An industrial pathway to emerging presodiation strategies for increasing the reversible ions in sodium-ion batteries and capacitors
Abstract
Sodium-ion batteries (SIBs) and capacitors (SICs) have been drawing considerable interest in recent years and are considered two of the most promising candidates for next-generation battery technologies in the energy storage industry. Therefore, it is essential to explore feasible strategies to increase the energy density and cycling lifespan of these technologies for their future commercialization. However, relatively low Coulombic efficiency severely limits the energy density of sodium-ion full cells, particularly in the initial cycle, which gradually decreases the number of recyclable ions. Presodiation techniques are regarded as effective approaches to counteract the irreversible capacity in the initial cycle and boost the energy density of SIBs and SICs. Their cyclic stability can also be enhanced by the slow release of supplemental sodium and high-content recyclable ions during cycling. In this review, a general understanding of the sodium-ion loss pathways and presodiation process towards full cells with high Coulombic efficiency is summarized. From the perspectives of safety, operability and efficiency, the merits and drawbacks of various presodiation techniques are evaluated. This review attempts to provide a fundamental understanding of presodiation principles and strategies to promote the industrial development of SIBs and SICs.
Keywords
INTRODUCTION
In the upcoming decades, the widespread adoption of clean and efficient energy storage systems will be necessary to combat climate change[1-5]. Metal-ion batteries[6-9], exemplified by lithium-ion batteries (LIBs), have received extensive attention due to their high energy density and low self-discharge and have been frequently applied in portable electronic devices, electric vehicles and grid-scale energy storage[6]. However, the limited and unevenly distributed lithium resources hinder the further development of LIBs[10,11]. It is therefore necessary to search for other energy storage technologies to substitute for LIBs. As a result of their significant abundance, high performance, low cost and similar physicochemical properties to LIBs,
It is without a doubt that increasing the cyclable sodium-ion content in a full-cell system can directly and efficiently improve its electrochemical performance by alleviating the sodium-ion loss in the initial cycle. Presodiation, known as the pre-doping of Na+, is an efficient method to prevent the capacity loss introduced by constrained sodium sources in the cathode, which can also boost the operating voltage and elevate the concentration of recyclable ions in SIBs[14,31-35] and SICs[36-38]. As indicated in Figure 1, under normal conditions, the active sodium ions in the cathode material are partly responsible for Na loss; however, the presodiated full cell can supply more active Na, which can compensate for the irreversibly recyclable Na, preventing Na loss in the cathode and the corresponding capacity decay. On this basis, the presodiation process is recognized as a practical method for bringing high-performance Na-ion full-cell manufacturing to fruition in the future. Based on the research on prelithiation in LIBs[33,39-42], several presodiation strategies[33,35,43] have been reported containing physical, chemical and electrochemical approaches. Considering the cathode side, mixing the suitable Na-containing additives and coupling them with
FUNDAMENTALS AND STRATEGIES OF PRESODIATION
Similar to LIBs, the electrode materials from SIBs also suffer from Na loss during electrochemical cycles, as shown in Figure 1, leading to the deterioration of capacity and energy density. In SIBs, the following three factors are primarily responsible for the irreversible capacity loss:
(i) Formation of SEI from electrolyte decomposition. The electrolytes of SIBs mainly contain carbonate ester solvent and sodium salt, which are prone to irreversible decomposition reactions at low potential to form SEI film[44,45], resulting in the reduction of Coulombic efficiency in the first cycle[44-47]. In particular, for an alloy anode that undergoes a significant volume change during Na storage[48-50], the SEI film continuously splits and reconstructs during electrochemical cycling, leading to a further increase in Na consumption.
(ii) Capture of Na+ from structural defects. Generally, the anode material has several structural flaws and sodiophilic functional groups that can permanently trap sodium ions and cause capacity deterioration[51,52]. In particular, for anode materials with a high surface area or porous structure, the Na+ loss will be promoted.
(iii) Na loss from side reactions. For instance, coordinated water is present in cathode materials, such as Prussian blue, which is vulnerable to electrolyte side reactions at high potentials and results in Na consumption[53]. From the perspective of the Na-ion full cell, the SEI will develop on the surface of the anode during the first charge cycle, which consumes partial Na+ from the energy storage system, causing a slight capacity loss and a drop in energy density.
If a second Na+ source can be provided in addition to the cathode compensating for the Na+ loss during charge and discharge, the capacity and energy density of SIBs can be further increased[33,43]. This process of providing an additional Na+ source is defined as presodiation. Additionally, the presodiation process can also increase the operating voltage and lower the electrolyte consumption during the formation of the SEI film in SICs. Among the strategies to enhance the initial Coulombic efficiency, such as surface engineering[54-56], structural regulation[57] and new materials design[58], the feasible presodiation technology appears more effective and enables the irreversible capacity to be activated, maximizing the energy density in SIBs. Presodiation methods vary in their benefits and drawbacks, and it is therefore crucial to comprehend the underlying mechanism.
Self-sacrificing Na-containing additives for cathodes
Recently, presodiation has been performed with the addition of supplementary Na-containing additives and a wide range of materials have been systematically investigated. Na-containing additives usually undergo electrochemical oxidation during the first charge-discharge operation, irreversibly releasing extra Na+ to compensate for the Na+ loss. For this, the decomposition potential of the additives should be lower than the working potential of the full cell to ensure that the Na-containing additives can be thoroughly electrochemically oxidized to release sufficient Na+ during the first charge[59].
There are many Na-containing additives that have been carefully studied for the presodiation of Na-ion full cells, including Na2C2O4[60], DTPA-5Na[59], NaCrO2[61], Na2O[62], Na2S[63,64], NaN3[65], and NaNiO2[66], which can be combined with the active cathode materials and provide sufficient extra Na+ sources during the first charge, as well as oxidizing the associated anions to release gases. Na2C2O4, as a typical sacrificial additive, is environmentally friendly, low cost and can achieve no additional residues after Na+ extraction. As shown in Figure 2A, Sun et al. systematically evaluated the role of Na2C2O4 in the presodiation of SICs[60]. They concluded that Na2C2O4 could be oxidized at ~3.7-4.0 V (vs. Na+/Na) to yield a specific capacity of
There are many Na-containing additives that have been carefully studied for the presodiation of Na-ion full cells, including Na2C2O4[60], DTPA-5Na[59], NaCrO2[61], Na2O[62], Na2S[63,64], NaN3[65], and NaNiO2[66], which can be combined with the active cathode materials and provide sufficient extra Na+ sources during the first charge, as well as oxidizing the associated anions to release gases. Na2C2O4, as a typical sacrificial additive, is environmentally friendly, low cost and can achieve no additional residues after Na+ extraction. As shown in Figure 2A, Sun et al. systematically evaluated the role of Na2C2O4 in the presodiation of SICs[60]. They concluded that Na2C2O4 could be oxidized at ~3.7-4.0 V (vs. Na+/Na) to yield a specific capacity of
Figure 2. (A) Schematic illustration of presodiation mechanics by introduction of Na2C2O4 implemented by initial charge process[60].
As shown in Figure 2B, Jo et al. reported a new penta-sodium diethylenetriaminepentaacetic acid salt (DTPA-5Na), which could be irreversibly oxidized to achieve an excellent charge capacity of nearly
As shown in Figure 2C, Shen et al. employed a NaCrO2 additive to achieve high capacity, low polarization, high energy density and excellent cycle stability in Na3V2O2(PO4)2F//HC full cells. During the first cycle, the full cell with NaCrO2 shows charge and discharge capacities of 308 and 118 mAh g-1[61], respectively, which are higher than the capacities of the full cell without additives (charge capacity of 132 mAh g-1 and discharge capacity of 50.7 mAh g-1). In addition to traditional cathode additives, Zhang et al. developed an electrocatalytically driven decomposition of Na2O with high Na+ content, which could provide a large number of recyclable Na+ without jeopardizing the integrity of the electrode materials, electrolytes and the overall battery [Figure 2D][62]. High sodium content (88%) sodium oxide (Na2O) can provide sufficient cyclable sodium ions that are electrocatalytically-driven by a highly active ruthenium@graphene (Ru@G) electrocatalyst to compensate the sodium loss during the initial SEI formation and following consumption. This additional electrocatalytically-driven cathode strategy not only provides numerous cyclable sodium but also has no adverse effects on the stability of the electrode materials, electrolyte or the whole battery system. All the steps were based on the current mature commercial battery fabrication process, which can efficiently ensure its potential practical application. Furthermore, this process does not induce unknown byproducts into sodium-ion full-cell systems. The catalytically-driven sodium-ion compensation was monitored by
In addition to experimental investigations, theoretical calculations are also useful tools for developing presodiation techniques. Zou et al. calculated the optimal binding energy of O-M (M = Li, Na or K) bonds in metal carboxylates[67-69]. After an in-depth analysis of the experimental results and density functional theory calculations, it was found that the cathode additive decomposition caused by irreversible decarboxylation is determined by the O-M (M = Li, Na or K) bond energy, which can be further affected by the electronic structure of the substituent and hardness/softness adjustment of metal elements. Furthermore, the bonding strength of O-M bonds can be regulated by the electron-donating effect of substituents and the low charge density of cations, resulting in a lower electrochemical oxidation potential.
The presodiation process by introducing Na-containing cathode additives has many advantages. First, it is straightforward and the total cost is determined by the cost of the additive substance, which is easy to commercialize and industrialize. Second, cathode additives have excellent environmental adaptability and high compatibility with current battery manufacturing technologies. However, there are still some remaining challenges facing cathode presodiation. For instance, the impact of cathode additive residues and emitted gases on the overall battery system is still not well understood at present. In particular, the released gases are likely to change the microstructure of cathode materials, which may have a significant influence on the long-time operation of the battery system.
Self-presodiation cathode materials
The introduction of sacrificial additives results in an increase in cathode mass and the inevitable generation of gases and byproducts, which restrains their commercial and industrial application[60]. To overcome the above-mentioned problems, the researchers proposed a Na-rich cathode as an alternative approach towards presodiation. The Na-rich cathode is a solid solution including supersaturated Na, which can be irreversibly released to the electrolytes during cycling, compensating for active Na loss. As shown in Figure 3A, the self-presodiation cathode compound O3-type Na0.9Cu0.11Ni0.11Fe0.30Mn0.48Ti0.10O2 was prepared by the quenching treatment, which can retain a high sodium content (nearly 0.9) in the crystal structure by inhibiting the precipitation of carbonate. The quenched materials maintain high Mn3+ and Na+ contents, which can compensate for Na consumption during initial charging by releasing Na+ activated by Mn3+ oxidation. Other transition metals are employed to supply capacity for subsequent cycles. In contrast, the structural evolution of the naturally cooled cathode material was investigated by in-situ temperature-variable XRD, indicating that the Na2CO3 layer formed on the surface of the cathode particles, accompanied by a large amount of Mn3+ oxidation caused by the reaction between Na+ precipitated from the layered oxide lattice and CO2 molecules in the air. The quenching procedure could significantly suppress the emergence of surface carbonates and preserve the long-range structure of Na0.9Cu0.11Ni0.11Fe0.30Mn0.48Ti0.10O2, particularly the lattice oxygen array architecture. Paired with a commercially available HC anode in Na-ion full cell, the quenching cathode delivered a higher energy density of 256 Wh kg-1, representing a ~9.9% increase compared with that of the naturally cooled cathode[70].
In addition, another Na-rich cathode, Na4V2(PO4)3, was systematically investigated by Mirza et al.[71]. As shown in Figure 3B, the electrochemical presodiation strategy was applied, in which Na3V2(PO4)3 (Na3VP) was first converted to Na4V2(PO4)3 (Na4VP) by a sodium foil and then the desodiation process of Na4VP was performed below 2.2 V vs. Na+/Na. The whole reaction process was characterized by operando XRD. During this process, the additional Na per formula unit of Na4VP is extracted into the electrolyte to compensate for the irreversible Na depletion and the corresponding Na3VP generated after desodiation from Na4VP is directly regarded as the cathode. As a result, the Na4PV//HC full cell achieves an excellent energy density of 265 Wh kg-1, which is 76% higher than that of the Na3VP//HC full cell. The reversible capacities of the
Direct contact with sodium foil/powder
Learning from the prelithiation process of LIBs employing metallic Li or Li powder[72], metallic Na has also been widely explored in direct contact with anode materials for presodiation. As shown in Figure 4A,
Figure 4. (A) Schematic illustration of synthesis process of Na-Sn alloy anode and corresponding electrochemical performance during first cycle[73]. (B) Schematic of direct contact with Na metal[74]. (C) Schematic illustration of ultrasonic dispersion of sodium metal powder and electrode preparation[75].
Similar to Li metal, metallic Na is extremely active and difficult to store stably and safely in air, so the presodiation with Na metal or powder can only be performed in an oxygen- and water-free glove box. Simultaneously, the manufacture of metallic Na powder is laborious and the risk of thermal runaway exists when the anode and metallic Na powder are pressure coated. Additionally, excessive Na powder input will promote the growth of Na dendrites and cause safety problems, so accurate calculations of the amount of Na metal or powder are required. Given these drawbacks, several researchers have experimented with a variety of solutions. For instance, an ultrasound-assisted synthesis of Na powder was reported by
Chemical presodiation for anodes
Chemical presodiation, similar to chemical prelithiation[76-79], is rapidly gaining popularity as a reliable and efficient presodiation technique that can substitute for the conventional operation of directly employing active Na metal. Generally, this process involves soaking sodium metal into an organic ether solvent containing naphthalene(Naph)/biphenyl (Bp), followed by electron transfer between sodium metal and Naph/Bp resulting in the production of highly active polycyclic aromatic sodium and the generation of a complex with ether solvent (Na-Naph or Na-Bp). Because of the potential difference, the Na-Naph or
In contrast to conventional wet chemical presodiation, Liu et al. proposed a continuous presodiation process by solution spraying, where 0.1 M Na-Naph in tetrahydrofuran (THF) solvent was sprayed with a precise dosage of Na-Naph (38 µL cm-2) onto commercially available HC anodes, followed by drying to eliminate any remaining Naph and THF [Figure 5A][32]. The results indicate that the presodiation treatment boosts the reversible capacity by 60 mAh g-1, the initial Coulombic efficiency by 20.0% and the energy density from 141 to 240 Wh kg-1 for the Na0.9[Cu0.22Fe0.30Mn0.48]O2//HC full cell. Interestingly, after chemical presodiation, a stable SEI film is generated on the surface of the HC anodes, which effectively reduces the irreversible loss of Na during the initial stage. To suppress the decomposition of electrolytes during battery assembly, Zheng et al. used Na-Naph in a DME solvent as the presodaition reagent to perform an ultrafast chemical pretreatment, as shown in Figure 5B[80]. Presodiation treatment successfully raises the initial Coulombic efficiency of rGO to 96.8% and results in the decomposition of the Na-containing complex to generate an artificial SEI layer on the anode surface. As a result of the suppressed decomposition of the excessive electrolyte by the artificial SEI, a homogenous and inorganic-rich SEI film generated on the surface of rGO, facilitated rapid interfacial ion transfer. Therefore, an outstanding capacity of 198.5 mAh g-1 at 5 A g-1 is displayed by the presodiated rGO anode.
Figure 5. (A) Schematic illustration of chemical presodiation of commercial HC anode with a Naph-Na solution[32]. (B) Schematic diagram of ultrafast presodiation of reduced graphene oxide (rGO) anode in using Na-Naph dissolved in DME (top) and the
Referring to the traditional prelithiation process, Cao et al. reported a liquid-phase immersion presodiation method, as shown in Figure 5C[81]. To finish the presodiation process, a Na2Ti6O13 cathode was submerged into the stable liquid Na-Naph-DME for 10 min, followed by rinsing with a DME solution. As a result, the initial Coulombic efficiency of Na2Ti6O13 in the half cell is significantly boosted to 100% from 65%. The presodiation treatment could raise the initial efficiency from 40% to 80% in a Na3V2(PO4)3//Na2Ti6O13 full cell and the electrode after presodiation still exhibited high rate capability and cycle performance. To raise the initial Coulombic efficiency of commercial HC, Liu et al. developed a feasible and efficient chemical presodiation method, in which the HC anode was submerged into a DME solution containing Na-Bp and the presodiation level could be carefully regulated by varying the immersion time [Figure 5D][30]. The presodiated HC anode shows a dramatically increased initial Coulombic efficiency by 30%, originating from the provided extra Na sources by presodiation treatment. The Na3V2(PO4)3//NaxHC full cell demonstrates a significantly improved energy density and capacity retention using this presodiated HC anode.
The chemical presodiation strategy can easily regulate the presodiation degree by changing the soaking time and Na+ concentration in the solution. Compared with Na metal, the safety of liquid sodium sources is significantly improved, which can remain safe even in harsh conditions with water.
Electrochemical presodiation
The electrochemical presodiation involves two steps of assembling and disassembling the half cell[43]. Firstly, the anode is assembled with Na metal in a half cell and then pre-cycled to generate the stable SEI film on the anode surface before disassembling. During electrochemical presodiation, the current density should be sufficiently low to ensure the integrity and uniformity of the SEI film. The detailed electrochemical presodiation process is given in Figure 6A[82]. By assembling a Na//PH5 (or Na//HC) half cell, the PH5 and HC are both successfully presodiated during the first discharge process. Consequently, the full cell
Figure 6. (A) Schematic illustration of electrochemical presodiation of PH5[82]. (B) Scheme of voltage-driven presodiation process of Sb@ZMF/C anode and full cell configuration[83]. (C) Charge-discharge voltage profiles of Na-Sb@ZMF/C||NaVPO4F model after presodiation (left) and specific capacity and Coulombic efficiencies of Na-Sb@ZMF/C||NaVPO4F, Na-Cu||NaVPO4F and Na||NaVPO4F full cells at 0.5 C (right)[83].
CONCLUSIONS AND OUTLOOK
Sodium-based energy storage devices provide a highly economic, efficient and sustainable alternative for large-scale electrochemical energy storage systems. However, many challenges are remaining towards further commercialization and industrialization, such as the low initial Coulombic efficiency and unsatisfactory energy density. The presodiation technique is considered as an effective method to alleviate the above issue, not only compensating for irreversible Na+ depletion but also facilitating the energy density, rate performance and cycle lifespan. The presodiation by introducing self-sacrificing Na-containing additives for the cathode is seen to be a simple process without any complex operation. However, the introduction of Na-containing additives increases the weight of SIBs, causing the reduction of energy density and additional reactions. Unavoidably, the electrochemical oxidation of sacrificial reagents will generate gases or solid byproducts, which will reduce the battery system security or affect the electrochemical performance. How to alleviate the adverse consequences induced by the above issues will be the focus of future research.
In comparison, self-presodiation cathode materials are regarded as superior materials due to their “zero dead mass” and lack of gas release during the electrochemical process. Notably, the self-presodiation method is strongly associated with the development of high-performance Na-rich cathodes. In addition to presodiation for cathodes, presodiation for anodes has also attracted significant attention. Physical presodiation based on direct contact with Na foil/powder is the most direct method but the handling of high-risk Na foil/powder limits the industrialization of this method. In contrast, chemical presodiation technique offers greater potential for application in the manufacture of commercial electrodes because of the high feasibility. The presodiation reagent involves a THF or DME solution containing Na-Naph/Na-Bp, which can maintain its stability in dry air. The Na storage mechanism during the chemical presodiation is different from that during the electrochemical cycle, which may result in an additional side reaction during the following electrochemical cycles in the full cell. Furthermore, the anion type in the presodiation solution may also influence the formation of SEI film, which is necessary for further study. Different from chemical presodiation, electrochemical presodiation by precycling in a half cell can make the anode presodiated in real cell conditions. The Na storage mechanism and SEI film are in accordance with those in the normal electrochemical process. It is easy to regulate the presodiation degree by controlling the cut-off voltage during discharge. The greatest challenge is the complex procedure, including assembling the half cells, disassembling the half cells and reconstructing the full cells, which is unfeasible for industrialization.
Although presodiation technology has been extensively investigated, there remain significant issues that need to be resolved urgently, as shown in Table 1. In particular, the underlying mechanics of various presodiation methods are still mysterious and need further investigation. In-situ characterization methods, including in-situ XRD, spectroscopy, and TEM, need to be applied during the first charge and discharge to understand the aforementioned mechanism. In addition, whether there is a difference between the conventional SEI film and the SEI film formed after presodiation needs to be systematically evaluated, especially considering the morphology and composition of the SEI film. As powerful tools, theoretical calculations should be used to analyze the presodiation process, which can reveal the presodiation mechanism from the electronic and atomic scales. To comprehend and grasp such crucial factors, in-depth research should be conducted to promote the further development of Na-based energy storage devices.
Comparison of different presodiation strategies and possible research directions
Side | Method | Disadvantage | Research direction |
Cathode | Self-sacrificed materials | Residual materials, gas release | Presodiation mechanism In-situ characterization Theoretical calculation New self-presodiation cathode design |
Self-presodiation | Limited materials | ||
Anode | Direct contact | Dangerous | |
Chemical presodiation | Air-sensitive, complex | ||
Electrochemical presodiation | Dangerous, disassembly |
Overall, the current presodiation technique for SIBs is still in its infancy due to it being quite different from that of LIBs and therefore requires further exploration to pave the route from basic scientific research to industrialization. The fundamental issues, such as the Na storage mechanism and SEI formation process during chemical presodiation, should be intrinsically addressed, which benefits the development of presodiation technique. This review provides feasible principles and strategies of presodiation to help researchers to gain a comprehensive understanding of the presodiation process.
DECLARATIONS
Authors’ contributionsConceived the idea, designed the manuscript: Gao XW
Prepared most figures: Liu ZM, Lai QS, Chen H
Wrote the paper: Mu JJ, Gao XW, Wang D, Yang DR
All authors participated in the writing and revision and commented on the manuscript.
Availability of data and materialsNot applicable.
Financial support and sponsorshipThis work was supported by the National Natural Science Foundation of China (Grant No.52272194 and 52204308), LiaoNing Revitalization Talents Program (No. XLYC2007155), the Fundamental Research Funds for the Central Universities (N2025018, N2025009), China Postdoctoral Science Foundation (2022M710639).
Conflicts of interestAll authors declared that there are no conflicts of interest.
Ethical approval and consent to participateNot applicable.
Consent for publicationNot applicable.
Copyright© The Author(s) 2022.
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How to Cite
Mu, J. J.; Liu, Z. M.; Lai, Q. S.; Wang, D.; Gao, X. W.; Yang, D. R.; Chen, H.; Luo, W. B. An industrial pathway to emerging presodiation strategies for increasing the reversible ions in sodium-ion batteries and capacitors. Energy Mater. 2022, 2, 200043. http://dx.doi.org/10.20517/energymater.2022.57
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