2020-03-05 11:31:27
Lingzhu Zhaoa, Jingchuan Fua, Zhi Dua, Xiaobo Jiaa, Yanyu Qua, Feng Yua,b, Jie Du
1.Introduction
Cellulose powders (Aladdin, 90μm), PEG (600 g mol−1), sodium hydroxide (NaOH, Xilong Scientific, AR), urea (Aladdin, AR), epi- chlorohydrin (ECH, Aladdin, AR), polyvinylidene fluoride (PVDF, Solvay, battery grade), N-methyl-2-pyrrolidone (NMP, Aladdin, GC) and Ketjen black carbon (Akzo Nobel N·V, battery grade) were com- mercially obtained. Lithium ion batteries (LIBs) with higher energy and power density are highly advisable energy sources due to the growing demand for portable electronics in recent years [1,2]. Lithium metal, offering higher theoretical specific capacity (3860 mAh g−1) and lower redox potential (−3.04 V vs SHE) than graphite, is rated to be an ideal al- ternative anode material for the higher energy density. However, the formation and the growth of undesired lithium dendrites could be hardly inhibited by traditional liquid electrolyte during repetitive charge/discharge cycles, so the practical usage of lithium metal anode has been limited by lithium dendrites [3,4]. For the traditional liquid lithium ion batteries, the separator could be ultimately pierced by the uneven deposition and lithium dendrite formation, which results in cell internal short circuits and a series of serious safety problems including thermal runaway and explosion.
The research and application of the solid polymer electrolyte (SPE) can not only avoid these issues, but also improve the safety performance of the battery [7]. So far, SPE has been proved to be an effective substitution for the liquid electrolyte to suppress the lithium dendrite growth because of the excellent electrochemical stability with lithium metal and good mechanical strength of SPE [6]. Nevertheless, the low ionic conductivity under ambient temperature and the poor interfacial compatibility with electrodes are the big drawbacks of SPE, which hinders its practical application [7,8]. By contrast, a gel polymer electrolyte which is prepared by plasticizing the SPE with liquid electrolyte, combines the advantages of both liquid electrolytes and SPE. The liquid electrolytes entrapped in GPE are beneficial to enhance the interface stability of electrode/electrolyte, leading to relatively higher ionic conductivity and lower interface resistance under room tem- perature compared with SPE [8,9]. Unfortunately, the gelled polymer matrices always suffer from inferior mechanical strength [10]. For ex- ample, Poly (ethylene oxide) (PEO) as well as its derivatives have been investigated systematically as the promising host materials of GPEs because of the coordination and dissociation interaction between ethylene oxide (EO) and lithium ions [11–13]. But PEO-based GPE has a labile structure and poor mechanical properties. Therefore, the poor mechanical strength of GPEs is the big obstacle to restrain the lithium dendrite.
In order to improve the mechanical properties and the thermal stability of GPE, some researchers utilize electrospinning technology or chemical crosslinking method to fabricate GPE materials [14–17]. For instance, Xiaoyuan Yu research group has prepared a gel polymer electrolyte based on poly (vinylidene fluoride)/poly (propylene carbo- nate) (PVdF/PPC) by electrospinning technology. The GPE showed good mechanical property and high ionic conductivity of 4.05 × 10−3 S cm−1. Nevertheless, the extensive energy consumption and exceeding low-production prevent the practical commercial applications of this approach in LIBs. In recent years, Dong Xu et al. have designed a 3D cross-linked chitosan-poly (ethylene glycol)- based GPE by a facile and eco-friendly process. The prepared gel polymer electrolyte showed developed mechanical strength (5.5 MPa) [19]. Even though this GPE owned an admirable lithium ion transfer number (0.869), the ionic conductivity (2.74 × 10−4 S cm−1) at 25 °C in this work was relatively lower compared with other GPEs. In order to further meliorate the mechanical property and ionic conductivity of GPEs, they also prepared a special gel polymer electrolyte based on internally crosslinked and freeze-dried bacterial cellulose network with high strength [20]. The designed gel polymer electrolyte shared pre- ferable mechanical strength (49.9 MPa) and ionic conductivity at 25 °C (4.04 × 10−3 S cm−1) which is about ten times higher than that of chitosan-based GPE. Therefore, seeking a crosslinked polymer network as the matrix of GPE combined with good mechanical properties and high comprehensive performance for lithium ion batteries is an efficient strategy to promote the practical application of GPEs in the field of Liion battery.
Cellulose, the most abundant naturally macromolecule, is renewable, biodegradable, and affordable [21,22]_ENREF_13. The strong in- tramolecular and intermolecular hydrogen bonds give cellulose good thermal stability and mechanical property. At the same time, it was reported that cellulose has the ability to dissociate lithium salts, adsorb and retain the organic solvents, and also accelerate the migration of lithium ions [23,24]_ENREF_22. Polyethylene glycol (PEG), a flexible linear molecular chain comprised of numerous repetitive ether groups that is similar with the structure of PEO, is beneficial to promote the movement of lithium ions by continually coordination and dissociation interaction between ether groups and Li+. Thus, in this research, we prepared a cellulose/PEG composite GPE via one-step crosslinking method. In this work, PEG is expected to further improve the strength of cellulose membrane depending on the hydrogen bond interaction be- tween cellulose and PEG and meanwhile further promote the migration of lithium ions.
2.Experimental
2.1.Materials
Cellulose powders (Aladdin, 90μm), PEG (600 g mol−1), sodium hydroxide (NaOH, Xilong Scientific, AR), urea (Aladdin, AR), epi- chlorohydrin (ECH, Aladdin, AR), polyvinylidene fluoride (PVDF, Solvay, battery grade), N-methyl-2-pyrrolidone (NMP, Aladdin, GC) and Ketjen black carbon (Akzo Nobel N·V, battery grade) were com- mercially obtained. The liquid electrolyte was 1 M lithium bis (tri- fluoromethane sulfonyl) imide (LiTFSI, Aladdin)/sulfoxide (DMSO, Aladdin), which was prepared and stored in the argon glove box (moisture level < 1ppm).
2.2.Preparation methods
2.2.1.Preparation of cellulose/PEG composite membranes
The numerous hydrogen bonds can form close packing and the rigid molecular chains in bulk cellulose, thereby, the existence of strong self- aggregation forces makes the dissolution of cellulose an extremely hard process. Profiting from the cellulose alkali/urea aqueous solvent-system of Zhang research group [25,26], a cellulose solution (4.5wt %) was prepared by dissolving cellulose powders into a pre-cooled 7wt % NaOH/12wt% urea aqueous solution with stirring under room tem- perature. Then, air bubbles and the slightly remaining undissolved cellulose powders were removed via 5 min of centrifugation at 8000 rpm at 25 °C. Finally, clear cellulose solution was obtained. PEG with the various mass percentages (2.5%, 5%, 10%, 15% and 20%) was mixed with the cellulose solution to obtain a cellulose/PEG composite solution. Certain amounts of epichlorohydrin (ECH) were added to the mixed solution (1:20, V/V) as a crosslinking agent. Keep stirring for 30 min at ambient temperature. Then, the obtained sticky solution was decanted into molds and kept at 50 °C for 2 h to gelation. The obtained chemically cross-linked cellulose/PEG gels were immersed into DI water to wash and remove the remaining alkaline liquid. Finally, the gels were dried at 50 °C in drying oven to get cellulose/PEG membrane. The prepared composite membranes with different PEG mass percen- tages were named as CP-1, CP-2, CP-3, CP-4 and CP-5 respectively.
2.2.2.Preparation of cellulose/PEG gel polymer electrolyte
The obtained CP membranes were poked into circular slices (D/ R = 16mm/0.5 mm), and immediately immersed in the liquid electro- lyte of the Ar-filled glove box (moisture level < 1ppm) after disposing at 110 °C for 1 h by vacuum. The achieved GPEs were named as GCP-1, GCP-2, GCP-3, GCP-4 and GCP-5 and then used for further characterization.
2.3. The battery assembly
The CR-2032-coin cells were sealed in this work by installing the as- obtained GPE (T = 0.9 ± 0.1 mm) in the middle of a working elec- trode (NCM523) and a reference electrode (Li) in a glove-box. Herein, the ternary material NCM523 (LiNi0·5Co0·2Mn0·3O2) as cathode was synthesized in our lab [27]. The cathode piece was conducted through mixing evenly the NCM523, KB and PVDF by mass ratio of 8: 1: 1. The uniform slurry was smeared on a sheet of aluminum foil then dried under 80 °C for 4h. The coated aluminum foil was poked as discs (diameter 10 mm) and further dried by vacuum oven under 110 °C for 12 h for the cell assembly. The typical loadings of active material are 2–3 mg cm−2 in the cathode plate.
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