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• Reduction Roasting of Black Mass Recovered from NCM-based Spent Lithium-ion Batteries Using CH4 Gas
  Sang-Yeop Lee, Jae-Ho Hwang, Ho-Sang Sohn
  Resources Recycling.2025; 34(5): 93.     CrossRef

Transition metal chalcogenides are promising cathode materials for next-generation battery systems, particularly sodium-ion batteries. Ni₃Co₆S₈-pitch-derived carbon composite microspheres with a yolk-shell structure (Ni₃Co₆S₈@C-YS) were synthesized through a three-step process: spray pyrolysis, pitch coating, and post-heat treatment process. Ni₃Co₆S₈@C-YS exhibited an impressive reversible capacity of 525.2 mA h g^-1 at a current density of 0.5 A g^-1 over 50 cycles when employed as an anode material for sodium-ion batteries. However, Ni₃Co₆S₈ yolk shell nanopowder (Ni₃Co₆S₈-YS) without pitch-derived carbon demonstrated a continuous decrease in capacity during charging and discharging. The superior sodium-ion storage properties of Ni₃Co₆S₈@C-YS were attributed to the pitchderived carbon, which effectively adjusted the size and distribution of nanocrystals. The carbon-coated yolk-shell microspheres proposed here hold potential for various metal chalcogenide compounds and can be applied to various fields, including the energy storage field.

Lithium lanthanum titanium oxide (LLTO) is a promising ceramic electrolyte because of its high ionic conductivity at room temperature, low electrical conductivity, and outstanding physical properties. Several routes for the synthesis of bulk LLTO are known, in particular, solid-state synthesis and sol-gel method. However, the extremely low ionic conductivity of LLTO at grain boundaries is one of the major problems for practical applications. To diminish the grain boundary effect, the structure of LLTO is tuned to nanoscale morphology with structures of different dimensionalities (0D spheres, and 1D tubes and wires); this strategy has great potential to enhance the ion conduction by intensifying Li diffusion and minimizing the grain boundary resistance. Therefore, in this work, 0D spherical LLTO is synthesized using ultrasonic spray pyrolysis (USP). The USP method primarily yields spherical particles from the droplets generated by ultrasonic waves passed through several heating zones. LLTO is synthesized using USP, and the effects of each precursor and their mechanisms as well as synthesis parameters are analyzed and discussed to optimize the synthesis. The phase structure of the obtained materials is analyzed using X-ray diffraction, and their morphology and particle size are analyzed using field-emission scanning electron microscopy.

Tin/graphite composites are prepared as anode materials for Li-ion batteries using a dry ball-milling process. The main experimental variables in this work are the ball milling time (0–8 h) and composition ratio (tin:graphite=5:95, 15:85, and 30:70 w/w) of graphite and tin powder. For comparison, a tin/graphite composite is prepared using wet ball milling. The morphology and structure of the different tin/graphite composites are investigated using X-ray diffraction, Raman spectroscopy, energy-dispersive X-ray spectroscopy, and scanning and transmission electron microscopy. The electrochemical properties of the samples are also examined. The optimal dry ball milling time for the uniform mixing of graphite and tin is 6 h in a graphite-30wt.%Sn sample. The electrode prepared from the composite that is dry-ballmilled for 6 h exhibits the best cycle performance (discharge capacity after 50^th cycle: 308 mAh/g and capacity retention: 46%). The discharge capacity after the 50^th cycle is approximately 112 mAh/g, higher than that when the electrode is composed of only graphite (196 mAh/g after 50^th cycle). This result indicates that it is possible to manufacture a tin/graphite composite anode material that can effectively buffer the volume change that occurs during cycling, even using a simple dry ball-milling process.

Layered LiNi_0.83Co_0.11Mn_0.06O₂ cathode materials single- and dual-doped by the rare-earth elements Ce and Nd are successfully fabricated by using a coprecipitation-assisted solid-phase method. For comparison purposes, nondoping pristine LiNi_0.83Co_0.11Mn_0.06O₂ cathode material is also prepared using the same method. The crystal structure, morphology, and electrochemical performances are characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectrometer (EDS) mapping, and electrochemical techniques. The XRD data demonstrates that all prepared samples maintain a typical α-NaFeO₂-layered structure with the R-3m space group, and that the doped samples with Ce and/or Nd have lower cation mixing than that of pristine samples without doping. The results of SEM and EDS show that doped elements are uniformly distributed in all samples. The electrochemical performances of all doped samples are better than those of pristine samples without doping. In addition, the Ce/Nd dualdoped cathode material shows the best cycling performance and the least capacity loss. At a 10 C-rate, the electrodes of Ce/Nd dual-doped cathode material exhibit good capacity retention of 72.7, 58.5, and 45.2% after 100, 200, and 300 cycles, respectively, compared to those of pristine samples without doping (24.4, 11.1, and 8.0%).

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• Numerical approach for lithium-ion battery performance considering various cathode active material composition for electric vehicles using 1D simulation
  Heewon Choi, Nam-gyu Lim, Seong Jun Lee, Jungsoo Park
  Journal of Mechanical Science and Technology.2021; 35(6): 2697.     CrossRef
• Synthesis of CeVO4-V2O5 nanowires by cation-exchange method for high-performance lithium-ion battery electrode
  Xueliu Xu, Shiying Chang, Taofang Zeng, Yidan Luo, Dong Fang, Ming Xie, Jianhong Yi
  Journal of Alloys and Compounds.2021; 887: 161237.     CrossRef

This study investigates the viability of using a Na-ion battery with a tin(Sn) anode to mitigate the vulnerability caused by volume changes during discharge and charge cycling. In general, the volume changes of carbon material do not cause any instability during intercalation into its layer structure. Sn has a high theoretical capacity of 847 mAh g⁻¹. However, it expands dramatically in the discharge process by alloying Na-Sn, placing the electrode under massive internal stress, and particularly straining the binder over the elastic limit. The repeating strain results in loss of active material and its electric contact, as well as capacity decrease. This paper expands the scope of fabrication of Na-ion batteries with Sn by fabricating the binder as an auxetic structure with a unique feature: a negative Poisson ratio (NPR), which increases the resistance to internal stress in the Na-Sn alloying/de-alloying processes. Electrochemical tests and micrograph images of auxetic and common binders are used to compare dimensional and structural differences. Results show that the capacity of an auxetic-structured Sn electrode is much larger than that of a Sn electrode with a common-structured binder. Furthermore, using an auxetic structured Sn electrode, stability in discharge and charge cycling is obtained.

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• Highly Flexible and Conductive Electrodes through Combining Honeycomb and Butterfly Pattern Bio‐Inspired Structure for ECG Signal Recording
  Qi Hou, Min Wang, Chunyang Han, Kuiyang Gao, Ruiyao Liu, Guofeng Yao
  Advanced Materials Interfaces.2022;[Epub]     CrossRef

The high theoretical energy density (2600 Wh kg⁻¹) of Lithium-sulfur batteries and the high theoretical capacity of elemental sulfur (1672 mAh g⁻¹) attract significant research attention. However, the poor electrical conductivity of sulfur and the polysulfide shuttle effect are chronic problems resulting in low sulfur utilization and poor cycling stability. In this study, we address these problems by coating a polyethylene separator with a layer of activated carbon powder. A lithium-sulfur cell containing the activated carbon powder-coated separator exhibits an initial specific discharge capacity of 1400 mAh g⁻¹ at 0.1 C, and retains 63% of the initial capacity after 100 cycles at 0.2 C, whereas the equivalent cell with a bare separator exhibits a 1200 mAh g⁻¹ initial specific discharge capacity, and 50% capacity retention under the same conditions. The activated carbon powder-coated separator also enhances the rate capability. These results indicate that the microstructure of the activated carbon powder layer provides space for the sulfur redox reaction and facilitates fast electron transport. Concurrently, the activated carbon powder layer traps and reutilizes any polysulfides dissolved in the electrolyte. The approach presented here provides insights for overcoming the problems associated with lithium-sulfur batteries and promoting their practical use.

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• A one-step deposition method to prepare separators with carbon soot loading for lithium-sulfur battery
  Yueting Zhu, Jingjing Wang, Yanshu Wang, Ying Zhu, Yixuan Li, Shicheng Zhao
  Ionics.2022; 28(4): 1693.     CrossRef
• High thermal stability multilayered electrolyte complexes via layer-by-layer for long-life lithium-sulfur battery
  Jing Wang, Yufan Li, Xianmei Deng, Lei Yan, Zhiqiang Shi
  Ionics.2020; 26(11): 5481.     CrossRef

In this study, the compound Li₃BO₃ (LBO) is intended to be prepared by a polymeric complex method as a sintering aid for the densification of Li₇La₃Zr₂O₁₂ (LLZ) solid electrolyte. A polymeric precursor containing Li and B is heat-treated in an air atmosphere at a temperature range between 600°C and 800°C. Instead of LBO, the compound Li_2+xC_1-xB_xO₃ (LCBO) is unexpectedly synthesized after a heat-treatment of 700°C. The effect of LCBO addition on sintering behavior and ion conductivity of LLZ is studied. It is found that the LCBO compound could lead to significant improvements in the densification and ionic conductivity of LLZ compared to pure LLZ. After sintering at 1100°C, the density of the LLZ-12wt%LBO composite is 3.72 g/cm³, with a high Li-ion conductivity of 1.18 × 10⁻⁴ Scm^-1 at 28°C, while the pure LLZ specimen had a densify of 2.98 g/cm³ and Li-ion conductivity of 5.98 × 10⁻⁶ Scm^-1.

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• Characterization of Li1.5Al0.5Ge1.5(PO4)3 Solid Electrolyte with an Added Sintering Aid
  Hyun-Joon Lee, Liyu-Liu, Won-Jong Jeong, Seoung-Ki Lee, Bong-Ki Ryu
  Electronic Materials Letters.2023; 19(1): 55.     CrossRef

Ceramic powder, such as MgO, is added as a binder to prepare the green compacts of molten salts of an electrolyte for a thermal battery. Despite the addition of a binder, when the thickness of the electrolyte decreases to improve the battery performance, the problem with the unintentional short circuit between the anode and cathode still remains. To improve the current powder molding method, a new type of electrolyte separator with porous MgO preforms is prepared and characteristics of the thermal battery are evaluated. A Spherical PMMA polymer powder is added as a pore-forming agent in the MgO powder, and an organic binder is used to prepare slurry appropriate for tape casting. A porous MgO preform with 300 μm thickness is prepared through a binder burnout and sintering process. The particle size of the starting MgO powder has an effect, not on the porosity of the porous MgO preform, but on the battery characteristics. The porosity of the porous MgO preforms is controlled from 60 to 75% using a pore-forming agent. The batteries prepared using various porosities of preforms show a performance equal to or higher than that of the pellet-shaped battery prepared by the conventional powder molding method.

Fe₃O₄/Fe/graphene nanocomposite powder is synthesized by electrical wire explosion of Fe wire and dispersed graphene in deionized water at room temperature. The structural and electrochemical characteristics of the powder are characterized by the field-emission scanning electron microscopy, X-ray diffraction, Raman spectroscopy, field-emission transmission electron microscopy, cyclic voltammetry, and galvanometric discharge-charge method. For comparison, Fe₃O₄/Fe nanocomposites are fabricated under the same conditions. The Fe₃O₄/Fe nanocomposite particles, around 15-30 nm in size, are highly encapsulated in a graphene matrix. The Fe₃O₄/Fe/graphene nanocomposite powder exhibits a high initial charge specific capacity of 878 mA/g and a high capacity retention of 91% (798 mA/g) after 50 cycles. The good electrochemical performance of the Fe₃O₄/Fe/graphene nanocomposite powder is clearly established by comparison of the results with those obtained for Fe₃O₄/Fe nanocomposite powder and is attributed to alleviation of volume change, good distribution of electrode active materials, and improved electrical conductivity upon the addition of graphene.

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• Preparation of magnetic metal and graphene hybrids with tunable morphological, structural and magnetic properties
  Kyunbae Lee, Joonsik Lee, Byung Mun Jung, Byeongjin Park, Taehoon Kim, Sang Bok Lee
  Applied Surface Science.2019; 478: 733.     CrossRef

In the present work, we apply a technique that has been used for the expansion of graphite to multiwall carbon nanotubes (MWCNT). The nanotubes are rapidly heated for a short duration, followed by immersion in acid solution, so that they undergo expansion. The diameter of the expanded CNTs is 5-10 times larger than that of the asreceived nanotubes. This results in considerable swelling of the CNTs and opening of the tube tips, which may facilitate the accessibility of lithium ions into the inner holes and the interstices between the nanotube walls. The Li-ion storage capacity of the expanded nanotubes is measured by using the material as an anode in Li-ion cells. The result show that the discharge capacity of the expanded nanotubes in the first cycle is as high as 2,160 mAh/g, which is about 28% higher than that of the un-treated MWCNT anode. However, the charge/discharge capacity quickly drops in subsequent cycles and finally reaches equilibrium values of ~370 mAh/g. This is possibly due to the destruction of the lattice structures by repeated intercalation of Li ions.

Silicon alloys are considered promising anode active materials to replace Li-ion batteries by graphite powder, because they have a relatively high capacity of up to 4200 mAh/g, and are environmentally friendly and inexpensive ECO-materials. However, its poor charge/discharge properties, induced by cracking during cycles, constitute their most serious problem as anode electrode. In order to solve these problems, Si-Ge-Al alloys with porous structure are designed as anode alloy powders, to improve cycling stability. The alloys are melt-spun to obtain the rapidly solidified ribbons, and then ball-milled to make fine powders. The powders are etched using 1 M HCl solution, which gives the powders a porous structure by removing the element Al. Subsequently, in this study, the microstructures and the characteristics of the etched powders are evaluated for application as anode materials. As a result, the etched porous powder shows better electrochemical properties than as-milled Si-Ge-Al powder.

In this study, a finite element analysis approach is proposed to predict the fluid-structure interaction behavior of active materials for lithium-ion batteries (LIBs), which are mainly composed of graphite powder. The porous matrix of graphite powder saturated with fluid electrolyte is considered a representative volume element (RVE) model. Three different RVE models are proposed to consider the uncertainty of the powder shape and the porosity. Pwave modulus from RVE solutions are analyzed based on the microstructure and the interaction between the fluid and the graphite powder matrix. From the results, it is found that the large surface area of the active material results in low mechanical properties of LIB, which leads to poor structural durability when subjected to dynamic loads. The results obtained in this study provide useful information for predicting the mechanical safety of a battery pack.

Ni_1/3Co_1/3Mn_1/3(OH)₂ powders have been synthesized in a continuously stirred tank reactor via a co-precipitation reaction between aqueous metal sulfates and NaOH using NH₄OH as a chelating agent. The co-precipitation temperature is varied in the range of 30-80°C. Calcination of the prepared precursors with Li₂CO₃ for 8 h at 1000°C in air results in Li Ni_1/3Co_1/3Mn_1/3O₂ powders. Two kinds of obtained powders have been characterized by X-ray diffraction (XRD), scanning electron microscopy, particle size analyzer, and tap density measurements. The co-precipitation temperature does not differentiate the XRD patterns of precursors as well as their final powders. Precursor powders are spherical and dense, consisting of numerous acicular or flaky primary particles. The precursors obtained at 70 and 80°C possess bigger primary particles having more irregular shapes than those at lower temperatures. This is related to the lower tap density measured for the former. The final powders show a similar tendency in terms of primary particle shape and tap density. Electrochemical characterization shows that the initial charge/discharge capacities and cycle life of final powders from the precursors obtained at 70 and 80°C are inferior to those at 50°C. It is concluded that the optimum co-precipitation temperature is around 50°C.

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• A kinetic descriptor to optimize Co-precipitation of Nickel-rich cathode precursors for Lithium-ion batteries
  Seon Hwa Lee, Ki Young Kwon, Byeong Kil Choi, Hyun Deog Yoo
  Journal of Electroanalytical Chemistry.2022; 924: 116828.     CrossRef

Lithium-ion batteries (LIBs) are rapidly improving in capacity and life cycle characteristics to meet the requirements of a wide range of applications, such as portable electronics, electric vehicles, and micro- or nanoelectromechanical systems. Recently, atomic layer deposition (ALD), one of the vapor deposition methods, has been explored to expand the capability of LIBs by producing near-atomically flat and uniform coatings on the shell of nanostructured electrodes and membranes for conventional LIBs. In this paper, we introduce various ALD coatings on the anode, cathode, and separator materials to protect them and improve their electrochemical and thermomechanical stability. In addition, we discuss the effects of ALD coatings on the three-dimensional structuring and conduction layer through activation of electrochemical reactions and facilitation of fluent charge collection.

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• Atomic Layer Deposition for Powder Coating
  Seok Choi, Jeong Hwan Han, Byung Joon Choi
  Journal of Korean Powder Metallurgy Institute.2019; 26(3): 243.     CrossRef
• Formation of Uniform SnO2 Coating Layer on Carbon Nanofiber by Pretreatment in Atomic Layer Deposition
  Dong Ha Kim, Doh-Hyung Riu, Byung Joon Choi
  journal of Korean Powder Metallurgy Institute.2018; 25(1): 43.     CrossRef

As precursors of cathode materials for lithium ion batteries, Ni_1/3Co_1/3Mn_1/3(OH)₂ powders are prepared in a continuously stirred tank reactor via a co-precipitation reaction between aqueous metal sulfates and NaOH in the presence of NH4OH in air or nitrogen ambient. Calcination of the precursors with Li₂CO₃ for 8 h at 1,000°C in air produces dense spherical cathode materials. The precursors and final powders are characterized by X-ray diffraction (XRD), scanning electron microscopy, particle size analysis, tap density measurement, and thermal gravimetric analysis. The precursor powders obtained in air or nitrogen ambient show XRD patterns identified as Ni_1/3Co_1/3Mn_1/3(OH)₂. Regardless of the atmosphere, the final powders exhibit the XRD patterns of LiNi_1/3Co_1/3Mn_1/3O₂ (NCM). The precursor powders obtained in air have larger particle size and lower tap density than those obtained in nitrogen ambient. NCM powders show similar tendencies in terms of particle size and tap density. Electrochemical characterization is performed after fabricating a coin cell using NCM as the cathode and Li metal as the anode. The NCM powders from the precursors obtained in air and those from the precursors obtained in nitrogen have similar initial charge/discharge capacities and cycle life. In conclusion, the powders co-precipitated in air can be utilized as precursor materials, replacing those synthesized in the presence of nitrogen injection, which is the usual industrial practice.

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• Stabilization of High Nickel Cathode Materials with Core-Shell Structure via Co-precipitation Method
  Minjeong Kim, Soonhyun Hong, Heongkwon Jeon, Jahun Koo, Heesang Lee, Gyuseok Choi, Chunjoong Kim
  Korean Journal of Materials Research.2022; 32(4): 216.     CrossRef
• Spherical agglomeration of nickel-manganese-cobalt hydroxide in turbulent Batchelor vortex flow
  Xiaotong Sun, Jinsoo Kim, Woo-Sik Kim
  Chemical Engineering Journal.2021; 421: 129924.     CrossRef
• Design strategies for development of nickel-rich ternary lithium-ion battery
  Kyu Hwan Choi, Xuyan Liu, Xiaohong Ding, Qiang Li
  Ionics.2020; 26(3): 1063.     CrossRef
• Effect of Single and Dual Doping of Rare Earth Metal Ce and Nd Elements on Electrochemical Properties of LiNi_0.83 Co_0.11Mn_0.06O₂ Cathode Lithium-ion Battery Material
  Yoo-Young Kim, Jong-Keun Ha, Kwon-Koo Cho
  Journal of Korean Powder Metallurgy Institute.2019; 26(1): 49.     CrossRef
• Effects of Precursor Co-Precipitation Temperature on the Properties of LiNi1/3Co1/3Mn1/3O2 Powders
  Woonghee Choi, Chan Hyoung Kang
  Journal of Korean Powder Metallurgy Institute.2016; 23(4): 287.     CrossRef

Anodic aluminum oxide (AAO) has been widely used for the development and fabrication of nano-powder with various morphologies such as particle, wire, rod, and tube. So far, many researchers have reported about shape control and fabrication of AAO films. However, they have reported on the shape control with different diameter and length of anodic aluminum oxide mainly. We present a combined mild-hard (or hard-mild) anodization to prepare shape-controlled AAO films. Two main parameters which are combination mild-hard (or hard-mild) anodization and run-time of voltage control are applied in this work. The voltages of mild and hard anodization are respectively 40 and 80 V. Anodization was conducted on the aluminum sheet in 0.3 mole oxalic acid at 4°C. AAO films with morphologies of varying interpore distance, branch-shaped pore, diameter-modulated pore and long funnel-shaped pore were fabricated. Those shapes will be able to apply to fabricate novel nano-materials with potential application which is especially a support to prevent volume expansion of inserted active materials, such as metal silicon or tin powder, in lithium ion battery. The silicon powder electrode using an AAO as a support shows outstanding cycle performance as 1003 mAh/g up to 200 cycles.

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• Nano silicon encapsulated in modified copper as an anode for high performance lithium ion battery
  Jong-Keun Ha, Anupriya K. Haridas, Gyu-Bong Cho, Hyo-Jun Ahn, Jou-Hyeon Ahn, Kwon-Koo Cho
  Applied Surface Science.2019; 481: 307.     CrossRef

The composite of porous silicon (Si) and amorphous carbon (C) is prepared by pyrolysis of a nano-porous Si + pitch mixture. The nano-porous Si is prepared by mechanical milling of magnesium powder with silicon monoxide (SiO) followed by removal of MgO with hydrochloric acid (etching process). The Brunauer-Emmett-Teller (BET) surface area of porous Si (64.52 m²g⁻¹) is much higher than that before etching Si/MgO (4.28 m²g⁻¹) which indicates pores are formed in Si after the etching process. Cycling stability is examined for the nano-porous Si + C composite and the result is compared with the composite of nonporous Si + C. The capacity retention of the former composite is 59.6% after 50 charge/discharge cycles while the latter shows only 28.0%. The pores of Si formed after the etching process is believed to accommodate large volumetric change of Si during charging and discharging process.

The effects of particle size of Li-Si alloy and LiCl-KCl addition as a binder phase for raw material of anode were investigated on the formability of the thermal battery anode. The formability was evaluated with respect to filling density, tap density, compaction density, spring-back and compressive strength. With increasing particle size of Li-Si alloy powder, densities increased while spring-back and compressive strength decreased. Since the small spring-back is beneficial to avoiding breakage of pressed compacts, larger particles might be more suitable for anode forming. The increasing amount of LiCl-KCl binder phase contributed to reducing spring-back, improving the formability of anode powder too. The control of particle size also seems to be helpful to get double pressed pellets, which consisted of two layer of anode and electrolyte.

The electrochemical properties of cells assembled with the LiNiO₂ (LNO) recycled from cathode materials of waste lithium secondary batteries (Li[Ni,Co,Mn]O₂), were evaluated in this study. The leaching, neutralization and solvent extraction process were applied to produce high-purity NiSO₄ solution from waste lithium secondary batteries. High-purity NiO powder was then fabricated by the heat-treatment and mixing of the NiSO₄ solution and H₂C₂O₄. Finally, LiNiO₂ as a cathode material for lithium ion secondary batteries was synthesized by heat treatment and mixing of the NiO and Li₂CO₃ powders. We assembled the cells using the LiNiO₂ powders and evaluated the electrochemical properties. Subsequently, we evaluated the recycling possibility of the cathode materials for waste lithium secondary battery using the processes applied in this work.

FeS₂ has been widely used for cathode materials in thermal battery because of its high stability and current capability at high operation temperature. Salts such as a LiCl-KCl were added as a binder for improving electrical performance and formability of FeS₂ cathode powder. In this study, the effects of the addition of Li₂O in LiCl-KCl binder on the formability of FeS₂ powder compact were investigated. With the increasing amount of Li₂O addition to LiCl-KCl binder salts, the strength of the pressed compacts increased considerably when the powder mixture were pre-heat-treated above 350°C. The heat-treatment resulted in promoting the coating coverage of FeS₂ particles by the salts as Li₂O was added. The observed coating as Li₂O addition might be attributed to the enhanced wettability of the salt rather than its reduced melting temperature. The high strength of compacts by the Li₂O addition and pre-heat-treatment could improve the formability of FeS₂ raw materials.

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• Effects of Particle Size and Binder Phase Addition on Formability of Li-Si Alloy Powder for Thermal Battery Anode
  Sung-Soo Ryu, Hui-Sik Kim, Seongwon Kim, Hyung-Tae Kim, Hae-Won Cheong, Sung-Min Lee
  Journal of Korean Powder Metallurgy Institute.2014; 21(5): 331.     CrossRef

Cathode materials and their precursors are prepared with transition metal solutions recycled from the the waste lithium-ion batteries containing NCM (nickel-cobalt-manganese) cathodes by a H₂ and C-reduction process. The recycled transition metal sulfate solutions are used in a co-precipitation process in a CSTR reactor to obtain the transition metal hydroxide. The NCM cathode materials (Ni:Mn:Co=5:3:2) are prepared from the transition metal hydroxide by calcining with lithium carbonate. X-ray diffraction and scanning electron microscopy analyses show that the cathode material has a layered structure and particle size of about 10 μm. The cathode materials also exhibited a capacity of about 160 mAh/g with a retention rate of 93~96% after 100 cycles.