes onto a Gel-Film substrate (WFx4 6.0 mil, by Gel-Pak®). By using the micro-reflectance spectroscopy method [49, 56], which allows us to determine the thickness of the crystals, we select a single-layer MoS₂ flake and we place it onto the center of a beam-shaped, 250 µm thick polycarbonate (PC) substrate using an all dry deterministic transfer method [57–62].

The encapsulation process consists of using remote plasma-assisted vacuum deposition (RPAVD) to deposit a thin layer of adamantane plasma polymer to the surface of the sample. RPAVD is a useful method to deposit polymer-like layers of sensitive functional organic molecules that cannot be deposited in a direct Ar plasma due to excessive precursor fragmentation. Adamantane powder (> 99%) was purchased from Sigma-Aldrich and used as received. The deposition process consists of the controlled sublimation of adamantane powder in the downstream region of an Ar microwave electron cyclotron resonance (ECR) plasma. The deposition pressure was 10^− 2 mbar and the plasma power was 150 W. The temperature of the substrates was 2–3 ºC above room temperature, determined by a thermocouple connected to the sample holder in the same position as the substrates. The sample holder was placed about ~ 10 cm from the plasma and oriented upside down to reduce plasma interaction with the surface. The evaporation rate was monitored with a calibrated quartz crystal monitor (QCM). A set of films examined by spectroscopic ellipsometry was used to calibrate the QCM values to obtain reproducible thickness values. Besides, reference films on Si(100) were examined by spectroscopy ellipsometry to check the thickness in each deposition process. Full details regarding the plasma source and reactor geometry can be found elsewhere [35, 36]. Figure 1(b) shows an optical image of the single-layer MoS₂ flake before encapsulation and Fig. 1(c) shows the flake after deposition of 50 nm of adamantane. A contrast and color difference can be readily appreciated across the entire sample.

Variable angle spectroscopy ellipsometry was carried out with a VASE ellipsometer from J.A. Woollan Co.

Young modulus values were obtained in a NanoXP nanoindenter from MTS Nanosystems using the continuous stiffness (CSM) and low load dynamic contact (DCM) modules. The study was carried out using 5x1cm² ~ 500 nm thick adamantane plasma samples prepared in identical conditions on Si(100) and fused silica. The values obtained corresponded to a total of 70 indentations.

DATA AVAILABILITY:

The datasets generated during and/or analysed during the current study are available from the authors on reasonable request.

ACKNOWLEDGEMENTS:

A.C.G. acknowledges funding from the European Research Council (ERC) under the European Union's Horizon 2020 research and innovation program (Grant Agreement No. 755655, ERC-StG 2017 project 2D-TOPSENSE), the EU FLAG-ERA project To2Dox (JTC-2019-009), the Comunidad de Madrid through the CAIRO-CM project (Y2020/NMT-6661) and the Spanish Ministry of Science and Innovation (grant PID2020-118078RB-I00). Ana B. thanks the ERC Union's Horizon 2020 program (Grant Agreement No. 851929 StG 2019 project 3DScavengers). We also thank the Spanish Ministry of Science and Innovation AEI/10.13039/501100011033 (grants PID2020-118078RB-I00 and PID2019-110430GB-C21), the EU ERDF (FEDER) Program (A way of making Europe), and the Junta de Andalucía (grant P18-RT-3480, and EMERGIAUS-1381057 program)

AUTHOR CONTRIBUTIONS:

FC and HL fabricated 1L MoS₂ samples and performed uniaxial strain tests. JMO-P, FJA, AnaB and AngelB, performed the deposition of the adamantane and the characterization of its Young’s modulus. JOI and AC-G wrote the first draft of the manuscript, all co-authors contributed to the final version of the manuscript.

COMPETING INTERESTS:

The authors declare no conflict of interest.

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Improved strain engineering of 2D materials by adamantane plasma polymer encapsulation

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