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.

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

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

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.

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.