Physically Transient Field-Effect Transistors Based on Black Phosphorus

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Functional Inorganic Materials and Devices

Physically Transient Field-Effect Transistors Based on Black Phosphorus Min-Kyu Song, Seok Daniel Namgung, Taehoon Sung, Ah-Jin Cho, Jaehun Lee, Misong Ju, Ki Tae Nam, Yoon-Sik Lee, and Jang-Yeon Kwon ACS Appl. Mater. Interfaces, Just Accepted Manuscript • DOI: 10.1021/acsami.8b15015 • Publication Date (Web): 29 Oct 2018 Downloaded from http://pubs.acs.org on October 30, 2018

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ACS Applied Materials & Interfaces

Physically Transient Field-Effect Transistors Based on Black Phosphorus Min-Kyu Song†,‡, Seok Daniel Namgung†,‡, Taehoon Sung†,‡, Ah-Jin Cho†,‡, Jaehun Lee§, Misong Ju§, Ki Tae Nam§, Yoon-Sik Lee∥,⊥, Jang-Yeon Kwon*,†,‡

†School

of Integrated Technology, Yonsei University, Incheon 21983, South Korea

‡Yonsei

§Department

Institute of Convergence Technology, Incheon 21983, South Korea

of Materials Science and Engineering, Seoul National University, Seoul 08826, South Korea

∥School

of Chemical and Biological Engineering, Seoul National University, Seoul 08826, South Korea

KEYWORDS: transient electronics, black phosphorus, 2D transistors, bioresorbable devices, biodegradable FETs

ACS Paragon Plus Environment

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ABSTRACT

Black phosphorus (BP) has shown great potential as a semiconductor material beyond graphene and MoS2 because of its intrinsic bandgap and high mobility. Moreover, the biocompatibility of the final biodegradation products of BP has led to extensive research on biomedical applications. Herein, physically transient field-effect transistors (FETs) based on black phosphorus have been demonstrated using peptide insulator as a gate dielectric layer. The fabricated devices show high hole mobility up to 468 cm2V-1s-1 and on-off current ratio over 103. The combined use of black phosphorus, peptide, and molybdenum provides rapid disappearance of the devices within 36 hours. Dissolution kinetics and cytotoxicity of black phosphorus are assessed to clarify its availability to be applied in transient electronics. This work provides transient FETs with high degradability and high performance based on biocompatible black phosphorus.

1. INTRODUCTION Transient electronics, a recently proposed concept of implantable electronics, is an electronic system that dissolves in physiological condition at a programmed time. In contrast to conventional electronics that is designed to be durable and reliable for long-term operation, transient devices degrade and disappear after diagnosis or therapeutic function in the human body, thereby eliminating the need for secondary surgery to retrieve implanted devices and additional risks of infection. Moreover, these self-destructing devices will open up new applications, including ecological monitoring devices, disposable consumer electronics, and data-secure devices. The first demonstration of silicon electronics on silk substrates in 2009 has triggered a surge of research interest on transient electronics1, and a significant amount of extensive work, including transistor


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circuits2-8, biosensors9-11, memories12-13, batteries14-15, and triboelectric nanogenerators16, has been reported. Silicon nanomembrane (Si NM) is mostly used as a semiconductor material for transient electronics, mainly due to its degradability and high performance.17-18 Furthermore, the biocompatibility of Si NM has also been evaluated both in vitro and in vivo studies by means of cytotoxicity assays and animal models, respectively.3, 17 However, Si NM has its limits as an active layer of transient electronics in view of its slow dissolution, from a few days to weeks, 18 and brittle nature19. Slow dissolution directly refers to long-remaining time of host materials that may induce physical damage from remaining particles. After its function is completed, an implanted device is no longer needed and should disappear as soon as it can be designed to minimize any other side effects from remains. Other semiconductor materials applied in transient electronics including oxide semiconductors and polymers also have been reported. Zinc oxide shows rapid dissolution in biofluids and energy-harvesting characteristics.4 Polymer-based transient devices are designed to be dissolved in acidic condition with good flexibility.8 Nevertheless, these channel materials have relatively low mobility to realize high performance devices. None of the devices based on these semiconductor materials exceeds the mobility values over 1 cm 2V-1s-1. Therefore, there is still a need for new semiconductor materials with both high degradability and high performance. Black phosphorus (BP), also known as phosphorene, has attracted significant attention since its first isolation in 2014 owing to its outstanding intrinsic properties including high mobility up to 1000 cm2V-1s-1 and tunable bandgap ranging from 0.3 eV to 2 eV.20-21 As other two-dimensional materials, BP possesses atomically thin body and flexible nature. As phosphorus is the second most abundant mineral in the human body accounting for 1 % of the body weight and being required daily, BP, the most stable allotrope of phosphorus, has been expected to be biocompatible


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and thus can be a new platform in biomedical application. Various research has been reported biomedical applications of BP including photothermal cancer therapy,22-24 drug delivery,25-26 and biosensing.27-29 We report transient BP field effect transistors that provide short term operation and rapid dissolution. Since a peptide with a sequence of Tyr−Tyr−Ala−Cys−Ala−Tyr−Tyr (YYACAYY) shows great dielectric property and dissolves rapidly in water along with BP as we previously discovered, YYACAYY peptide insulator was used for gate dielectric layers. 30 Molybdenum (Mo), which is dissolvable in biofluid, was used as source, drain and gate metal.31 All components of the devices, including source, drain, gate, gate insulator, and channel, disappear within 36 hours in a physiological environment. The transient BP FETs show not only high degradability in biofluid but high electrical performance. The highest mobility and on-off current ratio among the devices was estimated to be ~468 cm2V-1s-1 and ~1200 respectively. Biocompatibility from cytotoxicity was also investigated by a LIVE/DEAD viability assay. The transient BP FETs we report here can be the building blocks for rapidly dissolvable and highly biocompatible transient electronics.


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2. EXPERIMENTAL SECTION Dissolution Tests. Dissolution rates of each component including BP, YYACAYY peptide, and Mo were examined. Bulk BP with 99.998% purity was purchased from Smart Element. BP flakes were exfoliated by a mechanical scotch-tape method and transferred onto 300-nm SiO2 /Si substrates in an Ar-filled glove box. BP flakes with thicknesses of 30-50 nm were identified by optical microscopy. We deposited 350-nm Mo on 300-nm SiO2 /Si substrates by RF sputter. A 4 wt % YYACAYY peptide solution was prepared by dissolving YYACAYY peptide powder in trifluoroacetic acid (Daejung, 99.0%) at room temperature and spin-coated onto 300-nm SiO2 /Si substrates at 4000 rpm for 60s. Prepared thin films on substrates were immersed in 37 °C deionized water and 1x phosphate buffered saline (PBS, Sigma Aldrich). Both water and PBS had pH 7.4. Thicknesses were measured at various times using AFM (XE-100, Park systems) and a surface profiler (D-100, KLA Tencor). Dissolution of BP was characterized using Raman spectroscopy (LabRAM ARAMIS, Horiba) with a laser source of λ = 532 nm and 5 mW. Fabrication of BP FETs. BP flakes were cleaved by mechanical exfoliation onto substrates in an Ar-filled glove box. The flakes with appropriate thicknesses were identified by optical microscopy. A Mo metal contact (30 nm) for source and drain was defined by following a photolithography step and deposited by RF sputter. After a lift-off step, the YYACAYY peptide solution was spin-coated. Additional mask-patterned deposition of Mo (30 nm) yielded the top gate metal. The exposure time to ambient air from exfoliation of BP to spin coating of YYACAYY peptide was controlled to be less than 10 minutes. Cytotoxicity of BP. Bulk BP was ground and exfoliated by ultrasonication in ultrapure water (Milli-Q) for 12 hours. NIH 3T3 mouse fibroblast cells were plated on to 24-well culture plates with a concentration of 105 mL-1. Volume of media per solvents for each well is 200 µL. After 48


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hours of incubation with a BP concentration (0, 6.25, 12.5, 25, 50, 100, 200, and 400 µg mL-1), cells were rinsed gently with Dulbecco’s phosphate buffered saline (D-PBS) and treated with 2 µM calcein AM and 4 µM EthD-1 in D-PBS. Calcein which is produced after acetoxymethyl ester hydrolysis of calcein AM by intracellular esterase emits green fluorescence. EthD-1 produces a strong red fluorescence when it is bound to nucleic acid. Cell counting was carried out with imageJ. (version 1.52a, NIH, Bethesda, MD) 3. RESULTS AND DISCUSSION Dissolution kinetics of BP were examined using atomic force microscopy (AFM) and Raman spectroscopy. Figure 1a shows images of a BP flake with a thickness of 40 nm at the various stages of dissolution in deionized water with physiological conditions (pH 7.4, 37 °C). The pristine flake was mechanically exfoliated by the conventional scotch-tape method and transferred onto 300nm-thick SiO2 thermally grown on Si substrates. Measured thicknesses of immersed BP were 40.43 ± 1.09 nm at 0 hour, 20.27 ± 2.18 nm at 12 hours, 10.85 ± 1.66 nm at 18 hours, and 0.99 ± 0.34 nm at 24 hours. As shown in figure 1b, BP flakes dissolved rapidly and linearly within 24 hours of immersion both in deionized water and in phosphate buffered saline (PBS, pH 7.4). Dissolution rates of BP in water and PBS are 1.81 nm/hour and 1.65 nm/hour, respectively. Dissolution rate commonly depends on ionic contents of solutions,18 but the dissolution rate of BP in PBS is not significantly different from its dissolution rate in deionized water implying that ion contents, such as phosphates and chlorides, in PBS don’t strongly affect the dissolution of BP. The total time for disappearance of BP depends strongly on the initial thickness of the pristine BP because of its linear dissolution rate. Total dissolution time can be shortened further, because the initial thicknesses of BP we employed here are generally thicker than that in previously reported


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data. This rapid dissolution of BP can minimize physical damage to the implanted site and prevents undesired immune response due to residue from slow dissolution. Several studies have shown that BP dissolves in water by a two-step reaction, P4 + 5O2 → P4O10 + 5e- and P4O10 + 6H2O → 4H3PO4.32-33 BP reacts with oxygen dissolved in water first and becomes phosphorus pentoxide (P4O10) which dissolves in water to form phosphoric acid (H3PO4).33 To verify this mechanism, dissolution behaviors of BP in N2-deaerated water were examined. As shown in Figure S1, immersed in O2-depleted water, the thickness of pristine BP was not changed, suggesting that hydrolysis of BP does not take place without dissolved oxygen. On the other hand, thickness of fully oxidized BP was decreased owing to dissolution of phosphorus pentoxide layers. Dissolution of pristine BP depends on oxygen partial pressure which causes oxidation of phosphorus. The final products from dissolution, including phosphates and phosphonates, are non-toxic and are involved in metabolism in the human body.23, 33-34 Raman spectroscopy was taken to study the dissolution of BP with a laser source of λ = 532 nm. Intensities of Raman spectra were normalized with respect to the Si peak (~520 cm -1) to clarify changes of each peak. The angle of the induced laser was fixed to exclude anisotropic effects on peak ratios. Pristine BP flakes showed three Raman peaks at 361 cm -1, 438.3 cm-1 and 465.9 cm-1, corresponding to three typical vibrational modes A1g, A2g, and B2g respectively. After immersion in 37 °C water, intensities of all peaks decreased (Figure 1c). After 20 hours of immersion, Raman peaks converged to zero, indicating that BP flakes were fully dissolved. Figure 1d shows the changes of the intensity ratios of the three peaks. The intensity of the out-of-plane A1g mode which linearly depends on thickness of BP, gradually declined in terms of immersion time, indicating that BP flakes were gradually dissolved with decreasing thickness. 35 The intensity of in-plane A2g mode also decreased gradually, while that of in-plane B2g mode showed less correlation with layer


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thickness. Different aspects among the three Raman vibrational modes probably result from the anisotropic changes in the electronic and optical properties of layered BP of different thickness.36 The Raman spectroscopy data doesn’t show any clear peak shift, meaning that there is no lattice deformation and no oxidized layer because the layer might be immediately dissolved after being formed. With dissolvable BP, we fabricated transient field-effect transistors with dissolvable materials. Figure 2a presents a schematic of fabricated transient BP field-effect transistors with a top-gate configuration. Based on our previous work, the YYACAYY peptide has great insulator properties with a high dielectric constant (k = 6.5) and is highly soluble in water. 30 The dissolution rates of the YYACAYY peptide in 37 °C water and PBS are 133.3 nm/m and 355 nm/m, respectively. The dissolution kinetics of YYACAYY peptide and Molybdenum are shown in Figure S2. Along with BP, the YYACAYY peptide is suitable for rapidly dissolvable transient devices. Thickness of the YYACAYY peptide was optimized for insulating property to 400 nm and the dissolution time of the YYACAYY peptide layer was less than three minutes. A few layers of BP were cleaved by the scotch-tape method on thermally oxidized Si substrates (300 nm SiO 2) in an Ar-filled glovebox. BP flakes with appropriate thickness were identified by optical microscopy. Photolithography was carried out to define source and drain on the flakes. Mo contact was deposited by DC sputter using a lift-off technique. The YYACAYY peptide was dissolved in trifluoroacetic acid (TFA) and spincoated onto the samples at 4000 rpm. Mo gate metal was defined by a shadow mask and deposited by DC sputter. Sputtered SiO2 (850 nm) and spin-coated crystallized silk (370 nm) served as device passivation to render the device stable in the human body during the functioning time. Figure S3 shows the cross-sectional transmission electron microscopy (TEM) images of the fabricated BP FETs.


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We examined the electrical characteristics of transient BP FETs. Figure 2b shows the transfer characteristics of BP for gate voltage swept from 10 V to -40 V with drain voltage of -0.1 V; the inset shows the output characteristics under gate voltage modulation from 10 V to -10 V. We extracted the field effect mobility of 141.5 cm2V-1s-1 from the conventional equation for μ = (dID/dVG) * [L/(WCiVD)] where μ is the field effect mobility, W and L are the width and length of the channel respectively, and Ci is the unit-area capacitance of the YYACAYY peptide gate dielectric and a current modulation of over 1.2 * 10 3 is observed. The transient BP FETs exhibit comparable performance to previously reported BP FETs. 20, 37-41 The highest field-effect mobility value among the samples was 468.4 cm2V-1s-1 with 4.07 mA mm-1 of on current. (Figure S4, Supporting Information). This high value of mobility is further comparable to the field-effect mobility of p-doped Si NM based transient transistors.3 High mobility transistors with high speed switching characteristic can be applied to RF transistor for communication between internal and external devices. To investigate transient operation of the device in the human body condition, transient BP FETs were immersed in water, and changes of electrical characteristics at various stages of degradation were measured. Without passivation, the transient BP FET stops operating within 20 seconds (Figure S5b, Supporting Information). After immersion in water, the BP FET degraded with decreasing on current because of increasing gate leakage caused by rapid degradation of the YYACAYY peptide insulator. Rapid dissolution of the dielectric layer caused a sudden operation stop. To ensure stable operation time in the human body condition, we applied a passivation layer on the devices with sputtered SiO2 and crystallized silk. With the passivation layer, the device operation was stable for eight minutes (Figure 2c and d). After the period of stable operation, the device rapidly stopped functioning, and drain current converged to zero. To control the operation


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time of the device, the thickness of the passivation layer and the crystallinity of the silk can be controlled. Physical dissolution of each component of the BP FETs was clearly identified with devices fabricated on glass substrates with the same structure as above. The devices were immersed in 37 °C water under ambient conditions. Figure 3 shows images of immersed BP FETs on glass substrates in water; the insets show the optical microscope images of a BP FET in the dashed circled region. After 15 hours of immersion, the YYACAYY peptide layer was fully dissolved, and all metals seemed to be partially dissolved. BP and other metal layers seemed to be thinner in optical microscope images. After 36 hours of immersion, the devices were invisible to the naked eye. Optical microscope images showed that the BP flake was fully dissolved and only a residue of metal remained. Because sputtered Mo leaves residue on glass, dissolution time can be reduced by using dissolvable substrates. We conclude that all components of the transient BP FETs physically dissolved within 36 hours. Physical damage on subdermal sites may induce inflammation and immune response even with high biocompatibility of components of implantable devices. Therefore, rapid disappearance of transient devices must be counted on time programming of dissolution to minimize side effects of implantation. Even with nontoxicity of the final biodegradation products of BP, we further examined the biocompatibility of BP flakes by a cytotoxicity assay to mouse fibroblast cells (NIH 3T3). Several studies on the cytotoxicity of BP nanosheets using various assays have been reported.22, 26, 42-43 However, results from MTT and WST assay can be interfered with by the properties of host material, as previously reported.44-45 In this case, BP can reduce formazan products leading to false results.42 We performed a LIVE/DEAD® staining assay to avoid reactions between BP and


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formazan products. Figure 4a shows the representative fluorescent images of the cells treated with BP flakes. Green and red dots indicate live cells and dead cells, respectively. Cell viabilities are summarized in Figure 4b. As concentration of BP increases, the normalized cell viability decreases and goes down abruptly at 100 µg mL -1. Below 50 µg mL-1 of BP concentration, NIH 3T3 fibroblast cells showed viability of over 90 %. The BP flakes used for a transistor do not exceed 5 µm laterally and 30 nm vertically. We found the maximum number of BP transistors with a cell viability over 90% can be achieved by assuming the size of BP to be 5 µm * 5 µm * 30 nm; 50 µg/mL of BP is equal to around 2.5 x 108 of BP flakes in 1 mL solution. BP shows not only the biocompatibility of its final product, but biocompatibility with itself.

4. CONCLUSION In conclusion, we fabricated transient field effect transistors using a few layers of black phosphorus. Compared to silicon nanowire, BP dissolves rapidly and exhibits comparable performance used as a channel material for a transient device. In addition to biodegradability, we investigated biocompatibility of BP itself by a cytotoxicity assay. The dissolution test of transient BP FETs suggests that the time for physical disappearance of the devices doesn’t exceed two days. BP has great potential for transient electronics that disappear rapidly after functioning. This work provides an important step toward to human-implantable electronics with higher feasibility.


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FIGURES Figure 1. Dissolution characteristics of black phosphorus. (a) AFM images of a BP flake at various stages of dissolution in 37 °C D.I water (pH ~7.4). (b) Change in thickness of BP flakes as a function of time in 37 °C D.I. water and PBS. Linear fits (solid lines) yield dissolution rates of 1.65 nm/hour (water) and 1.81 nm/hour (PBS). (c) Raman spectra and (d) peak ratios of a BP flake normalized to the Si peak after immersion in 37 °C D.I. water. Inset: Raman vibrational modes of BP.


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Figure 2. Performance of transient BP FETs. (a) A schematic of a transient BP FET on SiO 2/Si substrate. (b) Transfer characteristics of a transient BP FET at a drain voltage of -0.1 V. The insets show output characteristics of the same device (left) and an optical microscope image of the BP flake (right). (c) Changes of transfer characteristics at various stages of degradation with passivation. Inset shows a schematic of the passivated device. (d) The drain current at a gate voltage and a drain voltage of -10 V and -0.1 V as a function of immersion time in water. The device is passivated by SiO2 and crystallized silk.


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Figure 3. Dissolution of transient BP FETs on glass. Images at various stages of dissolution after (a) 0 hour, (b) 15 hours, (c) 24 hours and (d) 36 hours of immersion in 37 °C of deionized water. Insets show optical microscope images of a device.


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Figure 4. In vitro cytotoxicity evaluation of black phosphorus. (a) Fluorescent images of NIH 3T3 fibroblast cells at various concentrations of BP. Living cells are stained green and dead cells are stained red. (b) Normalized cell viability of NIH 3T3 fibroblast cells as a function of BP concentrations.


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ASSOCIATED CONTENT Supporting Information. Dissolution characteristics of black phosphorus in deaerated H2O; Dissolution characteristics of molybdenum; Cross-sectional TEM images of the BP FETs; Statistics of the BP FET performance; Transient operation of the BP FETs immersed in 37 °C D.I. water AUTHOR INFORMATION Corresponding Author * E-mail: [email protected] Present Addresses ⊥Nano

Systems Institute, Seoul National University, Seoul 08826, South Korea

ACKNOWLEDGMENT This work was supported by Samsung Research Funding Center of Samsung Electronics under Project Number SRFC-MA1401-51.


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ToC FIGURE


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Physically Transient Field-Effect Transistors Based on Black Phosphorus

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