Li- and Mn-rich layered oxide cathode materials for lithium-ion batteries: a review from fundamentals to research progress and applications

Hongge Pan *^a, Shiming Zhang ^a, Jian Chen ^b, Mingxia Gao ^a, Yongfeng Liu ^a, Tiejun Zhu ^a and Yinzhu Jiang ^a
aState Key Laboratory of Silicon Materials, School of Materials Science and Engineering, Zhejiang University, Hangzhou, 310027, P.R. China
^bSchool of Materials Science and Chemical Engineering, Xi'an Technological University, Xi'an, 710021, P.R. China

First published on 18th July 2018

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Hongge Pan

Hongge Pan received his PhD in Materials Science and Engineering from Zhejiang University in 1996 under a joint program between Zhejiang University and Institute of Physics, Chinese Academy of Sciences. Later that year, he joined Zhejiang University and became a Professor in 1999. His research is focused on energy materials for solid-state hydrogen storage and lithium batteries.

Shiming Zhang

Shiming Zhang received his BS degree in Chemical Engineering and Technology from Shanghai University of Electric Power, China, in 2010 and his MS degree in Applied Chemistry from Shanghai University of Electric Power, China, in 2013. He received his PhD degree in Materials Science under the supervision of Prof. Hongge Pan at Zhejiang University, China, in 2016. He mainly focuses on materials for advanced energy storage and conversion systems.

Mingxia Gao

Mingxia Gao received her PhD in Materials Science and Engineering from Zhejiang University in 2004. She is currently a professor at Zhejiang University. Her research is focused on solid-state hydrogen storage materials and electrode materials for rechargeable batteries.

Yongfeng Liu

Yongfeng Liu received his PhD in Materials Science and Engineering from Zhejiang University in 2005. He then moved to the National University of Singapore as a postdoctoral research fellow (working with Dr. Ping Chen). In 2007, he joined Zhejiang University as an Associate Professor. He became a Professor of Materials Science and Engineering at Zhejiang University. His research is focused on solid-state hydrogen storage materials and electrode materials for rechargeable batteries.

Design, System, Application In recent years, intensive efforts have been made to develop high-performance cathode materials of lithium-ion batteries (LIBs) for applications of high-end products such as power sources of electric vehicles (EVs) and 3C (computer, communication, and consumer electronics) products. However, the specific energy density of commercialized LIBs still cannot meet the ever-growing requirements of practical applications. Success in these fields will mostly depend on further studying and developing new electrode materials with higher-energy density. Li- and Mn-rich layered oxide (LMRO) cathode materials xLi2MnO3-(1 − x)LiMO2 (M = Co, Ni, Mn, Cr, etc.) have attracted the spotlight due to their high electrochemical capacity of over 280 mA h g−1 and high-energy density of over 1000 W h kg−1 which is nearly two times those of traditional cathode materials. The major goals of this review article are to highlight the recent developments and prospective advances of LMRO cathode materials and to give a broad picture of recent scientific research on LMRO cathode materials for high-performance LIBs.

1. Introduction

Lithium-ion batteries (LIBs) have been extensively used as power sources of electric vehicles (EVs), 3C (computer, communication, and consumer electronics) products, and energy storage devices for renewable energy and smart grids.^1–3 However, the specific energy density of commercialized LIBs still cannot meet the requirements for practical applications. Success in these fields will mostly depend on further studying and developing new electrode materials with higher energy density.^4,5 At present, several alternative cathode materials (layered LiCoO₂, LiNi_0.8Co_0.15A_l0.05O₂, LiNi_0.33Co_0.33Mn_0.33O₂, spinel LiMn₂O₄, olivine LiFePO₄, and so on) have been commercially utilized in LIBs. As shown in Table 1, layered LiCoO₂ and LiNi_1/3Co_1/3Mn_1/3O₂ oxide cathode materials which are the main cathode materials applied for current LIBs exhibit energy densities below 600 W h kg⁻¹ and spinel LiMn₂O₄ and olivine LiFePO₄ cathode materials also only deliver about 400 W h kg⁻¹ and 500 W h kg⁻¹, respectively. The low energy density of these cathodes limits their widespread applications for commercial LIBs, especially in the large-scale electric vehicle and energy storage fields.

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Li- and Mn-rich layered oxide (LMRO) cathode materials xLi₂MnO₃-(1 − x)LiMO₂ (M = Co, Ni, Mn, Cr, etc.) have attracted the spotlight due to their high electrochemical capacity of over 280 mA hg⁻¹ and high-energy density of over 1000 W h kg⁻¹ which is nearly two times those of traditional cathode materials.^6,7 The typical Li- and Mn-rich layered Li[Li_0.2Ni_0.2Mn_0.6]O₂ and Li_1.2Mn_0.54Ni_0.13Co_0.13O₂ cathode materials generally deliver an initial discharge capacity of over 250 mA h g⁻¹ at room temperature^8–10 and an anomalous high capacity of more than 350 mA h g⁻¹ at high temperature (over 50 °C).^11,12 It has been reported that the LMRO is composed of two phases, namely, a trigonal LiMO₂ phase (space group Rm) and a monoclinic Li₂MnO₃ phase (space group C2/m) (M = Ni, Co, Mn, Fe, Cr, etc.), and they are intergrowth on the nanoscale forming a nano dominated composition structure.^13–16 In the LMRO cathode materials, the Li₂MnO₃ phase can enhance the electrochemical capacity of the cathode because it transforms into an active LiMnO₂ phase after the first cycle, but Li₂MnO₃ itself has low electrochemical activity,^17–20 which can be activated by the LiMO₂ phase.^21–26 Therefore, the synergic effect between the Li₂MnO₃ phase and the LiMO₂ phase contributes to the higher electrochemical performance of the LMRO cathode materials. Moreover, the LMRO cathode materials are low cost and environmentally compatible. Therefore, the LMRO cathode materials are of interest as the next generation of cathode materials for high-energy density LIBs.

However, several scientific issues and challenges need to be overcome before realizing the commercial applications of the LMRO cathode materials, including their disputed crystal structure, ambiguous reaction mechanism, high initial irreversible capacity, poor cycle life, fast voltage fading, and poor rate capability. Various physical and electrochemical techniques are used to explore the crystal structure, reaction mechanism and electrochemical performance of the LMRO cathode materials. At present, there are three viewpoints about the long-term structure of the LMRO: (1) a solid solution with a monoclinic (C/2m) structure; (2) a solid solution with a trigonal (Rm) structure and (3) a composite structure with a monoclinic (C2/m) and trigonal (Rm) structure. Moreover, the local structures of the LMRO are also ambiguous. The reported reaction mechanisms of the LMRO cathode materials include: (1) mechanism of oxygen release; (2) mechanism of surface reaction; (3) mechanism of peroxide reaction and (4) mechanism of proton exchange.^13,27–31

The high initial irreversible capacity of the LMRO cathode materials mainly originate from the activation of the Li₂MnO₃ component at high voltages over 4.5 V, which causes the discharge capacity to decrease by 20–30% that of the charge capacity.³² The side reaction of the interphase between the cathode surface and the electrolyte, especially at high cutoff charge voltages over 4.6 V, is another reason leading to its initial irreversible capacity.^33,34 It is generally accepted that the phase transformation from layered to spinel structure occurs when the LMRO cathodes are charged to 4.8 V.^30,35,36 The gradual growth of the spinel phase results in voltage fading and capacity decay during cycling.³⁷ The dissolution of metal elements in the electrolyte also gives rise to capacity/voltage fading.³⁸ The low conductivity of LiMO₂ and Li₂MnO₃ oxides is one of the main reasons causing the poor rate capability of the LMRO cathode materials.^39–42 It has also been reported that the activity of the Li₂MnO₃ phase could damage the electrode surface structure which increases its interfacial impedance and decreases the Li⁺ ions' diffusion kinetics, which also severely causes the poor rate capability of the LMRO cathode materials.^43–45

Representative modification methods including chemical activation, doping/substitution, and surface coating are used to overcome these issues of high initial irreversible capacity, poor cycle life, fast voltage fading, and poor rate capability of the LMRO cathode materials. The chemical activation approach includes controlling the chemical composition and phase structure, acid treatment, pre-activation, etc.^54–58 Recently, surface coating of LMRO cathode materials with MnO_x,^59,60 Al₂O₃,^61,62 MoO₃,⁶³ TiO₂,⁶⁴ ZrO₂,⁶⁵ AlPO₄,^66,67 and AlF₃ (ref. 68 and 69) inert phases has been reported as an effective way to enhance the initial coulombic efficiency and cycling ability by preventing the electrode from being etched by acidic species and suppressing the dissolution of transition metal (TM) elements in the electrolyte. Ion doping/substitution with K⁺, Na⁺, Mg²⁺, Al³⁺etc. can stabilize the host crystal structure of the LMRO cathode materials by prohibiting the formation of the spinel phase during cycling and subsequently suppress capacity/voltage fading.^38,70–77

Herein, firstly we review the development history of the LMRO cathode materials and elaborate their fundamentals issues and challenges. Secondly, we review the latest research advances in the LMRO cathode materials, and then demonstrate and discuss their applications in full-cells and related key technical issues. Lastly, the prospects for future research on the LMRO cathode materials are also presented.

In contrast with other reviews about the LMRO cathode materials,^78–84 in this paper we systematically review the fundamentals, research progress and applications of the LMRO cathode materials and retrospects in detail the development history of the LMRO cathode materials in the past 30 years. Moreover, the synergistic effect mechanism, contributions of the Li, Ni, Co, Mn and O vacancies, local structure, mechanisms of peroxide reaction as well as dissolution of metal elements, solid electrolyte interphase (SEI) and electrolyte decomposition leading to capacity/voltage fading in the LMRO cathode materials are also systematically discussed. In this paper, the following sections are reviewed and discussed in sequence:

(1) Development history of the LMRO cathode materials;

(2) Fundamental issues of the LMRO cathode materials, which include the synergistic effect mechanism, the contributions of the Li, Ni, Co, Mn and O vacancies, the disputed crystal structure, and the ambiguous reaction mechanism;

(3) Challenges in the LMRO cathode materials, including the high initial irreversible capacity, capacity/voltage fading, and poor high rate capability;

(4) Improvement strategies and recent progress in the LMRO cathode materials, which include surface coating, ion doping/substitution, chemical activation, new binders, special morphology and so on;

(5) Applications of the LMRO cathode materials in full-cells;

(6) Prospects for future research on the LMRO cathode materials.

2. Development history of the LMRO cathode materials

The LMRO cathode materials can be traced back to the ‘90s. In 1991, Thackeray et al.⁸⁵ first reported that the lithium manganese oxide Li_2−xMnO_3−x/2 derived from Li₂MnO₃ could be used as the cathode material in LIBs. The electrochemically active Li_2−xMnO_3−x/2 phases were synthesized by chemical leaching of Li₂O from the rock salt phase Li₂MnO₃ (Li₂O–MnO₂) with an acid treatment method. The result demonstrated that the Li_2−xMnO_3−x/2 cathodes could deliver a discharge specific capacity of approximately 200 mA h g⁻¹. In the same year, they also found that the Li⁺ ions could reversibly insert and extract from the α-MnO₂ host framework and delivered a higher reversible electrochemical capacity of over 200 mA h g⁻¹.⁸⁶

In 1992, Thackeray et al.⁸⁷ reported that the lithium-manganese-oxide cathode materials from Li₂O–yMnO₂(Li₂MnO₃, y = 1) demonstrated a good electrochemical performance with a discharge specific capacity of 213 mA h g⁻¹.

In 1993, Thackeray et al.⁸⁸ obtained a lithiated compound Li_0.36Mn_0.91O₂ prepared from Li₂MnO₃ by acid digestion. The structure of Li_0.36Mn_0.91O₂ consists of alternate layers of trigonal prisms, partially occupied by Li⁺ ions, and edge-shared octahedra, which are almost completely occupied by Mn⁴⁺ ions. Lithiation of the Li_0.36Mn_0.91O₂ product with LiI formed the rock-salt phase Li_1.09Mn_0.91O₂, which can also be described as 0.2Li₂MnO₃–0.8LiMnO_2.21, in which the cubic close-packed oxygen array of the parent Li₂MnO₃ structure is regenerated. They firstly demonstrated that the layered Li_y(Li_1−zMn_z)O₂ compounds derived from Li₂MnO₃ can be used as cathode materials.

In 1997, Numata et al.⁸⁹ firstly reported that the lithium–manganese–cobalt oxide Li(Li_x/3Mn_2x/3Co_1−x)O₂(0 ≤ x ≤1) can be prepared as a solid solution between two kinds of layer structures, LiCoO₂ and Li₂MnO₃. In this solid solution, LiCoO₂ is the electrochemically active component, which shows poor cycling stability due to the instability of its structure during cycling. However, Li₂MnO₃ is the electrochemically inert component, which can effectively stabilize the structure of LiCoO₂ during cycling to improve its cycling stability.

From 1997 to 1999, Numata et al.^90–94 continually reported a series of Li(Li_x/3Co_1−xMn_2x/3)O₂ cathode materials and found that these cathode materials could deliver better cycling performance than the pure LiCoO₂ cathode material in the operation potential window between 2.5–4.3 V vs. Li/Li⁺.

In 1999, Kalyani et al.⁹⁵ found that the Li₂MnO₃ compound could be electrochemically activated by charging in a lithium cell up to 4.5 V for the first time, rather than by acid treatment.^85,87,88 Subsequent investigations showed that, at this high potential, the Li⁺ ions can be extracted from the Li₂MnO₃ phase accompanied by the release of oxygen from the electrode surface, resulting in a net loss of Li₂O from the structure. This finding is an important milestone for the development of the LMRO cathode materials, which suggests that the electrochemically inert Li₂MnO₃ material can be used as a cathode material at higher operation potential.

From 1999 to 2003, a series of Li- and Mn-rich materials, such as the Li₂MnO₃, Li[Ni_xLi_(1/3−2x/3)Mn_(2/3−x/3)]O₂, Li[Co_xLi_(1/3−x/3)Mn_(2/3−2x/3)]O₂, Li[Cr_xLi_(1/3−x3)Mn_(2/3−2x/3)]O₂, and Li[Li_0.1Ni_0.35−x/2Co_xMn_0.55−x/2]O₂ compounds were studied as cathode materials, which showed a higher discharge specific capacity of over 200 mA h g⁻¹ in the potential window of 2.0 to 4.8 V vs. Li/Li⁺.^{11,23,24,96–104}

In 2004, Thackeray et al.¹⁰⁵ began to use the two-component notation xLi₂MnO₃-(1 − x)LiMO₂ with M = Co, Cr, Ni and/or Mn instead of the equivalent layered notation Li[Li_x/(2+x)M_2/(2+x)]O₂ to monitor the compositional changes that occur in the electrode during electrochemical charge and discharge. The structural compatibility between the Li₂MnO₃ component (alternatively, in the layered notation, Li[Li_0.33Mn_0.67]O₂) and the LiMO₂ component, such as LiCoO₂, LiCrO₂, LiNi_0.8Co_0.2O₂ and LiMn_0.5Ni_0.5O₂, all of which have a rock salt-type structure, allows for the structural integration of the two components at the atomic level.

In the same year, Thackeray et al.¹⁰⁶ reported the xLi₂MO₃-(1 − x)LiMn_0.5Ni_0.5O₂ (M = Ti, Mn, Zr) cathode materials. They revealed that the Li₂MO₃ component can be structurally integrated into the LiMn_0.5Ni_0.5O₂ component to yield a domain composite structure, which is of short range order rather than a true solid solution.

In 2005, Thackeray et al.¹⁰⁷ first proposed the concept of Li- and Mg-rich layered oxide (LMRO) cathode materials derived from composite structures in which the layered Li₂MnO₃ component is structurally integrated with either the layered LiMO₂ component or with the spinel LiM₂O₄ component (M = Mn, Ni, Co). These cathode materials can be represented as xLi₂MnO₃-(1 − x)LiMO₂ and xLi₂MnO₃-(1 − x)LiM₂O₄, respectively. The LMRO cathode materials not only offer the advantages of low cost, stability and safety, but also deliver high capacity which is nearly two times higher than that of the LiCoO₂ cathode material. Therefore, the LMRO were considered as the next generation cathode materials of LIBs. After that, lots of studies focused on typical Li- and Mn-rich layered oxide cathode materials with composite structures composed of a Li₂MnO₃ component and a Li(Ni_1−x−yCo_xMn_y)O₂ component.^54,108,109

In the following years, lots of efforts have been done to further reveal the crystal structures, reaction mechanisms and relationship between the structure and the electrochemical performance of the LMRO cathode materials. Moreover, the strategies for improving the electrochemical performance of the LMRO cathode materials were also extensively carried out, such as incorporating other metal ions (Co, Ni, Mn, Cr, Fe, Mo, etc.) into the structure, chemical pre-activation, ion doping/substitution, surface coating, developing new binders, preparing special structures and so on.^{79–81,83,84,110}

In 2005, Bruce et al.⁹⁷ found that the Li[Li_0.2Ni_0.2Mn_0.6]O₂ cathode can deliver a charge specific capacity of over 390 mA h g⁻¹, a discharge specific capacity of 350 mA h g⁻¹ and an ICL of only 40 mA h g⁻¹ when cycled at the ambient temperature of 85 °C. The mechanisms of peroxide reaction and proton exchange were used to explain this higher electrochemical capacity of the LMRO cathode at a higher cycle temperature.

In 2006, Bruce et al.³² reported the oxygen release mechanism of a LMRO cathode by an in situ differential electrochemical mass spectrometry (DEMS) technique and Zhou et al.¹⁴ investigated in detail the oxygen release mechanism of the 0.5Li₂MnO₃–0.5LiMn_0.42Ni_0.42Co_0.16O₂ cathode in 2012, which helped to clearly understand the electrochemical behavior of the LMRO cathode during cycling.

In 2011, Komaba et al.¹¹¹ systematically investigated the reaction mechanisms of the Li_1.2Co_0.13Ni_0.13Mn_0.54O₂ cathode material by the synchrotron X-ray diffraction (SXRD), X-ray absorption spectroscopy (XAS), X-ray photoelectron spectroscopy (XPS), and time-of-flight secondary ion mass spectroscopy (SIMS) techniques to put forward a surface reaction mechanism.

In 2012, Boulineau et al.¹¹² found the presence of a defect spinel phase in the Li₂MnO₃ cathode material after the first charge due to the transfer of transition metal ions into the Li layers. In 2013, Mohanty et al.¹¹³ investigated the structural transformation in LMRO cathode materials by in situ XRD to further confirm the layered to spinel phase transformation in the LMRO cathode materials during cycling.

In 2010, Aurbach et al.,¹¹⁴ by a rigorous study with HRTEM, further confirmed that the 0.5Li₂MnO₃·0.5LiMn_1/3Ni_1/3Co_1/3O₂ cathode material is a two-phase composite comprising nanodomains of both the trigonal LiNiO₂-like structure and the monoclinic Li₂MnO₃ structure, which are closely integrated and interconnected with one another at the atomic level.

In 2013, Lu et al.¹¹⁵ modified Li(Li_0.2Mn_0.54Ni_0.13Co_0.13)O₂ by a surface cubic spinel phase coating prepared by a simple strategy of using surface treatment with various amounts (0–30 wt%) of Super P (carbon black). Results demonstrated that the phase transformation from the Li₂MnO₃-type structure to the spinel-like phase took place in the surface regions of the particles during the post annealing process, which led to the increase in both the initial coulombic efficiency and rate capability from 78% and 100 mA h g⁻¹ (charge capacity of 2500 mA g⁻¹) of the pristine material to 93.4% and 200 mA h g⁻¹, respectively.

In 2014, Guo¹¹⁶ demonstrated that the surface of the LMRO cathode material coated with a continuous delaminated MnO₂ nanolayer can effectively enhance the discharge capacity, initial coulombic efficiency, rate capability, and cycling stability of the LMRO cathode material. The LMRO coated with a 3 wt% MnO₂ nanolayer presented an initial discharge capacity and initial coulombic efficiency of 299 mA h g⁻¹ and 88%, respectively, the capacity retention after 50 cycles also reached 93%, and the discharge capacity can be 157 mA h g⁻¹ even at 5C. In the same year, Li et al.⁷³ reported that Li_1.20Mn_0.54Co_0.13Ni_0.13O₂ with in situ K⁺ doping exhibited a superior cycling stability of 85% with an initial capacity of 315 mA h g⁻¹ even after 110 cycles, which can be attributed to the K⁺ ion doping stabilizing the host layered structure by prohibiting the formation of spinel structure during cycling.

In 2016, Shi et al.¹¹⁷ reported that the 0.5Li₂MnO₃·0.5LiNi_0.8Co_0.1Mn_0.1O₂ cathode material with high nickel content exhibited much slower voltage decay during long-term cycling compared with the conventional LMRO cathode materials. The voltage decay after 200 cycles was only 201 mV.

In 2017, our group successfully resolved the cycling performance of Li_1.2Ni_0.13Co_0.13Mn_0.54O₂ cathode materials by combining the modification by a binder and Na⁺ ion doping strategies. We found that the sodium salt carboxymethyl cellulose (CMC) as a binder can significantly improve the cycling stability of the Li_1.2Ni_0.13Co_0.13Mn_0.54O₂ cathode materials with an initial discharge capacity of 291 mA h g⁻¹ and a capacity retention of over 79% after 500 cycles.¹¹⁸

3. Fundamental issues of the LMRO cathode materials

3.1. Synergistic effect mechanism between the Li₂MnO₃ phase and the LiMO₂ phase in the LMRO cathode materials

For the traditional layered LiMO₂ cathode materials, such as LiCoO₂, LiNi_0.5Mn_0.5O₂ and LiNi_0.33Co_0.33Mn_0.33O₂, their reversible capacities range from 130 to 160 mA h g⁻¹ with the upper cut-off charge voltage below 4.3 V vs. Li/Li⁺. In contrast, the reversible capacities of the LMRO cathode materials can be higher than 280 mA h g⁻¹ within a wider voltage range of 2.0–4.8 V vs. Li/Li⁺, which is nearly two times those of the traditional cathode materials. It has been reported that the LiCoO₂ cathode material can suffer from severe irreversible structure collapse when over 50% Li⁺ ions are extracted from its structure with a high operation potential window of over 4.4 V vs. Li/Li⁺.^119,120 In 1997, Numata et al.⁸⁹ firstly reported the LiCoO₂–Li₂MnO₃ solid solution as the cathode material for LIBs. In this solid solution, the Li₂MnO₃ component can effectively stabilize the structure of the LiCoO₂ component to improve its cycling stability. Moreover, it is surprising that the Co doped Li- and Mn-rich Li[Li_(1/3−x/3)Co_xMn_(2/3−2x/3)]O₂ cathode materials can deliver a discharge capacity of over 265 mA h g⁻¹ when cycled between 2.0 and 4.8 V vs. Li/Li⁺.^98,121,122 It was also found that the Ni doped Li- and Mn-rich Li[Ni_xLi_(1−2x)/3Mn_(2−x)/3]O₂ and Li[Li_(1−x)/3Mn_(2−x)/3Ni_x/3Co_x/3]O₂ cathode materials cycled between 2.0 and 4.8 V vs. Li/Li⁺ can deliver a discharge capacity of more than 230 mA h g⁻¹.^{11,12,21,23,54,105,108,109,123–132} The high electrochemical capacity of these cathode materials can be explained by the fact that, when charged to high potentials typically 4.5–4.8 V vs. Li/Li⁺, the extensive Li⁺ ions can be extracted from the Li₂MnO₃ component to yield an electrochemically active layered MnO₂ component and MnO₂ becomes LiMnO₂ during the discharge process, thereby enhancing the discharge capacity of these cathodes.^{96,97,133,134} A large number of efforts have been performed to improve the electrochemical performance of these materials by adjusting their components.

In order to explore the interaction between the Li₂MnO₃ and LiMO₂ components in the LMRO cathode materials, extensive efforts have been performed.^{78,84,107,135–138} Kumagai et al.¹⁰⁴ revealed that, for the Li(Li_(1−x/3)Co_xMn_(2−2x)/3)O₂ (0 < x < 1) cathode materials, the electrochemical capacity in the range between 0.2 < x < 0.6 increased during the initial few cycles, and then it slowly decreased with prolonged cycling; while in the range between 0.6 < x < 1, it exhibited a fast capacity loss with cycling (LiCoO₂ (x = 1)). In addition, Li(Li_0.2Co_0.4Mn_0.4)O₂ (x = 0.4) exhibited a high discharge capacity of 180 mA h g⁻¹ after 50 cycles, whereas Li₂MnO₃ and LiCoO₂ only showed a discharge specific capacity of 14 and 45 mA h g⁻¹ at the 50th cycle, respectively. Kim et al.¹³⁹ systematically studied the electrochemical behavior of the Li[Li_(1−x)/3Mn_(2−x)/3Ni_x/3Co_x/3]O₂ cathode series (0 < x < 1). The results demonstrated that the sample with x = 0.1 showed a low discharge capacity of 12 mA h g⁻¹; the sample with x = 0.5 showed the highest discharge capacity of 224 mA h g⁻¹; the sample with x = 1 delivered the lowest capacity retention. It can be concluded that the Mn element can effectively improve the electrochemical capacity and cycling stability of the LMRO cathode materials.

Moreover, Aurbach et al.¹⁴⁰ demonstrated that, in the xLi₂MnO₃-(1 − x)LiMn_1/3Ni_1/3Co_1/3O₂ (x = 0.3, 0.5, 0.7) cathode (Fig. 1), when x = 0.5, it showed the highest discharge capacity and rate capacity, and it demonstrated the best cycling stability with x = 0.7. The electrode with x = 0.3 showed the lowest discharge capacity and poor high rate capability. Ghanty et al.¹⁴¹ also investigated the electrochemical performance of the xLi₂MnO₃-(1 − x)Li(Mn_0.375Ni_0.375Co_0.25)O₂ (0 ≤ x ≤ 1) cathodes. As shown in Fig. 2(a and b), when x = 0.5, it showed a discharge capacity of 290 mA h g⁻¹ with an initial irreversible capacity loss (ICL) of 58 mA h g⁻¹ and a capacity retention of 76% after 50 cycles at 10 mA g⁻¹; when x = 0 and 0.25, it delivered the lowest discharge capacity, IRC and capacity retention; when x = 0.75 and 1, although it exhibited a lower discharge capacity, it had a higher IRC and higher capacity retention. Moreover, the results also indicated that the cathode with x = 0.25 showed a higher rate capability, but the cathode with x = 0.75 exhibited a poorer rate capability (Fig. 2(c)). Therefore, from the above reported results, it can be concluded that, in the LMRO cathode materials, the Li₂MnO₃ component can effectively stabilize the structure of the LiMO₂ component at high charge potential to improve its cycling stability.^142–144 Choi et al.¹⁴⁵ have revealed that the structure destruction of the Li[Ni_1/3Co_1/3Mn_1/3]O₂ cathode caused by the volume change during the charge/discharge process can be suppressed by modification of the Li₂MnO₃ component. Moreover, the activation of the Li₂MnO₃ component at high potential also significantly improves the electrochemical capacity of the LMRO cathode materials.¹⁴⁶ However, Li₂MnO₃ is also a low activity material which decreases the rate capability of the LMRO cathode materials.^{17–20,147–149} Moreover, Li₂MnO₃ can increase the ICL of the LMRO cathode materials. It is also found that the LiMO₂ component can significantly enhance the electrochemical activity of the Li₂MnO₃ component and the rate capability of the LMRO cathode materials.^21–26

It is clearly shown that there exists a synergistic effect between the Li₂MnO₃ component and the LiMO₂ component in the LMRO cathode materials. Our group has systematically investigated the relationship between the structures and the electrochemical performance of the Li_(2x+2)/(2+x)Ni_{(2−2x)/(6+3x)}Co_{(2−2x)/(6+3x)}Mn_{(2+4x)/(6+3x)}O₂ (XLNCMO) (0 ≤ X ≤1) cathode materials. The X-ray diffraction (XRD) with Rietveld refinement and high-resolution transmission electron microscopy (HRTEM) results demonstrated that the XLNCMO is composed of two phases, namely, a trigonal LiMO₂ phase (space group Rm) and a monoclinic Li₂MnO₃ phase (space group C2/m) (M = Ni, Co, Mn, Fe, Cr, etc.), and the two phases are intergrown on the nanoscale forming a nano dominated composition structure.^13–16 We revealed that there is an obvious synergistic effect between the Rm phase and the C2/m phase in the XLNCMO cathode materials with a mutually doped composite structure at the atomic level. As presented in Fig. 3(a and e), in the XLNCMO cathode materials, the C2/m phase can significantly improve the electrochemical capacity of the XLNCMO cathodes but it has a poor electrochemical activity. However, the Rm phase can activate the electrochemical activity of the C2/m phase, which can be called as a “catalyst”. Moreover, the C2/m phase can improve the cycling stability of the Rm phase during cycling which can be considered as a “stabilizer” (Fig. 3(b and f)). In addition, the Rm phase can effectively suppress the voltage fading of the XLNCMO cathode during cycling (Fig. 3(c and g)). It also should be noted that the C2/m phase can decrease the initial coulombic efficiency of the XLNCMO cathodes. Therefore, the synergistic effect between the Rm phase and the C2/m phase gives rise to the excellent overall electrochemical performance of the XLNCMO cathodes. The electrode with X = 0.5 demonstrated the best overall electrochemical performance with an initial capacity of 271 mA h g⁻¹ and an initial coulombic efficiency of 81% at a current density of 40 mA g⁻¹, enhanced cycling stability with a capacity retention of 96% after 120 cycles, and an excellent rate capability of 157 mA h g⁻¹ at 10C (200 mA g⁻¹) (Fig. 3(d and h)).¹⁵⁰

3.2. Contributions of Li, Ni, Co, Mn elements and O vacancies

In the LMRO cathode materials, the chemical states of the elements are Li⁺, Ni²⁺, Co³⁺, Mn⁴⁺, and O²⁻, respectively.^111,151 In the first charge process, in the first step from 2.0 to 4.4 V vs. Li/Li⁺, Li⁺ ions de-intercalate from the layered structure with the oxide of Ni²⁺/Ni⁴⁺ and Co³⁺/Co⁴⁺, and in the second step from 4.4 to 4.8 V, Li⁺ ions de-intercalate from the Li₂MnO₃ component accompanied by the O₂ release from the structure and then Li₂MnO₃ becomes an active MnO₂ component. At the following discharge process, Li⁺ ions reinsert into the layered structure accompanied by the reduction of Ni⁴⁺/Ni²⁺, Co⁴⁺/Co³⁺ and Mn⁴⁺/Mn³⁺.^80,81 It obviously indicates that Li, Ni, Co, Mn, and O play different roles in the LMRO cathode materials, which have a significant influence on their electrochemical performance.

3.3. Crystal structure of the LMRO cathode materials

It is clear that the LMRO cathode material is composed of the LiMO₂ component and the Li₂MnO₃ component. Fig. 4(a and b) show the trigonal LiMO₂ structure (space group: Rm, M = Co, Ni, Mn, Fe, Cr, etc.) and monoclinic Li₂MnO₃ structure (space group: C2/m) viewed from their [100] crystallographic direction, respectively. The Li₂MnO₃ structure can be reformulated with Li[Li_1/3Mn_2/3]O₂, which is very similar to the trigonal LiMO₂ structure. Therefore, it can be considered as a particular case of LiMO₂ with the TM layer consisting of a periodic sequence of one Li and two Mn atoms so that the Li is surrounded by six Mn atoms to form a honeycomb pattern (Fig. 4(c)). Both structures can be considered as a layered α-NaFeO₂-type rock salt structure, and all the octahedral sites are occupied by oxygen forming a close packed oxygen array structure.¹⁸² Presently the controversy focuses on whether the integrated LMRO material is a two-phase composite or a homogeneous solid solution. To understand the structural characteristics of the LMRO cathode materials is of great importance due to the strong correlation between the structure and the electrochemical performance. In this section, we will discuss the pristine structures of the LMRO cathode materials based on the average and local structures, as well as the phase diagram analysis.

3.4. Reaction mechanism of the LMRO cathode materials

In the past years, the mechanism of Li⁺ ion insertion/extraction from the LMRO cathodes has been extensively investigated. However, the real mechanism is still ambiguous, which cannot reasonably explain all electrochemical phenomena of the LMRO cathodes.^{29,35,92,97,196,228–234}

4. Challenges of the LMRO cathode materials

Amongst the reported cathode materials so far, the LMRO cathode materials, which can deliver a high specific capacity of over 280 mA h g⁻¹ and a high energy density of over 1000 W h kg⁻¹, have attracted much attention in recent years.^81,84 In addition, the LMRO cathode materials are economically attractive due to their high content of Mn, which is much cheaper and less toxic than Co and Ni. However, the LMRO cathode materials also suffer from several challenges: (1) large irreversible capacity loss (ICL) in the first cycle; (2) severe capacity/voltage fading during the cycling process; (3) poor rate capability.

4.1. High initial irreversible capacity of the LMRO cathode materials

The fundamentals of the high initial irreversible capacity of the LMRO cathode materials have been extensively investigated.^33,109 At present, it is accepted that the ICL of the LMRO cathode materials mainly originates from the release of oxygen and corrosion.^{32,109,248–250} It has been reported that, in the charge process of the LMRO cathode materials, the Li₂MnO₃ component needs to be activated at high voltages over 4.5 V to provide the high electrochemical capacity. In this process, the oxygen is released from the surface along with extensive Li⁺ ion extraction. The irreversible oxygen loss results in some of the extracted Li⁺ ions not being inserted back into the layered lattice in the subsequent discharge process, which results in an ICL of over 96 mA h g⁻¹ as calculated by eqn (3).³² Furthermore, the high ICL can also be attributed to the side reactions at the interphase between the cathode surface and the electrolyte to form Li₂CO₃, LiF etc. SEI layers, especially at high cutoff charge voltages over 4.6 V, and these reactions can consume the Li⁺ ions to reduce the reversible Li and consequently lead to the ICL of the LMRO cathode materials.^33,34

To date, it seems that the pre-activation of the Li₂MnO₃ component may be the best way to decrease the ICL of the LMRO cathode materials. The main way to pre-activate the Li₂MnO₃ component is acid treatment due to the formation of the active MnO₂ component.^55,251,252 Lu et al.¹¹⁵ also reported that the phase transformation from the Li₂MnO₃-type of structure to the spinel-like phase takes place in the surface regions of particles during the post annealing process, leading to the increase in initial coulombic efficiency from 78% to 93.4% (Fig. 22). Meanwhile, lots of studies showed that the pretreatment of the LMRO cathode materials by NH₃, H₂NO₃, Na₂S₂O₈ and (NH₄)₂S₂O₈ can effectively decrease the ICL due to the pre-activity of the Li₂MnO₃ phase.^54,55,253 Surface coating with VO₂, V₂O₅, Al₂O₃, Li₄Mn₅O₁₂, LiV₃O₈, and MoO₃ is also a very significant way to enhance the initial coulombic efficiency of the LMRO cathodes (Fig. 23).^{61,63,254,255} The surface coating, on the one hand, can inhibit the release of O₂ from the surface of the LMRO particles;^256–258 on the other hand, it can prevent the side reactions between the LMRO cathode materials and the electrolyte and prevent the formation of SEI films such as Li₂CO₃ and LiF.^33,34 Moreover, ion doping with K⁺, Na⁺, Ru⁴⁺, Fe³⁺, Mn⁴⁺ and Ti⁴⁺ can also improve the initial coulombic efficiency of the LMRO cathode materials.^77,259,260 It has been reported that Ti⁴⁺ and Ru⁴⁺ can form a stronger bond with O to suppress the release of O₂ in the first charge process.²⁵⁹

4.2. Capacity/voltage fading of the LMRO cathode materials

Nowadays, the greatest concern over the LMRO cathode materials is focused on their fast capacity and voltage fading. In this sub-section, we would like to discuss in detail the mechanisms and key factors which result in the capacity/voltage fading of the LMRO cathode materials.

4.3. Poor high rate capability of the LMRO cathode materials

Compared with the conventional layered LiNi_xMn_yCo_zO₂ (NMC) or LiMn₂O₄ spinel, the LMRO cathodes generally have lower conductivity due to the existence of the poorly conducting Li₂MnO₃ component.³²⁶ The relatively poor rate performance of the LMRO cathodes has to be taken into account when considering them as electrode materials, especially for practical applications in the EV and HEV fields. It is well known that the rate performance of the LMRO cathodes strongly depends on their kinetic factors, including the Li⁺ ion diffusion coefficient within the material structure and/or the charge transfer reactions that occur at the electrode/electrolyte interface.³²⁷

It has been widely considered that the low conductivity and poor kinetics of Li⁺ ion diffusion are the main reasons behind the poor rate capability of the LMRO cathodes.^39–44 Huang et al.³²⁸ found that the value of the D_Li⁺ decreased to its minimum at 4.55 V which might be associated with Ni²⁺ migration to occupy the 3b sites in the Li layers for the LMRO cathodes. In order to explore the rate controlled step of the LMRO cathodes, constant current potentiometric titration and electrochemical impedance spectroscopy (EIS) are carried out to calculate the kinetic parameters of the LMRO cathodes in the charge and discharge process (Fig. 31).^39,40 The results indicated that the activity of the Li₂MnO₃-like component controls the rate capability of the LMRO cathodes due to its large interfacial impedance and the poor kinetics of Li⁺ ion diffusion because it damages the electrode surface structure, leading to a high impedance.^43–45,329

Moreover, Xiao et al.⁴¹ reported that the formation of the spinel-like phase may be one of the main reasons leading to the poor kinetic performance of the LMRO cathodes (Fig. 32). Careful observation shows that the Li⁺ ion diffusion coefficients in the MnO₂ component are quite different between the charge and discharge process. The Li⁺ ion diffusion coefficient in the MnO₂ component is much higher during the initial Li⁺ ion de-intercalation process than that during the end of the Li⁺ ion intercalation process. This may be ascribed to severe concentration polarization at the end of the discharge process. At the beginning of the charge process, the cathode is fully lithiated, thus the Li⁺ ions can be easily removed from the surface lattice of the cathode particles. By contrast, at the end of the discharge process, most Li sites of the cathode particles have been fully lithiated, and it is much more difficult to find a Li vacancy in the cathode to insert more Li⁺ ions. Furthermore, it is also found that, during cycling, the cathode seems to show a slight increase of D_Li⁺ during the discharge processes. However, the layered-to-spinel structural transformation during the discharge process leads to voltage fading and may affect the Li⁺ ion diffusion process. However, the rate performance of this material is unsatisfactory with a significant increase of the polarization and a decrease of the discharge capacity observed in the voltage region below 3.5 V with an increase of cycling rates. The electrochemical kinetics of the Li[Li_0.2Ni_0.2Mn_0.6]O₂ cathode investigated by the galvanostatic intermittent titration technique (GITT) method demonstrate that the Li⁺ ion intercalation/de-intercalation reactions in this material are mainly controlled by Li₂MnO₃ and its activated MnO₂ components. The sluggish kinetics in the MnO₂ component plays an important role in determining the discharge capacity of the LMRO cathode, especially at high rates, while it shows much less effect on the charge process.

The kinetics of Li⁺ ion deintercalation in Li_1.12[Ni_0.5Co_0.2Mn_0.3]_0.89O₂ samples was studied by EIS and GITT.³³⁰ The D_Li⁺ values show analogical ∩−type variation in the full voltage range of 2.0–4.8 V, which is coincident with the behavior of Li⁺ deintercalation in Li_1.12[Ni_0.5Co_0.2Mn_0.3]_0.89O₂, and it greatly depends on the open-circuit voltage of the cell during the first charge process (Fig. 33(d and g)). The D_Li⁺ values calculated by EIS and GITT vary from 1.9 × 10⁻¹⁴ cm² s⁻¹ to 8.1 × 10⁻¹⁰ cm² s⁻¹ and 3.1 × 10⁻¹⁶ cm² s⁻¹ to 7.2 × 10⁻¹⁰ cm² s⁻¹, revealing that the electrode kinetics of Li_1.12[Ni_0.5Co_0.2Mn_0.3]_0.89O₂ is controlled by Li⁺ ion diffusion in the voltage range of 2.0–4.5 V. However, when the Li_1.12[Ni_0.5Co_0.2Mn_0.3]_0.89O₂ electrode is charged up to 4.5 V or higher the electrode kinetics of Li_1.12[Ni_0.5Co_0.2Mn_0.3]_0.89O₂ becomes controlled by the charge transfer reaction (Fig. 33(a–c, e and f)). Therefore, it cannot confirm the rate controlled step of the LMRO cathodes at present.

According to the above reasons, several corresponding strategies are performed: (1) ion doping/substitution with Na⁺, K⁺, Mg²⁺, Al³⁺, Ru³⁺, F⁻, B³⁻, etc. may be one of the best ways to improve the conductivity of the LMRO cathode materials. A large number of investigations have proved that ion doping/substitution can effectively improve the rate performance of layered oxide cathodes.^{70,72,331–338} (2) Surface coating which could stabilize the electrode/electrolyte interface, thus improving the ionic or/and electronic conductivity, has been repeatedly reported to enhance the rate performance of the LMRO cathode materials.^{59–69,312,339–341} In addition, conductive surface modification with conductive inert materials of carbon³⁴² as well as conducting polypyrrole,³⁴³ and ionic conductor Li₄Ti₅O₁₂ (ref. 344) is also a facile approach to enhance the rate capability of LMRO cathode materials. (3) Introducing a spinel-like phase on the surface of the bulk material can also effectively improve the rate capability of the LMRO cathode due to the 3D diffusion channel of the spinel-like phase.^{115,345–348} (4) Surface nitridation is also used to enhance the rate capability of the LMRO cathode materials by improving their surface conductivity.³⁴⁹ The details will be discussed in section 5.

4.4. Thermal stability of the LMRO cathode materials

The thermal stability of the LMRO cathode materials depends on the activation of the Li₂MO₃ component in the first cycle^14,262 and the structure transformation of the LMRO cathode materials during cycling.³⁵⁰ During the first charge, the thermal stability of the cathode is affected by charging over 4.5 V vs. Li⁺/Li (over 280 mA h g⁻¹ specific capacity). The probable cause is the formation of unstable oxidized oxygen in the later stage of Li₂MO₃ activation.²⁶²

Geder et al.³⁵¹ have systematically investigated the thermal stability of the LMRO cathode materials. They concluded that, for the LMRO electrodes with the same Li content, the onset temperature of decomposition during the second charge cycle is in fact higher than that during the first cycle. This could be due to the difference in the oxidation state of Ni, Co and Mn in the material during the first and the second charge–discharge. The enthalpy of decomposition of the electrode is observed to increase during the first charge cycle with the amount of Li removal, whereas enthalpies are much higher during the second charge cycle. The LMRO cathode material is found to be thermally more stable than LiCoO₂ but less stable than Li[Ni_1/3Co_1/3Mn_1/3]O₂. Overall, the amount of Li, amount of unstable oxygen, and oxidation state of Ni, Co and Mn all contribute to the thermal stability of the LMRO material, making it a very complicated system. Moreover, they found differences in the products of thermal decomposition of cathodes with the same Li content before and after the first charge by XRD and TGA-DSC analyses, as shown in Fig. 34. This further confirms the influence of the Li₂MO₃ component activation on the thermal stability of the active material. Further structural and calorimetric investigations of the material are underway to establish clear and distinct links between cycling-related structural changes and thermal stability as well as to elaborate the influence of long-term cycling and cut-off voltage on thermal stability.

Manthiram et al.³⁵² also found that the thermal stability of the LMRO cathode materials will decrease with an increasing amount of lithium vacancies in the charged sample as the vacancies may tend to get eliminated on heating. Furthermore, they revealed that the Ni- or Al-doped samples exhibit better thermal stability than the Li-doped samples with the same number of lithium vacancies at the fully charged state, implying that the nature of the constituent ions and the metal–oxygen bond strength have a profound effect on thermal stability. In addition, the oxyfluorides exhibit better thermal stability compared to the corresponding oxide analogs.

5. Improvement strategies and recent progress in the LMRO cathode materials

At present, significant improvements have been achieved for the LMRO cathode materials, such as enhanced initial coulombic efficiency, improved cycling performance and suppressed voltage fading, enhanced rate capability, by surface coating (with carbon, metal oxide, metal fluoride, metal phosphate, conversion materials, etc.),^353–368 ion doping (Li-site doping, TM-site doping and anion doping),^{246,369–378} developing new binders,^379–381 controlling the composition and morphology by various synthesis methods (co-precipitation, sol–gel, spray pyrolysis, freeze drying, spray drying, solid-state reaction with the assistance of molten salt, solvothermal, microwave irradiation and so on),^{143,144,147,152,382–385} and optimizing the electrolyte (including those based on ionic liquids and electrolyte additives).^{306,310,386–391} In this section, we will review the recent progress in overcoming these challenges in the LMRO cathode materials by various strategies.

5.1. Surface coating

Surface coating is an important strategy to improve the electrochemical performance by means of providing a protective layer to minimize the direct contact of the active material with the electrolyte or modifying the surface chemistry.³⁹² The surface coating has proven to be an effective way to improve the initial irreversible capacity, cycling performance, rate capability, and even thermal stability of the LMRO cathode materials.^{339,354,359,360,364,393–397} The main mechanisms for the positive effect of surface coating on the performance of the LMRO cathode materials include:⁸⁰ (1) forming a physical protection barrier that reduces the possible side reactions between the cathode materials and the electrolytes;^32,48,55 (2) suppressing metal ion dissolution from the cathode materials;^{35,59,66,265,291–293} (3) acting as a hydrogen fluoride (HF) scavenger to reduce the acidity of the non-aqueous electrolyte;^{35,59,66,265,291–293} and (4) modifying the cathode surface chemistry to improve the rate capability.^300,344 A series of coating materials, such as MnO_x,^59,60 Er₂O₃,²⁹⁴ Al₂O₃,^61,62,339 MoO₃,⁶³ TiO₂,⁶⁴ ZrO₂,⁶⁵ SiO₂,³⁹⁸ AlPO₄,^66,67 FePO₄,^312,340 Li₂TiO₃,³⁴¹ and AlF₃,^68,69 have been proven effective in improving the overall electrochemical performance of the LMRO cathode materials as displayed in Table 3.

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5.2. Ion doping/substitution

The ion doping strategy has been proved to be another effective way to improve the overall electrochemical performance of the LMRO cathodes, which includes cation ion doping, such as K⁺, Na⁺, Mg²⁺, Al³⁺, Ti⁴⁺, Nb⁵⁺, etc.,^{71,73,76,260,337,369,371,372,374,416–418} and anion ion doping, like F⁻, SO₄²⁻, PO₄³⁻, SiO₄⁴⁻, BO₃³⁻, BO₄⁵⁻, etc.,^{373,376,419,420} as shown in Table 4. The ion doping strategy is considered to suppress the formation of the spinel-like phase during cycling and enhance the electronic and ionic conductivity of the LMRO cathode materials.^{117,175,178,379,405,406,421,422} The performance, including electrochemical capacity, initial irreversible capacity, cycling performance and rate capability, can be improved by ion doping, through either affecting the microstructure or morphology or stabilizing the layered crystal structures.

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5.3. Nanostructured materials

Nanostructured materials have been extensively investigated in order to improve the electrochemical performance of the LMRO cathode materials, as shown in Table 5. As we all know, nanostructured materials can significantly decrease the diffusion pathway of Li⁺ ions in the insertion/extraction process, which can increase the high rate charge and discharge rate. Moreover, nanostructured materials can also increase surface/interface storage due to the large contact interface between the electrode material and the electrolyte. In addition, nanostructured materials can buffer the stresses caused by volume variation occurring during charge/discharge processes, and subsequently alleviate the capacity fading.^{188,431–456} Fu et al.⁴⁵⁷ have systematically investigated the relationship between the morphology and the electrochemical performance of the LMRO cathode materials. The electrochemical tests clearly illustrated that the performance of the different LMRO structures follows the order: microrods > microspheres> nanoplates > irregular particles. The distinct difference in the performance of the four LMRO cathode materials can be understood from their morphological and structural features. The microrods have a porous structure and 1D shape. The remarkable electrochemical performance of the LMRO microrods may result from the synergistic effect of the porous structure, 1D shape, nanoscale size, and robust microstructure. Firstly, the porous structure can provide large contact areas between the electrolyte and solid active material, more open channels for ion transfer, and more electrochemically active sites, which significantly improve the specific capacity and reaction kinetics. Secondly, the 1D shape can provide a short distance for Li⁺ ion diffusion along the confined radial dimension, facilitating Li⁺ ion diffusion.⁴³⁶ Lastly, the nanoscale size of the primary particle decreases the energy barrier for Li⁺ ion diffusion. Additionally, the robust secondary microstructure can enhance the structural integrity upon cycling and reduce the undesired side reactions, leading to superior cycling stability.

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Li et al.⁴³⁷ reported a hierarchical mesoporous Li[Li_0.2Ni_0.2Mn_0.6]O₂ cathode material composed of nanoparticles synthesized via ice templating. The as-prepared material exhibited remarkably enhanced electrochemical performance with a high capacity of 280.1 mA h g⁻¹, excellent cycling stability and superior rate properties. The enhanced electrochemical performance can be ascribed to the stable hierarchical microsized structure and the improved Li⁺ ion diffusion kinetics in the highly porous structure. Liu et al.⁴³⁴ reported an innovative approach to synthesize a three-dimensional (3D) nanoporous Li[Li_0.144Ni_0.136Co_0.136Mn_0.544]O₂ cathode material, directly occurring during deep chemical de-lithiation with carbon dioxide. The results illustrated that the as-prepared material presented a micrometer sized spherical structure that was typically composed of interconnected nanosized subunits with narrow distributed pores of 3.6 nm. As a result, this unique 3D micro-/nanostructure Li[Li_0.144Ni_0.136Co_0.136Mn_0.544]O₂ cathode material not only had a high tap density of over 2.20 g cm⁻³ but also exhibited excellent rate capability (197.6 mA h g⁻¹ at 1250 mA g⁻¹). The excellent electrochemical performance is ascribed to the unique nanoporous micro-nanostructure, which facilitates the Li⁺ ion diffusion and enhances the structural stability of the LMRO cathode materials. Wang et al.⁴³¹ prepared a hierarchical ball-in-ball hollow structure Li_1.2Mn_0.54Ni_0.13Co_0.13O₂ cathode material by a coprecipitation and two-step calcination method. The obtained cathode material delivered a discharge specific capacity of 193 mA h g⁻¹ at 750 mA g⁻¹ and a capacity retention of 87.6% after 400 cycles, and exhibited a high rate capacity of 132 mA h g⁻¹ at 10C; moreover, it also displayed a quite slow voltage fading of 240 mV and a high energy density of 668 W h kg⁻¹. The excellent electrochemical performance could be attributed to the combined merits of the multi-functional structure and composition, wherein the hierarchical hollow architecture facilitates efficient electron/ion transport and high structural stability, while multi-elemental components offer high reversible capacity. Wang et al.¹⁸⁸ reported an effective approach to fabricate a layered-spinel capped nanotube assembled 3D hierarchical architecture LMRO cathode material by a hydrothermal and ionic interfusion method. The unique 3D hollow hierarchical structure greatly shortens the pathways of the electron and Li ion transfer, while maintains the reliable structural stability. Moreover, the layered spinel multicomponent introduced more effective 3D Li⁺ ion diffusion channels (an excellent Li⁺ ion diffusion coefficient of 1.55 × 10⁻¹⁰ cm² S⁻¹) and offered a high coulombic efficiency. This 3D hierarchical architecture LMRO cathode material delivered a high capacity of 293 mA h g⁻¹ at 0.1C and a superior capacity retention of 89.5% after 200 cycles at 1C, and exhibited a high capacity of 202 mA h g⁻¹ even at 5C. The Li_1.2Ni_0.2Mn_0.6O₂ cathode material with a stable network flake structure has been synthesized through a facile resorcinol–formaldehyde (RF) organic carbon gel-assisted method. The stable network flake structure was assembled through a dense stack of nanoparticles with an average size of 50–200 nm. The Li_1.2Ni_0.2Mn_0.6O₂ cathode showed excellent rate capacity and cycling stability, and delivered an initial discharge capacity of 273.3 mA h g⁻¹ at 0.1C. When the discharge rate increased to 2C, an initial capacity of 196.7 mA h g⁻¹ and a capacity retention of 93.4% were yielded at a rate of 2C.⁴³³

5.4. Other strategies

Many other strategies were also developed to enhance the electrochemical performance of the LMRO cathode, including pre-activation,^54,55,253 surface treatment,³⁴⁹ integrated spinel-like phase and layered LMRO composites by structure design or pre-surface treatment,^253,461 developing new binders^379,380 and adjusting electrolyte components or additives,^{306,310,388,391} which are presented in Table 6.

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6. Applications of the LMRO cathode materials in full-cells

To date, there are several challenges on the practical applications of the LMRO cathodes in a full-cell configuration. The parameters and performance of the full-cells constructed with the LMRO as the cathode and different kinds of anodes are summarized in Table 7. It clearly shows that the LMRO cathodes in a full-cell system with silicon or graphite as the anode demonstrated excellent electrochemical performance.^474–476 Huang et al.⁴⁷⁵ reported that the Li_1.2Mn_0.534Ni_0.133Co_0.133O₂ cathode with silicon as the anode demonstrated an initial discharge capacity of 285.8 mA h g⁻¹, an initial coulombic efficiency of 83.3%, and a capacity retention of 93% after 180 cycles. In addition, impressive discharge capacities of 162.3 and 123.5 mA h g⁻¹ were obtained at high rates of 5C and 10C, respectively. Aurbach et al.⁴⁷⁷ found that the Li_1.2Ni_0.27Mn_0.40Co_0.13O₂ cathode with graphite as the anode exhibited an initial capacity of about 190 mA h g⁻¹ and a very stable cycle life of about 185 mA h g⁻¹ after 150 cycles at 0.2C. Zhou et al.⁴⁷⁸ systematically investigated the spherical Li[Li_0.2Ni_0.16Co_0.1Mn_0.54]O₂ cathode and silicon anode full-cell. The results showed that the particle size of the final product has an average diameter of about 10 μm, and the corresponding tap density was about 2.25 g cm⁻³. The electrochemical measurements indicated that the prepared cathode has a great initial columbic efficiency, reversible capacity, and cycling stability, which delivered a discharge specific capacity of 278 and 201 mA h g⁻¹ at 0.03C and 0.5C, respectively. When cycled at 0.1C, the Li[Li_0.2Ni_0.16Co_0.1Mn_0.54]O₂ cathode showed a discharge specific capacity of 226 mA h g⁻¹ with 95% retention capacity after 50 cycles. This full-cell illustrated a specific energy of 590 W h kg⁻¹ based on the total weight of the cathode and anode materials.

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Moreover, Qiu et al.⁴⁷⁹ reported that the Li_1.2Ni_0.15Mn_0.55Co_0.1O₂ cathode with Li₄Ti₅O₁₂ as the anode also showed excellent electrochemical performance with an initial discharge specific capacity of 232 mA h g⁻¹, an initial coulombic efficiency of 85%, and a capacity retention of 93% after 500 cycles. Chen et al.⁴⁸⁰ showed that, using Mn_0.8Co_0.2O as the anode, the 0.5Li₂MnO₃–0.5LiMn_0.5Ni_0.5O₂/Mn_0.8Co_0.2O full-cell can deliver a high reversible capacity of 205 mA h g⁻¹ and a particularly rather high volumetric energy density, which is about 31% higher than that of a Li-rich/graphite full-cell.

It has also been reported that the electrochemical performance of 18650 LIBs using Li_1.144Ni_0.136Co_0.136Mn_0.544O₂ as the cathode material and mesocarbon microbead (MCMB) as the anode material showed an excellent rate capability of 227 mA h g⁻¹ at 8C. In addition, it exhibited excellent cycle performance with a capacity retention of nearly 85% after 300 cycles in the voltage range of 2.5–4.5 V (vs. MCMB) at 0.2C.⁴⁷⁹

Another challenge of the LMRO cathode for assembling practical cells is its mismatch coulombic efficiency with the anode. The special coulombic efficiency match-up of the electrode materials is very crucial to achieve such a high energy density. The LMRO cathode materials have much higher reversible capacity (about 280 mA h g⁻¹) and energy density (1000 W h kg⁻¹) than other commercial cathodes but they have drawbacks of low initial coulombic efficiency (about 70–80%).⁸³ According to reported works, graphite anodes are hardly applied in the LMRO cathode full-cell systems because their low initial coulombic efficiency (usually 50–70%) would destroy a big fraction of the reversible capacity from the cathodes.^474,477 The efficiency loss is due to solid electrolyte interphase (SEI) formation by electrolyte decomposition, and the consumption of partial Li⁺ ions in the SEI film is irreversible in the initial charge–discharge process. However, it is surprising to find that the silicon and metal oxides anodes matched with LMRO cathode full-cell systems demonstrate a high coulombic efficiency of over 90%.^{475,476,478,480}

7. Prospects for future research on the LMRO cathode materials

The synergistic effect between the Li₂MnO₃ phase and LMO₂ phase in the LMRO cathode materials contributes to their high capacity of 280 mA h g⁻¹ and high-energy density of 1000 W h kg⁻¹. The high content Mn in the LMRO cathode materials can develop a nontoxic, less expensive, and high performance LMRO cathode. Therefore, the LMRO cathode material has been considered as a candidate cathode material for next generation high-energy density LIBs, especially in the EV field. However, several scientific issues and challenges need to be overcome before realizing their commercial applications, including their disputed crystal structures, ambiguous reaction mechanisms, high initial irreversible capacity, poor cycle life, fast voltage fading and poor rate capability.

This review demonstrates some of the pioneering ex situ and in situ material diagnostic studies that have been conducted in recent years to reveal the crystal structure and the electrochemical reaction mechanism, and to obtain deeper insights into the relationships between the structure and the electrochemical performance of the LMRO cathode materials. Furthermore, this review also discusses all kinds of strategies used to overcome the various challenges faced by the current LMRO cathode materials.

The recent research results demonstrate that the overall electrochemical performance of the LMRO cathode materials has been significantly improved. For example, the Mg ion doping in the LMRO cathode material enhanced the initial discharge specific capacity to 315 mA h g⁻¹, the coulombic efficiency to 87%, the capacity retention to 85% after 500 cycles and the rate capacity to 170 mA h g⁻¹ at 200 mA g⁻¹.⁴²⁵ The Er₂O₃ coating on the LMRO cathode material further importantly improved its overall electrochemical performance with an initial coulombic efficiency of 87% and almost no capacity decay after 300 cycles.²⁹⁴ Moreover, the Li[Li_0.2Ni_0.13Co_0.13Mn_0.54]O₂–0.4LiNiO₂ cathode with a Ni-rich bulk phase and an in situ precipitated Ni-rich spinel-like phase on the surface shows a large improvement in the initial average voltage of about 3.8 V and delivers an enhanced voltage retention of 94.1% and a capacity retention of 93.3% after 500 cycles.⁴²⁸ Even in the full-cell system, the LMRO cathode materials with a silicon anode also deliver a high electrochemical capacity of 285 mA h g⁻¹, an initial coulombic efficiency of 87%, a capacity retention of 93%, and a high rate capacity of 123 mA h g⁻¹ at a current density of 2500 mA g⁻¹.⁴⁷⁵ These technical indexes are far higher than those of the currently used cathode materials, such as LiCoO₂, LiFePO₄ and NCM listed in Table 1, which have completely met the technical requirements for use as cathodes in high-energy density LIB systems.

However, the practical applications of the LMRO cathode materials still face some challenges: firstly, the reported electrochemical performance at present is obtained under laboratory conditions; secondly, there are some technical issues that should be considered, such as the tap density of the electrode materials and the thickness of the electrode.

Conflicts of interest

There are no conflicts to declare.

Acknowledgements

This work was supported by the National Natural Science Foundation of PR China (No. 51571178), the Aerospace Science and Technology Innovation Fund of CASC, and the National Materials Genome Project (2016YFB0700600).

Notes and references

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