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Polypyrrole Wrapped V2O5 Nanowires Composite for Advanced Aqueous Zinc-Ion Batteries

Polypyrrole Wrapped V2O5 Nanowires Composite for Advanced Aqueous Zinc-Ion Batteries fenrg-08-00199 August 27, 2020 Time: 11:51 # 1 BRIEF RESEARCH REPORT published: 27 August 2020 doi: 10.3389/fenrg.2020.00199 Polypyrrole Wrapped V O Nanowires Composite for Advanced Aqueous Zinc-Ion Batteries 1 1 1 2 2 Xinghua Qin , Xinyu Wang , Juncai Sun , Qiongqiong Lu , Ahmad Omar and * * Daria Mikhailova 1 2 Institute of Materials and Technology, Dalian Maritime University, Dalian, China, Leibniz Institute for Solid State and Materials Research (IFW) Dresden e.V., Dresden, Germany Aqueous zinc-ion batteries (ZIBs) have obtained increasing attention owing to the high safety, material abundance, and environmental benignity. However, the development of cathode materials with high capacity and stable cyclability is still a challenge. Herein, Edited by: the polypyrrole (PPy)-wrapped V O nanowire (V O /PPy) composite was synthesized Yaolin Xu, 5 5 2 2 Helmholtz-Zentrum Berlin für by a surface-initiated polymerization strategy, ascribing to the redox reaction between Materialien und Energie, V O and pyrrole. The introduction of PPy on the surface of V O nanowires not 2 5 2 5 Helmholtz-Gemeinschaft Deutscher Forschungszentren (HZ), Germany only enhanced the electronic conductivity of the active materials but also reduced Reviewed by: the V O dissolution. As a result, the V O /PPy composite cathode exhibits a high 2 5 2 5 Soorathep Kheawhom, 1 1 specific capacity of 466 mAh g at 0.1 A g and a superior cycling stability with 95% Chulalongkorn University, Thailand capacity retention after 1000 cycles at a high current density of 5 A g . The superior Lian Yi Shao, Guangdong University of Technology, electrochemical performance is ascribed to the large ratio of capacitive contribution China 1 2C (92% at 1 mV s ) and a fast Zn diffusion rate. This work presents a simple method Ning Zhang, Hebei University, China for fabricating V O /PPy composite toward advanced ZIBs. 2 5 *Correspondence: Keywords: V O nanowires, surface-initiated polymerization, polypyrrole, cathode material, aqueous zinc-ion 2 5 Xinyu Wang battery [email protected] Qiongqiong Lu [email protected] INTRODUCTION Specialty section: The ever-increasing energy consumption, and limited fossil fuels, necessitates effective utilization This article was submitted to of renewable energy resources (Xu F. et al., 2020). For that purpose, large-scale efficient energy Electrochemical Energy Conversion and Storage, storage systems are desired (Shao et al., 2021). Although lithium-ion battery has found widespread a section of the journal applicability, it suffers from safety issues caused by flammable organic electrolytes as well as the Frontiers in Energy Research availability of Li source (Dong et al., 2020; Lu et al., 2020). Aqueous zinc-ion batteries (ZIBs) are Received: 01 July 2020 regarded as a suitable alternative for scalable energy storage systems, due to the usage of zinc metal Accepted: 29 July 2020 anode which, apart from high abundance and environmental friendliness, has a large theoretical Published: 27 August 2020 capacity (820 mAh g ) and a low redox potential [0.76 V vs. SHE (Wang F. et al., 2018; Citation: Wang et al., 2020b; Zhang et al., 2019a). Furthermore, the possibility of an aqueous electrolyte Qin X, Wang X, Sun J, Lu Q, endows an intrinsic non-flammability and high ionic conductivity (Wang et al., 2020a). However, Omar A and Mikhailova D (2020) corresponding ZIB cathode materials with high capacity and stable cyclability need to be further Polypyrrole Wrapped V O 2 5 explored (Zhang et al., 2019b). Nanowires Composite for Advanced Manganese oxides (Khamsanga et al., 2019; Wang J. et al., 2019), Prussian blue analogs (Liu Aqueous Zinc-Ion Batteries. et al., 2020; Zampardi and La Mantia, 2020), vanadium-based compounds (Yang et al., 2020), and Front. Energy Res. 8:199. doi: 10.3389/fenrg.2020.00199 some organic materials (Wang et al., 2020c) have been investigated as cathode materials for aqueous Frontiers in Energy Research | www.frontiersin.org 1 August 2020 | Volume 8 | Article 199 fenrg-08-00199 August 27, 2020 Time: 11:51 # 2 Qin et al. Polypyrrole Wrapped V O Nanowires Composite 2 5 ZIBs. Among those, vanadium-based materials, particularly PPy coating, indicating that the wrapping procedure has no vanadium oxides, are very attractive because of the advantage significant influence on the V O morphology (Figure 1B). 2 5 of high theoretical capacities due to multiple oxidation states The TEM image also confirms the nanowire morphology of the of vanadium. Unfortunately, the electrochemical performance of V O /PPy composite (Figure 1D). EDS elemental mappings 2 5 vanadium oxides in ZIBs is hindered by their poor electronic show the homogeneous distribution of C, O, V, and N throughout conductivity and noticeable solubility in the electrolyte (Zhang the entire V O /PPy composite, indicating the presence of PPy 2 5 et al., 2020). To address these issues, various strategies have (Figure 1C and Supplementary Figure S1B). been applied, such as using pre-insertion materials (V O H O) The XRD data of the V O nanowires mainly fit with the 2 5 2 2 5 (Wang X. et al., 2019), integration with carbon materials (Yan layered orthorhombic structure (JCPDS no. 40-1296), and typical et al., 2018), as well as electrolyte modifications (Wan et al., 2018). (001) and (003) reflection peaks are present (Figure 1E). A little Another viable approach is to incorporate conducting polymers amount of V O was also indexed and may be assigned to 4 7 along with V O (Du et al., 2020). Polypyrrole (PPy) is a widely the reduction of P123. The interlayer distance is estimated to 2 5 used conductive polymer, and V O /PPy composites have been be 0.96 nm by Bragg’s law from the (001) peak. This large 2 5 2C shown to exhibit enhanced performance in supercapacitors and distance is beneficial for Zn insertion/extraction during the LIBs (Wang J.G. et al., 2018). Therefore, with regard to aqueous electrochemical process. After the PPy coating, no significant ZIBs, an effective PPy coating can aid in enhancing the electronic change is observed in the XRD data, indicating that the layered conductivity of V O as well as help to reduce the solubility in structure was well maintained after the polymerization process. 2 5 the electrolyte. In order to confirm the PPy coating and identify the valence state Herein, V O nanowires were synthesized by a facile of vanadium in the V O /PPy composite, XPS was carried out. 2 5 2 5 hydrothermal method, and a surface-initiated polymerization Figure 1F shows the survey spectrum with the clear presence method was utilized to fabricate a PPy-wrapped V O of N 1s and C 1s, confirming the polymeric coating (see also 2 5 nanowire composite. V O served as the initiator to induce Supplementary Figure S2). Figure 1G shows the V 2p spectrum, 2 5 5C the polymerization reaction of pyrrole monomer at room with strong V 2p3/2 and V 2p1/2 peaks of V located at 517.6 eV 5C temperature due to the strong oxidizing property of V . and 525 eV, along with shoulder peaks at 516 eV and 523.8 eV, 4C Benefiting from the improved electronic conductivity and corresponding to V (Liu et al., 2019). The presence of a small 4C restricted V O dissolution due to the PPy layer, V O /PPy amount of V (9.3 at.%) corresponds to the oxygen vacancies 2 5 2 5 cathode delivered a higher specific capacity and rate performance generated in the V O surface due to the redox reaction between 2 5 in comparison to the pristine V O nanowire cathode. Therefore, V O and pyrrole. Previous studies on V O demonstrated 2 5 2 5 2 5 the V O /PPy composite is a promising high-performance that such vacancies enhance the electrochemical performance 2 5 cathode material for aqueous ZIBs toward large-scale energy (Liao et al., 2020). storage applications. The electrochemical performance of pristine V O and 2 5 V O /PPy composites is evaluated in aqueous ZIBs. Figure 2A 2 5 presents the rate capability of the pristine V O cathode and 2 5 V O /PPy composite cathode. The V O /PPy composite cathode 2 5 2 5 EXPERIMENTAL SECTION 1 1 delivers a high initial capacity of 466 mAh g at 0.1 A g , V O nanowires were synthesized by a facile hydrothermal as compared to the V O nanowire electrodes (425 mAh g ). 2 5 2 5 method according to previously reported literature (Wang J.G. Even at a very high current density of 5.0 A g , the V O /PPy 2 5 et al., 2018). 200 mg of obtained V O nanowires was dispersed composite cathode still possesses a higher discharge capacity of 2 5 into deionized water. Then, pyrrole (0.1 ml) dissolved in DMF 174 mAh g than that observed for the V O nanowire cathode 2 5 (4 ml) was slowly added to the above V O nanowire suspended (142 mAh g ). The results point to the better rate performance 2 5 solution and stirred for 24 h. The obtained V O /PPy was washed of V O /PPy composite in comparison to non-modified V O 2 5 2 5 2 5 carefully and dried in a vacuum oven. nanowire electrodes. The voltage-capacity plots for the V O /PPy 2 5 More detailed synthesis and characterization processes are composite at different current rates demonstrate that the redox available in electronic Supplementary Information. plateaus are well maintained even at a high current density of 5.0 A g (Figure 2B). In comparing to voltage-capacity plots for pristine V O , the overpotentials are slightly lower suggesting 2 5 improved kinetics due to the higher electrical conductivity of the RESULTS AND DISCUSSION composite (Supplementary Figure S3). V O nanowires were synthesized by the hydrothermal Based on the voltage profiles, the energy/power densities 2 5 method. The as-obtained V O nanowires show a diameter of the batteries were calculated and are shown in the Ragone 2 5 of approximately 15 nm with a cable-like nanostructure plot (Figure 2C). Impressively, the batteries base on the (Supplementary Figure S1A). The V O /PPy composites were V O /PPy composite cathode display a high energy density of 2 5 2 5 1 1 prepared using a surface-initiated polymerization strategy, as 235 Wh kg at a power density of 56 W kg and exhibit shown in Figure 1A. Owing to the strong oxidizing property a relatively high energy density of 100 Wh kg even at a of V O , the pyrrole monomer can be polymerized with V O high power density of 2335 W kg . Moreover, the V O /PPy 2 5 2 5 2 5 initiation, resulting in the surface coating of V O with PPy. composite cathodes are highly competitive among the aqueous 2 5 The morphology of V O nanowires was well-maintained after ZIBs based on the different cathodes: V O (Hu et al., 2017), 2 5 2 5 Frontiers in Energy Research | www.frontiersin.org 2 August 2020 | Volume 8 | Article 199 fenrg-08-00199 August 27, 2020 Time: 11:51 # 3 Qin et al. Polypyrrole Wrapped V O Nanowires Composite 2 5 FIGURE 1 | (A) Schematic illustrating the preparation of V O /PPy composite. Characterizations of the V O /PPy composite. (B) SEM image and (C) Corresponding 2 5 2 5 elemental mappings, (D) TEM image, (E) XRD patterns, (F) XPS survey spectrum, and (G) V 2p spectrum with fitting showing mixed valence of V after PPy coating. FIGURE 2 | Electrochemical performance of V O /PPy composites cathode in aqueous ZIBs. (A) Rate performance in comparison to pristine V O . (B) Voltage 2 5 2 5 - 1 - 1 profile plots at different current rates. (C) Ragone plot. (D) Cycling performance at 1A g and (E) Long-term cycling performance at 5A g , in comparison to pristine V O . 2 5 Frontiers in Energy Research | www.frontiersin.org 3 August 2020 | Volume 8 | Article 199 fenrg-08-00199 August 27, 2020 Time: 11:51 # 4 Qin et al. Polypyrrole Wrapped V O Nanowires Composite 2 5 TABLE 1 | Comparison of the initial capacity and cycling stability of V O /PPy 2 5 V O /PPy composite cathode exhibits a high initial capacity 2 5 composite with recent literature data on vanadium oxide-based cathodes 1 1 of 329 mAh g at 1 A g and a capacity retention of 94% in aqueous ZIBs. after 100 cycles, which is much higher than that of pristine V O cathodes (234 mAh g , 82%). Furthermore, long-term Electrodes Rate Initial Capacity References 2 5 (mA g ) capacity Retention cycling performance of the cathodes was evaluated, because it is (mAh g ) a key feature for practical applications. Even after 1000 cycles, the batteries based on the V O /PPy composite cathode show 2 5 V O /PPy 1000 329 94% (100 This work a reversible capacity of 174 mAh g with a capacity retention cycles) of 95%. In contract, pristine V O cathodes exhibit a poor 5000 174 95% (1000 2 5 cycles) cycling stability, with a specific capacity of only 93 mAh g K V O 1000 205 83% (50 cycles) Li S. et al., 0:25 2 5 after 1000 cycles corresponding to a capacity retention of 62% (Figure 2E). The strong capacity fading observed for pristine Na V O 1000 280 75% (50 cycles) Xie et al., 2020 1:25 3 8 V O cathode is most probably be a result of V O dissolution 2 5 2 5 a-Zn V O 4000 163 85% (1000 Sambandam 2 2 7 during cycling, which is minimized with the PPy coating for cycles) et al., 2018 the V O /PPy composite. Moreover, such a high cycling stability 2 5 V O nH O 6000 281.7 71% (900 Yan et al., 2018 2 5 2 for the V O /PPy composite is better compared to the recently 2 5 cycles) reported literature on aqueous ZIBs with vanadium oxide-based H V O 5000 173.6 94.3% (1000 He et al., 2017a 2 3 8 cathodes (Table 1). The high rate performance and stable long cycles) cycle life of the V O /PPy composite cathode are ascribed to 2 5 Li V O nH O 5000 252 92.1% (500 Yang Y. et al., x 2 5 2 cycles) 2018 the introduction of a conductive polymer PPy layer, which not (NH ) V O 1000 361.6 76.1% (100 Xu L. et al., only increases the electronic conductivity but also reduces the 4 2 6 16 cycles) 2020 dissolution of V O in the electrolyte. 2 5 The electrochemical kinetics of the V O /PPy composite 2 5 cathode was further investigated to understand the impressive NH V O (Yang G. et al., 2018), Na V (PO ) (Li et al., 2016), 4 4 10 3 2 4 3 heterogeneous vanadium oxide nanowire with V O nH O shell performance. Cyclic voltammetry (CV) was performed at various 2 5 2 and V O H O core (h-VOW) (Li X. et al., 2019), VS (He et al., scan rates from 0.1 to 1.0 mV s (Figure 3A). The CV curves 3 7 2 2 2017b), Zn V O (OH) (Chao et al., 2018), and NaV O /V O show similar redox peaks in the voltage window of 0.3–1.6 V. 3 2 7 2 6 15 2 5 (Lanlan et al., 2020). In addition, as shown in Figure 2D, the The characteristic peaks appeared at 0.5/0.7 V as well as 0.8/1.0 V, FIGURE 3 | The electrochemical kinetics of the V O /PPy composite cathode. (A) CV curves at different scan rates. (B) Log(peak current) vs. log(scan rate) plots for 2 5 2C different peaks marked in (A). (C) Capacity contribution ratios at different scan rates. (D) GITT curves. (E) Evaluated diffusion coefficients of Zn . Frontiers in Energy Research | www.frontiersin.org 4 August 2020 | Volume 8 | Article 199 fenrg-08-00199 August 27, 2020 Time: 11:51 # 5 Qin et al. Polypyrrole Wrapped V O Nanowires Composite 2 5 5C reflecting the redox processes in V O that is consistent with 2 5 the strong oxidizing property of V , the polymerization of the reported literature (Yang Y. et al., 2018; Zhang et al., 2018). The pyrrole monomer could be initiated at room temperature. Due capacity is regarded to be originated from two contributed parts: to the introduction of the conductive PPy layer, the V O /PPy 2 5 a surface-controlled capacitive part and a diffusion-induced part, cathode displayed a superior specific capacity and excellent as described in the literature (Ming et al., 2018): cycling stability. The outstanding electrochemical properties are explained by the large ratio of a capacitive-controlled process i D av (1) 1 (92% at 1 mV s ) and a fast zinc ion diffusion coefficient. Considering the excellent electrochemical performance, coupled In this equation, v is the scan rate, and a and b refer to with the safe and simple operation process of aqueous ZIBs, the adjustable parameters. The b values range from 0.5 to 1.0. V O /PPy composite cathode holds great promise for practical 2 5 Corresponding to b = 0.5, the observed capacity is fully diffusion- grid-level storage applications. induced. When the capacity is completely determined by a surface-controlled capacitive part, the b value is close to 1.0. The peak currents at different scan rates are plotted and fitted with a DATA AVAILABILITY STATEMENT linear function (Figure 3B). The b values are 0.51, 0.75, 0.61, and 0.64, which implies that the capacity of the V O /PPy composite 2 5 The raw data supporting the conclusions of this article will be cathode is simultaneously influenced by both the capacitive made available by the authors, without undue reservation. and diffusion processes. Furthermore, the capacity is divided as a capacitive-controlled part (k v) and diffusion-induced part 1= 2 (k v ) as described by the following equations: AUTHOR CONTRIBUTIONS 1=2 i D k vC k v (2) 1 2 All authors listed have made a substantial, direct and intellectual or contribution to the work, and approved it for publication. 1=2 1=2 i=v D k v C k (3) 1 2 The ratios of surface-controlled capacitive and diffusion- FUNDING induced parts with various scan rates are displayed in Figure 3C. The surface-controlled capacitive contribution ratio 1 1 This work was supported by the National Natural Science increases from 57% (0.1 mV s ) to 92% (1.0 mV s ), Foundation of China (21905037) and the Fundamental indicating that the batteries possess fast charge-transfer kinetics. Research Funds for the Central Universities (3132019328 The kinetics of the V O /PPy composite cathode is further 2 5 and 3132020151). evaluated by galvanostatic intermittent titration technique (GITT). The profiles in GITT curves of V O /PPy electrode 2 5 are well in coincidence with the galvanostatic charge–discharge ACKNOWLEDGMENTS profiles (Figure 3D). The zinc-ion diffusion coefficient during discharging–charging procedures for V O /PPy is 3.03 10 – 2 5 10 2 1 QL acknowledges the financial support from the China 1.46 10 cm S (Figure 3E), which is comparable to that of Scholarship Council (CSC). the reported aqueous ZIBs based on the V O @CNT composite 2 5 and porous V O nanofiber cathodes (Chen et al., 2019, 2020). 2 5 SUPPLEMENTARY MATERIAL CONCLUSION The Supplementary Material for this article can be found In this work, a surface-initiated polymerization strategy was online at: https://www.frontiersin.org/articles/10.3389/fenrg. utilized to synthesize PPy-wrapped V O nanowires. Owing to 2020.00199/full#supplementary-material 2 5 Dong, Y., Di, S., Zhang, F., Bian, X., Wang, Y., Xu, J., et al. (2020). 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Interfacial constructing flexible V2O5@polypyrrole core–shell nanowire membrane with superior Conflict of Interest: The authors declare that the research was conducted in the supercapacitive performance. ACS Appl. Mater. Interfaces 10, 18816–18823. absence of any commercial or financial relationships that could be construed as a doi: 10.1021/acsami.8b05660 potential conflict of interest. Wang, J., Wang, J.-G., Liu, H., Wei, C., and Kang, F. (2019). Zinc ion stabilized MnO2 nanospheres for high capacity and long lifespan aqueous zinc-ion Copyright © 2020 Qin, Wang, Sun, Lu, Omar and Mikhailova. This is an open-access batteries. J. Mater. Chem. A 7, 13727–13735. doi: 10.1039/c9ta03541a article distributed under the terms of the Creative Commons Attribution License Wang, X., Ma, L., and Sun, J. (2019). Vanadium pentoxide nanosheets in- (CC BY). The use, distribution or reproduction in other forums is permitted, provided situ spaced with acetylene black as cathodes for high-performance zinc-ion the original author(s) and the copyright owner(s) are credited and that the original batteries. ACS Appl. Mater. Interfaces 11, 41297–41303. doi: 10.1021/acsami. publication in this journal is cited, in accordance with accepted academic practice. No 9b13103 use, distribution or reproduction is permitted which does not comply with these terms. Frontiers in Energy Research | www.frontiersin.org 6 August 2020 | Volume 8 | Article 199 http://www.deepdyve.com/assets/images/DeepDyve-Logo-lg.png Frontiers in Energy Research Unpaywall

Polypyrrole Wrapped V2O5 Nanowires Composite for Advanced Aqueous Zinc-Ion Batteries

Qin, Xinghua; Wang, Xinyu; Sun, Juncai; Lu, Qiongqiong; Omar, Ahmad; Mikhailova, Daria
Frontiers in Energy Research – Aug 27, 2020
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fenrg-08-00199 August 27, 2020 Time: 11:51 # 1 BRIEF RESEARCH REPORT published: 27 August 2020 doi: 10.3389/fenrg.2020.00199 Polypyrrole Wrapped V O Nanowires Composite for Advanced Aqueous Zinc-Ion Batteries 1 1 1 2 2 Xinghua Qin , Xinyu Wang , Juncai Sun , Qiongqiong Lu , Ahmad Omar and * * Daria Mikhailova 1 2 Institute of Materials and Technology, Dalian Maritime University, Dalian, China, Leibniz Institute for Solid State and Materials Research (IFW) Dresden e.V., Dresden, Germany Aqueous zinc-ion batteries (ZIBs) have obtained increasing attention owing to the high safety, material abundance, and environmental benignity. However, the development of cathode materials with high capacity and stable cyclability is still a challenge. Herein, Edited by: the polypyrrole (PPy)-wrapped V O nanowire (V O /PPy) composite was synthesized Yaolin Xu, 5 5 2 2 Helmholtz-Zentrum Berlin für by a surface-initiated polymerization strategy, ascribing to the redox reaction between Materialien und Energie, V O and pyrrole. The introduction of PPy on the surface of V O nanowires not 2 5 2 5 Helmholtz-Gemeinschaft Deutscher Forschungszentren (HZ), Germany only enhanced the electronic conductivity of the active materials but also reduced Reviewed by: the V O dissolution. As a result, the V O /PPy composite cathode exhibits a high 2 5 2 5 Soorathep Kheawhom, 1 1 specific capacity of 466 mAh g at 0.1 A g and a superior cycling stability with 95% Chulalongkorn University, Thailand capacity retention after 1000 cycles at a high current density of 5 A g . The superior Lian Yi Shao, Guangdong University of Technology, electrochemical performance is ascribed to the large ratio of capacitive contribution China 1 2C (92% at 1 mV s ) and a fast Zn diffusion rate. This work presents a simple method Ning Zhang, Hebei University, China for fabricating V O /PPy composite toward advanced ZIBs. 2 5 *Correspondence: Keywords: V O nanowires, surface-initiated polymerization, polypyrrole, cathode material, aqueous zinc-ion 2 5 Xinyu Wang battery [email protected] Qiongqiong Lu [email protected] INTRODUCTION Specialty section: The ever-increasing energy consumption, and limited fossil fuels, necessitates effective utilization This article was submitted to of renewable energy resources (Xu F. et al., 2020). For that purpose, large-scale efficient energy Electrochemical Energy Conversion and Storage, storage systems are desired (Shao et al., 2021). Although lithium-ion battery has found widespread a section of the journal applicability, it suffers from safety issues caused by flammable organic electrolytes as well as the Frontiers in Energy Research availability of Li source (Dong et al., 2020; Lu et al., 2020). Aqueous zinc-ion batteries (ZIBs) are Received: 01 July 2020 regarded as a suitable alternative for scalable energy storage systems, due to the usage of zinc metal Accepted: 29 July 2020 anode which, apart from high abundance and environmental friendliness, has a large theoretical Published: 27 August 2020 capacity (820 mAh g ) and a low redox potential [0.76 V vs. SHE (Wang F. et al., 2018; Citation: Wang et al., 2020b; Zhang et al., 2019a). Furthermore, the possibility of an aqueous electrolyte Qin X, Wang X, Sun J, Lu Q, endows an intrinsic non-flammability and high ionic conductivity (Wang et al., 2020a). However, Omar A and Mikhailova D (2020) corresponding ZIB cathode materials with high capacity and stable cyclability need to be further Polypyrrole Wrapped V O 2 5 explored (Zhang et al., 2019b). Nanowires Composite for Advanced Manganese oxides (Khamsanga et al., 2019; Wang J. et al., 2019), Prussian blue analogs (Liu Aqueous Zinc-Ion Batteries. et al., 2020; Zampardi and La Mantia, 2020), vanadium-based compounds (Yang et al., 2020), and Front. Energy Res. 8:199. doi: 10.3389/fenrg.2020.00199 some organic materials (Wang et al., 2020c) have been investigated as cathode materials for aqueous Frontiers in Energy Research | www.frontiersin.org 1 August 2020 | Volume 8 | Article 199 fenrg-08-00199 August 27, 2020 Time: 11:51 # 2 Qin et al. Polypyrrole Wrapped V O Nanowires Composite 2 5 ZIBs. Among those, vanadium-based materials, particularly PPy coating, indicating that the wrapping procedure has no vanadium oxides, are very attractive because of the advantage significant influence on the V O morphology (Figure 1B). 2 5 of high theoretical capacities due to multiple oxidation states The TEM image also confirms the nanowire morphology of the of vanadium. Unfortunately, the electrochemical performance of V O /PPy composite (Figure 1D). EDS elemental mappings 2 5 vanadium oxides in ZIBs is hindered by their poor electronic show the homogeneous distribution of C, O, V, and N throughout conductivity and noticeable solubility in the electrolyte (Zhang the entire V O /PPy composite, indicating the presence of PPy 2 5 et al., 2020). To address these issues, various strategies have (Figure 1C and Supplementary Figure S1B). been applied, such as using pre-insertion materials (V O H O) The XRD data of the V O nanowires mainly fit with the 2 5 2 2 5 (Wang X. et al., 2019), integration with carbon materials (Yan layered orthorhombic structure (JCPDS no. 40-1296), and typical et al., 2018), as well as electrolyte modifications (Wan et al., 2018). (001) and (003) reflection peaks are present (Figure 1E). A little Another viable approach is to incorporate conducting polymers amount of V O was also indexed and may be assigned to 4 7 along with V O (Du et al., 2020). Polypyrrole (PPy) is a widely the reduction of P123. The interlayer distance is estimated to 2 5 used conductive polymer, and V O /PPy composites have been be 0.96 nm by Bragg’s law from the (001) peak. This large 2 5 2C shown to exhibit enhanced performance in supercapacitors and distance is beneficial for Zn insertion/extraction during the LIBs (Wang J.G. et al., 2018). Therefore, with regard to aqueous electrochemical process. After the PPy coating, no significant ZIBs, an effective PPy coating can aid in enhancing the electronic change is observed in the XRD data, indicating that the layered conductivity of V O as well as help to reduce the solubility in structure was well maintained after the polymerization process. 2 5 the electrolyte. In order to confirm the PPy coating and identify the valence state Herein, V O nanowires were synthesized by a facile of vanadium in the V O /PPy composite, XPS was carried out. 2 5 2 5 hydrothermal method, and a surface-initiated polymerization Figure 1F shows the survey spectrum with the clear presence method was utilized to fabricate a PPy-wrapped V O of N 1s and C 1s, confirming the polymeric coating (see also 2 5 nanowire composite. V O served as the initiator to induce Supplementary Figure S2). Figure 1G shows the V 2p spectrum, 2 5 5C the polymerization reaction of pyrrole monomer at room with strong V 2p3/2 and V 2p1/2 peaks of V located at 517.6 eV 5C temperature due to the strong oxidizing property of V . and 525 eV, along with shoulder peaks at 516 eV and 523.8 eV, 4C Benefiting from the improved electronic conductivity and corresponding to V (Liu et al., 2019). The presence of a small 4C restricted V O dissolution due to the PPy layer, V O /PPy amount of V (9.3 at.%) corresponds to the oxygen vacancies 2 5 2 5 cathode delivered a higher specific capacity and rate performance generated in the V O surface due to the redox reaction between 2 5 in comparison to the pristine V O nanowire cathode. Therefore, V O and pyrrole. Previous studies on V O demonstrated 2 5 2 5 2 5 the V O /PPy composite is a promising high-performance that such vacancies enhance the electrochemical performance 2 5 cathode material for aqueous ZIBs toward large-scale energy (Liao et al., 2020). storage applications. The electrochemical performance of pristine V O and 2 5 V O /PPy composites is evaluated in aqueous ZIBs. Figure 2A 2 5 presents the rate capability of the pristine V O cathode and 2 5 V O /PPy composite cathode. The V O /PPy composite cathode 2 5 2 5 EXPERIMENTAL SECTION 1 1 delivers a high initial capacity of 466 mAh g at 0.1 A g , V O nanowires were synthesized by a facile hydrothermal as compared to the V O nanowire electrodes (425 mAh g ). 2 5 2 5 method according to previously reported literature (Wang J.G. Even at a very high current density of 5.0 A g , the V O /PPy 2 5 et al., 2018). 200 mg of obtained V O nanowires was dispersed composite cathode still possesses a higher discharge capacity of 2 5 into deionized water. Then, pyrrole (0.1 ml) dissolved in DMF 174 mAh g than that observed for the V O nanowire cathode 2 5 (4 ml) was slowly added to the above V O nanowire suspended (142 mAh g ). The results point to the better rate performance 2 5 solution and stirred for 24 h. The obtained V O /PPy was washed of V O /PPy composite in comparison to non-modified V O 2 5 2 5 2 5 carefully and dried in a vacuum oven. nanowire electrodes. The voltage-capacity plots for the V O /PPy 2 5 More detailed synthesis and characterization processes are composite at different current rates demonstrate that the redox available in electronic Supplementary Information. plateaus are well maintained even at a high current density of 5.0 A g (Figure 2B). In comparing to voltage-capacity plots for pristine V O , the overpotentials are slightly lower suggesting 2 5 improved kinetics due to the higher electrical conductivity of the RESULTS AND DISCUSSION composite (Supplementary Figure S3). V O nanowires were synthesized by the hydrothermal Based on the voltage profiles, the energy/power densities 2 5 method. The as-obtained V O nanowires show a diameter of the batteries were calculated and are shown in the Ragone 2 5 of approximately 15 nm with a cable-like nanostructure plot (Figure 2C). Impressively, the batteries base on the (Supplementary Figure S1A). The V O /PPy composites were V O /PPy composite cathode display a high energy density of 2 5 2 5 1 1 prepared using a surface-initiated polymerization strategy, as 235 Wh kg at a power density of 56 W kg and exhibit shown in Figure 1A. Owing to the strong oxidizing property a relatively high energy density of 100 Wh kg even at a of V O , the pyrrole monomer can be polymerized with V O high power density of 2335 W kg . Moreover, the V O /PPy 2 5 2 5 2 5 initiation, resulting in the surface coating of V O with PPy. composite cathodes are highly competitive among the aqueous 2 5 The morphology of V O nanowires was well-maintained after ZIBs based on the different cathodes: V O (Hu et al., 2017), 2 5 2 5 Frontiers in Energy Research | www.frontiersin.org 2 August 2020 | Volume 8 | Article 199 fenrg-08-00199 August 27, 2020 Time: 11:51 # 3 Qin et al. Polypyrrole Wrapped V O Nanowires Composite 2 5 FIGURE 1 | (A) Schematic illustrating the preparation of V O /PPy composite. Characterizations of the V O /PPy composite. (B) SEM image and (C) Corresponding 2 5 2 5 elemental mappings, (D) TEM image, (E) XRD patterns, (F) XPS survey spectrum, and (G) V 2p spectrum with fitting showing mixed valence of V after PPy coating. FIGURE 2 | Electrochemical performance of V O /PPy composites cathode in aqueous ZIBs. (A) Rate performance in comparison to pristine V O . (B) Voltage 2 5 2 5 - 1 - 1 profile plots at different current rates. (C) Ragone plot. (D) Cycling performance at 1A g and (E) Long-term cycling performance at 5A g , in comparison to pristine V O . 2 5 Frontiers in Energy Research | www.frontiersin.org 3 August 2020 | Volume 8 | Article 199 fenrg-08-00199 August 27, 2020 Time: 11:51 # 4 Qin et al. Polypyrrole Wrapped V O Nanowires Composite 2 5 TABLE 1 | Comparison of the initial capacity and cycling stability of V O /PPy 2 5 V O /PPy composite cathode exhibits a high initial capacity 2 5 composite with recent literature data on vanadium oxide-based cathodes 1 1 of 329 mAh g at 1 A g and a capacity retention of 94% in aqueous ZIBs. after 100 cycles, which is much higher than that of pristine V O cathodes (234 mAh g , 82%). Furthermore, long-term Electrodes Rate Initial Capacity References 2 5 (mA g ) capacity Retention cycling performance of the cathodes was evaluated, because it is (mAh g ) a key feature for practical applications. Even after 1000 cycles, the batteries based on the V O /PPy composite cathode show 2 5 V O /PPy 1000 329 94% (100 This work a reversible capacity of 174 mAh g with a capacity retention cycles) of 95%. In contract, pristine V O cathodes exhibit a poor 5000 174 95% (1000 2 5 cycles) cycling stability, with a specific capacity of only 93 mAh g K V O 1000 205 83% (50 cycles) Li S. et al., 0:25 2 5 after 1000 cycles corresponding to a capacity retention of 62% (Figure 2E). The strong capacity fading observed for pristine Na V O 1000 280 75% (50 cycles) Xie et al., 2020 1:25 3 8 V O cathode is most probably be a result of V O dissolution 2 5 2 5 a-Zn V O 4000 163 85% (1000 Sambandam 2 2 7 during cycling, which is minimized with the PPy coating for cycles) et al., 2018 the V O /PPy composite. Moreover, such a high cycling stability 2 5 V O nH O 6000 281.7 71% (900 Yan et al., 2018 2 5 2 for the V O /PPy composite is better compared to the recently 2 5 cycles) reported literature on aqueous ZIBs with vanadium oxide-based H V O 5000 173.6 94.3% (1000 He et al., 2017a 2 3 8 cathodes (Table 1). The high rate performance and stable long cycles) cycle life of the V O /PPy composite cathode are ascribed to 2 5 Li V O nH O 5000 252 92.1% (500 Yang Y. et al., x 2 5 2 cycles) 2018 the introduction of a conductive polymer PPy layer, which not (NH ) V O 1000 361.6 76.1% (100 Xu L. et al., only increases the electronic conductivity but also reduces the 4 2 6 16 cycles) 2020 dissolution of V O in the electrolyte. 2 5 The electrochemical kinetics of the V O /PPy composite 2 5 cathode was further investigated to understand the impressive NH V O (Yang G. et al., 2018), Na V (PO ) (Li et al., 2016), 4 4 10 3 2 4 3 heterogeneous vanadium oxide nanowire with V O nH O shell performance. Cyclic voltammetry (CV) was performed at various 2 5 2 and V O H O core (h-VOW) (Li X. et al., 2019), VS (He et al., scan rates from 0.1 to 1.0 mV s (Figure 3A). The CV curves 3 7 2 2 2017b), Zn V O (OH) (Chao et al., 2018), and NaV O /V O show similar redox peaks in the voltage window of 0.3–1.6 V. 3 2 7 2 6 15 2 5 (Lanlan et al., 2020). In addition, as shown in Figure 2D, the The characteristic peaks appeared at 0.5/0.7 V as well as 0.8/1.0 V, FIGURE 3 | The electrochemical kinetics of the V O /PPy composite cathode. (A) CV curves at different scan rates. (B) Log(peak current) vs. log(scan rate) plots for 2 5 2C different peaks marked in (A). (C) Capacity contribution ratios at different scan rates. (D) GITT curves. (E) Evaluated diffusion coefficients of Zn . Frontiers in Energy Research | www.frontiersin.org 4 August 2020 | Volume 8 | Article 199 fenrg-08-00199 August 27, 2020 Time: 11:51 # 5 Qin et al. Polypyrrole Wrapped V O Nanowires Composite 2 5 5C reflecting the redox processes in V O that is consistent with 2 5 the strong oxidizing property of V , the polymerization of the reported literature (Yang Y. et al., 2018; Zhang et al., 2018). The pyrrole monomer could be initiated at room temperature. Due capacity is regarded to be originated from two contributed parts: to the introduction of the conductive PPy layer, the V O /PPy 2 5 a surface-controlled capacitive part and a diffusion-induced part, cathode displayed a superior specific capacity and excellent as described in the literature (Ming et al., 2018): cycling stability. The outstanding electrochemical properties are explained by the large ratio of a capacitive-controlled process i D av (1) 1 (92% at 1 mV s ) and a fast zinc ion diffusion coefficient. Considering the excellent electrochemical performance, coupled In this equation, v is the scan rate, and a and b refer to with the safe and simple operation process of aqueous ZIBs, the adjustable parameters. The b values range from 0.5 to 1.0. V O /PPy composite cathode holds great promise for practical 2 5 Corresponding to b = 0.5, the observed capacity is fully diffusion- grid-level storage applications. induced. When the capacity is completely determined by a surface-controlled capacitive part, the b value is close to 1.0. The peak currents at different scan rates are plotted and fitted with a DATA AVAILABILITY STATEMENT linear function (Figure 3B). The b values are 0.51, 0.75, 0.61, and 0.64, which implies that the capacity of the V O /PPy composite 2 5 The raw data supporting the conclusions of this article will be cathode is simultaneously influenced by both the capacitive made available by the authors, without undue reservation. and diffusion processes. Furthermore, the capacity is divided as a capacitive-controlled part (k v) and diffusion-induced part 1= 2 (k v ) as described by the following equations: AUTHOR CONTRIBUTIONS 1=2 i D k vC k v (2) 1 2 All authors listed have made a substantial, direct and intellectual or contribution to the work, and approved it for publication. 1=2 1=2 i=v D k v C k (3) 1 2 The ratios of surface-controlled capacitive and diffusion- FUNDING induced parts with various scan rates are displayed in Figure 3C. The surface-controlled capacitive contribution ratio 1 1 This work was supported by the National Natural Science increases from 57% (0.1 mV s ) to 92% (1.0 mV s ), Foundation of China (21905037) and the Fundamental indicating that the batteries possess fast charge-transfer kinetics. Research Funds for the Central Universities (3132019328 The kinetics of the V O /PPy composite cathode is further 2 5 and 3132020151). evaluated by galvanostatic intermittent titration technique (GITT). The profiles in GITT curves of V O /PPy electrode 2 5 are well in coincidence with the galvanostatic charge–discharge ACKNOWLEDGMENTS profiles (Figure 3D). The zinc-ion diffusion coefficient during discharging–charging procedures for V O /PPy is 3.03 10 – 2 5 10 2 1 QL acknowledges the financial support from the China 1.46 10 cm S (Figure 3E), which is comparable to that of Scholarship Council (CSC). the reported aqueous ZIBs based on the V O @CNT composite 2 5 and porous V O nanofiber cathodes (Chen et al., 2019, 2020). 2 5 SUPPLEMENTARY MATERIAL CONCLUSION The Supplementary Material for this article can be found In this work, a surface-initiated polymerization strategy was online at: https://www.frontiersin.org/articles/10.3389/fenrg. utilized to synthesize PPy-wrapped V O nanowires. Owing to 2020.00199/full#supplementary-material 2 5 Dong, Y., Di, S., Zhang, F., Bian, X., Wang, Y., Xu, J., et al. (2020). 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Interfacial constructing flexible V2O5@polypyrrole core–shell nanowire membrane with superior Conflict of Interest: The authors declare that the research was conducted in the supercapacitive performance. ACS Appl. Mater. Interfaces 10, 18816–18823. absence of any commercial or financial relationships that could be construed as a doi: 10.1021/acsami.8b05660 potential conflict of interest. Wang, J., Wang, J.-G., Liu, H., Wei, C., and Kang, F. (2019). Zinc ion stabilized MnO2 nanospheres for high capacity and long lifespan aqueous zinc-ion Copyright © 2020 Qin, Wang, Sun, Lu, Omar and Mikhailova. This is an open-access batteries. J. Mater. Chem. A 7, 13727–13735. doi: 10.1039/c9ta03541a article distributed under the terms of the Creative Commons Attribution License Wang, X., Ma, L., and Sun, J. (2019). Vanadium pentoxide nanosheets in- (CC BY). The use, distribution or reproduction in other forums is permitted, provided situ spaced with acetylene black as cathodes for high-performance zinc-ion the original author(s) and the copyright owner(s) are credited and that the original batteries. ACS Appl. Mater. Interfaces 11, 41297–41303. doi: 10.1021/acsami. publication in this journal is cited, in accordance with accepted academic practice. No 9b13103 use, distribution or reproduction is permitted which does not comply with these terms. Frontiers in Energy Research | www.frontiersin.org 6 August 2020 | Volume 8 | Article 199

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