Realization of a high voltage Ni rich layer LiNi0.5Co0.2Mn0.3O2 single crystalline cathode for LIBs by surface modification

Single crystalline ternary cathode material LiNi_0.5Co_0.2Mn_0.3O₂(NCM523) can operate at extremely high voltages and could offer exceptional energy density. The single crystal morphology is less easy to form the cracks and could express better structure stability compared to the polycrystalline counterpart. However, irreversible parasitic side reactions in the interface during cycling may lead to rapid electrochemical degradations. Herein, a simple chemical wet method that modifies the single-crystal NCM523 particles with Al₂O₃ coating is proposed. The coating layer can effectively suppress the phase transformation and irreversible phase transition on the NCM surface during cycling. Furthermore, the cladding layer can prevent the erosion of by-products such as HF. As a result, the Al₂O₃ modified NCM523 delivers a high specific capacity of 192.5mAh g^?1, excellent cycling stability and rate capability. The capacity retention was 91.7% after 50 cycles even at ultra-high cut-off voltage of 4.7 V. This surface engineering strategy paves the way to promote the development of small size single crystal NCM523 materials for next generation LIBs.     

Synthesis and characterization of mono-dispersion LiNi0.8Co0.1Mn0.1O2 micrometer particles for lithium-ion batteries

LiNi_0.8Co_0.1Mn_0.1O₂ cathode material for lithium-ion battery exhibits high capacity, but it suffers from interfacial side reactions and structural/thermodynamic instability, which leads to capacity reduction and safety problems. Cubic brick (Ni_0.8Co_0.1Mn_0.1)C₂O₄·2H₂O particles with micron size are synthesized by co-precipitation method. The oxalic precursor is sintered with lithium hydroxide to obtain cubic mono-dispersion LiNi_0.8Co_0.1Mn_0.1O₂ micrometer particles. Structural stability, cycling performance, rate capability and compacting density of the cubic mono-dispersion material are investigated. Conventional spherical and irregular mono-dispersion LiNi_0.8Co_0.1Mn_0.1O₂ are also prepared for comparison. The results reveal that the cubic mono-dispersion LiNi_0.8Co_0.1Mn_0.1O₂ dramatically enhances the structural stability and cycling performance at a little cost of capacity and rate capability.     

Effects of Al doping on the electrochemical performances of LiNi0.83Co0.12Mn0.05O2 prepared by coprecipitation

The Ni-rich LiNi_0.83Co_0.12Mn_0.05O₂ (NCM83) cathode materials have drawn intensive attention due to the high energy density and low cost. However, Ni-rich LiNi_1-x-yCo_xMn_yO₂ still has the fatal weakness of poor cycle stability, limiting its further wide application. Bulk doping is an effective means to enhance the cycle stability, yet the electrochemical performances are very sensitive to the doping quantity. Here a facile method of co-precipitation is adopted to coat (Ni_0.4Co_0.2Mn_0.4)_1-xAl_x(OH)_2+x on precursor particles of NCM83. Al ions diffuse evenly in the NCM83 particles after sintering. The cells are operated at a high cut-off voltage of 4.5 V. The discharge capacity of NCM83 is 187.8 mAh g^?1, and decays fast with cycles. The doped sample even exhibits a higher discharge capacity of 195 mAh g^?1, and the capacity retention is improved to 83.8% after 200 cycles.     

Nano SIMS characterization of boron- and aluminum-coated LiNi1/3Co1/3Mn1/3O2 cathode materials for lithium secondary ion batteries

The LiNi_1/3Co_1/3Mn_1/3O₂ powders required for the present study, obtained by coprecipitation method has been surface coated with boron and aluminum. The morphology and crystal structure of powders have been characterized using scanning electron microscopy, X-ray diffraction and X-ray photoelectron spectroscopy techniques. The elemental distribution of the coated samples analyzed by transmission electron microscopy images and nano secondary ion mass spectrometry indicates a thin uniform layer of [B, Al]₂O₃ on the surface of spherical LiNi_1/3Co_1/3Mn_1/3O₂. The surface-modified LiNi_1/3Co_1/3Mn_1/3O₂ has been explored as a cathode material for lithium secondary ion battery applications. The electrochemical charge–discharge results reveal that the capacity retention rate of coated LiNi_1/3Co_1/3Mn_1/3O₂ after 40 cycles at 1 C rate maintains 93% of the initial discharge capacity while the rate of bare LiNi_1/3Co_1/3Mn_1/3O₂ maintains only 88%. It is noticed that the small amounts of boron and aluminum coatings on the surface of LiNi_1/3Co_1/3Mn_1/3O₂ can significantly improve the electrochemical properties of electrode materials because of the suppression of reaction between the cathode and the electrolytes.     

An ultrafast synthesis method of LiNi1/3Co1/3Mn1/3O2 cathodes by flash/field‐assisted sintering

LiNi_1/3Co_1/3Mn_1/3O₂ as a promising cathode material in lithium‐ion batteries was synthesized by flash/field‐assisted sintering technique for the first time. This study showed that the current‐limited synthesis of LiNi_1/3Co_1/3Mn_1/3O₂ could be carried out at temperatures less than 400°C for only 8 minutes, compared with the conventional pressureless sintering at 850°C for 12 hours. X‐ray diffraction results showed the phase evolution from precursor mixtures to the final LiNi_1/3Co_1/3Mn_1/3O₂ products during flash/field‐assisted sintering process and a well‐layered structure without undesirable cation mixing in the as‐formed LiNi_1/3Co_1/3Mn_1/3O₂. Combined with the lowered sintering temperatures and reduced sintering time, the excellent electrochemical performance of flash/field‐assisted sintered LiNi_1/3Co_1/3Mn_1/3O₂ materials suggested that this technique could be an energy‐efficient approach for the synthesis of lithium‐ion battery cathode materials and other materials requiring high‐temperature heat treatment.     

Performance of LiNi1/3Co1/3Mn1/3O2 prepared from spent lithium-ion batteries by a carbonate co-precipitation method

Spherical LiNi_1/3Co_1/3Mn_1/3O₂ cathode particles were resynthesized by a carbonate co-precipitation method using spent lithium-ion batteries (LIBs) as a raw material. The physical characteristics of the Ni_1/3Co_1/3Mn_1/3CO₃ precursor, the (Ni_1/3Co_1/3Mn_1/3)₃O₄ intermediate, and the regenerated LiNi_1/3Co_1/3Mn_1/3O₂ cathode material were investigated by laser particle-size analysis, scanning electron microscopy–energy-dispersive spectroscopy (SEM-EDS), thermogravimetry–differential scanning calorimetry (TG-DSC), X-ray diffraction (XRD), inductively coupled plasma–atomic emission spectroscopy (ICP-AES), and X-ray photoelectron spectroscopy (XPS). The electrochemical performance of the regenerated LiNi_1/3Co_1/3Mn_1/3O₂ was studied by continuous charge–discharge cycling and cyclic voltammetry. The results indicate that the regenerated Ni_1/3Co_1/3Mn_1/3CO₃ precursor comprises uniform spherical particles with a narrow particle-size distribution. The regenerated LiNi_1/3Co_1/3Mn_1/3O₂ comprises spherical particles similar to those of the Ni_1/3Co_1/3Mn_1/3CO₃ precursor, but with a narrower particle-size distribution. Moreover, it has a well-ordered layered structure and a low degree of cation mixing. The regenerated LiNi_1/3Co_1/3Mn_1/3O₂ shows an initial discharge capacity of 163.5 mA h g^?1 at 0.1 C, between 2.7 and 4.3 V; the discharge capacity at 1 C is 135.1 mA h g^?1, and the capacity retention ratio is 94.1% after 50 cycles. Even at the high rate of 5 C, LiNi_1/3Co_1/3Mn_1/3O₂ delivers the high capacity of 112.6 mA h g^?1. These results demonstrate that the electrochemical performance of the regenerated LiNi_1/3Co_1/3Mn_1/3O₂ is comparable to that of a cathode synthesized from fresh materials by carbonate co-precipitation.     

Effects of precursor treatment with reductant or oxidant on the structure and electrochemical properties of LiNi0.5Mn1.5O4

LiNi_0.5Mn_1.5O₄, a lithium-ion battery cathode material, is prepared using co-precipitation via a two-step drying method with Ni-Mn mixed hydroxide as the precursor. This study examines the effects of precursor pretreatment with hydrazine (a reductant) or with H₂O₂ (an oxidant) in solutions of NiSO₄ and MnSO₄. The results indicate substantial differences in the structure and electrochemical properties of LiNi_0.5Mn_1.5O₄ depending on whether the precursor is pretreated with reductant or oxidant. For the hydrazine-treated precursor, the synthesized LiNi_0.5Mn_1.5O₄ has a very pure spinel phase and an ordered, octahedral crystal morphology (ca. 100-300 nm). In contrast, the material synthesized using the H₂O₂-treated precursor shows numerous impurity phases (Na_0.7MnO_2.05) with a layer-by-layer crystal structure. The control sample (prepared without precursor pretreatment) maintains an octahedral structure but still retains a few impurity phases of Na_0.7MnO_2.05. The electrochemical results show that LiNi_0.5Mn_1.5O₄ synthesized using a hydrazine-treated precursor has a higher specific capacity (especially under high discharge current) and a higher cyclic life than the control sample, whereas the sample using H₂O₂-treated precursor shows almost no special capacity due to changes in crystal structure.     

LiNi<Subscript>0.4</Subscript>Co<Subscript>0.3</Subscript>Mn<Subscript>0.3</Subscript>O<Subscript>2</Subscript> thin film electrode by aerosol deposition

LiNi_0.4Co_0.3Mn_0.3O₂ thin film electrodes are fabricated from LiNi_0.4Co_0.3Mn_0.3O₂ raw powder at room temperature without pretreatments using aerosol deposition that is much faster and easier than conventional methods such as vaporization, pulsed laser deposition, and sputtering. The LiNi_0.4Co_0.3Mn_0.3O₂ thin film is composed of fine grains maintaining the crystal structure of the LiNi_0.4Co_0.3Mn_0.3O₂ raw powder. In the cyclic voltammogram, the LiNi_0.4Co_0.3Mn_0.3O₂ thin film electrode shows a 3.9-V anodic peak and a 3.6-V cathodic peak. The initial discharge capacity is 44.6 μAh/cm², and reversible behavior is observed in charge-discharge profiles. Based on the results, the aerosol deposition method is believed to be a potential candidate for the fabrication of thin film electrodes.     

Comparison of structure and electrochemistry of Al- and Fe-doped LiNi1/3Co1/3Mn1/3O2

LiNi_1/3Co_1/3−xM_xMn_1/3O₂ (M = Fe and Al; x = 0, 1/20, 1/9 and 1/6) have been synthesized by firing the co-precipitates of metal hydroxides. The impacts of Fe and Al doping on the structure and electrochemical performances of LiNi_1/3Co_1/3Mn_1/3O₂ are compared by means of powder X-ray diffraction (XRD), scanning electron microscopy (SEM), and galvanostatic charge/discharge test as cathode materials for lithium ion batteries. These materials keep the same layered structure as the LiNi_1/3Co_1/3Mn_1/3O₂ host. It is found that Fe- and Al-doped LiNi_1/3Co_1/3Mn_1/3O₂ show different characteristics in lattice parameter and cycling voltage plateau with increasing dopant dose. More interestingly, low Al doping (x < 1/20) improves the structural stability while Fe doping does not have such effect even at low Fe content.     

Al-doped Ni-rich cathode powders prepared from the precursor powders with fine size and spherical shape

LiNi_0.8Co_0.15Al_0.05O₂ cathode powders with fine size and spherical shape were prepared by solid-state reaction method using the Ni-Co-Al-O precursor powders with fine size and spherical shape. The Ni-Co-Al-O precursor powders with fine size and filled inner structure were prepared by spray pyrolysis from the spray solution with drying control chemical additive (DCCA), citric acid and ethylene glycol. The one LiNi_0.8Co_0.15Al_0.05O₂ cathode powder with fine size and spherical shape was formed from the one precursor powder with spherical shape and filled morphology. The mean size of the spherical shape LiNi_0.8Co_0.15Al_0.05O₂ cathode powders was 1.1 μm. The initial discharge capacity of the LiNi_0.8Co_0.15Al_0.05O₂ cathode powders prepared from the spray solution with citric acid, ethylene glycol and DCCA was 200 mAh g⁻¹. The cycle properties of the cathode powders prepared from the spray solution with and without additives were compared.     

Properties of LiNi<Subscript>0.8</Subscript>Co<Subscript>0.1</Subscript>Mn<Subscript>0.1</Subscript>O<Subscript>2</Subscript> as a high energy cathode material for lithium-ion batteries

Nickel-rich layered materials are prospective cathode materials for use in lithium-ion batteries due to their higher capacity and lower cost relative to LiCoO₂. In this work, spherical Ni_0.8Co_0.1Mn_0.1(OH)₂ precursors are successfully synthesized through a co-precipitation method. The synthetic conditions of the precursors - including the pH, stirring speed, molar ratio of NH₄OH to transition metals and reaction temperature - are investigated in detail, and their variations have significant effects on the morphology, microstructure and tap-density of the prepared Ni_0.8Co_0.1Mn_0.1 (OH)₂ precursors. LiNi_0.8Co_0.1Mn_0.1O₂ is then prepared from these precursors through a reaction with 5% excess LiOH· H₂O at various temperatures. The crystal structure, morphology and electrochemical properties of the Ni_0.8Co_0.1Mn_0.1 (OH)₂ precursors and LiNi_0.8Co_0.1Mn_0.1O₂ were investigated. In the voltage range from 3.0 to 4.3 V, LiNi_0.8Co_0.1Mn_0.1O₂ exhibits an initial discharge capacity of 193.0mAh g^-1 at a 0.1 C-rate. The cathode delivers an initial capacity of 170.4 mAh g^-1 at a 1 C-rate, and it retains 90.4% of its capacity after 100 cycles.     

Spray-drying synthesized LiNi0.6Co0.2Mn0.2O2 and its electrochemical performance as cathode materials for lithium ion batteries

Layered LiNi_0.6Co_0.2Mn_0.2O₂ materials were synthesized at different sintering temperatures using spray-drying precursor with molar ratio of Li/Me = 1.04 (Me = transition metals). The influences of sintering temperature on crystal structure, morphology and electrochemical performance of LiNi_0.6Co_0.2Mn_0.2O₂ materials have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and charge-discharge test. As a result, material synthesized at 850 °C has excellent electrochemical performance, delivering an initial discharge capacity of 173.1 mAh g^− 1 between 2.8 and 4.3 V at a current density of 16 mA g^− 1 and exhibiting good cycling performance.     

Optimization of microwave synthesis of Li[Ni0.4Co0.2Mn0.4]O2 as a positive electrode material for lithium batteries

A positive electrode material for lithium ion battery applications was successfully synthesized using microwave irradiation. This microwave synthesis has several merits such as homogeneity of final product and much shorter reaction time compared to conventional synthetic methods. We synthesized spherical [Ni_0.4Co_0.2Mn_0.4](OH)₂ as a precursor by a co-precipitation method. The pelletized mixture of the precursor and lithium hydroxide was calcined under different reaction times and temperatures by applying 1200 W of microwave irradiation at 2.45 GHz. We determined the optimum conditions of microwave synthesis for positive electrode materials. The powders were characterized by X-ray diffraction, scanning electron microscopy, and electrochemical testing. The capacity, its retention, and thermal stability of Li[Ni_0.4Co_0.2Mn_0.4]O₂ synthesized by the microwave synthesis were comparable to the Li[Ni_0.4Co_0.2Mn_0.4]O₂ prepared by the high temperature calcination method.     

Novel synthesis of layered LiNi1/2Mn1/2O2 as cathode material for lithium rechargeable cells

A new solution combustion synthesis of layered LiNi_0.5Mn_0.5O₂ involving the reactions of LiNO₃, Mn(NO₃)₂, NiNO₃, and glycine as starting materials is reported. TG/DTA studies were performed on the gel-precursor and suggest the formation of the layered LiNi_0.5Mn_0.5O₂ at low temperatures. The synthesized material was annealed at various temperatures, viz., 250, 400, 600, and 850 °C, characterized by means of X-ray diffraction (XRD) and reveals the formation of single phase crystalline LiNi_0.5Mn_0.5O₂ at 850 °C. The morphology of the synthesized material has been investigated by means of scanning electron microscopy (SEM) and suggests the formation of sub-micron particles. X-ray photoelectron spectroscopy (XPS) and cyclic voltammetry (CV) studies on the synthesized LiNi_0.5Mn_0.5O₂ powders indicate that the oxidation states of nickel and manganese are +2 and +4, respectively. Electrochemical galvanostatic charge-discharge cycling behavior of Li//LiNi_0.5Mn_0.5O₂ cell using 1 M LiPF₆ in EC/DMC as electrolyte exhibited stable capacities of ∼125 mAh/g in the voltage ranges 2.8-4.3 V and 3.0-4.6 V and is comparable to literature reports using high temperature synthesis route. The capacity remains stable even after 20 cycles. The layered LiNi_0.5Mn_0.5O₂ powders synthesized by this novel route have several advantages as compared to its conventional synthesis techniques.     

Toward high stability single crystal material by structural regulation with high and low temperature mixing sinter

Single-crystal cathode materials are a potential research focus for high-nickel ternary cathode materials owing to their high compaction density and good electrochemical stability. However, in the traditional sintering process, lithium is lost because of the long-time and higher-temperature sintering, which reduces the migration energy barrier of Ni²⁺ and increases the degree of mixing of Li⁺ and Ni²⁺. Herein, for the first time, a method for short-time high-temperature sintering combined with low-temperature heat preservation is proposed to prepare LiNi_0.6Co_0.6Mn_0.2O₂ (NCM622) single crystal materials in a mixed molten salt system of LiOH and Li₂CO₃. In analyses of morphology, structure and electrochemical properties, the prepared NCM622 exhibits excellent cycling stability owing to an ordered layered structure and low cation mixing degree. The single-crystal material shows an excellent capacity retention of 93.19% (150.49–140.24mAh·g^?1) after 100 cycles at 1 C in the voltage range of 2.8–4.3 V. The single crystal particles exhibit reliable stability after long cycling without microcracks in the cycled particles. Furthermore, the preparation cost could be significantly reduced with a closed loop of the flux salt. The short-time high-temperature combined with the low-temperature holding sintering method may provide an effective strategy for the synthesis of other single-crystal materials with excellent electrochemical properties.     

Electrochemical performance and local cationic distribution in layered LiNi1/2Mn1/2O2 electrodes for lithium ion batteries

LiNi_1/2Mn_1/2O₂ electrodes with layered structure were synthesized by solid-state reaction between lithium hydroxide and mixed Ni,Mn oxides obtained from co-precipitated Ni,Mn carbonates and hydroxides and freeze-dried Ni,Mn citrates. The temperature of the solid-state reaction was varied between 800 and 950 °C. This method of synthesis allows obtaining oxides characterized with well-crystallized nanometric primary particles bounded in micrometric aggregates. The extent of particle agglomeration is lower for oxides obtained from freeze-dried Ni,Mn citrates. The local Mn⁴⁺ surrounding in the transition metal layers was determined by X-band electron paramagnetic resonance (EPR) spectroscopy. It has been found that local cationic distribution is consistent with α,β-type cationic order with some extent of disordering that depends mainly on the precursors used. The electrochemical extraction and insertion of lithium was tested in lithium cells using Step Potential Electrochemical Spectroscopy. The electrochemical performance of LiNi_1/2Mn_1/2O₂ oxides depends on the precursors used, the synthesis temperature and the potential range. The best electrochemical response was established for LiNi_1/2Mn_1/2O₂ prepared from the carbonate precursor at 900 °C. The changes in local environment of Mn⁴⁺ ions during electrochemical reaction in both limited and extended potential ranges were discussed on the basis of ex situ EPR experiments.     

Enhancing high-potential stability of Ni-rich LiNi0.8Co0.1Mn0.1O2 cathode with PrF3 coating

It is still a huge challenge to improve the safety and stability of Ni-rich (LiNi_0.8Co_0.1Mn_0.1O₂) cathode materials at elevated potential. Herein, the PrF₃ layer is employed to protect LiNi_0.8Co_0.1Mn_0.1O₂ (NCM811) via a simple wet chemical process. It was confirmed by XRD, HR-SEM, TEM, EDS, and XPS tests that PrF₃ is evenly covered throughout the surface of NCM811 without affecting the particle size and surface morphology. In particular, 1 wt% PrF₃ coated NCM811 exhibits excellent stability and rate capability with the capacity retention of 86.3% after 100 cycles at 1 C under a cut-off potential of 4.3 V, while the retention of pristine one is only 73.8%. Moreover, the capacity retention of 1 wt% PrF₃ coated samples enhances from 74.5% to 88.5% after 50 cycles at 1 C under higher cut-off voltage of 4.6 V. The superior performance for coated samples can be attributed to the fact that PrF₃ can effectively isolate the active material and the electrolyte from HF corrosion, and at the same time, reduce the generation of micro-cracks on the surface during prolonged cycles. Furthermore, as a physical barrier, PrF₃ alleviates the dissolution of transition metals in the electrolyte largely. These results suggest that the stability of NCM811 can be greatly upgraded at high voltage by PrF₃ coating.     

Characterization of yttrium substituted LiNi0.33Mn0.33Co0.33O2 cathode material for lithium secondary cells

LiNi_0.33−xMn_0.33Co_0.33Y_xO₂ materials are synthesized by Y³⁺ substitute of Ni²⁺ to improve the cycling performance and rate capability. The influence of the Y³⁺ doping on the structure and electrochemical properties are investigated by means of X-ray diffraction (XRD), scanning electron microscope (SEM), cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), X-ray photoelectron spectroscopy (XPS) and galvanostatic charge/discharge tests. LiNi_0.33Mn_0.33Co_0.33O₂ exhibits the capacity retentions of 89.9 and 87.8% at 2.0 and 4.0 C after 40 cycles, respectively. After doping, the capacity retentions of LiNi_0.305Mn_0.33Co_0.33Y_0.025O₂ are increased to 97.2 and 95.9% at 2.0 and 4.0 C, respectively. The discharge capacity of LiNi_0.305Mn_0.33Co_0.33Y_0.025O₂ at 5.0 C remains 75.7% of the discharge capacity at 0.2 C, while that of LiNi_0.33Mn_0.33Co_0.33O₂ is only 47.5%. EIS measurement indicates that LiNi_0.305Mn_0.33Co_0.33Y_0.025O₂ electrode has the lower impedance value during cycling. It is considered that the higher capacity retention and superior rate capability of Y-doped samples can be ascribed to the reduced surface film resistance and charge transfer resistance of the electrode during cycling.     

Preparation and characterization of LiNi0.8Co0.15Al0.05O2 with high cycling stability by using AlO2- as Al source

We report the preparation of a series of LiNi_0.8Co_0.15Al_0.05O₂ materials with different reaction time (10, 20, 30 and 40 h) of precursor and their electrochemical properties as cathode material for lithium-ion batteries (LIBs). The preparation of LiNi_0.8Co_0.15Al_0.05O₂ was divided into two steps: a co-precipitation process to obtain Ni_0.8Co_0.15Al_0.05(OH)₂ precursor and a calcination step with LiOH. During the co-precipitation process, AlO₂^- was employed as Al source so as to guarantee Ni²⁺, Co²⁺ and Al³⁺ co-precipitation. The impacts of different synthesis time of the precursor on crystal structure, morphology and electrochemical performance of LiNi_0.8Co_0.15Al_0.05O₂ were systematically investigated. The samples with various synthesis time of precursor possessed spherical morphology and a layered α-NaFeO₂ structure with R-3m space group. Especially, when the reaction time of precursor was 30 h, the LiNi_0.8Co_0.15Al_0.05O₂ had the weakest degree of Li⁺/Ni²⁺ ions mixing and the best uniformity and integrity. When used as cathode materials for LIBs, the LiNi_0.8Co_0.15Al_0.05O₂ with 30 h exhibited high discharge capacity, good cycling performance and remarkable rate capability. The maximum discharge capacity was 202.3 mAh g⁻¹ at 0.1 C and the capacity retention approached 99.4% after 100 cycles at 1 C. At 10 C, the discharge capacity exceeded 140 mAh g⁻¹, suggesting a possible application in the high rate LIBs. The excellent electrochemical performance might be attributed to the uniform co-precipitation of Ni²⁺, Co²⁺ and Al³⁺ and well layered structure with less Li⁺/Ni²⁺ mixing.     

Synthesis of LiNi1/3Co1/3Mn1/3O2 cathode materials by using a supercritical water method in a batch reactor

LiNi_1/3Co_1/3Mn_1/3O₂ and LiCoO₂ cathode materials were synthesized by using a supercritical water (SCW) method with a metal salt solution in a batch reactor. Stoichiometric LiNi_1/3Co_1/3Mn_1/3O₂ was successfully synthesized in a 10-min reaction without calcination, while overlithiated LiCoO₂ (Li_1.15CoO₂) was synthesized using the batch SCW method. The physical properties and electrochemical performances of LiNi_1/3Co_1/3Mn_1/3O₂ were compared to those of Li_1.15CoO₂ by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), and charge/discharge cycling tests. The XRD pattern of LiNi_1/3Co_1/3Mn_1/3O₂ was found to be similar to that of Li_1.15CoO₂, showing clear splitting of the (0 0 6)/(1 0 2) and (1 0 8)/(1 1 0) peak pairs as particular characteristics of the layered structure. In addition, both cathode powders showed good crystallinity and phase purity, even though a short reaction time without calcination was applied to the SCW method. The initial specific discharge capacities of the Li_1.15CoO₂ and LiNi_1/3Co_1/3Mn_1/3O₂ powders at a current density of 0.24 mA/cm² in 2.5-4.5 V were 149 and 180 mAh/g, and their irreversible capacity loss was 20 and 17 mAh/g, respectively. The discharge capacities of the Li_1.15CoO₂ and LiNi_1/3Co_1/3Mn_1/3O₂ powders decreased with cycling and remained at 108 and 154 mAh/g after 30 cycles, which are 79% and 89% of the initial capacities. Compared to the overlithiated LiCoO₂ cathode powders, the LiNi_1/3Co_1/3Mn_1/3O₂ cathode powders synthesized by SCW method had better electrochemical performances.