High-performance bilayer flexible resistive random access memory based on low-temperature thermal atomic layer deposition

Abstract

We demonstrated a flexible resistive random access memory device through a low-temperature atomic layer deposition process. The device is composed of an HfO2/Al^sub 2^O3-based functional stack on an indium tin oxide-coated polyethylene terephthalate substrate. After the initial reset operation, the device exhibits a typical bipolar, reliable, and reproducible resistive switching behavior. After a 10^sup 4^-s retention time, the memory window of the device is still in accordance with excellent thermal stability, and a 10-year usage is still possible with the resistance ratio larger than 10 at room temperature and at 85°C. In addition, the operation speed of the device was estimated to be 500 ns for the reset operation and 800 ns for the set operation, which is fast enough for the usage of the memories in flexible circuits. Considering the excellent performance of the device fabricated by low-temperature atomic layer deposition, the process may promote the potential applications of oxide-based resistive random access memory in flexible integrated circuits.

Fang et al. Nanoscale Research Letters 2013, 8:92 http://www.nanoscalereslett.com/content/8/1/92

NANO EXPRESS Open Access

High-performance bilayer flexible resistive random access memory based on low-temperature thermal atomic layer deposition

Run-Chen Fang, Qing-Qing Sun*, Peng Zhou*, Wen Yang, Peng-Fei Wang and David Wei Zhang

Abstract

We demonstrated a flexible resistive random access memory device through a low-temperature atomic layer deposition process. The device is composed of an HfO2/Al2O3-based functional stack on an indium tin oxide-coated polyethylene terephthalate substrate. After the initial reset operation, the device exhibits a typical bipolar, reliable, and reproducible resistive switching behavior. After a 104-s retention time, the memory window of the device is still in accordance with excellent thermal stability, and a 10-year usage is still possible with the resistance ratio larger than 10 at room temperature and at 85C. In addition, the operation speed of the device was estimated to be 500 ns for the reset operation and 800 ns for the set operation, which is fast enough for the usage of the memories in flexible circuits. Considering the excellent performance of the device fabricated by low-temperature atomic layer deposition, the process may promote the potential applications of oxide-based resistive random access memory in flexible integrated circuits.

Keywords: Flexible memory, Atomic layer deposition, Low temperature

Background

Since flexible electronic system (FES) appeals to be light, convenient, has conformal contingence with the crooked surface, and excellent interfaces with humans, it ought to be a prospective existing form of electronic product to substitute its clumsy predecessors manufactured and packaged by traditional bulk silicon technology [1,2]. Up to now, multifarious electronic components, such as integrated circuits (ICs) [3,4], active matrix organic light-emitting diodes [5], sensors [6], radiofrequency identification antennas [7], and solar cells [8,9], have been fabricated on flexible substrates and are delved by many researchers. As we know, among all the components used in ICs, good and reliable memories [10,11] will maximize the functionality of ICs, and it is also important for the FES.

Among all the memories, nonvolatile resistive random access memory (RRAM) is the most promising candidate because of its low power consumption, high speed, simple structure, and high packaging density, compared

with its counterparts such as flash memory and DRAM [12-14]. Currently, oxides, such as STO [15], HfO2 [16],

NiO [17], Al2O3 [18], ZnO [19], and GO [20], have received much interest in resistive switching research. Among the oxides mentioned, HfO2 has been profoundly studied and contains great potentiality to be put into applications. However, the application of HfO2-

based RRAM on flexible substrate is still rare.

In recent years, atomic layer deposition (ALD) has emerged as a new technique for depositing films, particularly for fabricating oxide films. Owing to its self-limiting mechanism during the process, excellent step coverage and conformal thickness of the film can be achieved [21]. Although the deposition of oxide film by ALD on bulk silicon is very mature, seldom had researchers used this method to deposit films on flexible substrate. The main reason is that the flexible substrate could not undergo high-temperature processing above 200C, except in some cases such as depositing films using plasma-enhanced atomic layer deposition under low temperature where plasma damage and degradation of the step coverage is unavoidable [22].

* Correspondence: mailto:[email protected]

Web End [email protected] ; mailto:[email protected]

Web End [email protected] State Key Laboratory of ASIC and System, Department of Microelectronics, Fudan University, Shanghai 200433, China

2013 Fang et al.; licensee Springer. This is an Open Access article distributed under the terms of the Creative Commons Attribution License (http://creativecommons.org/licenses/by/2.0

Web End =http://creativecommons.org/licenses/by/2.0), which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

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In this letter, we fabricated a bilayer flexible RRAM device based on HfO2/Al2O3 films under low temperature, with resistive layers deposited using a low-temperature ALD process at 120C and the electrodes sputtered by direct current (DC) magnetron reactive sputtering at room temperature. The devices fabricated by these methods exhibit impressive resistive switching characteristics with reliable data retention properties under room temperature and elevated temperature up to 85C.

Methods

Flexible RRAM was fabricated on polyethylene terephthalate (PET) substrate coated by indium tin oxide (ITO) conducting film, and ITO serves as the bottom electrode in our devices. During the process, the substrate was fixed on a 3-in wafer with polyimide tapes in order to maintain sufficient mechanical support. The Al2O3 layer was deposited by 41 cycles of low-temperature

ALD at 120C with trimethyl aluminum (TMA) and water

Figure 1 The XPS spectra. (a) Al 2p and O 1s peaks at the surface and in the bulk of the Al2O3 film. (b) Hf 4f and O 1s peaks at the surface and in the bulk of HfO2 film.

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as precursors. Subsequently, the HfO2 layer was deposited by 67 cycles within the same framework using tetrakis (ethylmethylamino)hafnium (TEMAH) and water as precursors. TMA was pulsed at room temperature, and TEMAH was heated to 85C to offer enough evaporation pressure. Al2O3 film was deposited with a pulse time of 0.1 and 0.2 s for TMA and water, and the purging time for TMA and water was 5 and 20 s, respectively. The deposition method of HfO2 was derived from our previous work[23]. Finally, a 50-nm TiN top electrode was sputtered on the resistive layer by DC magnetron reactive sputtering through a metal shadow mask with a diameter of 400 m.

The thicknesses of the HfO2 and the Al2O3 layer were estimated to be 10.1 and 4.9 nm by Sopra GES5E spectroscopic ellipsometry. X-ray photoelectron spectroscopy (XPS) of HfO2 and Al2O3 on the PET substrate was performed using a Kratos Axis Ultra DLD XPS (Kratos Analytical, Ltd., Manchester, UK). Electrical properties at room temperature and at 85C of the device were assayed using an Agilent B1500A (Agilent Technologies, Inc., Santa Clara, CA, USA) semiconductor parameter analyzer and an Agilent B1525A high-voltage semiconductor pulse generator. Impedance of high and low resistance states was analyzed by an Agilent 4294A precision impedance analyzer. The device was tested with top biased and grounded bottom electrodes.

Results and discussion

The XPS spectra of HfO2 and Al2O3 films are respectively shown in Figure 1a,b. In Figure 1a, the binding energies of Al 2p in the bulk and at the surface of the Al2O3 film are both at 73.9 eV, and the binding energies of O 1s in the bulk and at surface of the Al2O3 film

show that the Al-O bond is at about 530.8 eV without any shifts. In Figure 1b, the bulk and surface XPS spectra of the HfO2 film illustrate that the binding energies of the Hf 4f5/2 and 4f7/2 are at the positions of about

18.4 and 16.7 eV, respectively, with a 1.7-eV spin-orbit splitting. From the O 1s spectrum in Figure 1b, the Hf-O bond is at 530 eV in the interior and at the surface of the HfO2 film [24]. However, from the surface XPS of O 1s in both Al2O3 and HfO2, the existence of -OH is observed with a peak at around 532 eV. This is either incorporated by residue water precursors during the process because of the high desorption energy of water at low temperatures or exposing the film to the atmosphere (CO2 and moisture) before XPS measurement[23]. The XPS qualification report shows that the ratios of the O/Al in the bulk of the Al2O3 film and the O/Hf in the bulk of the HfO2 are about 1.7 and 2, respectively, which means that our films obtained at low temperature are almost stoichiometric.

Typical I-V characteristics of the device are shown in Figure 2, which indicates a bipolar resistive switching.

The initial resistance state of the TiN/HfO2/Al2O3/ITO flexible RRAM (schematically shown in the inset of Figure 2) device was found (curve 1) to be even lower than the low resistance state (LRS) of the device, and an excess negative voltage was applied to reset the device to high resistance state (HRS). The initial reset voltage and current were 3 V and 10 mA, respectively. This phenomenon was not observed in RRAMs grown at high temperatures, except in some cases after high-temperature annealing [25-27]. We attribute this phenomenon to the high density of defects in the film grown at low temperature. As with our low-temperature ALD processing using H2O as oxidant, it is inevitable that there will be some incomplete reactions during the process, such as residual -OH groups, fixed positive charges, and oxygen vacancies. It is considered that when the density of defects exceeds the percolation theory threshold value, the resistance of the insulating layer will be lower than the typical value [26,28]. This large density of defects may be very suitable for RRAM applications which work dependently on the defects. After the initial reset operation, the set operation was achieved by sweeping a positive voltage from 0 to 1.5 V with 1 mA of current compliance to protect the device from a hard breakdown (curve 3). An abrupt increase of current was observed at 1 V, and the device was set to LRS (approximately 650 ). A negative bias was then applied to the device by a sweep from 0 to 1 V, and a sudden descent of current occurred at 0.6 V, indicating that the device was reset to HRS with a reset current in the same magnitude as the set current.

To further investigate the conduction mechanism in the flexible RRAM, the I-V curves of the ON and OFF states were re-plotted in a dual logarithmic plot. As shown in Figure 3a, the logarithmic plot and linear fitting of the previous I-V curve for the device in LRS show

Figure 2 The initial reset operation and the typical resistive switching characteristics of the flexible RRAM. Inset: the photograph and schematic structure of the device.

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Figure 3 Dual logarithmic plots of the currentvoltage characteristics. (a) ON state device, (b) OFF state device under negative bias, and (c) OFF state device under positive bias.

a typical ohmic conduction with a slope of 0.95, which is considered to be the formation of conductive filaments in the memory cell during the set process. On the other hand, the conduction mechanism of the device in HRS seems to be more complicated, with considerable disparities in negative and positive sweepings. The fitting result for the device in HRS under negative bias is presented in Figure 3b, and the slopes of the curve differ from each

other under different voltages. When the electric field is small, the I-V slope is about 1.08, which conforms to ohmic conduction. However, when the voltage enters into the high electric field, the relationship between logarithm voltage and logarithm current turns to be an aV2 + bV relation, which is the classical space charge-limited conduction (SCLC). However, for the conduction behavior of the OFF state in devices under positive bias (Figure 3c), the slope is estimated to be 1.27 when the electric field is small, and the slope raises to 3.77 when the electric field is large enough until it approaches the compliance current (1 mA). As it is widely accepted that in oxide-based films the electron hops across the film through the body oxygen vacancies or defects, we attribute the conduction mechanism for the device in HRS under positive bias to be the trap-assisted tunneling (TAT) conduction [29]. When a negative bias was applied on the device, electrons are injected from the top electrode (TE) to the oxide and then proceed to the bottom electrode (BE). The resistance of TE to oxide is much larger than that of oxide to BE. As a result, the current is limited by the available electron in the oxide and leads to SCLC conduction. On the other hand, when a positive voltage was applied on the device, electrons are injected from BE to the oxide and then proceed to the TE. The current is limited by the traps available in the oxide near TE. As a result, the conduction mechanism will possibly be TAT.

Figure 4 shows the data retention characteristics of the flexible RRAM device at room temperature and under high temperature up to 85C. Both HRS and LRS were read at 0.1 V for 104 s, and a predetermination of the long-term retention was made. At room temperature, no significant degradation of the memory window was

Figure 4 Read disturbance test for device after 104-s retention time under room temperature and at 85C. No significant degradation of resistance ratio was observed under room temperature, and there is a slightly parallel descent of the HRS and LRS at 85C.

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observed, with the HRS ascending slightly. It suggests that sufficient memory margin still exists when the device undergoes decade employment. At elevated temperature (85C), even with descents of both LRS and HRS, the memory window is still in accordance with excellent thermal stability, and a 10-year usage is still possible, with the resistance ratio larger than 10.

The speed of the set and reset operations with different pulse widths at 5 V is exhibited in Figure 5, and the resistance state of the device after the pulse was read at0.1 V. We found that the resistive switching phenomenon occurs when the pulse width is larger than 500 ns for reset operation and 800 ns for set operation. The operation speed of the memory cell is a little faster than some cases before [22,30].

Stable and reproducible switching characteristics have been displayed in Figure 6 with a consistent 400 switching cycle without failures by DC sweeping. The sweeping voltage was applied from 0 to 2 V for set and 0 to 2 V for reset with a reading voltage of 0.1 V at room temperature. In Figure 6a, the result of the endurance test shows that memory ratio remains above 10:1 all along. Furthermore, statistics of the resistances and operation voltages are conducted separately according to the endurance test result. The resistance distributions of the LRS and HRS have been shown in Figure 6b, and we can find that only a small dispersion, with almost 90% of the LRS around 0.6 k and 80% of the HRS around 10 k, existed during the switching. In addition, Figure 6c shows the operation voltage distributions for set and reset. It can be obviously observed that almost 99% of the reset voltages are near 2 V and almost 85% of the set voltages are around 1 V. Through all the statistical results and previous test result, we can conclude that

Figure 6 The DC endurance test of the device. Voltage sweeping was from 0 V to 2 V for set and from 0 V to 2 V for reset at room temperature, with a reading voltage of 0.1 V. (a) The continuous program and erase test, (b) the statistical result of the set and reset voltages, and (c) the statistical result of the resistance distributions of the LRS and HRS.

Figure 5 The behavior of the TiN/HfO2/Al2O3/ITO/PET memory cell under different pulses. HRS and LRS are read at 0.1 V, and the set and reset operations of the devices were achieved with different pulsing widths at 5 V.

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our flexible RRAM is characterized with high uniformity and reliability.

To inspect the equivalent circuit model of the device, we measured the impedance of the device in HRS and LRS in the Z-Z () mode by applying 20 mV of AC small signal (40 Hz to 110 MHz) to the device. Figure 7 shows the Nyquist plot (Z-Z0, Z, and Z0 represent the absolute value of imaginary parts and real parts of the impedance) of the device in the LRS and HRS. In Figure 7a, one semicircle is observed in the LRS, indicating the equivalent RC parallel circuit model. Parameters from the fitting results reveal the existence of a tiny capacitance and a big resistance, which is in consonance with the conductive filament (CF) theory that when the RRAM is in LRS, it is mainly a resistance formed by the CF [10]. On the other hand, the calculated parameters for the HRS are shown in the inset of Figure 7b, and the device exhibits two different semicircles which indicate the complex equivalent circuit model that contains two RC parallel sections in series. In the LRS of the device,

conducting filaments are formed in the device, and as a result, the device can be considered as a resistor with small resistance and a capacitor (the area without formed filaments) with small capacitance. On the other hand, when the device is in HRS, conducting filaments are ruptured at a certain position in the oxide. The ruptured place will induce an additional tunneling resistor with big resistance and a capacitor with big capacitance.

Conclusions

In conclusion, a highly reliable and uniform flexible RRAM based on the TiN/HfO2/Al2O3/ITO structure, fabricated by a low-temperature process, was investigated. The fresh cell shows an ultra-low resistance state, and after the initial reset operation, a typical bipolar reliable and reproducible resistive switching behavior was demonstrated. It is found that the memory window is still in accordance with excellent thermal stability after a 104-s

retention time, and a 10-year usage is still possible with the resistance ratio larger than 10 at room temperature and at 85C. The resistance of the LRS and HRS exhibits a very concentrated distribution with almost 90% of the LRS around 0.6 k and 80% of the HRS around 10 k. The developed low-temperature process for the memories may promote the potential applications of oxide-based RRAM in flexible ICs.

Competing interestsThe authors declare that they have no competing interests.

Authors' contributionsRCF carried out the sample fabrication and drafted the manuscript. WY carried out the device measurements. PZ and PFW participated in writing the manuscript and in the discussion of results. QQS and DWZ participated in the design of the study and performed statistical analysis. All authors read and approved the final manuscript.

Authors' informationRCF received his B.S. degree in Physics and Electronics from Nanjing Information Engineering University, Nanjing, China in 2010. He is currently studying at the School of Microelectronics, Fudan University for his Master's degree. His research interests include flexible memory and device design. QQS received his B.S. degree in Physics, his M.S. and Ph.D. degrees in Microelectronics and Solid state Electronics from Fudan University, Shanghai, China in 2004 and 2009, respectively. He is currently an associate professor at the School of Microelectronics in Fudan University. His research interests include fabrication and characterization of advanced metal oxide semiconductor field effect transistors, mainly high-k dielectric-based devices. He is also interested in design, fabrication, and characterization of advanced memory devices, such as resistive switching memory devices and Flash. PZ received his B.S. degree in Physics and Ph.D. degree in Optics from Fudan University, Shanghai, China in 2000 and 2005, respectively. He is currently an associate professor at the School of Microelectronics, Fudan University. His research interests include fabrication and characterization of advanced metal oxide semiconductor field effect transistors, advanced memory devices, and graphene device. WY received her B.S. degree in Physics and Electronics from Henan University, Henan, China in 2010. She is currently studying at the School of Microelectronics, Fudan University for her Ph.D. degree. Her research interests include low-power circuit, memory and device design, and theoretical and experimental investigations of two dimensional materials. PFW received his B.S. and M.S. degrees from Fudan University, Shanghai, China in 1998 and 2001, respectively, and his Ph.D. degree from the

Figure 7 The Nyquist plots. (a) LRS and (b) HRS from impedance measurements. Their fittings to the equivalent circuits (solid line) and the circuit models as well as their parameters werealso presented.

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Technical University of Munich, Mnchen, Germany in 2003. Until 2004, he was with the head of the Memory Division of Infineon Technologies in Germany on the development and process integration of novel memory devices. Since 2009, he has been a professor at Fudan University. His research interests include design and fabrication of semiconductor devices and development of semiconductor fabrication technologies such as high-k gate dielectrics and copper/low-k integration. DWZ received his B.S., M.S., and Ph.D. degrees in Electrical Engineering from Xian Jiaotong University, Xian, China in 1988, 1991, and 1995, respectively. In 1997, he was an associate professor at Fudan University, Shanghai, China, where he has been a full professor since 1999. He is currently the Dean of the Department of Microelectronics and the Director of the Fudan-Novellus Interconnect Research Center. He has authored more than 200 referred archival publications and is the holder of 15 patents. More than 50 students have received their M.S. or Ph.D. degrees under his supervision. His research interests include integrated-circuit processing and technology, such as copper interconnect technology, atomic layer deposition of high-k materials; semiconductor materials and thin-film technology; new structure dynamic random access memory (RAM), Flash memory, and resistive RAM; and metal oxide semiconductor FET based on nanowire and nanotube and tunneling FET.

AcknowledgmentsThis work was supported by NSFC (grant nos. 61076114 and 61106108), the Shanghai Educational Development Foundation (10CG04), SRFDP(20100071120027), the Fundamental Research Funds for the Central Universities, and the S&T Committee of Shanghai (10520704200).

Received: 1 November 2012 Accepted: 27 January 2013 Published: 19 February 2013

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doi:10.1186/1556-276X-8-92Cite this article as: Fang et al.: High-performance bilayer flexible resistive random access memory based on low-temperature thermal atomic layer deposition. Nanoscale Research Letters 2013 8:92.