Nickel-Rich Cathode Precursor Synthesis By Taylor Vortex Reactor

Although earlier adoption of continuous stirred tank reactors (CSTRs) were successfully employed in the synthesis of cathode precursor to day; there are still engineering challenges with the CSTRs, which makes several manufacturers to seek for alternative reactor systems. Typically, the CSTRs are modified (and still being modified based on the requirement of application) in order to overcome the common issues like: low reproducibility, product efficiency, very long stabilization times due to low mass transfer rate, hard to maintain the stability of the co-precipitation system, particle over growth by time and, etc. Here, we report an advanced manufacturing system, Taylor Vortex Reactor (TVR), for the cathode precursor synthesis, which overcomes many complexities encountered in CSTRs. The talk will discuss the scalability of TVR as an alternative way of manufacturing cathode precursors and the outcomes of different scales will be compared. Acknowledgement Funding for this work from the Office of Vehicle Technologies of the U.S. Department of Energy, Office of Energy Efficiency and Renewable Energy, is gratefully acknowledged. The submitted abstract has been created by UChicago Argonne, LLC, Operator of Argonne National Laboratory (“Argonne”). Argonne, a U.S. Department of Energy Office of Science laboratory, is operated under Contract No. DE-AC02-06CH11357.

Layered Ni-rich cathode material, Li[NixMnyCo1−x−y]O2 (x ≥ 0.8), is one of the most prospective materials for rechargeable lithium-ion batteries (LIBs) due to its high capacity. However, significant challenges remain in order to improve capacity retention during cycling and thermal-abuse tolerance of this material. As one of the promising approaches to overcome barriers, a series of core-shell structured cathode materials with the overall bulk composition of LiNi0.8Mn0.1Co0.1O2 is produced via co-precipitation method where Ni-rich composition (LiNi0.9Mn0.05Co0.05O2) with higher capacity is particle core and Mn-rich composition with higher stability is particle surface. It is challenging to design and implement heterogeneous structured particles with synergistic effects by combining the advantages of each composition. It is particularly important to develop a process of producing economically and quickly each type of these cathode particles, in which the Ni-rich composition and the Mn-rich composition change continuously or discretely from the particle core to the particle surface. To achieve this goal, a continuous rapid synthesis process for the production of heterogeneous structured cathodes was developed at ANL MERF based on an advanced Continuous Stirred Tank Reactor (CSTR) system and a Taylor Vortex Reactor (TVR) system. A detailed description of the developed process to mass-produce heterogeneous structured materials economically and rapidly will be presented. The excellent physical and electrochemical properties of Ni-rich NMC cathodes with core-shell or core-gradient particle structures produced by this advanced process will be reported. The produced heterogeneous structured cathodes and commercially available normal NMC materials will be compared through analysis of coin half cell, pouch full cell, SEM, EDS, ICP-MS, DSC, EIS, and other advanced characterization techniques.

Lithium ion batteries have been utilized in a wide range of applications. On-going research and development efforts are expanding the application of these materials for use in electric vehicles and household energy storage solutions. Much of these efforts have focused on improving the performance of lithium ion battery materials through achieving alterations to the composition of the cathode material, which has been seen as the limiting factor in terms of capacity and overall battery lifetime. For example, LiNi1/3Mn1/3Co1/3O2 (often referred to as NMC 111) is becoming a material of focus for commercial-scale production. A significant challenge in synthesizing this material is the propensity for Ni/Li based cation mixing in the octahedral sites of the product. While several studies have correlated the synthetic and processing methods with observations for cation mixing and electrochemical performance of the final material, these studies have not performed an in-depth analysis of the cation mixing phenomenon in situ on a mechanistic level. A detailed investigation is presented on the correlations between the processing conditions (e.g., thermal and compositional) for NMC 111 using a pre-lithiated precursor material. The relationship between cation mixing, sintering temperature and sintering time, as well as potential methods for the reversal of cation mixing were investigated through the use of in situ, variable temperature XRD methods. The importance of this knowledge and determining the ideal processing conditions for NMC 111 (and by extension, cathode materials in general) is further demonstrated through a final analysis of the quality of Li+ distribution in these materials as assessed by microscopy techniques and electrochemical coin cell tests.

The demand of rechargeable batteries had increased significantly every year during the last decade, driven for the needs associated with technological development (portability, high performance of electronic devices and vehicles). Lithium ion battery is a device of mayor consumption, and it is designed for energy storage and conversion based on intercalation electrodes. Nowadays the efforts are directed to the improvement and replacement of current battery components: anode, cathode (LiCoO2) electrolyte, with materials that have higher efficiency in terms of energy, power, cost, reliability, life time and safety. In recent years there has been significant interest in polyanion-based active materials as safe alternatives for the traditional oxide cathodes. For example, phosphate phases such as LiFePO4 [1], Li3V2(PO4)3, [2], Li2.5V2(PO4)3, [3], LiVOPO4, [4,5] and LiVP2O7[6] have all been proposed. Therefore, the search of new cathode materials is an important task for researchers in materials science. The possibility of using sodium directly in lithium ion cells allows the study of new compositions and structures. In this research work a series of four compounds with formula Na3V2-xAlx(PO4)2F3 (x= 0, 0.02, 0.05, 0.1) were prepared, characterized and applied as cathode materials in lithium ion batteries. These materials were synthesized by sol-gel Pechini method. Aqueous solutions containing appropriate amounts of NH4VO3, NH4H2PO4 and NaF were poured into a mixture of citric acid and ethylene glycol solution. Mixture was then heat treated under reflux at 80°C until gel formation. Fresh samples were heated at 300°C under air to eliminate volatile matter. Resulting powders were grinded and formed into pellets for reaction between 300 to 650°C under nitrogen atmosphere. Thermal stability of materials was evaluated by simultaneous termogravimetric and differential analysis (TGA-DTA). Morphological and microstructural characterization were carried out with field emission scanning electron microscopy (FESEM), textural analysis by N2 physisorption with BET method; chemical composition and crystallographic parameters were determined with Induced coupled plasma – optic emission spectroscopy (ICP-OES), energy dispersive X-ray spectroscopy (EDXS) and X-ray powder diffraction (XRD); the application of materials as cathodes in lithium ion batteries was evaluated through electrochemical charge discharge experiments. Electrodes were prepared using a mixture of each synthesized materials, conductive carbon and PVDF binder. CR2032 coin cells were assembled inside a glove box under Ar atmosphere, using LiPF6electrolyte and Li° as anode. Experiments were performed using a MacPile II by Biologic. Thermal analysis of sol-gel reaction products exhibited an exothermic even between 550 and 750°C attributed to the crystallization of the fluorophosphates. Results from XRD analysis showed that Al doped Na3V2(PO4)2F3 crystalline phase was formed at 650°C for 8h. According to cell parameters Na3V2(PO4)2F3 can incorporate aluminum content up to x=0.1, without the presence of secondary phases or structural transitions. Granular morphology and small particles size of about 40 to 100 nm were observed, this can be attributed to the effect of residual carbon within samples (8% by weight) since this inhibits particle grown and also allows contact among particles, improving electrical conductivity. Materials present average porous size of about 20nm, with surface area of 30m2/g. The sample with x=0.05 of Aluminum content, presents the best textural properties. This material also presents high specific charge/discharge capacity (123/101 mAh/g at a 4.4 V vs Li cell) and good capacity retention (82%), in comparison to the material without doping (128/63 mAh/g and 49% of capacity retention). Aluminum doping of Na3V2(PO4)2F3phase permitted the stabilization of the structure related to cycling processes. These results are promising for future application of the material in lithium and sodium ion batteries. Keywords: Pechini, cathodes, phosphates, lithium ion batteries References [1] A.K. Padhi, K.S. Nanjundaswamy, C. Masquelier, J.B. Goodenough, J. Electrochem. Soc. 144 (1997) 2581. [2] M.Y. Saidi, J. Barker, H. Huang, J.L. Swoyer, G. Adamson, Electrochem. Solid-State Lett. 5 (2002) A149. [3] C. Yin, H. Grondey, P. Strobel, L.F. Nazar, Chem. Mater. 16 (2004) 1456. [4] B.M. Azmi, T. Ishihara, H. Nishiguchi, Yusaku Takita, J. Power Sources 146 (1–2) (2005). [5] J. Gaubicher, T. Le Mercier, Y. Chabre, J. Angenault, M. Quarton, J. Electrochem. Soc. 146 (1999) 4375. [6] J. Barker, R.K.B. Gover, P. Burns, A. Bryan, Electrochem. Solid-State Lett. 8 (9) (2005) 446.

Antimony oxychloride/graphene aerogel composite as anode material for sodium and lithium ion batteries

Nowadays, Lithium ion batteries (LIBs) can be found in every corner of our daily life. However, safety and cost of lithium ion batteries are the two major issues. Aqueous rechargeable lithium ion batteries are believed to be the promising candidates for LIBs due to nonflammable，low cost higher ionic conductivity of aqueous electrolyte [1]. To reduce the cost of aqueous lithium-ion cells, researchers focus on developing methods to synthesize electrode material in an energy efficient way. It has been reported that TiP2O7 has a low intercalation /de-intercalation potential (2.6 V versus Li/Li+) [2], which makes it a promising anode material for aqueous lithium-ion batteries [3,4]. One report demonstrated a solid-state synthesis method annealing at 300◦C for 2 hours, annealing at 800◦C for 3 hours and cooling to room temperature for 4 hours [5]. The solid-state synthesis route is very common in industrial applications due to its simplicity. However, the long calcining duration and high temperature requirement increases the processing cost for the electrode materials. One report applied microwave to synthesize C-NaTi2(PO4)2, the negative electrode for aqueous sodium ion batteries [6]. Functional electrode materials can be synthesized in less than 20 minutes. In this work, a very fast microwave synthesis method was developed to produce C-TiP2O7 (Carbon and TiP2O7 Composite material). The precursor consists of (NH4)2HPO4 and anatase TiO2 in a molar ratio of 2:1, with 10wt%, 15wt% and 20wt%(the weight percent is relative to the precursor mixture) graphite added. After being ball milled together for 1 hour, the mixture was heated in a microwave oven (CEM Discover Proteomics System) for 10 minutes at 150W. The SEM figure shows the surface of Graphite-TiP2O7 composite, and the particle size of Graphite-TiP2O7 composite is around 40nm (Figure 1a). In XRD test (Figure 1b), the pattern of product matches with the reference pattern (JCPDS #38-1468) at major peaks (511), (600), (630), (721), (660), (933). The products we get from this method are tested in cyclic voltammetry tests, which shows promising electrochemical performance (Figure 2a); after ten cycles, the specific capacity of 10% Graphite-TiP2O7 composite maintains 107.4 mAh/g. (Figure 2b). Figure 1 a) SEM of Graphite-TiP2O7 composite. B) XRD patterns of Graphite-TiP2O7 composite and reference peaks. Figure 2 a) Second cycles of cyclic voltammetry curves of 10% Graphite-TiP2O7 composite, 15% Graphite-TiP2O7 composite and 20% Graphite-TiP2O7 composite in 1 M Li2SO4 at scan rate 0.5 mV/s in range of −0.5 V and −1.6 V versus MSE. b) Discharge cycling performance of Graphite-TiP2O7 composite. The total synthesis time is only 10 minutes for heating and 30 minutes for cooling, which is much less than for traditional solid state synthetic methods. Reference: Kim H, Hong J, Park K Y, et al. Aqueous Rechargeable Li and Na Ion Batteries[J]. Chemical Reviews, 2014, 114(23):11788.Aravindan V, Reddy M V, Madhavi S, et al. Hybrid supercapacitor with nano-TiP2O7, as intercalation electrode[J]. Journal of Power Sources, 2011, 196(20):8850-8854.Wang H, Huang K, Zeng Y, et al. Electrochemical properties of TiP2O7, and LiTi2(PO4)3, as anode material for lithium ion battery with aqueous solution electrolyte[J]. Electrochemical Acta, 2007, 52(9):3280-3285.Rai A K, Gim J, Song J, et al. Electrochemical and safety characteristics of TiP2O7 –graphene nanocomposite anode for rechargeable lithium-ion batteries[J]. Electrochemical Acta, 2012, 75(4):247-253.Wu W, Shanbhag S, Wise A, et al. High Performance TiP2O7 Based Intercalation Negative Electrode for Aqueous Lithium-Ion Batteries via a Facile Synthetic Route[J]. Journal of the Electrochemical Society, 2015, 162(9): A1921-A1926.Wu W, Mohamed A, Whitacre J F. Microwave Synthesized NaTi2(PO4)3 as an Aqueous Sodium-Ion Negative Electrode[J]. Journal of the Electrochemical Society, 2013, 160(3): A497-A504. Figure 1

Thanks to the promotion of new energy vehicles, the industry of lithium-ion batteries has ushered in its booming period. The current industry of lithium ion batteries is in rapid development with great potential. Therefore, many researchers have turned to focus on lithium ion batteries to obtain better lithium ion batteries. In this paper, the literature review of cathode materials for lithium ion batteries is to be carried out from the following aspects, including the overview of lithium ion batteries, their basic performance indexes, and the classification and preparation methods of cathode materials. Besides, the present situation and modification strategies of cathode materials for lithium ion batteries will be further analyzed, so as to improve their electrochemical performance.

Natural graphite (NG) has been attracted as a promising anode material for lithium ion batteries due to its appropriate charge/discharge profile, high reversible capacity and low cost. However, high irreversible capacity and low capacity retention at first cycle have influenced on its practical use. Although low cost is the main advantage of natural graphite, the material cost of natural graphite should be reduced further in order to be used for electric vehicles (EVs) and energy saving systems (ESS). Generally, pristine natural graphite contains various impurities such as Al, Fe, and Si. For commercial use, pristine natural graphite should be refined since the impurities would have a negative effect on both electrolyte and electrode of lithium ion batteries. The purity grade of natural graphite can be classified based on the purification process. As the requirement for high purity increases, more purification steps are needed, resulting in high manufacturing cost. Therefore, the main issue for the application of natural graphite as an anode active material is to use low-purity natural graphite with purification process as less as possible. In this regard, effect of Fe as impurity on the electrochemical performance of the low-purity natural graphite as anode active material for lithium ion batteries was investigated in this study. Natural graphite powders with 5 wt% Fe (05Fe) and 10 wt% (10Fe) were synthesized by combustion method from the raw materials of Fe(III)(NO3)3 9H2O (Alfa Aesar) and high-purity spherical natural graphite (POSCO CHEMTECH) by calcination at 500 °C in air atmosphere. The morphology of the natural graphite powders was observed by scanning electron microscopy (SEM, JSM-5900, JEOL, Japan). The particle size of each powder was measured by a dynamic light scattering method (ELS 6000 zeta potential and particle size analyzer, Otsuka Electronics, Japan). Powder X-ray diffraction (XRD, MAX-2500, RIGAKU, Japan) analysis was conducted using Cu Kα radiation with a wavelength λ = 1.5406 Å. The crystallite sizes (La and Lc) were calculated on the basis of the d002XRD lines by application of the Scherrer’s equation. The crystallinity of the natural graphite powders was investigated by Raman spectroscopy (LabRAM, Horiba Jobin-Yvon, Japan). The concentrations of impurities in the natural graphite were determined by an inductively coupled plasma atomic emission spectrophotometer (ICP-AES). A working electrode paste was fabricated from a mixture of natural graphite with a binder consisting of carboxymethylcellulose (CMC)/styrene-butadiene rubber (SBR) and carbon black (Super-p) as a conductive agent dissolved in D.I. water. The weight ratio of graphite to binder (CMC:SBR:Super-p=2:2:1) was 95:2:2:1. The prepared paste was coated onto 10㎛ Cu foil by using a doctor blade and then dried under vacuum at 120 °C for 12 h. Electrochemical performance was evaluated using CR2032 coin-type cells with a 20 μm thick Cellgard 2300 porous membrane separator and 1 M LiPF6-EC/DMC (1:1 in volume ratio) electrolyte. Lithium metal foil was used as a counter electrode. All of the samples studied in this work were treated by sphericalization and the sphericalized natural graphite maintained a spherical shape after the calcination process at 500 °C for 4 h. All the samples have both hexagonal and rhombohedral phases which are the typical structure of natural graphite. Fe2O3 peaks (JCPDS card #33-0664) were indexed at 2θ = 33.1°, 35.6°, 62.4°, and 63.9°, respectively. The most of Fe2O3particles were located on a surface of natural graphite, based on the EDX mapping and back-scattered electron (BSE) images. The irreversible capacity during the charge-discharge reactions increased with increasing the Fe content. However, the cycle retention of the 05Fe, 10Fe, and NG are comparable. Therefore, it may be possible to use unrefined natural graphite as an anode active material for lithium-ion rechargeable batteries.

Aqueous rechargeable lithium ion batteries (ARLBs) are the promising candidates for long term energy storage [1]. TiP2O7 has been reported as a promising anode material for ARLBs due to its appealing and stable intercalation/deintercalation potential, [2,3]. Today, a traditional solid-state synthesis method has been reported to synthesize TiP2O7, which takes about 9 hours [4]. In previous work, a fast microwave synthesis method was applied to synthesize TiP2O7, which takes only 40 minutes [5]. The idea was informed by the report about microwave synthesis of NaTi2(PO4)2, which is an aqueous sodium ion batteries anode material [6]. In this work, more complete material characterizations and long-cycle tests have been conducted for both of 10% graphite-TiP2O7 composite and pure TiP2O7 electrode materials as prepared previously [5]. Figure 1a presents the X-ray diffraction patterns of graphite-TiP2O7 composite and pure TiP2O7, from which it can be demonstrated that crystalline TiP2O7 and graphite-TiP2O7 composite are produced. The Scherrer formula is used to calculate average crystal size of graphite-TiP2O7 composite and pure TiP2O7., which are 46.9nm and 37.4nm respectively. Figure 1b shows the surface morphology of pure TiP2O7 (top) and graphite-coated TiP2O7 composite (bottom)respectively. The surface of carbon coated TiP2O7 is much smoother than pure TiP2O7, which indicates graphite layer is coated and it may protect TiP2O7’s structure against dissolution during cycling. Figure 2a is the thermogravimetric analysis (TGA) of graphite-TiP2O7 composite, which shows 82.3% of active material exists in the composite. Figure 2b presents the stability of graphite-TiP2O7 composite under the rate of 0.5C. It also demonstrates that after coated with graphite, the electrode material gives much better electrochemical performance. Carbon coating is essential for electrode material synthesized through microwave method, which stabilized the material’s structure for better electrochemical performance. Figure 1 a) XRD patterns and b) SEM of Graphite-TiP2O7 composite and Pure TiP2O7. Figure 2 a) Thermogravimetric analysis of Graphite-TiP2O7 composite. b) Long-cycle tests on Graphite-TiP2O7 composite and Pure TiP2O7. Reference: Li W , Dahn J R , Wainwright D S . Rechargeable Lithium Batteries with Aqueous Electrolytes[J]. Science, 1994, 264(5162):1115-1118.Wang H, Huang K, Zeng Y, et al. Electrochemical properties of TiP2O7, and LiTi2(PO4)3, as anode material for lithium ion battery with aqueous solution electrolyte[J]. Electrochemical Acta, 2007, 52(9):3280-3285.Chen L , Gu Q , Zhou X , et al. New-concept Batteries Based on Aqueous Li+/Na+ Mixed-ion Electrolytes[J]. Scientific Reports, 2013, 3(6):1946.Wu W, Shanbhag S, Wise A, et al. High Performance TiP2O7 Based Intercalation Negative Electrode for Aqueous Lithium-Ion Batteries via a Facile Synthetic Route[J]. Journal of the Electrochemical Society, 2015, 162(9): A1921-A1926.Haosheng Song, Jiang Chang, Jinming Wu, Wei Wu, Jay Whitacre. Microwave Synthesized TiP2O7/Carbon Composites for Use in Aqueous Lithium-Ion Batteries. The Electrochemical Society - Meeting s, 13 Apr 2018, pp. 507.Wu W, Mohamed A, Whitacre J F. Microwave Synthesized NaTi2(PO4)3 as an Aqueous Sodium-Ion Negative Electrode[J]. Journal of the Electrochemical Society, 2013, 160(3): A497-A504. Figure 1

In this work, precursor for Li1.14Mn0.53Ni0.28Co0.19Oylayered-layered spinel cathode material was synthesized by carbonate co-precipitation method using a Taylor Vortex reactor. In a similar fashion, we also utilize a 20L continuous stirred tank reactor (CSTR) to produce and compare the cathode materials with same composition. Recently, layered-layered spinel structures are explored to mitigate the voltage fade issue to some extent. Even though these materials deliver lower capacities than the Li- and Mn- rich (LMR-NMC) materials, they have the key feature of “spinel induced” structures which make the voltage fade relatively less compared to LMR-NMC materials. Here, by adopting Taylor Vortex reactor, we demonstrate that the usage of Taylor Vortex Flow shows good advantages to produce highly crystalline, spherical and dense cathode precursors in a relatively short residence time compared to CSTR. The particle size and distribution of the synthesized cathode powders are analyzed using particle size analyzer (PSA) and are confirmed with scanning electron microscopy (SEM). The composition and the phase determination of the cathode materials are characterized by inductively coupled plasma mass spectroscopy (ICP-MS) and X-ray diffraction (XRD). These cathode materials were electrochemically tested using Voltage Fade protocol of Argonne National Laboratory.

The improvement in energy density of lithium ion batteries (LIBs) is primarily focused on the increase of the specific capacity of active materials and the cell voltage.[1] Transition metal (TM) oxide-based cathodes materials reach a high specific capacity through the optimization of the chemical composition with a higher Ni content and can be cycled up to 4.6 V.[2] However, the electrochemical performance of Ni-rich cathode materials depends strongly on their physical properties such as particle size, specific surface area or surface characteristics. The poor rate capability and capacity retention as well as the high first cycle irreversible capacity loss (ICL) and the low volumetric energy density of electrodes have to be improved by specific design of the particle shape. A spherical morphology with a narrow size distribution is the preferred particle shape and can only be synthesized during the co-precipitation of TM-hydroxides or -carbonates by a continuously stirred tank reactor (CSTR). Additionally, the CSTR-process allows a further improvement of the cathode materials during the synthesis of core-shell and full concentration-gradient particles.[2] In this work, the design and the operating principle of a novel Couette-Taylor-Flow-Reactor (CTFR) is evaluated regarding the synthesis of spherical shaped Ni-rich TM-precursors. The CTFR offers a continuous process and is constructed by two co‐axial arranged cylinders with a small gap and a low working volume. The rotational motion of the inner cylinder induces a turbulent Taylor‐vortex flow. Above the suitable Taylor number (Ta), a periodic and stable turbulent fluid motion is formed, which increases the fluid shear and the local concentration of educts and promotes the agglomeration of precipitates to uniform spherical particles with narrow particle size distribution.[3] Based on the co-precipitation of Ni-rich TM-precursors by a continuous CTFR, the influence of the reaction conditions on the properties of TM-precursor is investigated. The rotational speed, residence time, temperature and pH-value were varied in a broad range. The growth behavior of the particles, regarding the morphology, particle size distribution, tap density and chemical composition of TM-precursors as well as for lithiated cathode materials are investigated. The electrochemical properties of the corresponding cathode materials with their unique particle morphology in dependence of the co-precipitation conditions are comprehensively evaluated for finding the optimal synthesis conditions. [1] J. Betz, G. Bieker, P. Meister, T. Placke, M. Winter, R. Schmuch, Adv. Energy Mater. 2018, 1803170/1-18.[2] H. Li, P. Zhou, F. Liu, H. Li F. Cheng, J. Chen, Chem. Sci, DOI: 10.1039/c8sc03385d.[3] J.-M. Kim, S.-M. Chang, J.-H. Chang, W.-S- Kim, Colloids and Surfaces A: Physicochem. Eng. Aspects (2011) 384, 31-39.

Biomass carbon micro/nano-structures derived from ramie fibers and corncobs as anode materials for lithium-ion and sodium-ion batteries

Lithium ion batteries have been popularly used as the rechargeable power sources in consumer electronics due to their high energy storage density since the first commercial lithium ion battery launched by Sony in 1991. Graphite is still commonly used as anode material for commercial Lithium ion batteries due to its low redox potential close to Li+/Li, good cycling stability, low cost, and environmental friendliness.[1] However, the performance of current lithium ion batteries, which use graphite as the anode material, cannot satisfy requirements of fast charge Lithium ion batteries. The volume expansion/contraction of the graphite associated with the lithium insertion and extraction process, which results in loss of inter-particle electronic contract, consequently, lead to poor cycling stability. Another consideration of graphite is their safety caused from lithium dendrite formation due to its low Lithium intercalation potential at about 0 V (vs. Li/Li+). [2] The search for new anode materials for lithium ion batteries has been an important way to satisfy the ever-growing demands for better performance with higher energy/power densities, improved safety and longer cycle life. Recently, Li2MnO3 was investigated as an anode material for lithium ion battery.[3] Li2MnO3 exhibits much higher capacity than conventional carbon-based materials and a very stable cycling performance. In this work, as-prepared Li2MnO3/graphene composite material shows the enhanced reversible specific capacity and the rate performance compared with that of pristine Li2MnO3 . It was found that the conductivity of Li2MnO3/graphene was significantly improved by forming a conductive graphene network throughout the insulating Li2MnO3.

As the global demand for more powerful and long-lasting energy storage solutions continues to grow, Li-rich Mn-rich layered oxides (LMR) emerges as a promising class of next-generation cathode materials for lithium-ion batteries. The LMR material stands out due to its impressive electrochemical specific capacity, surpassing 280 mAh g–1, along with a high discharge voltage exceeding 3.5 V. It also boasts a remarkable specific energy density close to 1000 Wh kg–1, all while maintaining a relatively lower cost.Current synthesis methods often rely on batch coprecipitation reactions followed by the calcination of precipitated Mn-rich precursors. However, the inherent challenges of batch reactions, particularly in terms of reproducibility and quality, prompt the exploration of more sophisticated approaches. Moreover, the transition from benchtop experiments to large-scale production introduces a distinct set of challenges. Parameters that work seamlessly on a smaller scale may not translate as effectively when producing the material at the kilogram scale. This scaling-up process involves navigating complexities such as chemical handling risks, and challenges related to reaction heat transfer and mixing efficiency. These factors collectively underscore the difficulties in achieving precise control over critical precursor characteristics, including primary and secondary particle size, morphology, tap density, and stoichiometry.In response to these challenges, this presentation will discuss an innovative approach. High-quality Li-rich Mn-rich materials are synthesized using continuous coprecipitation, facilitated by a pre-pilot scale Taylor Vortex Reactor (TVR) at the Materials Engineering Research Facility (MERF) in Argonne National Lab (ANL). This emerging synthesis technology offers a scalable solution for the production of high-quality cathode materials. This presentation will delve into the intricacies of the synthesis process, providing valuable insights into the relationship between the characteristics of the synthesized LMR precursors and their subsequent impact on cathode performance.

A comparative study on the production of Ni1/3Co1/3Mn1/3C2O4 cathode precursor material for lithium-ion batteries using batch and slug-flow reactors