A rechargeable Na-Zn hybrid aqueous battery

Journal of Power Sources 321 (2016) 257e263

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A rechargeable Na-Zn hybrid aqueous battery fabricated with nickel hexacyanoferrate and nanostructured zinc Ke Lu a, Bin Song b, Jintao Zhang a, **, Houyi Ma a, * a

Key Laboratory for Colloid and Interface Chemistry of State Education Ministry, School of Chemistry and Chemical Engineering, Shandong University, Jinan 250100, China b Jiangsu Key Laboratory for Carbon-Based Functional Materials and Devices, Institute of Functional Nano and Soft Materials (FUNSOM), Soochow University, Suzhou 215123, China

h i g h l i g h t s

g r a p h i c a l a b s t r a c t

Aqueous Na-Zn hybrid batteries were assembled based on NiHCF and Zn electrodes. The aqueous battery showed an average operating voltage of 1.5 V. The aqueous Na-Zn battery exhibited high energy density (62.9 Wh kg1).

a r t i c l e i n f o

a b s t r a c t

Article history: Received 18 December 2015 Received in revised form 4 March 2016 Accepted 2 May 2016

Rechargeable aqueous batteries are very attractive as a promising alternative energy storage system, although their reversible capacity is typically limited. A new rechargeable Na-Zn hybrid aqueous battery with nickel hexacyanoferrate (NiHCF) cathode and the nanostructured zinc anode is fabricated. The rational combination of two materials with mild aqueous electrolyte renders the devices with an average operating voltage close to 1.5 V, higher specific capacity of 76.2 mAh g1, and a good cycling stability with 81% capacity retention for 1000 cycles. These remarkable features can provide guidance for the development of rechargeable batteries from the naturally abundant electrode materials with neutral aqueous electrolytes. © 2016 Elsevier B.V. All rights reserved.

Keywords: Hybrid aqueous batteries Ion insertion Metal hexacyanoferrates Electroplated zinc

1. Introduction Along with the large-scale proliferation of consumer electronic devices [1], global efforts have been spend on the development of various rechargeable batteries, such as lithium-ion (Li-ion), nickel/ metal hydride (Ni-MH) and lead-acid batteries [2e7]. Reversible insertion of lithium, sodium, potassium or zinc ions in mild

* Corresponding author. ** Corresponding author. E-mail addresses: [email protected] (J. Zhang), [email protected] (H. Ma). http://dx.doi.org/10.1016/j.jpowsour.2016.05.003 0378-7753/© 2016 Elsevier B.V. All rights reserved.

aqueous solution would allow the creation of potentially safe and cheap battery chemistries [2,8e13]. Specifically, sodium-based aqueous electrochemical storage devices with advantages of rich raw material resource, low cost, and mild reaction condition, hold great promise for future large-scale electrical energy storage systems without the safety concerns related to highly toxic and flammable organic solvents [14e16]. In addition, the ion conductivity of an aqueous electrolyte is generally about two orders of magnitude higher than those of non-aqueous electrolytes [5,17,18]. Prussian blue (PB) and its analogues with open framework crystal structures are highly promising electrode materials in

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alkali-ion batteries because of their unique properties, such as chemical stability and high environmental compatibility [2,9e13,16,18]. The electrochemical properties of these materials were commonly investigated in a three-electrode configuration with organic electrolytes. However, only a few of rechargeable aqueous batteries with Liþ, Naþ or Kþ shuttles (e.g., CuHCF//AC/PPy [19], Na2NiFe(CN)6//NaTi2(PO4)3 [20], and Ni1Zn1HCF//TiP2O7 [21,22]) have been reported, and the drawbacks of low operation voltage, limited cycling stability and relatively complicated experimental procedures have to be addressed for promising applications. For the configuration of a high-performance rechargeable battery in an aqueous electrolyte, it is important to select suitable anode materials in order to couple with a hexacyanoferrate material. Zinc with low potential (0.78 V vs. standard hydrogen electrode potential), high theoretical capacity (820 mAh g1), innate safety, and low cost has been used as a highly promising anode candidate to fabricate rechargeable aqueous batteries [2,23e27]. However, the reversible insertion/deletion of divalent Zn2þ among the electrode materials cannot be achieved easily, which significantly limits the development of Zn-based rechargeable batteries [27]. Herein, rechargeable aqueous battery composed of an intercalation nickel hexacyanoferrate (NiHCF) cathode and an electroplated hierarchical porous Zn anode has been fabricated (illustrated in Scheme 1). During the charging/discharging process, metal ions (e.g., Naþ) inserted or extracted from the open framework channels of NiHCF (A sites, Faradaic reactions) along with the dissolution/ deposition of metal ions (Zn2þ) at Zn anode in an aqueous electrolyte. The battery operated in the potential range of 0.9e1.9 V show high specific capacity (76.2 mAh g1) and acceptable cycling stability. The combination of aqueous electrolytes with Naþ and Zn2þ ions renders the fabrication of rechargeable battery without using the toxic organic electrolyte and highly activated metals (e.g., Li, Na) in ambient air, exhibiting the potential practical applications.

2. Experimental details 2.1. Materials synthesis NiHCF nanoparticle was synthesized by a simple coprecipitation method [13,32]. Simultaneous, drop-wise addition of 40 mL of 10 mM Ni(NO3)2 and 40 mL of 5 mM K3Fe(CN)6 into 40 mL

deionized (DI) water. The mixture was continuously stirred for 2 h at room temperature. The obtained precipitates were washed with DI water, and then dried under vacuum at room temperature. The nanostructured Zn was deposited on a Cu foil via galvanostatic electrodeposition in an electrolyte containing 150 g L1 NaOH and 15 g L1 ZnO. A Zn plate was used as the counter electrode, and the distance between the working electrode and the counter electrode was 8 cm. The deposition process was carried out at current density of 5 A dm2 with different deposition times at room temperature. During deposition the electrolyte was agitated with a magnetic stirrer. 2.2. Materials characterizations Fourier transform infrared (FTIR) spectra were recorded in the transmission mode on a NicoletiS10 FTIR spectrophotometer. The crystal phase of the as-synthesized materials was characterized by X-ray powder diffraction (XRD) measurements. X-ray photoelectron spectra (XPS) were collected on a Thermo ESCALAB 250 X-ray photoelectron spectrometer. Nitrogen adsorption and desorption isotherms were performed by NOVA 2200e instrument (USA). The morphology and microstructures were investigated by scanning electron microscope (SEM, JEOL JSM-6700F) and transmission electron microscope (TEM, FEI Quanta 200F). 2.3. Electrochemical measurements The cathode was prepared by mixing active materials, acetylene black, and poly(vinylidene)fluoride (PVDF) with a weight ratio of 80:15:5. The homogeneous slurries were deposited onto Ni mesh current collectors and dried under vacuum. Cyclic voltammetry (CV) measurement was performed using three-electrode cell with a platinum sheet and a saturated calomel electrode (SCE) as the counter and reference electrodes, respectively. Electrochemical impedance spectroscopy (EIS, Zahner IM6) measurements were carried out with the potential amplitude of 5 mV over the frequency range from 100 kHz to 50 mHz. The coin cells (CR2032) were fabricated by coupling NiHCF cathode with Zn anode and the optimized cathode/anode mass ratio was 1:1.5 (Fig. S1). An aqueous solution of 0.5 M Na2SO4 and 50 mM ZnSO4 was used as the electrolyte. Galvanostatic charge-discharge cycle tests were conducted in the voltage range of 0.9e1.9 V on a Land 2001A battery test system. 3. Results and discussion

Scheme 1. Schematic illustration of the redox process for the NiHCF//Zn battery during the charge-discharge processes.

The sharp and intense peaks at 36.5 , 39.2 , 43.3 and 54.4 are the characteristic peaks for (002), (100), (101) and (102) planes of Zn (JCPDS No. 04-0831) [28]. In addition to one peak from Cu substrata (marked with a # symbol), no other secondary phases are observed, suggesting the successful deposition of pure Zn on Cu substrate (Fig. 1a). For the sample of NiHCF, the characteristic XRD pattern are indexed to the diffraction peaks of hydrated Ni3(Fe(CN)6)2 with face-centered cubic PB crystal structure [9]. The uniform porous structure of NiHCF with good crystallinity is highly accessible to cations, which would be benefit for the reversible intercalation process. As a result, the good stability and rate performance of batteries would be expected. The survey XPS confirms the presence of Ni, Fe, C, and N elements (Fig. 1b). High-resolution XPS data (Fig. 1c) shows that Fe 2p3/2 and Fe 2p1/2 peaks are located at ca. 710.4 and 724.1 eV, suggesting that the element Fe in NiHCF is present in the chemical state of Fe3þ [13,16,29]. The Ni 2p3/2 and Ni 2p1/2 were found at the binding energies of about 855.1 and 872.7 eV, indicating the existence of Ni2þ [30]. For the FTIR spectra (Fig. 1d), the peaks at


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Fig. 1. (a) XRD patterns of NiHCF and Zn. Inset is the framework of Prussian blue (PB). (b) XPS spectra of NiHCF. (c) Core level spectra of Fe 3p and Ni 2p for NiHCF. (d) FTIR spectra of NiHCF.

2072 cm1 and 2152 cm1 are assigned to the characteristic peaks of PB analogues and the CN ligand bridged to FeIII and NiII ions (e.g., FeIII-CN-NiII), respectively, confirming the formation of metalorganic framework in NiHCF (inset of Fig. 1a) [13,29].

The SEM image of the electroplated Zn anode material exhibits a hierarchical flake-like shape with micrometer size (see Fig. 2a). The nanostructured Zn anode would provide large electrochemically electrolyte/electrode active surface areas, thus enables good

Fig. 2. (a) SEM image of Zn. (b) SEM and (c) TEM images of NiHCF. (d) TEM image with the corresponding element mapping images of NiHCF. (e) EDX results of NiHCF.

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electrochemical performance. The SEM image (Fig. 2b) reveals that NiHCF is consisted of large agglomeration particles with diameters in the range of 40e80 nm. As shown in the TEM image (Fig. 2c), the NiHCF particles are interconnected with each other to form a three dimensional networks. The EDX mapping of NiHCF sample (Fig. 2d) exhibits the uniform distribution of C, N, Fe and Ni elements, indicating that NiHCF is a single phase containing a mixture of these elements. The surface area and pore size distribution of NiHCF were tested by the nitrogen adsorption-desorption isotherm measurements (Fig. S2, Supporting information). The pore size distribution reveals that the pore sizes are centered at ~29 nm and the BET specific surface area is 228 m2 g1. The continuously porous network of NiHCF composed of small particles would generate large electrochemically electrolyte/electrode active surface areas and is benefit to the rapid ion diffusion throughout the material. Cyclic voltammetry (CV) curves of the NiHCF cathode were recorded in various electrolytes with different cations (Liþ, Naþ, Kþ and Zn2þ). As shown in Fig. 3, these redox peaks can be attributed to the reversible conversion between Fe3þ and Fe2þ accompanied by the intercalation/deintercalation of cations (Liþ, Naþ, Kþ, and Zn2þ) in the cyano-bridged metallic rigid framework. However, the obviously different shapes of CV curves indicate cations have significant impact on the charge storage process of NiHCF. The high potential (0.76 V vs. SCE) and the low current density indicate that the insertion of Zn2þ ions into NiHCF is not easy, which may limit the configuration of rechargeable battery using Zn2þ ion as a shutter in an aqueous electrolyte. It is likely that the increased electrostatic interaction and the steric effect between insertion ions (divalent ions, Zn2þ) and host atoms would result in low electrochemical activity and slow kinetics when inserted into the open framework [27,31,32]. The potential for Li2SO4 electrolyte is much lower but the current density is lower too. Especially, the distorted CV curve is observed for NiHCF electrode in Li2SO4 electrolyte. In aqueous electrolyte, the hydrated Liþ would be dehydrated when inserted into the porous channels of NiHCF. The ions are rehydrated in the reverse process [33]. Although the ionic radius of Liþ ion is the smallest among the electrolytes used, the insertion/deletion through the channels of NiHCF is not able to be achieved easily due to the ion hydration. For the electrolytes of Na2SO4 and K2SO4, the highly reversible peaks with symmetric shapes suggest the highly reversible nature of the structural changes during the cations extraction/insertion process, which would lead to the superior cycling stability of the electrode material. The higher current

Fig. 3. CV curves of NiHCF cathode material with different insertable cations (Liþ, Naþ, Kþ and Zn2þ) in 0.5 M Li2SO4 (black), 0.5 M Na2SO4 (red), 0.5 M K2SO4 (blue), and 1 M ZnSO4 (green). (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)

density suggest that Naþ would be the best insertion ion, which would benefit to the reaction kinetic and cycling stability of NiHCF, although the intercalation potential of Naþ for NiHCF is lower than those of Zn2þ and Kþ. In order to improve the utilization of Zn, nanostructured porous Zn deposited on Cu foil via an electroplating method is used as an anode in the present study [34]. In comparison with the flat Zn plate, the larger current density (Fig. S3a) of nanostructured Zn electrode suggests the large active surface area, which would enhance the battery performance. The addition of ZnSO4 in the electrolyte is favorable to the kinetic reaction and the reversibility of Zn electrode, which is evidenced by the larger current density and symmetrical redox peaks in comparison to the non-featured CV curve of Zn electrode in pure Na2SO4 electrolyte (Fig. S3b). EIS measurements were carried out at open circuit potential to examine the fundamental behaviors and to compare the charge transport kinetics of NiHCF in different electrolytes (Supporting information, Fig. S4a). The above results are coinciding well with the CV results and demonstrate the feasibility of NiHCF// Zn system for aqueous rechargeable battery. On the basis of the above discussion, nanostructured Zn and NiHCF were coupled to fabricate rechargeable battery in an aqueous electrolyte. As shown in Fig. 4a, the redox peaks at 1.02/ 1.13 V (vs. SCE) for Zn electrode are ascribed to the reversible dissolution/deposition of Zn whereas the redox peaks for NiHCF are located at 0.32/0.47 V. Because of the large potential differences, Zn and NiHCF, are assembled into a battery system via incorporating the reversible cation intercalation and the deposition/dissolution of Zn in a mild aqueous electrolyte. The CV curve of the full cell is shown in Fig. S5 (Supporting information). The observed two obvious anodic peaks at ca. 1.47 and 1.76 V can be attributed to the extraction of Naþ and/or the oxidation of Zn, respectively. Meanwhile, the full cell exhibits a distinct cathodic peak at 1.40 V, which can be ascribed to the reversible intercalation of Naþ into NiHCF along with the deposition of Zn. As seen, cathode electrode reaction is related to the insertion/extraction of the electrochemically active ions (e.g., Naþ) into/from NiHCF, but anode electrode reaction involves the deposition and dissolution of zinc metal. The electrochemical properties of NiHCF//Zn battery are further evaluated by galvanostatic measurements. Fig. 4b shows the charge/discharge profiles at various current densities. The charge curves of NiHCF// Zn battery show a pair of plateaus in the potential range of 0.9e1.9 V, indicating that the reversible conversion between Fe3þ and Fe2þ along with the insertion/extraction of Naþ ions. Fig. 4c shows dQ/dV peak of NiHCF//Zn cell tested at 100 mA g1 where full-cell potential of 1.9 V matches the voltage difference between cathode and anode peaks (see CV curves of individual electrodes, Fig. 4a). The dQ/dV profile is in accordance with the CV analysis. Two sodium-ion button batteries were connected in series to power a small red or green LED (Fig. S4b). The two anodic peaks, indicative of a two-step extraction for active ions from the NiHCF lattice, can be ascribed to the deintercalation of Naþ and possibly divalent Zn2þ ions, which are in good agreement with the full cell’s CV results (Fig. S5). The sloping, S-shaped discharge potential profile indicates the intercalation mechanism, which is also consistent with previous reports on PB analogues [9,19,35]. For comparison, the full batteries with different electrolytes were also fabricated and tested under the similar conditions. The corresponding discharge curves are shown in Fig. 4d. At a current of 100 mA g1, the specific capacities of batteries based on the mass loading of NiHCF are 76.2, 70.2, 64.5 and 47.2 mAh g1 in Na2SO4, K2SO4, Li2SO4 electrolyte with ZnSO4, and pure ZnSO4, respectively. In good agreement with the CV measurements (Fig. 3), the battery with Na2SO4 electrolyte exhibits the best performance in terms of the discharge plateau and the largest specific capacity. Thus, the combination of NiHCF/nanostructured zinc metal as the cathode/


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Fig. 4. (a) CV curves of Zn and NiHCF in an aqueous solution of 0.5 M Na2SO4 and 50 mM ZnSO4. (b) Charge and discharge curves of the NiHCF//Zn battery at different current densities based on the NiHCF electrode. (c) dQ/dV curve of NiHCF//Zn cell tested at 100 mA g1. (d) Discharge curves of NiHCF-Zn cell measured in four different electrolytes.

anode materials, and Na2SO4 as the electrolyte enable the beneficial conditions for battery operation. Notably, an energy density as high as 62.9 Wh kg1 is achieved on the basis of the total weight of both electrode materials (Fig. 5c), which is comparable with those of

lead acid and low-voltage aqueous rechargeable lithium batteries [33,36]. In addition, the battery also exhibited a high rate capability. As shown in Fig. 5a, the rate capability of the NiHCF//Zn cell is tested

Fig. 5. (a) Rate capability and (b) cycle life and Coulombic efficiency of the NiHCF//Zn batteries with various electrolytes at a current density of 500 mA g1. (c) Ragone plots of NiHCF//Zn battery. (d) Nyquist plots of the battery before and after 1000 cycles of galvanostatic charge-discharge at 500 mA g1. Inset in d shows enlarged spectra at high-frequency range.

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Table 1 Comparison of the electrochemical performance of metal-ion batteries between this work and the previous reports. Materials

Cell type

Electrolyte

Capacity

Cycling stability/cycles

Ref.

ZnHCF//Zn Na1.72MnFe(CN)6//Na KNiFe(CN)6//Na CuHCF//AC/PPy Na2NiFe(CN)6//NaTi2(PO4)3 a-MnO2//Zn Na0.95MnO2//Zn NiO//Zn CuHCF//Zn Na2Zn3(Fe(CN)6)2//Na CuHCFe//MnHCMn Na1.63Fe1.89(CN)6//Na Na0.44MnO2//AC Na3V2(PO4)3/C//Zn FeFe(CN)6/carbon cloth//Na NiHCF//Na Na2CoFe(CN)6//Na Na1þxFeFe(CN)6//Na NiHCF//Zn

Full-cell Half-cell Half-cell Full-cell Full-cell Full-cell Full-cell Full-cell Full-cell Half-cell Full-cell Half-cell Full-cell Full-cell Half-cell Half-cell Half-cell Half-cell Full-cell

Aqueous Nonaqueous Nonaqueous Aqueous Aqueous Aqueous Aqueous Aqueous Aqueous Nonaqueous Aqueous Nonaqueous Aqueous Aqueous Nonaqueous Nonaqueous Nonaqueous Nonaqueous Aqueous

65.4 mAh g1 134 mAh g1 55 mAh g1 54 mAh g1 100 mAh g1 210 mAh g1 60 mAh g1 155 mAh g1 53 mAh g1 56.4 mAh g1 23 mAh g1 150 mAh g1 45 mAh g1 86 mAh g1 82 mAh g1 68 mAh g1 148 mAh g1 103 mAh g1 76.2 mAh g1

81%/100 (300 mA g1) 93.1%/30 (0.05 C) 100%/180 (100 mA g1) 100%/1000 (10 C) 88%/250 (5 C) 100%/100 (6 C) 90%/1000 (4 C) 60%/500 (1 A g1) 96.3%/100 (60 mA g1) 85.2%/50 (10 mA g1) 100%/1000 (10 C) 90%/200 (25 mA g1) 100%/1000 (4 C) 68%/200 (50 mA g1) 75%/200 (0.5 C) 100%/50 (10 mA g1) 90%/200 (100 mA g1) 97%/400 (20 mA g1) 81%/1000 (500 mA g1)

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by varying the current density from 100 to 1000 mA g1. No obvious decay was observed after 20 charging/discharging cycles at the same current density. When the current rate was restored to 100 mA g1 after 80 cycles, the capacity was recovered to 76 mAh g1, suggesting the excellent rate capability and high reversibility even under high-rate operation condition. The longterm cycling stability of the battery and Coulombic efficiency were investigated by a continuous cycling test at 500 mA g1. As shown in Fig. 5b, the capacity retention is around 81% (76%, 70% capacity retention for batteries in K2SO4 and Li2SO4 electrolytes, respectively) with a Coulombic efficiency of nearly 99% over 1000 cycles. The loss of capacity may arise from the slow dissolution of cathode material and the limited reversibility [9,25e27]. As can be seen, the capacity retention of the battery at high-rate operation is around 90% (vs. 70% at lower current density after 500 cycles) (Fig. 5b and S6). The electrochemical performances of aqueous metal-ion batteries reported recently are summarized in Table 1. Overall, the cycling performance and discharge capacity of the NaZn hybrid aqueous battery is highly competitive with that of aqueous metal-ion batteries. For example, the aqueous battery based on CuHCF cathode and AC/PPy anode exhibited a capacity of 54 mAh g1 at 1 C rate [19]. The aqueous battery based on Zn// ZnHCF achieved a specific capacity of 65.4 mAh g1 at 1 C rate [2]. Na1.72MnFe(CN)6 nanomaterial used as a cathode material in sodium battery showed a capacity of 134 mAh g1 at 6 mA g1 [10]. Nyquist plots of a battery before and after the cycling stability tests at the current density of 500 mA g1 (Fig. 5d) exhibit a semicircle in high-frequency region and a sloped line in low-frequency region. Obviously, the resistances were increased significantly after longterm stability test. During the long-term cycling stability measurement, the changes on the channels and skeletons of NiHCF due to the repeated intercalation process of ions may deteriorate the pathways for fast electron and ions transfer, leading to the increasing resistances for ion migration (semi-circle) and iondiffusion (Warburg tail). As a result, the slightly decay of specific capacity was also observed. It is worthwhile to note that the cycling stability would be improved by increasing the crystallinity of NiHFC in order to maintain the uniform porous structure, and also improving the reversibility of ion intercalation process.

(NiHCF) with the electroplated Zn electrode. The measurements of various cation (Liþ, Naþ, Kþ and Zn2þ) insertion in NiHCF have revealed that the intercalation process have a great impact on the electrochemical behaviors of electrode materials. The experiment results exhibited that the incorporation of Naþ containing electrolyte with small amount of ZnSO4 is benefit to improve the intercalation process and the reversibility of electrodes, rendering the configuration of aqueous battery with high specific capacity, high efficiency, and acceptable cycling stability (capacity retention over 81% after 1000 cycles). Even though there is still a long way before its practical application, with good engineering and further exploration, the cost-effectiveness, performance scalability and safety of NiHCF//Zn cells can make it a viable alternative to current Li-based systems. Acknowledgements This work was supported by the National Natural Science Foundation of China (21373129). Appendix A. Supplementary data Supplementary data related to this article can be found at http:// dx.doi.org/10.1016/j.jpowsour.2016.05.003. References [1] [2] [3] [4] [5] [6] [7] [8] [9] [10] [11] [12]

4. Conclusions We have demonstrated the fabrication of rechargeable battery in aqueous electrolytes by coupling an intercalation cathode

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