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Achieving High Energy-High Power Density in a Flexible Quasi-Solid-State Sodium Ion Capacitor Hongsen Li, Lele Peng, Yue Zhu, Xiaogang Zhang, and Guihua Yu Nano Lett., Just Accepted Manuscript • DOI: 10.1021/acs.nanolett.6b02932 • Publication Date (Web): 08 Aug 2016 Downloaded from http://pubs.acs.org on August 10, 2016

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Achieving High Energy-High Power Density in a Flexible Quasi-Solid-State Sodium Ion Capacitor Hongsen Li,† ‡ Lele Peng,† Yue Zhu,† Xiaogang Zhang,* ‡, Guihua Yu*†

† Materials Science and Engineering Program and Department of Mechanical Engineering, The University of Texas at Austin, TX, 78712, USA. ‡ Jiangsu Key Laboratory of Materials and Technologies for Energy Conversion, College of Material Science and Engineering, Nanjing University of Aeronautics and Astronautics, Nanjing 210016, China

KEYWORDS: Sodium ion capacitor, Solid-state, Conducting gel polymer, High energy density, High power density, Energy storage

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ABSTRACT: Simultaneous integration of high energy output with high power delivery is a major challenge for electrochemical energy storage systems, limiting dual fine attributes on a device. We introduce a quasi-solid-state sodium ion capacitor (NIC) based on a battery type urchin-like Na2Ti3O7 (NTO) anode and a capacitor type peanut shell derived carbon (PSC) cathode, using a sodium ion conducting gel polymer as electrolyte, achieving high energy-high power characteristics in solid state. Energy densities can reach 111.2 Wh kg-1 at power density of 800 W kg-1, and 33.2 Wh kg-1 at power density of 11200 W kg-1, which are among the best reported state-of-the-art NICs. The designed device also exhibits long-term cycling stability over 3000 cycles with capacity retention ~86%. Furthermore, we demonstrate the assembly of a highly flexible quasi-solid-state NIC and it shows no obvious capacity loss under different bending conditions.


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Due to the limited natural resources and serious warming threats in the global scale, it is desperately required for human beings to cope with the environmental and energy problems.1,

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Accordingly, in the near future, it will be necessary to build a carbon-

reducing society supported by the renewable energy such as wind, wave and solar.3, 4 The utilization of these intermittent energy resources highlights the need for high-performance cost-effective electrochemical storage devices able to store and deliver energy efficiently.5 Supercapacitors, has matured significantly over the last decade, could be a viable solution.6, 7 They store charges through accumulation of ions at the high-surfacearea carbon surface (non-faradaic surface reactions), providing the abilities that can be charged and discharged rapidly with long-term lifetime.8 In view of that, when combined with the renewable energy resources, supercapacitors can potentially demonstrate their effectiveness and merits. Aside from the above advantages, the low energy density characteristics seriously restrict their further development.9 Alternatively, rechargeable ion batteries show competitive superiority in energy density through faradaic ion insertion reactions, but the power density and cycle life of the batteries are far from satisfactory.10, 11

As a result, it is urgent to develop the future energy storage systems, combining the

complementary features of high power supercapacitor and high energy rechargeable ion batteries, for many applications from portable electronics to public transportation, in which high energy-high power delivery and uptake and long-term cycle life are required.12 Recently, lithium ion capacitors have been explored to achieve the desired performance and become the focus of the researchers to realize different storage mechanisms at both electrodes in a device, wherein the supercapacitor type cathode


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endures fast charge-discharge processes, and the rechargeable ion battery type anode stores large capacitance.13-15 For example, the lithium ion capacitor based on TiC//pyridine derived carbon (in 1 mol L-1 LiPF6 solution/ethylene carbonate electrolyte) delivered an energy density of 101.5 Wh kg-1 (achieved at 450 W kg-1), and an outstanding cycle stability (~82% retention after 5000 cycles) within the voltage range of 0.0-4.5 V.16 At the same time, the fact that easily accessible global lithium reserves largely exist in politically sensitive or remote area, driving the research towards energy storage systems beyond lithium ions.17-19 Accordingly, replacing lithium with sodium to construct the sodium ion capacitors offers the opportunity to build the device integrated the features of potentially lower cost and high performance.20 In the past three years, the sodium ion capacitor technology has gained great advances and the performance can also be comparable to lithium ion capacitors.5, 21-23 Lim et al. reported a type of sodium ion capacitor based on Nb2O5@C/rGO50 anode and activated carbon (MSP20) cathode in 1 mol L-1 NaPF6 solution/ethylene carbonate/dimethyl carbonate electrolyte. The device delivered a maximum energy density of ca. 76 Wh kg-1 with the power density of ca. 80 W kg-1.24 However, most of the hybrid devices explored thus far used the liquid electrolytes, which leads to a concern about potential safety. For these hybrid devices, their electrolytes are almost universally based on combinations of liner and cyclic alkyl carbonates.25 The high volatility and flammability of these organic electrolytes pose a serious safety issue for their use in the consumer (especially for flexible and wearable applications) and transportation markets. Hence, an efficient solution to avoid these crucial risks is realizing solid-state storage devices using solid-state electrolytes or quasisolid-state electrolytes.26


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Herein, we design a quasi-solid-state sodium ion capacitor based on an urchin-like NTO battery-type anode and PSC supercapacitor-type cathode. A kind of sodium ion conducting gel polymer using the P(VDF-HFP) membrane as the matrix was used as the electrolyte.27 The designed hybrid device integrated the advantages of both the sodium ion batteries and the supercapacitors, pushing the energy density, power density and safety to a high level. We further assembled a flexible quasi-solid-state sodium ion capacitor, which has not been reported previously on the hybrid device. To produce the urchin-like NTO, a facile hydrothermal method combined with heat treatment was employed (see Experimental section for more details, Supporting Information). Shown in Figure 1a is scanning electron microscopy (SEM) image of the prepared NTO products, revealing an urchin-like morphology. The STEM image in Figure S1 (Supporting Information) further reveals that the diameter of NTO nanofibers on the surface of NTO microspheres is in the range of 10-20 nm. Figure 1b presents an X-ray diffraction (XRD) pattern of the resultant urchin-like NTO indexed to PDF file 59-0666, implying that the hydrothermal products are pure phase of NTO.28 Furthermore, Figure 1b insert schematically shows the crystal structure of NTO along the a-axis. The basic unit is a block of six TiO6 octahedrons, which extends out of the plane as a zig-zag ribbon of octahedrons limited to three in width.29, 30 A two-dimensional sheet of the composition (Ti3O7)2- centred on the (100) plane is formed by the corner-shared identical blocks. Shown in Figure 1c is the SEM of the peanut shell derived carbon, resembling a macroscopically open sponge morphology. The corresponding XRD pattern of the PSC shows two inconspicuous broad diffraction peaks that are indexed as (002) and (100), indicative

of

its

much

lower

ordering.

The

Nitrogen

adsorption-desorption


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characterization is also measured and the results are shown in Figure S2 (Supporting Information). Specifically, the BET surface area is 1900.5 m2 g-1 and total pore volume is 0.86 cm3 g-1 with an average pore diameter of 1.94 nm, indicative of the considerable porosity and high surface areas of the PSC.

Figure 1. (a-b) SEM image and XRD patterns of urchin-like NTO, inset shows the crystallographic arrangements of NTO. (c-d) SEM and XRD pattern of PSC cathode material. The scale bars in (a) and (c) is 500 nm. The electrochemical properties of the NTO anode and PSC cathode are evaluated by a constant charge-discharge test in half cells using the sodium ion conducting gel polymer as the electrolyte. Shown in Figure S3 (Supporting Information) are the SEM images of the P(VDF-HFP) membrane, which is the matrix of the quasi-solid-state electrolyte before gelling. There are abundant pores on the surface of the membrane with the diameter of 1~2 µm which is beneficial to absorb and retain the organic electrolyte.


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Figure 2a shows the representative charge-discharge profiles of the NTO anode at a current density of 0.1 A g-1 between 0.01 and 2.5 V. A reversible capacity of 227 mAh g-1 can be achieved, and it shows smooth curves, little polarization and a low average operating voltage of ~0.35 V. The first charge-discharge curves of the NTO anode are shown in Figure S4a (Supporting information). Further rate tests reveal that the urchinlike NTO enables a high rate capability, providing high cycling stability with rapid changes of the current densities. It demonstrates a stable capacity of 210 mAh g-1 at the current density of 0.2 A g-1, and 200, 192, 188, 184, and 175 mAh g-1 at current density of 0.4, 0.6, 0.8, 1 and 2 A g-1, respectively. It is believed that the present urchin-like NTO is a promising battery type electrode in the hybrid ion capacitors which necessitate a high power anode with high rate capability to balance the kinetics gap between the slow faradaic anode and the fast physical capacitor type cathode in order to optimize the energy and power densities. Shown in Figure 2c is the long-term cycling performance of the NTO at a current density of 1 A g-1. The capacity retention is 95.1% after 1000 cycles, corresponding to a very low capacity fading rate. This cycling stability of these urchinlike NTO is superior to that of other reported NTO-based anode materials.31-33 In addition, the cyclic voltammetry (CV) of the NTO is also tested and shown in Figure S5a (Supporting Information). The typical charge-discharge curves of the PSC as the cathode are displayed in Figure 2d. It shows a large discharge capacity of 153 mAh g-1 with good reversibility. The rate capability of the PSC is also tested as shown in Figure 2e. It is clear that the electrode displays stable capacities at each tested current density. The charge-discharge curves of PSC at different current densities are shown in Figure S6b (Supporting Information). Figure 2f demonstrates the cycling stability and the


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corresponding coulombic efficiency of PSC. The electrode’s capacitance remains stable over 1000 cycles with no noticeable decay, indicating a long-term cycling stability in the cell. The appealing sodium ion storage characteristics combined with outstanding rate capability and cycling stability of both the NTO anode and PSC cathode in half cells is beneficial to improve the property when assembled into hybrid ion capacitors.

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50 20 0

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200 400 600 800 1000 Cycle number

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Figure 2. The electrochemical characteristics of urchin-like NTO and PSC in half cells. (a) The typical charge-discharge profiles of NTO between 0.01 and 2.5 V at a current density of 0.1 A g-1. The corresponding rate capability (b) and cycling performance (c) with coulombic efficiency over 1000 cycles at the current density of 1.0 A g-1. (d) The typical discharge-charge profiles of peanut shell carbon between 1.5 and 4.2 V at a current density of 0.1 A g-1. The corresponding rate capability (e) and cycling performance (f) with coulombic efficiency over 1000 cycles at the current density of 1.0 A g-1.


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Following the detailed electrochemical characterization of the NTO anode and PSC cathode, a quasi-solid-state sodium ion capacitor using the sodium ion conducting gel polymer as the electrolyte is assembled and characterized. Shown in Figure 3a is a schematic illustration of the coin cell assembled and charge storage mechanism of the NIC with two ends concurrently constructed with high performance NTO and PSC to overcome the kinetics discrepancy. During the charging process, the NTO anode undergoes reversible sodium ion insertion whereas the PSC cathode involves electric double layer capacitance with ClO4- anions. The above reactions are reversed during the discharging process. Figure 3b displays the photos of the prepared porous P(VDF-HFP) membrane (top) and its gel polymer electrolyte (bottom). The colour of the membrane changed from white to transparent, indicating the organic electrolyte successfully entrapped into the pores of the P(VDF-HFP) matrix. In Figure 3c, the galvanostatic charge-discharge curves of the quasi-solid-state sodium ion capacitor at current densities from 0.4 A g-1 to 3.2 A g-1 displays a symmetric quasi-triangular shape, indicating the combination of the different storage mechanisms (faradaic reactions and non-faradaic reactions). The Ragone plot in Figure 3d represents the trade-off between energy and power densities in the quasi-solid-state sodium ion capacitor described herein. A high energy density of 111.2 Wh kg-1 is achieved at a power density of 800 W kg-1, which is calculated from the total mass of both electrodes. It can still retain an energy density of 33.2 Wh kg-1 at a high power density of 11200 W kg-1, demonstrating the exceptional power delivery of the present sodium ion system. It is instructive to compare the present urchin-like NTO//PSC device to the state-of-the-art reported sodium ion capacitors and other energy storage systems such as lithium ion capacitors and lithium ion batteries to


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clarify the high energy-high power feature of the proposed design. Although reasonable performances

are

obtained

by

reported

literatures

such

as

AC//MCMB,34

AC//V2O5/CNT,35 AC//NaxH2-xTi3O7,36 Na3V2(PO4)3//Na3V2(PO4)3,37 PHPNC//TiC16 and LMO//CN-LTO-NMS,38 the sodium ion capacitor presented here demonstrates the most promising energy-power delivery. Moreover, our quasi-solid-state sodium ion capacitor using the sodium ion conducting gel polymer as the electrolyte even compare favorably with the device using liquid organic electrolyte (glass fiber as the separator). Indeed, unlike the present results, high energy output is generally accompanied by a low power delivery (Figure S7, Supporting Information). This is probably attributed to the higher sodium ionic conductivity of the gel polymer electrolyte than that of the commercial separator.27 Shown in Figure S8 (Supporting Information) is the impedance plots of the urchin-like NTO//PSC NIC using the liquid electrolyte and quasi-solid-state electrolyte, respectively. The resistance of device using the gel polymer electrolyte is much less than that of the device using liquid electrolyte combined commercial glass fiber separator. This may be because the polarity of the P(VDF-HFP) matrix buffers the movement of large ClO4- anions. The cycling stability of the urchin-like NTO//PSC quasi-solid-state NIC (shown in Figure 3e) is investigated at the current density of 3.2 A g-1, and the device maintains its columbic efficiency ca. 100% up to 3000 cycles with capacity retention of ca. 86%. In contrast to half cells which demonstrate good cycling performance with no noticeable decay during cycle tests, the device showed capacitance decay. The possible reasons may be due to an increase in the interfacial resistance and loss of active sodium ions with cycling.39, 40


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Figure 3. Electrochemical performance of the assembled quasi-solid-state sodium ion capacitors. (a) Schematic of a coin cell type sodium ion capacitor. (b) Photos of the prepared porous P(VDF-HFP) membrane and its gel polymer electrolyte. (c) Galvanostatic charge-discharge curves from 0.5 to 3.5 V at different current densities. (d) Ragone plots for the urchin-like NTO//PSC compared with other literature works. The energy and power densities and capacitance were calculated based on the total weight of the anode and cathode materials. (e) Cycling stability of the quasi-solid-state sodium ion capacitors. In order to explore the potential application of the present quasi-solid-state sodium ion capacitor, a flexible device is fabricated, following the significant trend of portable and wearable electronics which require high flexibility, performance and safety.41-44 Figure S9 (Supporting Information) schematically illustrates the fabrication process of the flexible quasi-solid-state NIC. The whole device, consisting of foil/poly bag film, gel polymer electrolyte, cathode and anode, is safer and thinner than the common liquid


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electrolyte based hybrid device. No organic liquid electrolyte is used in the device or device fabrication, thus the designed NIC potentially increases the safety and reduce the complicated fabrication cost. Furthermore, the flexible quasi-solid-state NIC are efficient, compact and they can fit the various size requirement of commercial electronics. Figure 4a shows the schematic illustration of the structure of a flexible quasi-solid-state NIC, which is sealed by two thin pieces of foil/poly bag film. To demonstrate the flexibility of the as-fabricated hybrid ion devices, the device is unrolled in flat and rolled with a mandrel of four different diameters (shown in Figure 4b and 4c inset) to evaluate its electrochemical behavior under different bending states. Encouragingly, there is no obvious capacity loss under different bending conditions, suggesting its remarkable mechanical robustness and great potential to be used for practical application. Furthermore, Figure 4d shows that the present flexible quasi-solid-state NIC is able to power a commercial desk lamp and a UT capacitor logo consisting of 50 red LEDs, demonstrating its high energy-high power characteristics.


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Figure 4. (a) Schematic illustration of the structure of the quasi-solid-state sodium ion capacitor. (b) Diagram of the flexible quasi-solid-state sodium ion capacitor under various bending conditions. (c) Stability of capacitive performance of the quasi-solid-state sodium ion capacitor collected at different bending conditions (the inset shows the flexibility with different mandrel radius). (d) A commercial desk lamp and a UT capacitor logo consisting of 50 red LEDs powered by the assembled quasi-solid-state sodium ion capacitor under rolled state. In summary, a quasi-solid-state sodium ion capacitor has been developed based on the urchin-like NTO and PSC as anode and cathode materials, respectively, using a sodium ion conducting gel polymer as electrolyte. Such a sodium ion capacitor can exhibit a battery-like high energy characteristics and a supercapacitor-like high power and long cycle life because of the integrated storage mechanisms. A maximum energy density of 111.2 Wh kg-1 can be achieved at a power density of 800 W kg-1 based on the total mass of the electrode materials. The device can also exhibit an outstanding cycling stability with ca. 86% capacity retention after 3000 cycles. The observed superior electrochemical performance is among the best reported hybrid ion capacitors up to present. Furthermore, a flexible quasi-solid-state sodium ion capacitor is fabricated, and it is robust enough to work under harsh mechanical deformation conditions with no significant capacity loss. These findings provide an opportunity for the further development of hybrid ion capacitor for a wide range of high energy-high power required electronic applications. ASSOCIATED CONTENT Supporting Information.


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Detailed experimental procedures and supplementary characterization methods including STEM, SEM, BET, CV, Charge-discharge and EIS test of the prepared samples. This material is available free of charge via the Internet at http://pubs.acs.org. AUTHOR INFORMATION Corresponding Author * E-mail: [email protected] * E-mail: [email protected] Author Contributions H. L. and L. P. equally contributed to this work. Notes The authors declare no financial competing interest. ACKNOWLEDGMENT G.Y. acknowledges the funding support from the Welch Foundation Grant F-1861, ACS Petroleum Research Fund award (55884-DNI10) and Alfred P. Sloan Research Fellowship. X.Z. acknowledges financial support by the National Program on Key Basic Research Project of China (973 Program, No. 2014CB239701), National Natural Science Foundation of China (No. 51372116, 51504139). H.L. acknowledges the Funding for Outstanding Doctoral Dissertation in NUAA (BCXJ14-10), Funding of Jiangsu Innovation Program for Graduate Education (KYLX_0255), Fundamental Research Funds for the Central Universities and the Priority Academic Program Development of Jiangsu Higher Education Institutions.


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