Metal- and binder-free dual-ion battery based on green synthetic nano-embroidered spherical organic anode and pure ionic liquid electrolyte
Abstract
Dual-ion batteries (DIBs) have attracted extensive attention and investigations due to their inherent wide operating voltage and environmental friendliness. Nevertheless, the vast majority of DIBs employ metal-based anode active materials or electrolytes, which are relatively costly and unsustainable. Moreover, the utilization of binders and current collectors in the preparation of cathodes and anodes reduces the energy density to a certain extent, which weakens the advantages of DIBs. Here, we synthesized three types of binder-free nano-embroidered spherical polyimide anode materials composed entirely of renewable elements, paired with pure ionic liquid electrolyte without metal elements and flexible self-supporting independent graphite paper cathode without current collector, to construct a class of totally metal and binder-free DIBs. It significantly improves specific discharge capacity, energy density, cyclic stability, and fast charging performance while remarkably reducing costs and self-discharge rate. Additionally, we overcame the drawbacks of conventional synthesis methods and innovatively prepared nanoscale polyimide materials by a green and facile hydrothermal method, which effectively minimizes synthesis costs and avoids risks. This novel battery system design strategy will promote the advancement of low-cost, high-performance DIBs and could be a promising candidate for large-scale energy storage applications.
Keywords
INTRODUCTION
The high energy density, long cyclic life, and no memory effect of lithium-ion batteries (LIBs) enable them to occupy a major share of the electrochemical energy storage (EES) market since their commercialization and are widely used in portable electronic devices and electric vehicles[1-4]. However, the scarcity and uneven distribution of metal resources, such as lithium and cobalt, drive up the manufacturing and usage costs of LIBs year by year, rendering it difficult to achieve large-scale grid-level energy storage applications. Against such a background, there is an urgent requirement to develop novel battery systems to meet the imminent demand for green and sustainable energy storage programs[5-8]. Different from LIBs, dual-ion batteries (DIBs) allow the simultaneous participation of anions and cations in the electrochemical reaction during charging and discharging, and electrolyte is the singular source of active ions[9-12]. Additionally, inexpensive graphite can be employed to avoid the use of expensive transition metal-based materials as the cathode. This unique reaction mechanism endows DIBs with high cost-effectiveness, suitable operating voltage, and environmental friendliness, which have continuously attracted great interest and research enthusiasm from researchers in recent years[13-15].
Currently, the anode of DIBs is mainly based on inorganic materials such as carbonaceous materials[16-18], alloy-based materials[19-21] and transition metal-based compounds[22-24], which are based on intercalation, alloying, and transformation reactions to accomplish the storage of active ions, respectively. Unfortunately, DIBs based on these electrodes usually undergo structural exfoliation and volume expansion during cycling, causing poor stability, low specific discharge capacity (SDC), and a reduced initial Coulomb efficiency (ICE). In particular, this is not in line with the development concept of "green and sustainable batteries"[25,26]. The key technology for green, sustainable DIBs is the exploration of organic anode materials composed entirely of renewable elements from nature. Organic materials are considered as excellent candidates for the next generation of green and sustainable EES due to their inherent merits of being metal-free and widely available, eco-friendly, cost-effective, and structurally well-designed[27-33]. However, an understanding of their application in DIBs is still in its infancy. Several organic materials have been reported, such as polycyclic aromatic hydrocarbon[34,35], nitrogen/sulfur-containing organics[36,37], carbonyl compounds[38,39], and so on. Organic carbonyl compounds are of great research fascination owing to their simplified synthetic route, unique multi-electron reaction, and structural diversity[40]. Unfortunately, small molecule carbonyl compounds inevitably dissolve in organic electrolytes, leading to terrible cyclic stability and accelerated capacity degradation, limiting their application in large-scale energy storage. Numerous attempts have been made by investigators to avoid dissolution and achieve excellent electrochemical performance. Due to their composition of organic cations and inorganic anions, ionic liquids have a broad electrochemical window. They are kinetically stable, free of solvent molecules, and non-flammable. Therefore, a feasible alternative is to adopt ionic liquids instead of traditional organic solvents[41-43]. Particularly, ionic liquids operate both as solvents and as active ions participating in electrochemical reactions, not only effectively preventing dissolution but also avoiding the use of electrolyte metal salts. Another feasible approach is to design organic polymers with stable inactive backbones and highly redox-active carbonyl functional groups such as polyimide (PI) electrode materials[44]. Additionally, employing nano-engineering design strategies can further increase the active sites of electrode materials and facilitate the transport of active ions and electrolyte penetration, which is beneficial for improving the SDC and electrode reaction kinetics[45,46]. Nevertheless, the application of PI as anodes for DIBs has rarely been reported. One of the main challenges is the dilemma of synthesis, followed by a long (> 8 h) polycondensation reaction at high temperatures (> 200 °C) under a catalyst and N2 atmosphere, and the final product also needs to be baked in a tube furnace at high temperatures (> 300 °C) for more than 8 h to remove the solvent[47,48]. As a consequence, the whole procedure is time-consuming and costly, with certain technical challenges and safety risks. In this regard, it is essential to explore a cost-effective, energy-saving, green, and safe synthesis path to obtain comparable or even superior performance.
Herein, after continuous trial and exploration, we have developed a simplified one-step green synthesis strategy, and three types of PI nano-anode materials can be obtained directly by hydrothermal reactions at 160 °C for 6 h. Besides, the straightforward adoption of independent graphite paper (GP) with self-supporting capability as the cathode and current collector, and the anode is binder-free, which greatly improves the discharge capacity and energy density. Combined with a pure ionic liquid electrolyte, a dual-ion full battery system without metal elements and binder is constructed. The reaction principle of the electrodes and the working mechanism of the battery are investigated through a series of physical and chemical characterizations. Such innovative DIBs with outstanding electrochemical performance furnish insight into the establishment of greener and sustainable EES systems and are expected to be applied in large-scale energy storage.
EXPERIMENTAL
Materials
Pyromellitic anhydride, o/m/p-phenylenediamine (o/m/p-PDA), N-methylpyrrolidone (NMP), and GP were purchased from Macklin. Glass fiber diaphragm (GF/A), conductive agent (Super P), carbon-coated aluminum foil, and CR2025 type cell shells were purchased from Clorod. N-butyl-N-methylpyrrolidinium bis(trifluoromethanesulfonyl)imide ionic liquid was purchased from Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences. Unless otherwise stated, no further treatment was required for all materials.
Synthesis of o-PDI, m-PDI, and p-PDI
Firstly, homophthalic anhydride and o/m/p-PDA are added sequentially to 110 mL of deionized water in a 1:3 molar ratio and stirred overnight at room temperature on a magnetic stirrer, then poured into a reaction kettle equipped with 250 mL PTFE liner and finally reacted hydrothermally in an oven at 160 °C for 6 h. After cooling to room temperature, the reaction was filtered with water, methanol, and ethanol successively and dried in a freeze dryer for 48 h. The as-prepared samples were named as o-PDI, m-PDI, and p-PDI.
Materials characterizations
Scanning electron microscopy (SEM) images and energy-dispersive X-ray spectroscopy (EDX) spectra and corresponding mappings were acquired on a scanning electron microscope (Merlin, ZEISS, Germany).
Battery assembly and measurements
In order to evaluate the electrochemical performance of the dual ion battery, the full battery was assembled by using CR-2025 type button cells in a super glove box (H2O < 0.01 ppm, O2 < 0.01 ppm), in which the cathode is directly employed with independent GP with self-supporting capability. As for the preparation of the anode, o/m/p-PDI and Super P are mixed in the ratio of 6:4 and added to a weighing bottle containing NMP without any binder added. Magnetic stirring was done overnight to form a homogeneous slurry, which was later coated on top of the carbon-coated aluminum foil with a coating thickness of 100 μm. The coating is then transferred to a vacuum drying oven at 100 °C for 12 h. Both the cathode and anode are cut into 14 mm diameter discs and placed in a glove box for use. The mass loading of the anode is
RESULTS AND DISCUSSION
Physical characterizations
As shown in Supplementary Schematic 1, three types of PI materials (o-PDI, m-PDI, and p-PDI) were synthesized by using three phenylenediamine isomers (o/m/p-PDA) and pyromellitic dianhydride (PMDA) through a green hydrothermal polycondensation reaction and freeze-drying. Figure 1A-C presents the SEM of the as-prepared o-PDI, m-PDI, and p-PDI, respectively, which all exhibit an embroidered spherical morphology. The elemental mapping in Figure 1D and Supplementary Figures 1 and 2 shows that the C, N, and O elements are uniformly distributed. Specifically, each hydrangea is composed of nanoscale flakes with thicknesses between 10~20 nm and displays a three-dimensional porous network interleaved structure. This distinctive nano-morphology configuration facilitates adequate electrolyte infiltration, diffusion, and storage of active ions, thus improving the ion transport kinetics, rate capability, and discharge capacity. Besides,
Figure 1. Characterizations of the o-PDI, m-PDI, and p-PDI. (A-C) SEM. (D) Elemental analysis. (E) FT-IR. (F) XRD. (G-J) XPS. (K) TGA. (L and M) N2 adsorption/desorption curves and pore size distributions.
The structural stability of the materials was investigated via the dissolution of the electrode sheets in electrolyte and TGA, respectively. The Pyr14TFSI ionic liquid electrolyte placed with PMDA, o-PDI, m-PDI, and p-PDI electrode sheets, respectively, showed no variations with time migration and remained clear and transparent even after one month [Supplementary Figure 6], indicating that o-PDI/m-PDI/p-PDI exhibits excellent stability in this ionic liquid. This is supported by the TGA curves in Figure 1K, where the three phenylenediamine isomers decomposed at ~150 °C with significant mass loss, and the PMDA monomer also decomposed at around ~250 °C with poor stability. On the contrary, the stability of o/m/p-PDI increased noticeably, with the onset decomposition temperature of o-PDI and p-PDI reaching up to
Electrochemical performance and kinetics of o-PDI, m-PDI, and p-PDI
A Pyr14TFSI ionic liquid electrolyte-based button-type battery was used to probe the active ion storage capacity and reaction kinetics of the electrodes. Supplementary Figure 7 shows the two-electrode cyclic voltametric (CV) curves based on PMDA electrodes at different cycles scanned from the open circuit voltage in the negative direction at a rate of 1 mV/s. No redox peaks appear, indicating that no electrochemical redox reaction occurs and the PMDA electrode cannot store active ions[61,62]. Interestingly, when replaced with the o-PDI/m-PDI/p-PDI electrode, two pairs of sharp redox peaks emerge, as shown in Figure 2A-C, respectively, and all the CV curves overlap, indicating excellent cycling reversibility and stability. Figure 2D and Supplementary Figure 8A-C depict the GCD curves based on PMDA, o-PDI, p-PDI, and m-PDI anodes, respectively. The full battery system, on the basis of PMDA anodes, exhibits two inclined curves without charge/discharge plateaus [Supplementary Figure 8A]. In contrast, the systems based on m-PDI, o-PDI, and p-PDI anodes all display typical active ion insertion/de-insertion behavior with two pairs of symmetrical charge/discharge plateaus [Figure 2D and Supplementary Figure 8B and C], respectively, in accordance with the CV curves. Similar to the GCD curves, the dQ/dV curves in Supplementary Figure 9 indicate that the charging and discharging processes of o-PDI, p-PDI, and m-PDI are divided into two regions except for PMDA, which represent the various stages of insertion and de-insertion, respectively[63-65]. The electrochemical storage behavior and reaction kinetics of o-PDI, m-PDI, and p-PDI were further analyzed by CV curves at different scan rates (0.2/0.4/0.6/0.8/1 mV/s), and the results are summarized in Figure 2E and Supplementary Figure 10A and B. All of the CV curves manifest an analogous silhouette and well-defined redox peaks, which indicate a stable electrochemical performance[23,66]. The voltammetric response of the electrode at various scan rates can be quantified based on the power-law relationship
Figure 2. Electrochemical performance and kinetic characterizations of o-PDI, m-PDI, and p-PDI electrodes. (A-C) CV tests at 1 mV/s. (D) GCD curves. (E) CV curves at various scan rates and (F) The corresponding b values derived from i = avb. (G) Pseudocapacitance ratio of m-PDI at 1 mV/s. (H) Contribution of pseudocapacitance at different scan rates. (I) Linear relationship between i and the square root of v.
Quantitatively, the capacitive contribution is calculated based on Dunn’s method: i = k1v + k2v1/2, where k1 and k2 are constants, and k1v and k2v1/2 represent the pseudocapacitance contribution and the diffusion contribution, respectively. Consequently, the pseudocapacitance contributions of o-PDI, m-PDI, and p-PDI electrodes at 1 mV/s are 0.69, 0.95, and 0.89 (the red-filled part in Figure 2G and
Electrochemical performance of o//G-DIB, m//G-DIB, p//G-DIB
The proof-of-concept full batteries based on o-PDI/m-PDI/p-PDI anodes, GP cathodes, and Pyr14TFSI ionic liquid electrolytes were constructed respectively to further investigate the electrochemical performance for various systems (abbreviated as o//G-DIB, m//G-DIB, p//G-DIB). In particular, GP is a type of conductive carbon material featuring self-supporting flexibility capability without current collectors
Figure 3. Electrochemical performances of o//G-DIB, m//G-DIB, and p//G-DIB. (A-C) GCD curves at different rates. (D) dQ/dV curves of m//G-DIB. (E) Rate performance. (F) EIS and its fitting diagram. (G) Cyclic performance at 2 C. (H) The medium discharge voltage during cycling. (I) The long-term cyclic performance under 10 C.
The cyclic performance of o//G-DIB, m//G-DIB, and p//G-DIB at 2 C is compared, as shown in Figure 3G, where the reversible initial specific discharge capacities of o//G-DIB and p//G-DIB are 94 and 104 mA h g-1, respectively, and the capacity retentions after 850 cycles are 99% and 99.5%, respectively. Apparently, the
A low self-discharge rate is an essential performance parameter for full batteries to achieve practical applications, and unfortunately, DIBs are often criticized for exhibiting a comparatively high self-discharge rate. On this basis, the self-discharge performance of o//G-DIB, m//G-DIB, and p//G-DIB was tested separately by fully charging the batteries first and then completely discharging them after 10 h of resting. The results are presented in Figure 4A-F and Supplementary Figure 22, according to the self-discharge rate calculation formula: S = (C - Cr)/CT*100%, where S denotes the self-discharge rate, C and Cr are the SDCs without and after resting, respectively, and T refers to the resting time[23,80]. It can be calculated that the self-discharge rates of o//G-DIB, m//G-DIB, and p//G-DIB are 0.00817, 0.00371 and 0.00603 h-1, respectively, which are significantly lower than the currently reported battery systems, as shown in
Figure 4. Self-discharge and fast charging performance. GCD curves of (A-C) Unresting and (D-F) Resting for 10 h. (G-I) The first ten cycles of charging at 20 C and discharging at 1 C and (J-L) Corresponding cyclic performance.
Working mechanism and reaction principle
Taking the m//G-DIB system as a typical representative, the unique active ion storage mechanism of cathodes/anodes and the variations of chemical bonds during charging and discharging were investigated by FT-IR, Raman, and XPS. Figure 5A and Supplementary Figure 23 illustrate the FT-IR characterization of the anode under different charging and discharging states. The symmetric and asymmetric stretching vibration peaks of C=O located near 1,742 and 1,769 cm-1 basically disappear after being completely charged [Figure 5A], and the characteristic peak of C-O appears near 1,270 cm-1 [Supplementary Figure 23]. Meanwhile, it is evident from the fitted high-resolution N1s spectra that N-S and N-F characteristic peaks appeared at 402 and 399 eV, respectively, after completely charged [Figure 5B and
Figure 5. The investigations of energy storage mechanism based on cathodes and anodes. (A) FT-IR and (B) the fitted high-resolution
From the above characterizations, combined with the CV, dQ/dV, and GCD curves in Figure 2, it can be concluded that the working mechanism of the full battery is depicted in Figure 5E. The electrode reactions involved are shown in (1) to (3): during charging, the active cations and anions in the electrolyte move toward the cathode and anode, respectively, and participate in the electrochemical reactions. Conversely, during the discharge process, the cations and anions return to the electrolyte from the cathode and anode, respectively. Additionally, as shown in Figure 5F, only one coin battery is able to light the LED and successfully charge the smartwatch, indicating a great prospect for practical applications.
Anode: x(o/m/p - PDI)n+ Pyr14+ + 2nxe- ↔ (o/m/p - PDI)nx(Pyr14)2nx
Cathode: yC + 2nxTFSI- ↔ Cy (TFSI)2nx+ 2nxe-
Overall: x(o/m/p-PDI)n+ 2nxPyr14+ + yC + 2nxTFSI- ↔ (o/m/p - PDI)nx(Pyr14)2nx+ Cy(TFSI)2nx
Such excellent electrochemical performance is greatly dependent on the superior structural stability of the cathode and anode. To appreciate this, a combination of XRD, Raman, and FT-IR techniques was employed to characterize the electrodes during the charge and discharge process. For the GP cathode, as depicted in Figure 6A and B, the signal of the 002 characteristic peak located at 26.5° decreases gradually during the charging process and drops to a minimum after being completely charged, implying the formation of graphite intercalation compounds (GICs) accompanied by a reduction in crystallinity due to the intercalation of TFSI-[67,75,86]. It can be corroborated by Raman that during the charging process, the graphite layers adjacent to the intercalation layers become highly charged owing to the formation of GICs, and the G peak located at 1,580 cm-1 undergoes a blue shift accompanied by a weakening of the signal
Figure 6. XRD, Raman, and FT-IR characterizations at different charge and discharge states. (A, B, F) XRD and (C, D, G) Raman and FT-IR spectrums of the cathode and anode based on the selected stages. (E) The IG/ID values based on different charging and discharging stages. (H) Electrochemical performance comparison of recently reported work in DIBs.
CONCLUSIONS
In summary, three types of PI anode materials with distinctive nano-morphologies, o-PDI, m-PDI, and p-PDI, could be synthesized on a large scale by an innovative green and mild hydrothermal strategy, which breaks through the technical drawbacks of the traditional synthesis of PIs. Through a combination of a series of physicochemical characterizations and electrochemical measurements, it is proved that m-PDI shows the most excellent performance due to the homogeneous and well-dispersed lamellar structure, the maximum specific surface area and pore size, the optimum ion diffusion coefficient, and the highest pseudocapacitance ratio. Matching with the GP cathode with self-supporting flexibility and Pyr14TFSI pure ionic liquid electrolytes, the binder and metal-free o//G-DIB, m//G-DIB, and p//G-DIB full battery systems are constructed, and they exhibit outstanding electrochemical performances: (1) high specific discharge capacities of 144, 222 and 168 mA h g-1 at 0.2 C, respectively, and energy densities of 409.8 and
DECLARATIONS
Acknowledgments
The authors would like to acknowledge the financial support from the National Natural Science Foundation of China (No. 22075089) and the Fundamental and Applied Fundamental Research Project of Zhuhai City (No. 22017003200023).
Authors’ contributions
Prepared the o/m/p-PDI, assembled the dual-ion batteries, and performed most of the electrochemical experiments and physicochemical characterizations: Wu H
Supervised the project: Fang Y, Yuan W
Analyzed the data and co-wrote and discussed the whole paper: Wu H, Luo S, Zheng W, Li L, Fang Y,
Availability of data and materials
The data are made available upon request to authors.
Financial support and sponsorship
This work was financially supported by the National Natural Science Foundation of China (No. 22075089) and the Fundamental and Applied Fundamental Research Project of Zhuhai City (No. 22017003200023). The authors would like to thank Jian-ming Liu from the Shiyanjia Lab (www.shiyanjia.com) for the support of SEM, XRD, and Raman testing.
Conflicts of interest
All authors declared that there are no conflicts of interest.
Ethical approval and consent to participate
Not applicable.
Consent for publication
Not applicable.
Copyright
© The Author(s) 2024.
Supplementary Materials
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Wu, H.; Luo, S.; Zheng, W.; Li, L.; Fang, Y.; Yuan, W. Metal- and binder-free dual-ion battery based on green synthetic nano-embroidered spherical organic anode and pure ionic liquid electrolyte. Energy Mater. 2024, 4, 400015. http://dx.doi.org/10.20517/energymater.2023.75
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