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Flexible Multistate Data Storage Devices Fabricated Using Natural Lignin at Room Temperature Youngjun Park, and Jang-Sik Lee ACS Appl. Mater. Interfaces, Just Accepted Manuscript • DOI: 10.1021/acsami.6b14566 • Publication Date (Web): 12 Jan 2017 Downloaded from http://pubs.acs.org on January 13, 2017

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ACS Applied Materials & Interfaces

Flexible Multistate Data Storage Devices Fabricated Using Natural Lignin at Room Temperature Youngjun Park & Jang-Sik Lee*

Department of Materials Science and Engineering, Pohang University of Science and Technology (POSTECH), Pohang 790–784, Republic of Korea

KEYWORDS Lignin, resistive switching memory, multi-level data storage, flexible electronics, biomemristors

ACS Paragon Plus Environment

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ABSTRACT The growing interests for bioinspired and sustainable electronics have induced research for biocompatible and biodegradable materials. However, conventional electronic devices have been restricted due to its non-biodegradable and sometimes harmful and toxic material, which even cause environmental issues. Here, we report resistive switching memory (ReRAM) device based on lignin, which is a biodegradable waste product of the paper industry. The active layer of the device can be easily formed using a simple solution process on a plastic substrate. The memory devices show stable bipolar resistive switching behavior with good endurance and retention. Appropriate control of the maximum reset voltage and compliance current can yield multi-bit data storage capability with at least four resistance states, which can be exploited to realize highdensity memory device. The resistive switching mechanism may be a result of formation and rupture of carbon-rich filaments. These results suggest that lignin is a promising candidate materials for an inexpensive and environmentally benign ReRAM device. We believe that this study can initiate a new route toward development of biocompatible and flexible electronics.


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INTRODUCTION Organic polymer materials have excellent flexibility, light weight, and versatile functionality, so they have great potential to overcome the problems of conventional inorganic materials for electronic devices.1-2 However, traditional organic materials are prepared using complex chemical synthesis and assembly, which use a large amount of energy and may release environmental issue. To overcome these problem, natural biopolymers from organisms have been considered for electronic applications3-6. The use of biopolymers offer feasibility for wearable, biocompatible and implantable electronics7. In addition, biopolymers have advantages including simple fabrication, environmental neutrality and application in flexible electronic device8-9. Lignin is an amorphous and heterogeneous polymer that composes 20 to 28 % of wood.10-11 Lignin is one of the most abundant natural biopolymers on earth, but it has been regard as waste products in paper industry,12 and only a small fraction is used as a low-value biomass13. Lignin has advantages for use in electronic devices. It possesses the phenol group, which can be oxidized to form the quinone group that can release electrons by redox reactions.14 In addition, lignin with good thermal stability and high carbon content can be easily fabricated using a solution process.15-16 Furthermore, this compound is inexpensive, ecologically benign, and biodegradable, which are useful traits in bio-inspired and implantable electronics.15,

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Electronic devices based on lignin, such as supercapacitors, lithium ion batteries, and sensors have been reported,10, 20-22 but further research can contribute to the development of application for this biopolymer. In particular, application as a memory device, which is used for data storage and processing, is necessary for the development of biocompatible electronics. Resistive switching random access memory (ReRAM) for next-generation high-density information storage has been also fascinated field due to its scalability, fast write/erase speeds,


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good reliability, and low power consumption23-25. In particular, ReRAM that uses biopolymers as an active layer can achieve both biocompatible and flexible properties.26-28 Compared to conventional memory devices, biopolymer-based ReRAM is inexpensive and easy to fabricate on a large area29. However, existing biopolymer ReRAM memory device have low-density storage capability, which hinders their application as future memory devices. Thus, multilevel resistive switching is a promising method to achieve high-density memory device.30 Although some papers have reported multilevel data storage using biopolymer31, there are still required further development. Therefore, multilevel memory device based on lignin could be an effective way to achieve high-density biopolymer ReRAM. In this study, we fabricate flexible ReRAM based on biopolymer as the switching layer on the plastic substrate. The lignin layer is formed by solution process at room temperature polyethylene terephthalate (PET) substrate coated with indium tin oxide (ITO). The as-fabricated memory device shows reliable and reproducible resistive switching behavior, even under bending. The device also shows stable and uniform information storage capability in four distinct multilevel resistance states. This study demonstrates that a memory device based on biopolymer can contribute to fabrication of environmentally benign electronics. We believe that this research based on lignin provides an important step in development of flexible, biocompatible, and implantable electronics.

EXPERIMENTAL SECTION Device fabrication The flexible ReRAM device was fabricated on ITO-coated PET substrate. The PET substrate had first been ultrasonically cleaned in acetone, 2-propanol, and distilled water for 15 min, then


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dried using N2 gas. To achieve high coverage of biopolymer active layer, the cleaned substrate was treated with UV ozone prior to spin coating. Lignin solution was prepared using low sulfonate alkali lignin powder (Sigma-Aldrich) in 1 M NH4OH16. The lignin was dissolved (1 wt %) in the 1 M NH4OH then mixing for 24 h under ambient temperature Lignin was spin-coated onto the flexible substrate for 5 s at 500 rpm, then for 40 s at 1200 rpm. The formed lignin thin film was dried at ambient condition for 24 h, then a 100-nm-thick Au top electrode with 100-µm diameter was deposited on the lignin layer by using thermal deposition. Characterization The electrical characteristics of fabricated lignin-based ReRAM were analyzed using a semiconductor parameter analyzer (4200SCS, Keithley) at ambient temperature. During electrical measurement of the memory device, the ITO bottom electrode was grounded while electrical bias was applied to the Au top electrode.

RESULTS AND DISCUSSION Lignin is an aromatic polymer that has complex chemical structure and the main component of the cell walls with cellulose and hemicellulose (Figure 1a).13,

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We fabricated a flexible

Au/lignin/ITO/PET ReRAM device on the ITO coated flexible PET substrate (Figure 1b, c). Au was used as a top electrode to avoid formation of metallic filaments. Thickness of fabricated lignin layer is about 100 nm (Figure S1). The electrical characteristics of lignin-based memory device were demonstrated under a direct current (DC) at 0.01 V/step. During electrical measurement, the DC bias voltage was applied to the Au top electrode, and the ITO bottom electrode was grounded. The as-fabricated device showed typical bipolar resistive switching behavior without an initial forming process, which


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causes high power consumption (Figure 2a). When negative DC bias was swept from 0 V to -2 V with compliance current of 10-3 A, the current increased at set voltage (-0.81 ± 0.19 V) from 10-6 A to 10-3 A (compliance current); this change indicates that the resistance state changed from high resistance state (HRS) to low resistance state (LRS). The LRS state was stably maintained during sweeping back from -2 V to 0 V. During the following sweep to the opposite polarity from 0 V to 2 V, the current gradually decreased and the device recovered to initial HRS state by exceeding reset voltage (0.76 ± 0.22 V). The device exhibited stable resistive switching behavior for 100 cycles with a reasonable memory window. In the LRS region, the resistance was slightly changed between negative and positive after repeated many cycles during DC sweep. The phenomena is thought to be related to the Joule heating, which is switching mechanism of the lignin-based device. However, the phenomena did not affect the memory sensing for 100 consecutive cycles. To demonstrate further the stability of the device during 100 consecutive cycles, the cumulative probability distributions of LRS and HRS were plotted (Figure 2b). The resistance distribution during 100 cycles was investigated at 0.2 V read voltage. The resistance remained stable in LRS, or HRS without obvious degradation. These results demonstrated that the memory device based on lignin has sufficient uniformity and reliability for nonvolatile ReRAM applications. Multilevel resistive switching behavior, which is important to overcome the limitation of the low-density storage of organic memory,32 could be achieved using lignin-based memory device. Current-voltage (I-V) characteristics of lignin-based memory showed three distinct HRSs (00, 01, 10 states) during positive voltage sweep with different maximum reset voltages VRESET = 2, 2.5, and 3 V (Figure 3a). The LRS (11 state) was almost the same during each of the three reset sweep. We speculate that a few unruptured conductive filaments exist within the lignin switching


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layer after the first 2 V reset sweep, if this is the case, further application of a positive bias > 2V could rupture the residual conductive filaments more completely during the reset process. The results demonstrate that the resistance of the lignin-based ReRAM device could be controlled by modulating the range of the reset voltage. Switching margin of the multilevel resistance state is directly related to the sensing of memory devices. The lignin-based memory device shows that On/Off ratio of multilevel states is ~ 50, 125, and 333, respectively. It is reported that operation of reliable multilevel resistive switching behavior was successfully demonstrated by optimization of device structure or using a programming algorithm, despite small switching margin.33-35 Therefore, it is thought that the biopolymer memory device is sufficient to be used as the multilevel memory device in real device applications. To investigate the stability and reliability for multilevel resistive switching operation, we measured the number of rewritable cycles of the lignin-based ReRAM device (Figure 3b). The resistance states were measured at read voltage VREAD = 0.2 V after applying the maximum reset voltage (2 V, 2.5 V, or 3 V). The measured resistance of 00, 01, 10, and 11 states was 1.29 × 105 to 1.35 × 105 Ω, 4.8 × 104 to 5.5 × 104 Ω, 1.6 × 104 to 2.4 × 104 Ω, and 300 to 680 Ω, respectively. The three HRSs and LRS were stable with distinct resistance for the 15 cycles in each multilevel state. We also measured the multi-bit data storage capability by using pulse measurement to confirm the feasibility of consecutive data storage operations at different multilevel resistance states (Figure 3c). Positive reset pulses (10 ms) at VRESET = 2.1 V, 2.6 V and 3.1 V were applied to form the different HRSs, and a negative reset pulse (10 ms) at VRESET = -3 V was used to form the LRS. A read pulse with amplitude 0.2V was applied after applying each set pulse and reset pulse. The memory device showed that information could be stored in at least four resistance states by controlling the amplitude of


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VRESET pulse. This results showed that multilevel resistive switching operation can be achieved in the lignin-based ReRAM device by imposing either a DC voltage sweep or an AC voltage pulse. Data retention properties of multilevel resistive state in this lignin-based ReRAM were measured (Figure 3d). Three HRSs and LRS were distinguished under constant voltage at 0.2 V, and the states were stable with no obvious degradation during stress for > 1000 s. In addition to control the range of reset voltage for multilevel switching, we also investigated whether multilevel switching could be realized by modulating the current compliance. The I-V characteristics of the lignin-based ReRAM device were measured under different compliance currents (Figure S2). The distinct two LRSs was observed by applying different compliance currents (5 × 10-4 A or 10-3 A) to the device, whereas off-state resistance was almost unchanged regardless of applied compliance current. It indicates that the LRS states depend on the magnitude of compliance current and that at least three multilevel states can be realized by imposing different compliance current. This results showed that multilevel operation can be realized by controlling compliance as well reset voltage, and the lignin-based ReRAM device is suitable for multilevel switching applications in high-density biopolymer-based memory devices. A flexible memory device is essential for application in information storage, implantable electronics, bio-integrated medical devices, and wearable systems. To assess the applicability of the ReRAM in a flexible memory device, we fabricated a lignin-based ReRAM device on PET substrate. To measure the memory performance under bending condition, Compressive or tensile bending stress were imposed on the device by fixing it to the 15 mm radius of curvature (Figure 4a). Resistive switching behavior did not degrade noticeable despite applied mechanical stress. A bending test was performed to measure the mechanical and electrical stability after repeated bending to a 15-mm radius of curvature (Figure 4b). The lignin-based ReRAM device was bent


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repeatedly from the initial flat to a bending condition. The current of HRS and LRS were measured at VREAD = 0.2 V. The on/off current ratio did not change much, and stable resistive switching behavior was observed for 100 bending cycles. These results demonstrated that ligninbased ReRAM device has a sufficient mechanical stability for future flexible memory devices. To investigate the switching and conduction mechanism of the device, the I-V curve of ligninbased memory device was plotted as log I-log V at the negative voltage sweep region (Figure S3). The fitted curves indicate that space-charge-limited conduction (SCLC) is dominant conduction mechanism for HRS and Ohmic conduction is dominant mechanism for LRS. The fitted I-V curve in the HRS region showed two distinguishable regions; the low voltage region was linear (I ~V), whereas the high voltage region showed quadratic behavior (I ~V2) before the set process.36 It is attributed to traps due to defects of switching layer. When the applied bias is low, there are a lot of thermally generated free charge carriers compared to injected carrier, which shows Ohmic conduction.4, 37 When the applied bias is increased, the sufficient electric field to fill all trap centers is applied, injected carriers are dominant for conduction until set process. In contrast, the fitted curve in the LRS region showed only Ohmic conduction. It indicates a filamentary switching mechanism by forming conductive path connected between two electrodes.38-39 It is possible that Au can be penetrated into the lignin film during deposition of Au top electrode. In our case all fabricated devices showed very insulating state (HRS) initially. So we believe Au doesn’t participate in resistive switching memory operations. Also, to confirm the effect of electrode materials and existence of interface states between Au and lignin layer, we fabricated the lignin-based memory devices with different metal electrodes. Al and Mg were used for top electrode and similar resistive switching behavior was observed (Figure S4). This result suggested that the resistive switching behavior is not related to the electrode materials and


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do not form interface state between electrode and lignin. The switching mechanism of ligninbased memory device may be a result of formation and rupture of conductive filament. There are two suggested filamentary switching mechanisms to explain resistive switching behavior in polymer based memory device; metallic filament conduction and carbon-rich filament conduction. Metallic filament conduction forms the conductive filament by dissolving of metal ions from the top electrode material, and their subsequent migration; this mechanism has been verified experimentally40-41. However, in the Au/lignin/ITO/PET structure used here, an inert metal (Au) is used as a top electrode, it is virtually impossible to dissolve by applying bias. Also, the resistive switching behavior was observed regardless of the electrode material (Figure S4). In addition, pre-forming process is required for formation of metallic filament27, 42; this behavior was not observed in this device, so this may be the evidence that metallic filament does not form. Furthermore, the lignin-based memory can be operated regardless of bias polarity (Figure S5), so it is indicated that switching behavior is inherent characteristics of switching layer. A possible underlying switching mechanism of the memory is the carbon-rich filament conduction. The carbon-rich filament conduction is a results of conductive filament formation due to the inherent characteristics of the polymer switching layer regardless of the species of the top electrode; this process has also been confirmed experimentally.43-44 Also, lignin can be carbonized and converted to amorphous carbon or graphite structures by proper thermal energy.45 Thus, carbon atoms in the lignin layer may contribute to the resistive switching of the device. When bias is applied to the electrode, Joule heating facilitates a local breakdown at the weakest point of the switching layer; as a result voids can be formed. An increase of bias further promotes the local breakdown, which is pyrolysis; the localized carbon-rich region surrounded by voids is formed.43, 46-47 The carbons may be amorphous carbonaceous matrix. The more heat


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was generated by applying the higher bias, the amorphous carbon region (with poor conductivity due to sp3 hybridization) can be locally changed graphite-like region (with high conductivity region due to sp2 hybridization); as a result, the resistance changes from HRS to LRS.48-51 Although, the formed carbon material at the LRS may be a stable, but it can be ruptured by Joule heating, which has been confirmed experimentally.52 Also, rupture can be affected by the length, diameter, and volume fraction.53 The increased thermal energy caused by current concentration through a narrow conduction path induces rupture of the carbon filament at the weakest point and make a nanogap at the center of the filament, so the HRS forms.43-44, 47, 52 The reversible switching occur by applying a proper bias to induce electric field across the nanogap. It can lead to the migration of atoms in the formed carbon-rich region and cause regrowth of ruptured filament; as a results, the resistance changes to LRS.48, 54 Lignin has a high density of carbon atoms, so the conductive carbon-rich filaments that form during the local breakdown of lignin layer may be wide and numerous.47 Therefore, when the reverse bias for reset applied, the formed carbon-rich filaments do not all completely, but just partially rupture, so the device switches back gradually to the HRS.

CONCLUSIONS We introduce flexible biopolymer memory devices using lignin as resistive switching layer on PET substrate. Lignin is inexpensive and environmentally benign, so it has application for a resistive switching layer. The fabricated devices exhibited reliable and reproducible bipolar resistive switching behavior with an acceptable memory window for 100 consecutive DC cycles. The lignin-based memory devices showed the feasibility of multi-bit data storage in at least four states by controlling the maximum reset voltage and compliance current. They have also good


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mechanical flexibility under bending. The switching behavior may be related to the carbon atom and Joule heating in the lignin layer, which could form and rupture carbon-rich filaments in an applied electric field. This study demonstrates that lignin is a promising candidate material for bio-inspired and biocompatible ReRAM. We believe that this flexible and biocompatible memory device provides an important step in development of implantable and bioinspired electronics.


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Figure 1. (a) Schematic and structure of lignin in lignocellulose (b) Schematic structure of flexible Au/Lignin/ITO/PET device. (c) Photograph of memory array on flexible substrate.


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Figure 2. (a) I-V characteristics of the lignin based memory structure under 100 consecutive cycles. (b) Cumulative probability of the HRS and LRS


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Figure 3. Multilevel operation of the lignin based device (a) I-V characteristics with different maximum reset voltages (b) Multilevel resistance states with different reset voltage under DC sweeping mode and (c) a pulse mode. (d) Retention characteristics for all four states.


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Figure 4. Mechanical flexibility test of memory device. (a) I-V characteristics under flat and compressive conditions. Insets : photographs of the device under compressive and tensile states, respectively. (b) Bending stability of lignin ReRAM over repetitive 100 bending cycles. Inset one bending cycle during bending test.


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ASSOCIATED CONTENT Supporting Information. Cross sectional SEM image of lignin layer, I-V characteristics of lignin-based memory with different compliance current, measured and fitted log scale I-V curve in negative sweep, effect of different top electrodes on switching behavior, and I-V charateristics of the device with positive set process in Figure S1-S5. This materials are available free of charge via the Internet at AUTHOR INFORMATION Corresponding Author *[email protected] Author Contributions J.-S.L. conceived and design the experiments. Y.P. performed experiments under the supervision of J.-S.L. J.-S.L. and Y.P. wrote the paper ACKNOWLEDGMENT This

work

was

supported

by

National

Research

Foundation

of

Korea

(NRF-

2016M3D1A1027663, NRF-2015R1A2A1A15055918). This work was also supported by Future Semiconductor Device Technology Development Program (10045226) funded by the Ministry of Trade, Industry & Energy (MOTIE)/Korea Semiconductor Research Consortium (KSRC). In addition, this work was partially supported by Brain Korea 21 PLUS project (Center for Creative Industrial Materials).


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