2025, Vol. 36 
b School of Materials Science and Chemical Engineering, Ningbo University, Ningbo 315211, China;
c College of Physics Science and Technology, Kunming University, Kunming 650214, China;
d School of Information Engineering, College of Science and Technology, Ningbo University, Ningbo 315300, China
With the fast depletion of fossil fuels and the increasing demand for renewable clean energy, there is an urgent need to develop high performance of energy storage systems with low cost, long lasting, and environmentally friendly [1–3]. Currently, the commercial lithium-ion batteries (LIBs) have been widely applied in many fields due to its merits of high energy & power density, and the mature technology [4]. Noticeably, the safety issues, high cost, and the limited resources of LIBs remain challenges, thus it is essential to explore new ways to achieve more efficient energy storage systems [5–7]. In recent years, the aqueous rechargeable zinc-ion batteries (ZIBs) are attracting increasing attention owing to their advantages such as high safety, low cost, abundant resources, high theoretical specific capacity (820 mAh/g, 5854 mAh/L), and zinc’s low redox potential (0.76 V vs. standard hydrogen) [8–11]. The energy storage mechanism of ZIBs is similar to LIBs, that the Zn ions would reversibly transport between the Zn anode and the manganese or vanadium-based compounds cathode during the repeated charge/discharge process [12–15]. However, the zinc ions prefer to deposit onto the screw dislocations of the zinc anode due to the uneven electric field distributions, which would lead to the generation of the unwanted zinc dendrites and the shortened cycle life [16]. Moreover, the side reactions such as self-corrosion and hydrogen evolution reaction (HER) during cycling can result in the formation of inactive by-products (such as ZnO, Zn(OH)2, Zn4SO4(OH)6·nH2O) on the Zn electrode surface, thus deliver poor electrochemical energy storage ability [17–19].
Nowadays, it was revealed that the electrolyte optimization [20–23], interface modification [24,25], and the structural design could effectively improve the cyclability and structure stability of the Zn anode [26–29]. Among of them, the interface optimization has been widely recognized as one of the most promising approaches because of its facile process, large-scale preparation, and the good compatibility, which can favorably bring enhanced electrochemical performance of the Zn-ion batteries [30]. Specifically, the interlayer (such as TiO2 [31], ZrO2 [32], nano-CaCO3 [33], GO [34], graphite [35]) located at between the Zn anode and the separator can not only function as an efficient spatial shielding to block the direct contact between the electrolyte and the Zn anode, but also effectively reduce the side reactions, and suppresses the hydrogen evolution during the charge/discharge process. Also, the introduction of the protective interlayer could achieve a uniform electric field, thus well balance the surface charge of the electrode, facilitate the uniform migration of Zn2+, and provide abundant nucleation sites to circumvent the dendrite formation. The non-conductive polymers with polar groups (such as polyamide [36], polypyrrole [37]) were also employed as buffer layer to improve the Zn2+ transporting and promote the uniform zinc deposition. Therefore, the rational strategies and methodologies for fabricating efficient protective layer show promise and the positive Zn plating/stripping behaviors require to be further developed and regulated, which make it a substantial step for the industrialization to build high properties of ZIBs.
In this work, as illustrated in Fig. 1, the phosphorus-doped carbon (P-C) thin film was employed as a useful protective layer for Zn anode after the facile plasma enhanced chemical vapor deposition (PECVD) process. The as-constructed P-C/Zn electrode can positively regulate the interface electric field and the ion flux during cycles, thus energetically alleviate the dendrites formation and volume change of the Zn anode. Therefore, the uniform and homogeneous Zn stripping/plating behaviors were achieved during cycling, and the P-C/Zn anode symmetric cells impressively exhibit stable operation for over 1000 h at a current density of 2 mA/cm2 and a constant capacity of 2 mAh/cm2. Specially, the P-C/Zn||MnO2 full cell demonstrated a high specific capacity of around 252.5 mAh/g after 700 cycles under the current density 2 A/g. It is believed that the employment of this carbon protective layer with positive effects provide valuable guideline to construct more reliable Zn ion batteries or other energy storage systems. From Fig. 2a, compared with the bare Zn electrode, it is clearly seen that the as-modified zinc foil with light blue color after the plasma-enhanced chemical vapor deposition (PECVD) process. Moreover, as shown in Figs. 2b and c, the protective layer of the phosphorus-doped carbon (P-C) thin film is uniformly and densely coated on the rough surface of the pristine zinc electrode. As displayed in Fig. S1 (Supporting information), the thickness and particle size of the deposited protective thin film are 30 nm and 10 nm, respectively. The crystalline property of the P-C/Zn electrode was then characterized by X-ray diffractometer (XRD) as demonstrated in Fig. 2d. Apparently, all peaks match well with the Zn (Zn-PDF #04–0831) electrode, which implies that the outmost P-C thin film is amorphous [38]. In addition, as shown in Fig. 2e and Fig. S2 (Supporting information), scanning electron microscope (SEM) image of the P-C/Zn electrode and its corresponding element mappings obviously reveal that the phosphorus-doped carbon layer is conformally and successfully distributed on the bare Zn foil substrate. Signals of C and P obtained from the energy dispersive spectrometer (EDS) pattern indicate that the successfully deposition of the functional P-C layer after the PECVD procedure, and the existence of F can be attributed to the formation of ZnF and the CFx during the reaction process [39]. In addition, as displayed in Fig. 2f and Fig. S3 (Supporting information), compared with the pristine Zn electrode, the X-ray photoelectron spectrometer (XPS) spectrum of the P-C/Zn electrode clearly embraces strong C and F signals, which suggest the generation of the optimized carbon protective layer after the CF4 plasma treatment. In Fig. 2g, for the C 1s of the P-C/Zn electrode, the peaks at about 284.8, 286.6 and 289.8 eV can be assigned to C-C, C-O-C and O-C꞊O bonds, respectively. An extra peak located at 292.3 eV belongs to the C-F [40]. For the overlapped energy region of P 2p and Zn 3s signals, as displayed in Fig. 2h, the peaks at 132.6, and 139.2 eV are the chemical state of P 2p and Zn 3s for the P-C/Zn electrode [41]. As thus, it is well identified that the P-doped carbon layer was well deposited on the bare Zn electrode based on the above recorded information.
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| Fig. 1. (a) Schematic diagram of P-C/Zn synthesis process. Illustration of the different electrochemical behaviors between the (b) bare Zn and (c) the optimized P-C/Zn electrodes. Hydrogen evolution reaction (HER). | |
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| Fig. 2. (a) Optical photograph of the bare Zn and P-C/Zn electrodes. Planar-view SEM images of (b) bare Zn and (c) P-C/Zn electrodes. (d) XRD pattern of bare Zn and P-C/Zn electrode. (e) SEM image of the P-C/Zn electrode and its corresponding element mappings of C, P, Zn and EDS pattern. (f-h) Survey, C 1s, and P 2p XPS spectra of P-C/Zn electrode. | |
To study the favorable effect of P-C layer on the Zn anode, the long-term sustainability and cyclability of symmetrical cells assembled with bare Zn and P-C/Zn anodes under a constant areal current density and capacity were then investigated and implemented as shown in Fig. 3. From Figs. 3a and b, it was observed that the symmetrical cell of P-C/Zn||P-C/Zn delivered a lower voltage hysteresis than the bare Zn||bare Zn (33.7 vs. 38.2 mV) upon 1000 h at a current density of 1 mA/cm2 and a capacity of 1 mAh/cm2. Moreover, as displayed in Figs. 3c–f, the overall overpotential of P-C/Zn||P-C/Zn symmetrical cell are around 34.8 and 67.4 mV, which are still much better than the bare Zn||bare Zn (48 mV, 91.5 mV) under the higher current density and capacity (2 mA/cm2, 2 mAh/cm2; 5 mA/cm2, 1 mAh/cm2). Long-life time of 1000 and 500 h clearly demonstrate that the superb stable cyclability of the optimized P-C/Zn electrode. The bare Zn||bare Zn obviously failed after 500 and 100 h can be ascribed to the short circuit induced by the Zn dendrites formation during cycling. Impressively, as displayed in Figs. 3g and h, the P-C/Zn||P-C/Zn symmetrical cell apparently achieved stable Zn plating/stripping behaviors during the rate capability test particularly at higher current densities. The P-C/Zn-based symmetrical cell could cycle over 150 h and embraced lower voltage polarization than the bare Zn||bare Zn symmetrical cell (27, 35, 55, 71, 116 vs. 33, 45, 82, 115, 196 mV) at various current densities of 0.5, 1.0, 3.0, 5.0, and 10.0 mA/cm2 with a constant areal capacity of 1.0 mAh/cm2. The achieved attractive cycling stability and facilitated kinetics during the Zn ions plating/stripping process highlight the protective capability of the as-constructed P-doped carbon thin-film layer.
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| Fig. 3. Voltage-time profiles of the symmetric cells with different Zn anodes at (a, b) 1 mA/cm2 with 1 mAh/cm2, (c, d) 2 mA/cm2 with 2 mAh/cm2 and (e, f) 5 mA/cm2 with 1 mAh/cm2. (g, h) Rate performance of different symmetric cells at various current densities with a fixed areal capacity of 1 mAh/cm2. | |
To well investigate the positive effects of the P-C thin layer on the performance of Zn electrode, the electrochemical activities between the bare Zn and P-C/Zn anodes were further systematically examined and studied as shown in Fig. 4. Obviously, as depicted in Fig. 4a and Fig. S4 (Supporting information), the P-C/Zn||P-C/Zn symmetrical cell still presents lower nucleation overpotential and superior stability than the bare Zn||bare Zn (21.4 vs. 33.6 mV) and indicates that the reduced energy barrier during the Zn plating process, which is helpful to bring the promoted electrochemical kinetics for abundant Zn ions storage. In Fig. 4b, the linear sweep voltammetry (LSV) result reveals that the P-C/Zn anode exhibits a more negative potential response (-0.118 V vs. -0.091 V) than the bare Zn anode, which proves that the P-C/Zn anode could more effectively inhibit the hydrogen evolution reaction (HER) [42]. Moreover, as shown in Fig. 4c, the P-C/Zn electrode presents higher corrosion potential (-0.009 V vs. -0.008 V) and lower corrosion current density (0.914 mA/cm2 vs. 1.094 mA/cm2) than the bare Zn electrodes and clearly demonstrates that the increased corrosion resistance induced by the P-C layer, which is favorable to suppress the side reactions and obtain high Zn plating/stripping reversibility [43,44]. The asymmetric cells of P-C/Zn and bare Zn||Cu were assembled and characterized as displayed in Fig. 4d and Fig. S5 (Supporting information). In sharp contrast, compared with the bare Zn anode, the reduced polarization voltage and the higher reversibility of the P-C/Zn anode (55 vs. 96 mV) again identifies that the facilitated electrochemical kinetics. In Fig. 4e, cyclic voltammetry (CV) was conducted in both P-C/Zn||Cu and bare Zn||Cu half-cells at a scan rate of 5 mV/s. Compared to the bare Zn anode, the P-C/Zn||Cu half-cell exhibits a higher initial potential (-61 mV vs. -95 mV), which is consistent with the reduced nucleation overpotential and further verifies that the P-C layer can well promotes the Zn deposition [45].
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| Fig. 4. (a) Nucleation overpotential between the bare Zn and P-C/Zn anodes with 1 mA/cm2 and 2 mAh/cm2. (b) LSV curves in 2 mol/L ZnSO4 at current density of 12.5 mA/cm2. (c) Tafel curves of two electrodes in 2 mol/L ZnSO4 electrolyte. (d) The comparison diagram of voltage gaps of bare Zn||Cu and P-C/Zn||Cu asymmetric cells. (e) CV curves of bare Zn||Cu and P-C/Zn||Cu half cells at a scan rate of 5 mV/s. (f) Chronoamperograms of P-C/Zn and bare Zn anodes at -150 mV overpotential. SEM image of cycled (g) P-C/Zn and (h) bare Zn anodes after 2 cycles at 0.5 mA/cm2 with a capacity of 5 mAh/cm2. (i) Optical images of the patterned Zn anode before and after 5 cycles at 0.5 mA/cm2 with a capacity of 6 mAh/cm2. (j-m) SEM images of cycled patterned Zn anodes for different areas. | |
In addition, the diffusion behavior of Zn ions on the anode surfaces was studied by chronoamperometry (CA) technique as shown in Fig. 4f. Benefiting from the P-C thin film protective layer, the P-C/Zn anode dropped slowly and eventually stabilized after 40 s, which suggests that the zinc migration behavior was optimized from a brief two-dimensional diffusion to a continuous three-dimensional diffusion, thus positively facilitating the uniform Zn deposition and preventing dendrite growth [46]. In Figs. 4g and h, the surface of the P-C/Zn anode clearly produced less uneven structures than the bare Zn anode after cycling and further verified the advantageous impact of the additional P-C layer. From Figs. 4i-m, it was seen that the patterned Zn anode displayed clear boundary and the surface of the patterned Zn electrode with P-C coating showed relatively flat, dense, and smooth characteristic, confirming the favorable protective effect of the functional P-C layer on the zinc anode. However, the patterned Zn anode without modification distinctly exhibited a rough surface and generated a large number of microflakes and protrusions, reflecting a very uneven zinc stripping/plating process. As displayed in Fig. S6 (Supporting information), the surface morphology of the P-C/Zn anodes even under higher current densities still can be well reserved and maintained. As a consequence, the outmost P-C layer enables enough adsorption sites and rapid pathways for ion diffusion, facilitates the uniform distribution of Zn2+ at the interface, and efficiently balances the electric field during the repeated Zn plating/stripping process. The distinct diffraction peaks in the bare Zn anode are ascribed to the formation of by-products of Zn4SO4(OH)6·5H2O, which indicates that the good protective effect of the optimized P-C layer (Fig. S7 in Supporting information). Additionally, as observed in Fig. S8 (Supporting information), the in-situ optical microscopy was used to further study the electrochemical behaviors of Zn2+ ions between the bare Zn and P-C/Zn anodes. Obviously, the surface of the bare Zn anode randomly and unevenly produced large Zn particles during the entire plating process. However, the plated Zn electrode with smaller size was almost uniformly deposited across on the whole optimized P-C/Zn anode, which again implied that the employment of the P-doped carbon protective layer was favorable to prevent the dendrites formation during cycling.
Full cells of bare Zn||MnO2 and P-C/Zn||MnO2 were assembled and evaluated based on the polycrystalline MnO2 cathode (Fig. S9 in Supporting information) toward the potential practical applications. As exhibited in Fig. 5a, both the P-C/Zn||MnO2 and bare Zn||MnO2 full cells display similar CV contours, which implies that the additional P-C thin film coated on the Zn electrode does not negatively affect the MnO2 cathode [46]. The increased current intensity in the CV curve of the P-C/Zn anode is due to the reduced polarization effect and the promoted ion diffusion kinetics during the Zn plating/stripping process [46]. Moreover, as shown in Figs. 5b and c, the charge-discharge profiles of P-C/Zn||MnO2 full cell in different cycles apparently demonstrates smaller voltage polarization and superior conformity, proving higher electrochemical activity and reversibility, and the corresponding voltage plateaus are also well consistent with the above CV results. Impressively, as depicted in Fig. 5d, compared with the bare Zn||MnO2 full cell, the P-C/Zn||MnO2 full cell delivered higher capacity (243 vs. 138 mAh/g) and superb capacity retention ability (98.3% vs. 66%) after 700 long-term cycles under the current density of 2.0 A/g, which is also comparable with previously reported surface modification strategies based on the carbon materials (Table S1 in Supporting information). The increased capacity appeared in the first 100 cycles and stabilized during the remained cycles can be attributed to the successive redox reactions of the MnO2 electrode [47]. Lower charge transfer resistance of the P-C/Zn||MnO2 full cell (15.4 vs. 51.1 Ω) further proved that the enhanced electrochemical kinetics (Fig. 5e). The improved electrochemical energy storage ability of the full cell construction illustrates that the additional P-C coating could largely prevent the dendrites growth and the side reactions during the repeated cycles.
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| Fig. 5. Electrochemical performance of between the bare Zn||MnO2 and P-C/Zn||MnO2 full cells. (a) CV curves at a scan rate of 0.3 mV/s. Charge-discharge curves of (b) P-C/Zn||MnO2 and (c) bare Zn||MnO2 full cells at 2.0 A/g. (d) Cycling performance at 2.0 A/g after the CV test and (e) EIS pattern of pristine bare Zn||MnO2 and P-C/Zn||MnO2 full cells. Here, Rs, Rct, constant phase-angle element (CPE), and W1 represent the ohmic resistance, charge transfer resistance, double layer capacitance, and the Warburg impedance, respectively. | |
In summary, an effective phosphorus-doped carbon layer coated on the Zn (P-C/Zn) anode was successfully constructed via using the plasma-enhanced chemical vapor deposition (PECVD) technique and significantly delivered improved energy storage ability for high-performance aqueous Zn-ion battery. The artificial protective P-C layer produces a stable electrolyte/electrode interface and efficiently suppresses the corrosive side reactions of the Zn anode. The diffusion energy barrier and the nucleation overpotential are greatly reduced, which is helpful to bring fast and uniform Zn2+ flux transportation during cycles. Therefore, the P-C/Zn||P-C/Zn symmetric cell achieved attractive stable plating /stripping performance upon 1000 h at a current density of 2 mA/cm2. Moreover, the P-C/Zn||MnO2 full cell maintained a high reversible capacity of 252.4 mAh/g after 700 cycles at a current density of 2 A/g. This promising strategy with optimized electrode/electrolyte interface could offer numerous opportunities for the development of high-performance dendrite-free zinc anodes.
Declaration of competing interestThe authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.
CRediT authorship contribution statementLong Huang: Writing – original draft, Investigation. Jian Pu: Writing – original draft, Investigation. Yunyu Zhao: Investigation. Xiangxiang Fang: Investigation. Yingjian Yu: Writing – review & editing, Resources. Yuan Li: Investigation. Jinyan Ma: Investigation. Yuejin Zhu: Investigation. Fang Hu: Investigation. Chuang Yue: Conceptualization, Investigation, Writing – review & editing.
AcknowledgmentsThis work is financially supported by the National Natural Science Foundation of China (Nos. 61904090 and 62464010), Project (No. 202306) of State Key Laboratory of Physical Chemistry of Solid Surfaces (Xiamen University).
Supplementary materialsSupplementary material associated with this article can be found, in the online version, at doi:10.1016/j.cclet.2025.110989.
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