Existence of Resistive Switching Memory and Negative Differential

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Existence of Resistive Switching Memory and Negative Differential Resistance State in Self-Colored MoS2/ZnO Heterojunction Device Mayameen S. Kadhim, Feng Yang, Bai Sun, Wentao Hou, Haixia Peng, Yunming Hou, Yongfang Jia, Ling Yuan, Yanmei Yu, and Yong Zhao ACS Appl. Electron. Mater., Just Accepted Manuscript • DOI: 10.1021/acsaelm.8b00070 • Publication Date (Web): 04 Mar 2019 Downloaded from http://pubs.acs.org on March 5, 2019

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ACS Applied Electronic Materials

Existence of Resistive Switching Memory and Negative Differential Resistance State in Self-Colored MoS2/ZnO Heterojunction Device Mayameen S. Kadhim,†, ‡ Feng Yang,*,†,‡ Bai Sun,*,‡ Wentao Hou,ƪ Haixia Peng,§ Yunming Hou,‖ Yongfang Jia,‡ Ling Yuan,‡ Yanmei Yu,‡ and Yong Zhao,*, †,‡ † School

of Electrical Engineering, Key Laboratory of Magnetic Levitation Technologies and Maglev Trains, Ministry of Education of China, Southwest Jiaotong University, Chengdu, Sichuan 610031, China ‡ Superconductivity and New Energy R&D Center, Southwest Jiaotong University, Chengdu, Sichuan 610031, China § Department of Electrical and Computer Engineering, University of Waterloo, Waterloo, Ontario N2L 3G1, Canada ƪ College of Materials Science and Technology, Nanjing University of Aeronautics and Astronautics (NUAA), Yudao Street 29, 210016 Nanjing, China ‖ Oil Testing and Perforating Company of Daqing Oilfield Limited Company, Daqing, Heilongjiang 163000, China * Author to whom correspondence should be addressed. Email: [email protected]; [email protected]; [email protected] ABSTRACT: A resistive switching random access memories (RRAM) have occupied great scientific and industrial interest for next-generation data storage technology because of their advantages of nonvolatile behaviour, low power consumption, high density, rapid writing/erasing speed and simple operating system. In this work, the wide spectrum with selfcolored ZnO layers on the Ti foil is obtained by varying the sputtering time, and the colors of these ZnO films can be tuned by covered a MoS2 layer. Further, an existence of resistive switching (RS) memory and negative differential resistance (NDR) state in MoS2/ZnO heterojunction device was demonstrated, in which the bright yellow Ag/MoS2/ZnO/Ti device shows the best performance with long time endurance. This work opens up an opportunity for exploration of the multifunctional components in future electronic applications. Keywords: Resistive switching, Negative differential resistance, Self-colored, Heterojunction, Memory device.

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INTRODUCTION It is well known that the material colors are manufactured by interference influences rather than produced from dyes.1 These conventional chemicals (pigments and dyes) can form chemical colors by selectively absorbing and reflecting specific wavelengths of visible light.2 Indeed, the colors of structurally painted films shift agree with Bragg’s law, which shows that optical path length is a function of the index of refraction and film thickness. Thus, the light initially reflected from the top-film surface undertakes constructive and deconstructive interferences with light reflected on the essential substrate interface.3,4 Generality of these films belongs to functional modification, besides of creating the metal surface elegantly they improve the coarseness of surface and protect it from corrosion. Moreover, the nice colors of nature include both chemical and physical colors. The selfcolored films can be grown-up on many metals substrates such as titanium, steel, niobium, tantalum and zirconium.5 Recently, there are many methods used in coloring various metals such as electrochemical technique6,7 and magnetic sputtering method8,9 etc. However, the magnetron sputtering technique is a dominant method of syntheses of thin films which is extensively used at each of laboratory or industrial rules for the preparation of various types of single, multi oxides or other oxide-based composite layers.8 Then, the thin film interference is interference between light reflected from the top and bottom surfaces of a thin film. Where, the thin film has a thickness of t less than a few times of the wavelength of light λ. Furthermore, color is contributed indirectly with λ, and since all interference relies in some method on the ratio of λ to the size of the sample included, we should expect to get diverse colors for various thicknesses of a film.3

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In previous reports, the resistive switching device can be synthesized with a wide diversity of materials, such as binary metal oxides,10 perovskites11,12 and molecules.13 Among the binary metal oxides, ZnO and MoS2 are especially motivating for researchers because it can compose a wealthy assortment of nanostructures.14 Besides, the resistive switching performance has been broadly reported, and understanding the switching mechanism can help develop the stability and scalability of devices.9 Resistive random access memory (ReRAM) has been considered the most promising next-generation nonvolatile memory.15 Our work firstly demonstrate that a spectrum of colors of the passive film on Ti foil can be achieved by regulated the sputtering time while maintaining other experimental conditions constant. As shown in Figure 1, with the increasing of sputtering time, the color of the passive ZnO layers can be gradually diversified: brown → light yellow → purplish blue → orange → blue → pink. While the color of the MoS2 layers on the ZnO (at different thickness for ZnO layer and same thickness for MoS2 layer) can be gradually diversified: silver green → purple → bright yellow → green → orange → yellow. These passive colored layers are varied according to the internal refraction between the layers and other optical properties such as absorption, reflection and transmission behaviours of the light incident on it and which will be explained in detail later. Additionally, the coexistence of RRAM features and the NDR effect was observed at room temperature. The collection of these features makes the device with a nice surface a perfect candidate for memory application in multifunctional electronic devices in the future.

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Figure 1. The relationship between the colors and the thickness of layers.(A) ZnO/Ti at the various thickness (30, 50, 100, 150, 200 and 250) nm of ZnO layer; (B) MoS2/ZnO/Ti at the same thickness of MoS2 layer (50 nm) for all.

EXPERIMENTAL SECTION Ti substrates with dimensions of 2.0 cm × 1.5 cm had been ultrasonically cleaned in ethanol and deionized water before deposition. Then the ZnO and MoS2 films were deposited on Ti foil substrates with thickness of 100 m by the magnetic sputtering process. The thickness of the ZnO layers was regulated to (30, 50, 100, 150, 200 and 250 nm) by adjusting the sputtering time (3, 5, 10, 15, 20 and 25 min), and the MoS2 film has one thickness (50 nm) for all devices because we fixed the time at 5 min in this step. The detailed experimental procedures and as-prepared samples are presented in Figures S1-S3 of the Supporting Information. Finally, the top electrode of Ag was deposited by utilizing a metal shadow mask. Consequently, the devices with Ag/ZnO/Ti, Ag/MoS2/Ti and Ag/MoS2/ZnO/Ti sandwich structure were collected. The schematic diagram of the preparation process is shown in Figure 2.

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Figure 2. The preparation process of Ag/MoS2/ZnO/Ti device in which the Ag as the top electrode, the ZnO and MoS2 film as the active layers and Ti foil as the bottom electrode.

RESULTS AND DISCUSSION Ellipsometry is an appropriate and precise method for the measurement of thicknesses and refractive indexes of extremely thin films on solid surfaces and the calculation of optical constants of reflecting surfaces.16 While the light is reflected at the top surface, the change in intensity and state of polarisation of the returned beam can be calculated by the optical properties of the reflecting interface as shown in Figure 3a.17,18 When the light reflects from a medium having (n) index of refraction larger than that of the medium in which the light is travelling through, and a 180º phase change (or a λ/2 shift) occurs. Additional, the interference of light consisted of two types of constructive and destructive interference as shown in equations (1-2). 1  2t   m   2 n 

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(1) Constructive



2t  n

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(2) Destructive

In this formula, t is the thickness of thin film, λ is the wavelength of the light, n is the index of refraction of materials, and m is integer number (0, +1, -1, +2, -2 …etc.).3, 17 The cross-section morphology of the device was characterized using a scanning electron microscope (SEM), as shown in Figure 3b. Consequently, we utilized the SEM results (Figure 3b) to recognize the thickness of ZnO and MoS2 layers additional to SE analysis. At the same time, the structural analysis of the colored anodic film on Ti foils was calculated by X-ray diffraction (XRD) analysis, as shown in Figure 3d. Thus the XRD pattern of our samples is displayed in peaks marked with * representing ZnO film, while the peaks marked with # corresponds to MoS2, and ♦ is assigned to Ti element. Then the pink curve represents to Ag/ZnO/Ti device. Therefore, it is noted that just * and ♦ sign that’s mean both of ZnO and Ti compound peak in this device. In addition, each of green and blue curves illustrate Ag/MoS2/Ti and Ag/ZnO/MoS2/Ti devices respectively, we can find the ♦ and # signs mean Ti, S and MoS2 compounds peak. Additional, the * sign represent to ZnO film in blue curve shows the ZnO material peak.

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Figure 3. (a) Interference performance of light on the surface of the thin film and schematic of the interference behavior. (b) The cross-section SEM image of Ag/MoS2/ZnO/Ti device, (c) The diagram of Ag/MoS2/ZnO/Ti device. (d) The X-ray diffraction (XRD) testing of asprepared device.

At the same time, we displayed the schismatic diagram of our devices, and we have represented each layer with a specific color as shown in Figure 4(a1-a3). Figure 4(b1-b3) shows the I-V curve for each Ag/ZnO/Ti, Ag/MoS2/Ti and Ag/MoS2/ZnO/Ti device, in which we can observe the current starting increases at 0.75 V in the forward voltage scan and step by step decreases at a voltage of ~1.0 V in the reverse voltage scan in both of Ag/ZnO/Ti and Ag/MoS2/ZnO/Ti devices, as shown in Figure 4b1 and Figure 4b3 respectively. But for Ag/MoS2/Ti device, the initial increase in the current at ~0.5 V in the 7



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forward voltage scan and gradually decreases at a voltage of ~0.75 V in the reverse voltage scan as shown in Figure 4b2. After positive part, the I-V curves with an appearance of negative differential resistance (NDR) performance (when the current decreases at the increase in the voltage) are detected only for Ag/MoS2/ZnO/Ti device, as shown in Figure 4b3. Consequently, we noticed the Ag/MoS2/ZnO/Ti device has a negative differential resistance (NDR) in additional to resistive switching (RS) behaviour compared with the other two devices, meaning this device has multifunctional performance. In this situation, the resistance memories of both the HRS and the LRS for each device were estimated as shown in Figure 4(c1, c2 and c3), in which we can see that the memory retention of these devices can reach 100 cycles.

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Figure 4. (a) The diagram of devices Ag/ZnO (100 nm)/Ti, Ag/MoS2 (50 nm)/Ti and Ag/MoS2 (50 nm)/ZnO (100nm)/Ti respectively. (b) The first cycle at a voltage range from -1.0 V to 1.0 V for each device. (c) The resistance–cycle number curve in a positive bias voltage of 0.5, 0.525 and 0.4 V respectively.

In order to investigate the switching and conduction mechanisms for our devices, the I–V curve of the first sweeping cycle in the positive and negative voltage regions has schemed and curve-fit on a log-log scale in Figure 5. The first part of the curve in the positive region (HRS) displays Ohmic conduction behavior, demonstrating that the charges crossed through the Ag anode into the MoS2 and ZnO layers, respectively.

Figure 5. (a, c and e) The logarithmic plots of I–V curve in positive bias region, (b, d and f) in negative bias region for Ag/MoS2 (50 nm)/ZnO (100 nm)/Ti, Ag/ZnO (100 nm)/Ti and Ag/MoS2 (50 nm)/Ti device, respectively.

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The slope of this first section is around ~1.0, indicating an Ohmic conductance behavior. When the applied voltage is increased, the second section of the curve has a linear relation with a slope of ~2.3, ~1.84 and ~2.5, respectively, which indicates the relation of I ∝

Vm,

suggesting the conduction performance depends on the classical trap-controlled space charge limited conduction (SCLC).19,20 It seems that the charge transfer happens between the Ag anode and the active layers. This can be demonstrated by the formation of Ag conductive filaments.21,22 After that, the LRS region can be fitted with a slope of approximately ~1.209, 1.17 and 0.99 in positive part for all devices respectively. In this study, the space charge limited conduction (SCLC) model should be responsible for the RS performances, which can be explained by the Equation (3): V m1 J  2 m1 d

(3)

Here, the J is the current density; the V is the bias voltage, the d is the thickness of the active layer, and the m is the fitting index. If m = 0, the I-V characteristics imply Ohmic law (I ∝ V), but when m = 1, that means Child’s square law (I ∝ V2) happened. When m = 2, the current slope rise (I ∝ Vx, x>2) with a high field, wherefore the conductive filament forms,23 which is certain by Equation (4):24,25

9 V2 J  i  3 8 d

(4)

Here, J is the current density, εi is the permittivity of the oxide, μ is the mobility, d is the thickness of the oxide layers, and θ is the ratio of free and shallow trapped charge. In the device, Ag as the top electrode can be formed easily a conducting filament because the Ag atoms can be ionized into Ag ions under the electric field, which could be explained as: Ag → Ag+ + e− 10


(5)

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Then, the Ag+ drifts across the active layer under the high electric field, and the Ag accumulates progressively and forms conducting filament leading to the resistance decrease and the SET process has been completed. In particular, the negative differential resistance (NDR) in additional to resistive switching (RS) behavior was found compared with two others device. Therefore, this device has multifunctional performance because it will be multifaceted and can use differently in more complex devices. The colors of the ZnO/Ti device can be realized by regulating the process time, with the increasing of time (3, 5, 10, 15, 20 and 25 min), the color of the thin films can be progressively varied with various thickness of ZnO film, which can be estimated from this analysis and the same case with different colors when we deposited MoS2 on ZnO/Ti device as shown in Supplementary Information. Furthermore, the effect of particle size of ZnO is important to show more explanation of our work. When the thickness of ZnO layer is less than 100 nm, it will show the quantum dot behavior. Therefore, it will lead to the increase of band gap of ZnO due to quantum confinement effect. As shown in Figure S4, the size of ZnO nanoparticles at the surface of 30 nm thickness ZnO layer is about 9 nm with an estimated bandgap of 3.48 eV. For 100 nm thickness ZnO layer, the grain size is about 30-50 nm, the bandgap is close to that of the bulk ZnO (3.37 eV). It compare with materials at a thickness equal or more than 100 nm will be at bulk material behavior in this time, which will lead to a decrease of the band gap compare with last one. For this purpose, a quantitative description of the quantum size effect derived by Brus was used as follows in equation (1).26 ,27

Eg  Eg

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bulk

h2 1 1 1.8e 2  2 [ *  *] r o  r 8r m e mh …………. (6)



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Here, the me* and mh* are the effective masses of the electrons and holes respectively, εo is the permittivity of free space and εr is the relative permittivity of the material. Here me*= 0.24, mh*= 0.59 and εo = 8.854×10−12 Farads/m. Figure 6(a) display the band gap and work function for each material in the Ag/MoS2/ZnO/Ti device.28 Clearly, the barrier height would increase when the trend field of built-in field is the matching as the trend of the external filed. Then, the depletion region would be expanded and resulted in show high resistance (Figure 6). Moreover, if the trend of the built-in field is opposite to the trend of the external field, the barrier height would be reduced, and the depletion region would be narrowed, showing a low resistance state. Thus, when applying a positive voltage (reverse bias) on the Ti electrode, the interference of Ti/ZnO would display high resistance state because the depletion region would be extended. With the thickness of ZnO is increased, the electron traps (oxygen vacancy defect) will also rise and then leading to larger schottky barrier height which contributes to the presence of NDR more clearly. Also, when the thickness of ZnO layer is less or equal 30 nm, the band gap of ZnO will increase according to quantum confinement effect as mentioned above, which further lead to decrease of the barrier height. On contrary, when the thickness of ZnO layer is more than 100 nm, it will lead to decrease of the band gap of ZnO. Besides, the current density JSE can be correlated to the electric field (E) and temperature (T) by the Schottky equation as shown in Equation (7). J ES 

 q ( B  qE / 4 ) 4qm* ( KT ) 2 exp[ ] 3 h KT

(7)

Where m* is the electron effective mass in the oxide, k is Boltzmann’s constant, T is the temperature, h is Planck’s constant, E is the electric field across the oxide, ΦB is the junction barrier height, and ε is the permittivity of the oxide. Thus the increase of this barrier limits the motion of the electrons and in

a correct sense prevents them from crossing or passing easily as shown in Figure 6(b-e).

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Figure 6. (a) The bandgap diagram of Ag/MoS2/ZnO/Ti device. The first cycle I-V curve of Ag/MoS2/ZnO/Ti device at different thickness of ZnO layer (b) 30 nm, (c) 100 nm. (d) and (e) The schematic diagram to explain the Schottky barrier with change in the thickness of thin film (the red balls are the electrons).

In order to further understand the RS and NDR progress, it will be described the conduction mechanisms in details. In Ag/MoS2/ZnO/Ti device the Ag ions move from top to bottom electrode that leads increase the electric conduction between two electrodes.21,29 Then the conductive filaments start to grow with the electric field passing to the top electrode as shown in Figure 7a and b respectively. This is the cause of the production of Ag conductive filaments between the top electrode Ag and the bottom electrode Ti. That means the device has arrived at LRS.30,31 So, after the “Set” process, the device stays to be in the LRS until sufficient high potential of opposite polarity (< VReset) is applied to electrochemically rupture the Ag filaments to “Reset” the device.30-33 Thus, the HRS is achieved as shown in Figure 7c and d respectively. Subsequently, the negative differential resistance (NDR) will appear as shown in Figure 7e. When the voltage is increased in negative voltage region, the current will start decrease, and

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the reason of this phenomenon is because the barrier height of the junction between materials will increase and prevent the electrons from passing easily as previously explained.

Figure 7. The proposed RS and NDR mechanisms at the Ti/ZnO/MoS2/Ag and interfaces. (a) The Ag ions start to move from top to bottom electrode (HRS). (b) The conductive filaments start to grow with the electric field passing to the top electrode (Set process). (c) The device stays in the LRS. (d) The rupture in Ag filaments (Reset process). (e) The negative differential resistance (NDR) will appear. (f) The conductive filaments start to grow again with the negative electric field passing to the top electrode (LRS).

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Electron traps are produced by a diversity of defects (such as oxygen vacancy, lattice mismatch, etc.) in the crystal, and the traps can absorb the inserted electrons under the conduction band. It is well known that the Ti substrate has chemisorbed oxygen surroundings. Therefore, it can cause a larger amount of oxygen vacancies at the ZnO/Ti interface, which could induce a high density of interface formation. With a starting applied voltage, the electrons were inserted and trapped by oxygen vacancies and additional defects were generated at the MoS2/ZnO/Ti interface. With the rise of the bias voltage, the built-in electric field is increased, leading to the diffusion of the oxygen vacancies and trapped electrons. Accordingly, the current reduced as the internal electric field of the interface barrier layer was sufficiently large to overcome the influence of the applied voltage, which rises the formation of the negative differential resistance (NDR).

CONCLUSIONS In summary, the ZnO and MoS2 films with dominance colors can be successfully prepared by magnetron sputtering technique, and their colorations can be adjusted easily by tuning the thickness of ZnO and MoS2 films. Also, the coexistence of resistive switching (RS) memory and negative differential resistance (NDR) performance at room temperature was achieved in Ag/MoS2/ZnO/Ti device. Through mechanism analysis, it is considered the RS behavior between high resistance state and low resistance state is generally produced by the formation and rupture of Ag conductive filaments. This work is useful for developing reliable nonvolatile self-colored memristors with bi-functional (RS and NDR) electronic and colorful devices for applications in the future.

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Supporting Information The supporting information is available free of charge on the ACS Publications website. The plot of preparation process to Ag/ZnO/Ti, Ag/MoS2/Ti and Ag/MoS2/ZnO/Ti device; the schematics to display the relation among different thickness with various colors and I-V curve performance for Ag/ZnO/Ti and Ag/MoS2/ZnO/Ti devices.

AUTHOR INFORMATION * Corresponding Authors Email: [email protected], [email protected], and [email protected] Author Contributions F. Yang, M. S. Kadhim and B. Sun contributed equally to this work. F. Yan and B. Sun conceived and designed the experiments. The manuscript was finished through the assistances of all authors. 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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Existence of Resistive Switching Memory and Negative Differential

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