| Cite this article as: |
Lingyun Xiong, Hao Fu, Weiwei Han, Manxiang Wang, Jingwei Li, Woochul Yang, and Guicheng Liu, Robust ZnS interphase for stable Zn metal anode of high-performance aqueous secondary batteries, Int. J. Miner. Metall. Mater., 29(2022), No. 5, pp.1053-1060. https://dx.doi.org/10.1007/s12613-022-2454-z
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Aqueous Zn metal batteries have garnered considerable attention as a fantastic potential for portable devices and electric vehicles due to their high specific capacity, low cost, non-toxicity, and high safety abilities [1–4]. Importantly, the metallic Zn anode possesses an appropriate redox potential of −0.762 V vs. the standard hydrogen electrode, which is more balance kinetics than other anode metals (Li [5–8], Na [9–14], K [15], Mg [16]) to allow it suitable for use in mildly acid aqueous electrolyte systems [17]. Nevertheless, the self-corrosion, hydrogen evolution reaction (HER), and dendrite growth during cycling markedly decrease the Coulombic efficiency (CE) and the service life [18–20]. To address those essential concerns, it is therefore critical to improve the stability and reversibility of metallic Zn.
Various techniques have recently been described to control dendrite formation and side reactions, including electrolyte modification, bulk Zn surface structure optimization, and passivation layer fabrication [21–24]. Among them, the artificial layer, in particular, has attracted substantial attention because of its great controllability, superior protection, and diversified options [25–27]. Due to the high complexity of the battery internal environment during cycling, the passivation layer should meet the fundamental requirements: (i) sufficient mechanical and chemical stability in the medially acid electrolyte to ensure its endurance protection function; (ii) excellent adhesion property with Zn substrate; (iii) high Zn-ionic conductivity and non-electrical conductivity to allow oxidation and reduction of metallic Zn underneath the artificial layer [28–30].
To date, numerous advancements have been accomplished in the field of artificial layers, such as polymer, ZnF2, and ZnO passivation layers, etc. [31–33]. Of note, the thickness of passivation layers plays a vital role in the Zn-ion diffusion and redox dynamic of metal during Zn plating/strapping. For instance, Shin et al. [34] designed stable solid-electrolyte interphase on Zn metal surface by cross-linked gelatin for dendrite-free Zn metal batteries. The protection layer with optimal thickness obviously increases the Zn-ion diffusion coefficient. Recently, ZnS has been reported as a potential protection layer for dendrite-free Zn metal anodes with long service life and high performance, thanks to its chemical inertness and high Zn-ion transference number [23]. Unfortunately, the reported ZnS layer was developed via a vapor–solidreaction at temperatures as high as 350°C, resulting in poor compatibility between high growth temperature of ZnS and low melting point (419.5°C) of Zn metal. Matter of fact, the high temperature can induce serious metal aging and an uncontrollable thickness of the ZnS passivation layer, resulting in poor physical and chemical properties of Zn substrate and a decline in anode performance repeatability [35]. Compared to the vapor–solid reaction, the moderate hydrothermal condition with low temperature is more suitable for the synthesis of thickness-controlled ZnS artificial layers, avoiding aging of the Zn metal.
Herein, a ZnS artificial layer with the controllable thickness was in-situ synthesized on Zn metal surface via two-step reactions, i.e., oxidation and orientating sulfuration reaction, consisting of liquid-phase hydrothermal (LPH) and vapor-phase hydrothermal (VPH) processes. The stable chemical property and unbalanced charge distribution of the ZnS layer endow the modified Zn metal anode with multifunctional features: desirable anti-corrosion, inferior hydrogen evolution reaction, and remarkable inducement of Zn plating. While too thick passivation layer could decrease the diffusion kinetics of Zn-ion in anodes. Therefore, the effects of the ZnS artificial layer with various thicknesses on dendrite growth and side reactions were systematically investigated to realize high CE and long service life of Zn metal anodes for aqueous secondary batteries.
In a typical synthesis process, 80 mL deionized water and 5 cm2 Zn foil were firstly heated at 120°C in a 100 mL Teflon-lined stainless-steel autoclave for 1, 3, and 6 h to obtain Zn@ZnO samples named as Zn@ZnO-1, Zn@ZnO-2, and Zn@ZnO-3, respectively, by the LPH reaction. Subsequently, the resulting Zn@ZnO and 2 g thiourea were annealed at 160°C in a Teflon-lined stainless-steel autoclave for 6 h by the VPH process to obtain Zn@ZnS samples of Zn@ZnS-1, Zn@ZnS-2, and Zn@ZnS-3, respectively.
Morphologies and section images of pure Zn, Zn@ZnO, and Zn@ZnS samples were detected by field emission scanning electron microscopy (FESEM, Hitachi S-4800). Lattice structures of pure Zn, Zn@ZnO, and Zn@ZnS samples were checked by the X-ray diffractometer (XRD, Ultima IV, Rigaku) measurements with scanning from 10° to 80°. Contact angles of pure Zn and Zn@ZnS samples were measured by the rame-hart instrument (model 250, America).
Electrochemical performances of Zn@ZnS and pure Zn anodes were systemically demonstrated using Zn@ZnS||Zn@ZnS symmetric, Zn@ZnS||Ti half, and Zn@ZnS||NH4V4O10 (HVO) full cells. All cells were assembled into CR2032 coin cells with 80 μL electrolytes (2 mol·L−1 ZnSO4) and tested at room temperature. The LANHE battery test system (CT-3001A, Wuhan, China) was conducted to evaluate charging-discharging performance. Cyclic voltammetry (CV),Tafel corrosion curve, and electrochemical impedance spectroscopy (EIS, frequency range of 0.001–105 Hz) were carried out on a Biologic VMP electrochemical station (Princeton Applied Research). Specifically, the CV measurement for half and full cells were assessed at a scan rate of 2 mV·s−1 and 0.1 mV·s−1. Tafel corrosion curves were tested at 1 mV·s−1 with the three-electrode system.
The synthesis process of the Zn@ZnS is illustrated in Fig. 1(a) and Fig. S1(a). First, the Zn@ZnO was synthesized by the LPH oxidation (Eq. (1)). The thickness of the ZnO layer was easily controlled by adjusting the reaction time.
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Zn+H2O→ZnO+H2↑ |
(1) |
Afterward, a VPH sulfidation was employed by the addition of thiourea to produce the Zn@ZnS through Eqs. (2) and (3). Due to the reducibility of H2S, the ZnO of the Zn@ZnO was transferred to ZnS and tightly grown on the surface of the Zn substrate.
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CH4N2S+2H2O→H2S↑+2NH3↑+CO2↑ |
(2) |
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H2S+ZnO→ZnS+H2O |
(3) |
SEM measurements were performed to quantificationally investigate the thickness of the ZnO layer on Zn substrates. As described in Fig. S1(b)–(d), with controlling hydrothermal time to 1 h, the thickness of the ZnO layer is 0.50 μm (Zn@ZnO-1). After increasing the growth time to 3 and 6 h, the ZnO-thicknesses are 0.75 μm (Zn@ZnO-2) and 1.00 μm (Zn@ZnO-3), respectively. Obviously, the ZnO-thickness increases with the extended hydrothermal time. Therefore, after the sulfuration reaction, the thicknesses of the ZnS layers in Zn@ZnS-1, Zn@ZnS-2, and Zn@ZnS-3 are 0.52 μm, 0.75 μm, and 1.00 μm (Fig. 1(b)–(d)), correspondingly, demonstrating that the ZnS-thickness in Zn@ZnS samples could be easily controlled by the adjusting ZnO-thickness during LPH step. It’s worth mentioning that some fault areas on the surface that aren’t completely covered by the ZnO layer (yellow circle in Fig. S1(e) are primarily caused by partial oxidation of the Zn substrate during the short hydrothermal period. Correspondingly, Zn@ZnS-1 behaves a similar phenomenon on the surface after sulfuration (Fig. 1(e)). In contrast, with increasing LPH time, complete and uniform surfaces of ZnO layers were obtained on Zn@ZnO-2 (Fig. S1(f)) and Zn@ZnO-3 (Fig. S1(g)), resulting in homogeneous surface morphologies of Zn@ZnS-2 (Fig. 1(f)) and Zn@ZnS-3 (Fig. 1(g)). To further confirm the chemical state of the S and Zn atoms, X-ray photoelectron spectroscopy (XPS) spectra characterizations of Zn@ZnS-2 were given in Fig. S2. The Zn 2p spectrum (Fig. S2(a)) presents two contributions, Zn 2p3/2 and Zn 2p1/2, located at 1022.8 and 1046.3 eV, respectively. Whereas the Zn@ZnS-2 displays the binding energies of S 2p3/2 and S 2p1/2 at 161.9 and 163.2 eV, respectively.
In what follows, the crystal structure and corresponding synthesis evolution mechanism were revealed by XRD measurements (Fig. 1(h) and (i)). All the Zn@ZnO samples display obvious peaks at around 36.2° (002), 38.9° (101), and 43.2° (100), which are consistent with the standard card of pure Zn (PDF # 65-3358). The strong peaks of ZnO crystal are observed in Zn@ZnO-2 and Zn@ZnO-3 samples at 31.77°, 34.42°, and 36.25°, which are assigned to the (100), (002), and (101) planes. The intensity of the ZnO peaks in Zn@ZnO-3 is higher than that of Zn@ZnO-2 electrodes, suggesting that the amount and degree of crystallinity of ZnO improve as the LPH time increases. After the sulfuration reaction, both of the Zn@ZnS-2 and Zn@ZnS-3 present distinct signals assigned to ZnS (111) at 28.53°, and ZnS (220) at 47.45°, respectively. While there is no visible ZnO signal in the Zn@ZnO-1 sample, this could be partly related to the incomplete reaction on the Zn surface and the low crystallinity of the ZnO [36]. Accordingly, Zn@ZnS-1 also has essentially little ZnS signal because of the low crystallinity of ZnS.
Thicknesses of the passivation layer play a critical role in the electrochemical properties of Zn electrodes. In an aqueous system, metallic Zn electrodes are suffered from corrosion in the neutral acid electrolyte, causing inferior CE and short service time of batteries [37]. Firstly, the anti-corrosive quality of ZnS was investigated by linear sweep voltammetry and Tafel plots. As displayed in Fig. 2(a), the corrosion potentials of Zn@ZnS-1, Zn@ZnS-2, and Zn@ZnS-3 are −1.037, −1.036, and −1.035 V, respectively. To sharp contrast, the pure Zn electrode exhibits a corrosion potential of –1.039 V, which is more negative than ZnS modified Zn foil, implying that the ZnS protector efficiently improves the chemical stability of Zn metal by suppressing the self-corrosion reaction.
To investigate the different thicknesses of the ZnS layer for the anodic electrochemical properties, EIS measurements were carried out to explore the effect of the ZnS layer on the interface impedance at the fresh state of symmetric cells (Fig. 2(b)). The fitting equivalent circuit model was given in Fig. S3 and the fitting data was shown in Table S1. The semicircle in the high-frequency region corresponds to charge transfer resistance (Rct). The pure Zn electrode delivers a high Rct of 687 Ω, which is much higher than that of the ZnS-modified Zn electrodes, illustrating that the ZnS protection layer enhances charge-transfer kinetics. The contact angles were conducted by dropping deionized water on metallic electrodes (Fig. S4) of pure Zn, Zn@ZnS-1, Zn@ZnS-2, and Zn@ZnS-3 exhibit 120°, 72°, 48°, and 38°, respectively, hinting that the ZnS layer effectively decreases the surface tension between the metallic electrode and aqueous electrolyte to conduct the reaction dynamics and decrease the interface resistance [38]. Compared with Zn@ZnS-2 and Zn@ZnS-3, Zn@ZnS-1 electrode displays higher Rct (334 Ω), ascribing to the partial exposure of Zn surface. Conversely, because of the excessively thick ZnS-protective barrier, Zn@ZnS-3 exhibits a higher Rct (267) than Zn@ZnS-2 (94), reflecting that long-distance ion transfer occurs (Fig. 2(b)) [39].
The effect of the ZnS layer for the Zn nucleation formation dynamic was evaluated by the chronoamperometry measurement under a bias current density of −5 mA·cm−2. As plotted in Fig. 2(c), the pure Zn electrode presents an initial nucleation voltage of −1.49 V with an overpotential of 282 mV. The Zn@ZnS-1, Zn@ZnS-2, and Zn@ZnS-3 electrodes display −1.25, −1.22, and −1.27 V of nucleation voltages, respectively, with the corresponding overpotentials of 153, 102, and 163 mV. The smaller nucleation formation and overpotential of Zn@ZnS electrodes demonstrate that the ZnS layer accelerates Zn-ion diffusion at the Zn@ZnS interphase to create metallic Zn due to the unbalanced charge distribution of the bonding connection between the S and Zn atoms [40]. Notwithstanding, the overpotential and initial nucleation voltage decrease as the ZnS layer thickens, similar to the Rct trend, since too much ZnS layer thickness retards Zn-ion diffusion [34].
Linear sweep voltammetry analyses (Fig. 2(d)) were implemented to inspect HER at a scanning rate of 2 mV·s−1 in 0.1 mol·L−1 Na2SO4 electrolyte. At the current density of −2 mA·cm−2, corresponding potentials of pure Zn, Zn@ZnS-1, Zn@ZnS-2, and Zn@ZnS-3 are −1.72, −1.76, −1.79, and −1.82 V, respectively. The reduced potential trend of Zn@ZnS electrodes suggests that the more thickness of the ZnS, the better anti-HER ability, implying that the ZnS layer skillfully improves the chemical stability of the Zn metal electrodes, which benefits not only the safety but also high CE and long cycling life for batteries. As a result of the excessively thick protective layer, ion transfer kinetics are inhibited, causing Zn-ion diffusion to be impeded. Therefore, from the abovementioned electrochemical properties of Zn@ZnS electrodes, the Zn@ZnS-2 is considered as the optimal electrode for high-performance Zn-metal batteries by virtue of stability, suppression abilities of self-corrosion and HER reactions, and the optimized charge-transfer and nucleation formation.
To reveal the reversibility of Zn2+ during stripping/plating, the long cycling performance of Zn@ZnS-2 and pure Zn electrodes in symmetric cells were provided (Fig. 3(a)). The Zn@ZnS-2 electrode yields service life for 300 h at a current density of 0.5 mA·cm−2 with a capacity of 0.25 mAh·cm−2. In stark contrast, the pure Zn electrode sustains 56 h of cycling life. The longer cycling life of the Zn@ZnS-2 electrode is mainly attributed to the Zn-ion fast diffusion and nucleation formation caused by the ZnS protection layer [40], leading to a uniform deposition and dendrite-free during Zn trapping/plating process. After 20 cycles, the pure Zn electrode exhibited spherical dendrites (Fig. S5(a)), attributed to the inhomogeneous plating and the by-product formation, leading to short service life. In sharp contrast, the Zn@ZnS-2 electrode showed a smooth and dense morphology (Fig. S5(b)), providing a dendrite-free electrode devoted to a long cycling life. To further confirm the phenomenon, the corresponding XRD patterns of pure Zn and Zn@ZnS after 20 cycles were presented in Fig. S5(c). Smaller peaks of Zn4(SO4)(OH)6·xH2O were detected in the cycled-pure Zn surface, demonstrating that the by-product was formed during cycling. On the other hand, on the Zn@ZnS-2 electrode, there was no signal of the Zn4(SO4)(OH)6·xH2O by-product, showing that the ZnS protector effectively inhibited by-product production and devoted to a dendrite-free electrode. Importantly, the obvious ZnS peaks further prove that the robust ZnS artificial is extremely stable and unlikely to be damaged during the trapping/platting process, which is contributed to the long service life electrode in the batteries system. Meanwhile, the overpotential of Zn@ZnS-2 is as low as 42 mV, which is smaller than that of the pure Zn electrode (64 mV, Fig. 3(b)), suggesting that the ZnS layer increases the redox kinetics of Zn during the charging/discharging process.
Coulombic efficiency, an important point for the reversibility of Zn-ions for metal anodes, was evaluated by galvanostatic cycling in a half cell with a current density of 5 mA·cm−2. Fig. 3(c) displays that the pure Zn electrode expresses a low average CE of 94.5% with only maintaining 66 cycles. While the Zn@ZnS-2 electrode harvests a high CE of 98.2% after 200 cycles (Fig. 3(c)), which illuminates that the ZnS passivation layer suppresses the strict side reaction and dendrite growth, such as HER reaction and “dead Zn” formation, to achieve excellent reversibility of metallic Zn. Correspondingly, the voltage-capacity curves (Fig. 3(d)) presents that the hysteresis voltages of pure Zn and Zn@ZnS-2 electrodes are 131 and 78 mV, respectively, attributing to the rapid redox kinetics of Zn metal conducted by the ZnS layer.
To demonstrate the full cell performance of the Zn@ZnS electrode, HVO (Fig. S6) was employed as the cathode. As shown in Fig. 4(a), rate performances of Zn@ZnS electrode are 326, 270, 170, 93 mAh·g−1 at current densities of 0.2, 0.5, 1, and 2 A·g−1, respectively. The corresponding voltage-capacity curves were depicted in Fig. S7. When the current density recovered to 0.2 A·g−1, the capacity maintains 300 mAh·g−1, which is almost the same as the initial performance, displaying excellent capacity recoverability. Contrastingly, the pure Zn-based batteries deliver inferior capacities of 298, 234, 99.8, and 14.8 mAh·g−1 at 0.2, 0.5, 1, and 2 A·g−1, respectively, demonstrating unstable and lower capacity at high current density. Especially, when the cycling current returns to 0.2 A·g−1, the capacity is only 240 mAh·g−1 with poor recoverability. The great rates performance and the good recoverability of Zn@ZnS-2 electrode are attributed to the remarkable protection ability of ZnS artificial layer with stability, outstanding optimized charge transfer, and nucleation formation characterizations. The corresponding voltage–capacity curves at the current density of 0.2 A·g−1 were given in Fig. 4(b). The charging/discharging capacities of pure Zn and Zn@ZnS are 329.4/318.2 and 339.9/338.8 mAh·g−1, respectively, corresponding CE of 96.6% and 99.7%. The Zn@ZnS electrode clearly possesses a higher initial CE and capacity with a lower polarization voltage than the pure Zn electrode, stating that the ZnS protective layer considerably improves the reversibility and activity of Zn2+ during cycling, thanks to the ZnS protection role prevents the dead Zn formation.
In addition, the CV characteristic of Zn@ZnS and pure Zn electrodes at a voltage scanning rate of 0.1 mV·s−1 were depicted in Fig. 4(c). When compared to a pure Zn electrode, the Zn@ZnS anode produces a larger redox current peak. As a result, the Zn@ZnS electrode presents a higher capacity and activity during cycling, which is in accordance with charging–discharging performance. Furthermore, the oxidation peak of Zn@ZnS anode shifts to the lower voltage, and the reduction peak shifts to the higher voltage during the charging/discharging process, suggesting that the ZnS layer facilitates the redox of metallic Zn with a lower polarization [41–42]. Moreover, the Rct for Zn@ZnS is only 201 Ω, whereas the Rct for pure Zn is as high as 288 Ω, showcasing that the Zn@ZnS has slightly faster charge-transfer kinetics (Table S2). It’s ascribed to the unbalanced charge distribution characteristics of the ZnS protection layer between the S and Zn atoms, which accelerates the Zn2+ diffusion at Zn@ZnS interphase, reduces the internal resistance, and increases effective reaction interface to achieve higher utilization and capacity.
A stable ZnS interphase was developed on the Zn metal surface through a two-step hydrothermal method based on oxidation–orientation sulfuration, achieving an accurately controllable thickness of the ZnS layer. The specially designed orientation sulfuration reaction for synthesizing the ZnS layer not only avoids the aging of the Zn metal at high temperature but also realizes the in-situ growth of the ZnS passivation layer. The optimized Zn@ZnS electrode exhibits promising anti-HER reaction and dendrite growth suppression abilities during cycling. Consequently, it delivers a high CE of 98.2% and a lower hysteresis voltage of 78 mV in half cells and long cycle lifespan of 300 h with a low overpotential of 42 mV at the current density of 0.5 mA·cm−2 in symmetric cells, and outstanding rate performance of 326, 270, 170, and 93 mAh·g−1 at the current densities of 0.2, 0.5, 1, and 2 A·g−1, respectively, in Zn@ZnS||HVO full cell. Considering this feasible and moderate strategy in terms of effectively inhibiting the HER reaction and dendrite-free for Zn anodes, it is expected to be applied in other metal anodes for large-scale applications in the future.
This work was financially supported by the National Research Foundation funded by the government of the Republic of Korea (Nos. 2020R1I1A1A01072996 and 2021K2A9A2A06044652), and the National Natural Science Foundation of China (Nos. 52111540265 and 51874272).
The authors declare no conflict of interest.
The online version contains supplementary material available at https://doi.org/10.1007/s12613-022-2454-z.
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