Metal Ions Redox Induced Repeatable Nonvolatile Resistive

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Metal Ions Redox Induced Repeatable Nonvolatile Resistive Switching Memory Behavior in Biomaterials Liang Zheng, Bai Sun, Shuangsuo Mao, Shouhui Zhu, Pingping Zheng, Yong Zhang, Ming Lei, and Yong Zhao ACS Appl. Bio Mater., Just Accepted Manuscript • DOI: 10.1021/acsabm.8b00226 • Publication Date (Web): 20 Jul 2018 Downloaded from http://pubs.acs.org on July 22, 2018

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ACS Applied Bio Materials

Metal Ions Redox Induced Repeatable Nonvolatile Resistive Switching Memory Behavior in Biomaterials Liang Zheng,†,‡ Bai Sun,*,†,ƪ Shuangsuo Mao,†,ƪ Shouhui Zhu,†,ƪ Pingping Zheng,†,ƪ Yong Zhang,†,‡,§ Ming Lei,*,†,‡,§ and Yong Zhao,*,†,‡,ƪ,§ †

Key Laboratory of Advanced Technology of Materials (Ministry of Education), Superconductivity and New Energy R&D Center (SNERDC), Southwest Jiaotong University, Chengdu, Sichuan 610031, China ‡ Key Laboratory of Magnetic Levitation Technologies and Maglev Trains, Southwest Jiaotong University, Chengdu, Sichuan 610031, China ƪ School of Physical Science and Technology, Southwest Jiaotong University, Chengdu, Sichuan 610031, China § School of Electrical Engineering, Southwest Jiaotong University, Chengdu, Sichuan 610031, China

ABSTRACT: The resistance random access memory (RRAM) based on biomaterials has great potential application in the sustainable electronic devices with the advantages of sustainable, green and environment-friendly, and it can offer a potential route for developing bio-RRAM devices, which would be a competitive bench in development of multipurpose memory devices. In our work, the banana peel, an ubiquitous useless waste, is introduced as an intermediate insulating material to preparing resistive switching memory device with Ag/Banana peel/Ti structure, in which the superior switching memory performance with a lager HRS/LRS resistance ratio and long retention characteristics are revealed. Moreover, the coexistence of memristor effect, capacitance effect and NDR phenomenon are observed in our device. The repeatable nonvolatile resistive switching memory behaviors are attributed to the redox properties of metal cations contained in biomaterials. Keywords: Resistive switching, Biomaterials, Negative differential resistance, Redox, Environment-friendly. 1

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INTRODUCTION With the rapid development of information science and continuous progress of electronic devices technology, the internet era has entered into people's life in an all-round way. Connecting devices are becoming inseparable, such as: computers, mobile phones and intelligent wearing devices. Attentively, storage technology plays a key role in the connecting devices. Research on storage devices has became a hotspot in recent years.1-3 With the development of storage technology, the faster read-write speed, higher storage capacity, higher integration density, and lower power consumption become the stringent issues.4-8 Traditional storage technologies such as dynamic random access memory (DRAM) have gradually failed to meet the rapid development of electronic devices.9-11 Many new storage technologies have been arisen, such as superconducting-magnetic memory (MRAM),12 atomic memory (ARAM),13 phase-change memory (PCRAM),14,15 ferroelectric memory (FRAM)16 and resistive switching memory (RRAM).17,18 Although MRAM and PCRAM are classified as more credible, they are limited by scalability or power consumption issues,19 ARAM and FRAM are complicated in structure and have higher preparation cost and/or operating cost. By contrast, RRAM has a simple structure and higher memory density, which makes it meet the needs of the era. The resistance switching memory rely on the resistance switching effect,20-22 which means that a resistance of materials can be switched between a high resistance state (HRS or "OFF" program) and a low resistance state (LRS or "ON" program) under an applied electrical impulse. When HRS are marked as logic "0" and LRS as logic "1", the resistor-swap cell can be used as a storage unit for information in the electronic applications. Currently, there are many researches on resistive switching memory device, various semiconductors and insulator materials have been assembled into memories as the interlayer, such as MOS2,23 MnO-CeO2,24 2


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carbon nanotube,25 TiO2,26 and so on. Although the rapid upgrading of electronic devices brings convenience to people's lives, it brings a heavy burden to our environment, especially for the consumption of non-renewable resources because of the rapid replacement.27,28 Therefore, the development of a bio-based memory devices are gaining more and more attention, the devices with Metal/Bio-materials/Metal structure are continuously detected.29-31 Banana, musa banana plantain, is one kind of rich raw materials. Annual output is about 1,200 tons in China, and banana is generally the best choice for vitamin supplements. However, the usage of banana peel is scarce, which have been currently just used as fertilizer or discarded in most countries.32 If banana peel can be used as a raw material for assembly of memory devices, it will have many advantages, such as easy to draw, low cost, environmentally friendly and biodegradable. In this paper, a bio-materials based memory devices with Ag/banana peel/Ti structure was prepared. The device hold large switching resistance ratio and excellent cycling performance at ambient temperature, further the nonvolatile switching behavior based on electrochemical redox is demonstrated. This superior bio-RRAM device with resistive switching effect holds great potential multifunctional application in physics, biology, biomedicine, and so on.

EXPERIMENTAL SECTION Preparation of materials. A unsalted of typical banana and its peel have been collected. The peels were washed with distilled water for several times, chopped into small pieces and dried in thermostat at 40 oC until completely desiccation. Subsequently, the dried banana peels were crushed and then uniformly dissolved in alcohol, the resulting alcohol solution was passed through a suction filter to remove particles larger than 40 mesh in size, then put the selected solution in the oven until they

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attains constant weight, and the powder was stored in dry environment. The prepared banana peel powder with micron size has been obtained.

Figure 1. The device preparation process.

Preparation of device. Glass substrates with a dimensions of 3.0 cm × 1.5 cm had been ultrasonic cleaned in acetone, ethanol and deionized water before deposition. Then the Ti bottom electrode was deposited on the glass substrate by radio frequency magnetron sputtering technique at ambient temperature, and the basic deposition parameters was as follow: chamber pressure was 1.0 × 10-5 Pa, the sputtering atmosphere was in 2.0 Pa (99.999%) Ar, the sputtering time was 20 min. Secondly, the precursor gel was spread on the Ti electrode by spin coating, and the precursor gel was prepared by mixing the banana peel powder and polyvinylidene fluoride binder in a mass ratio of 8:1, a few drops of N-methyl-pyrrolidone were put to make a slurry, and polyvinylidene fluoride and N-methyl-pyrrolidone are non-toxic 4


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and biodegradable materials. After pectin film deposition, the specimen was dried at 42 oC in vacuum for 5.0 hours to exclude moisture. Ultimately, the Ag top electrodes with the acreage of ~2.0 mm2 were deposited on the banana peel film, thus the device with Ag/Banana peel/Ti structure was assembled. The preparation process diagram is shown in Figure 1. The drugs used in the experiment are purchased from sigma. Characteristics. Structural information of banana peel powder was obtained by X-ray diffraction (XRD, Philips X'Pert MRD) with Cu Kα radiation. Cross section morphology and composition of the banana peel powder were obtained in FESEM (JSM-7001) with an energydispersive spectroscopy (EDS) instrument. In the test of resistive switching memory behaviour, all the electric measurements were performed by the electrochemical workstation (CHI-660E) using cyclic scanning model with Ag as the top and the Ti acts bottom electrodes at ambient temperature.

RESULTS AND DISCUSSION A schematic illustration of the preparation route of Ti/banana peel/Ag structure is shown in Figure 1. The structural analysis of banana peel powder is studied by XRD in Figure 2(a), the XRD result matched well to Potassium Chloride (KCl) PDF card 000411476 with space-group of Pm-3m, and the banana peel powder exhibit (200) and (220) peaks at about 28.2° and 40.6°, correspondingly. Notably, a weak diffraction peak at about 21.2° appear, which corresponds to (002) graphitic plane, indicating that the banana peel powder contain amorphous carbon.33 The EDS spectra of banana peel powder are presented in Figure 2(b). In general, it is well known that banana peel is rich composed of C, O, K and Na elements. In addition, F, S and Cl also appear in the data, the reason for the F element may be from the binder PVDF. The atomic mass fraction of C is as high as 74.94 %, and the atomic mass fractions of K and Na are 1.9 %

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and 1.72 %, respectively. The thickness of banana peel powder film by spin coating method on Ti bottom electrode is about 75 µm, as shown in Figure 2(c). Underneath, the thickness of Ti bottom electrode cover on glass substrates by radio frequency magnetron sputtering technique is approximately 500 nm in Figure 2(d), it can be seen that our bio-based memory device has a simple and clear structure.

Figure 2. (a) XRD spectra of as-prepared banana peel powder. (b) EDS spectra of banana peel powder, illustration shows atomic mass fraction. (c) Cross section images of the device. (d) A close-up cross-section photo of the Ti bottom electrode.

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The performance of the resistance switching memory devices with Ag/banana peel/Ti structure are investigated by the typical current-voltage relationship (I-V) shown in Figure 3(a), which reflects prominent resistive switching effects from the hysteresis loops of the I-V characteristics. During the test, the voltage sweep is carried out from 0 V → 6.0 V→ -6.0 V → 0 V with scanning speed of 0.1 V·s-1 over a hundred laps between the Ag top electrode to Ti bottom electrode respectively. Figure 3(b) is one circle of the hysteresis loops of the currentvoltage characteristics curve of Ag/banana peel/Ti structure. The inset shows the negative region of current-voltage (I-V) curves in double log scale, insinuating a stable and repeated negative differential resistance (NDR) phenomenon can be existed in our structure. The I-V curves exhibit irregularly rectangular shape, which is typical for electric double layer capacitor (EDLC) behavior.34 This behavior is usually manifested in activated carbon materials and conductive polymers in organic electrolytes, indicating that energy storage occurs via the electric double layer.35-37 Primitively, the device changes its resistance state from original state to low resistance state (LRS), when the applied potential is gradually increased to 6.0 V. Thereafter, the hysteresis curves show asymmetry, in the course of voltage reduction, the open circuit voltage (about 0.6 V, the observed voltage is non-zero when the current is zero in the hysteresis curves) and short circuit current (about -0.1 µA, the observed current is non-zero when the voltage is zero in the hysteresis curves) are observed. The origin of the phenomenon may be attributed to a displacement current Id adding to the conductive part Ic. The relationship between Id and total current ( I ) are determined in Eq:38 Id =

d (Cv ) d (v ) d (C ) =C +v dt dt dt

I = Ic + Id

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(1)

(2)


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Id = d(CV)/dt is due to voltage variation (CdV/dt) and capacitance variation V(dC/dt). Ulteriorly, when applied voltage is scanned to about -6.0 V, our device repeatedly exhibit a "Reset" process from LRS to HRS. Notably, there is a recessed part with a better capacitance storage performance at approximately -1.8 V in the process "3". The complete change state makes up the memory principle for memory devices and reflects superior memory performance and good sustainability.

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Figure 3. (a) The typical I-V characteristics curve of Ag/Banana peel/Ti structure. (b) One of the hysteresis loops of the current-voltage characteristics. The inset shows the negative region of I-V curves in double log scale for Ag/Banana peel/Ti structure. (c) The resistance cycle number curve with 160 cycles under a positive bias voltage of -1.0 V. (d) Retention test of the Ag/Banana peel/Ti memory device under a -1.0 V continuous read voltage.

The HRS/LRS resistance ratio is a key parameter to judge the performance of memory device. Figure 3(c) shows the resistance values through 160 times test, the two curves represent HRS and LRS respectively. Due to the concave curve of our equipment, the voltage value of 1.0 V is chosen to calculate of the resistance. It shows that the LRS basically remains constant while the HRS displays a gradual upward trend with the increasing cycle number. In addition, the HRS exhibits a positive temperature coefficient of resistance, which is contrary to the conventional non-metallic material. The possible reason is that as the temperature increases, the free electrons and oxygen vacancies inside the biofilm will undergo violent movement. In particular, the higher the temperature induces the faster the movement. As its movement speeds up, it will cause collisions between electrons and electrons, affecting the directional movement of electrons in the metal, resulting in increased resistance, when the number of cycles reaches 140 laps, the HRS gradually stabilizes, and we can assume that the inherent nature of the material tends to be stable, indicating that the resistive switching characteristic is highly outstanding and greatly stable with larger memory window in this state. In the first ten laps, the values of HRS and LRS are ~118 MΩ and ~6 MΩ respectively, and the HRS/LRS resistance ratio is ~20. When the HRS changes to 357 MΩ at 140 laps, the HRS/LRS resistance ratio is ~60. The growth of HRS is essentially linear with a slope of about 1.7, which indicating that banana-peel-based RRAM devices could have high OFF/ON resistance ratios as large as ~60

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and it also generally signifies a lower failure rate during read-write operation for data storage. Figure 3(d) shows a plot of configuration versus test duration under same voltage with a logarithmic scale abscissa. The storage performance of Ag/Banana peel/Ti structure device becomes better over time, and the possible trend of high resistance state will gradually increase in continuing testing, which does not accordance with conventional memristor current tend as reaching infinity as the voltage approaches the origin, and this trend will add more choices for our practical application. Attentively, Figure 4(a) reveals the cumulative probability distribution of the HRS and LRS resistance at a read voltage of -1.0 V for the first cycle of different samples with Ti/banana peel/Ag structure. It can be clearly seen that under the same preparation conditions, the high resistance and low resistance of the sample can be changed within a small fluctuation range, indicating that the samples are more reproducible.

Figure 4. (a) The cumulative probability distribution of the HRS and LRS resistance at a read voltage of -1.0 V for the Ag/Banana peel/Ti device. (b) The positive region of I-V curves in double log scale for Ag/Banana peel/Ti structure, the solid spheres are experimental data and the

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straight lines are the linear fitting curves according to the theoretical models, the non-solid part is the fourth area of the axis of I-V curve.

For better device performance and data retention property, the mechanisms of Ag/Banana peel/Ti resistive switching structure are thoroughly studied. The I-V curve of the first sweeping cycle in the positive voltage regions for the Ti/banana peel/Ag device is plotted and fitted on double log scale in Figure 4(b). The slope of the linear fit is approximately 0.27 and 0.12, The possible cause is the result of the combination of Ohmic and capacitive effects.17 When the slope of the linear fit more than 1.0, the conduction behavior to abide by the classical trapcontrolled Space Charge Constraint (SCLC).39 Specifically, it may be oxygen vacancy and electrolytic migration of metal cations through an insulator interlayer (banana peel) results in the formation of metallic filaments in resistive switching devices.40-42 The complete mechanism process is shown in Figure 5(a-f). The Ag is very active as the top electrode in the device, which will be easily ionized to Ag ions in the reading and writing process,43,44 the process could be described as: Ag → Ag + + e−

(3)

The K atom is also rich in Ag/Banana peel/Ti structure resistive switching device,45 and the K atom can be ionized to K ions in the running process as same as Ag, the process could be described as: K → K + + e−

(4)

Additionally, it is also known that banana peels are also rich in a large amount of Na from EDS, which will probably make our equipment more performance.40 It can be ionized as: Na → Na + + e−

(5)

Figure 5(a) shows the banana peel layer between Ti bottom electrode and Ag top electrode like sandwich. Ag atoms, K atoms, Na atoms and oxygen vacancies pass through insulating

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layer driven by the electric potential between anode and cathode as demonstrated in Figure 5(b). They can form conductive filaments at high potential in Figure 5(c). K ions, Na ions and oxygen vacancy in the insulating layer with Ag ions in top electrode together gradually form new connection under the potential impact. This is the reason why the conductivity of the insulating layer is suddenly increased to complete the "ON" state or the "SET" process in Figure 5(d). After "ON" state, the device will remain "ON" state until enough applied reverse voltage, subsequent Ag+, Na+ and K+ drift back to top electrode by driven electric-field as shown in Figure 5(e), then the status will change as "OFF" state after "RESET" process in Figure 5(f). Furthermore, the NDR effect is perpetually present in the negative bias region of I-V curves, for our memory cells, most of the oxygen vacancies are easily accumulated at the interface of Ti/Bio-film because of potentially Ti oxide and supply from reversible reaction of hydroxyl functional groups which are the common component of biological materials.29,46 This reaction process could be described by Eq:47

H 2O + VO + O×O + ↔ 2 OH −

(6)

Where VO and O×O stand for oxygen vacancies and oxygen in lattice, respectively. Excessive accumulation of oxygen vacancies will replace the conduction of the Ag filament in the bottom region, thus, a stable and meaningful NDR effect is observed in negative region of I-V curves. According to the above results, the interchange between HRS and LRS states can be explained by the

separation and closure of conductive filaments in the insulating layer, which are the major mechanism in Ag/Banana peel/Ti structure device.

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Figure 5. Schematic diagram of the proposed transfer process. (a) The original state with Ag top and Ti bottom electrodes. (b) Ag+ ion, K+ ion, Na+ ion and O vacancy movement under positive bias voltage. (c) Connection of two electrodes via conductive filament. (d) Set process. (e) High resistance state. (f) Reset process

CONCLUSIONS The repeatable nonvolatile resistive switching memory device based on nature banana peel were prepared by spin coating technique combined with radio frequency magnetron sputtering technique. The results confirm that the Ag/Banana peel/Ti structure device hold high OFF/ON resistance ratio (~60) and long retention characteristics (160 times circulation). In addition, the co-existence of memristor effect, capacitance effect and NDR phenomenon is

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observed in the device, this work gives ours a new guide towards of fabricating bio-memristor for next-generation nonvolatile bio-RRAM applications.

AUTHOR INFORMATION Corresponding Authors *E-mail: [email protected] (B. Sun); [email protected] (M. Lei); [email protected] (Y. Zhao) Author Contributions B. Sun and L. Zheng contributed equally for this work. B. Sun conceived and designed the experiments. The manuscript was written through contributions of all authors. S. Mao, S. Zhu and P. Zheng make a detailed and useful discussions and electric test. All authors have discussed related results and approval to the final version of the manuscript. Notes The authors declare no competing financial interest.

ACKNOWLEDGMENTS This work was supported by the National Magnetic Confinement Fusion Science Program (No. 2013GB114003-1, 2013GB110001), the National Natural Science Foundation of China (No. 51377138, 11504303), the 863 Program (No. 2014AA032701), the Sichuan Province Science Foundation (No. 2017JY0057), the application Infrastructure Projects in Sichuan Province (No. 2017JY0057) and the China Postdoctoral Science Foundation Founder Project (No. 158795).

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Figure 1 90x54mm (300 x 300 DPI)





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Figure 3 118x120mm (300 x 300 DPI)





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TOC Graphic 70x61mm (300 x 300 DPI)


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Metal Ions Redox Induced Repeatable Nonvolatile Resistive

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