• Journal of Powder Materials
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• v.23 no.2
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• pp.136-142
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• 2016

As precursors of cathode materials for lithium ion batteries, $Ni_{1/3}Co_{1/3}Mn_{1/3}(OH)_2$ powders are prepared in a continuously stirred tank reactor via a co-precipitation reaction between aqueous metal sulfates and NaOH in the presence of $NH_4OH$ in air or nitrogen ambient. Calcination of the precursors with $Li_2CO_3$ for 8 h at $1,000^{\circ}C$ 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 $Ni_{1/3}Co_{1/3}Mn_{1/3}(OH)_2$. Regardless of the atmosphere, the final powders exhibit the XRD patterns of $LiNi_{1/3}Co_{1/3}Mn_{1/3}O_2$ (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.

• Korean Journal of Materials Research
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• v.34 no.10
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• pp.475-481
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• 2024

Lithium-ion batteries are widely used in various advanced devices, including electric vehicles and energy storage devices. As the application range of lithium-ion batteries expands, it will be increasingly important to improve their gravimetric and volumetric energy density. Layer-structured oxide materials have been widely adopted as cathode materials in Li-ion batteries. Among them, LiNiO₂ has attracted interest because of its high theoretical capacity, ~274 mAh g^-1, assuming reversible one Li⁺-(de)intercalation from the structure. Presently, such layered structure cathode materials are prepared by calcination of precursors. The precursors are typically hydroxides synthesized by coprecipitation reaction. Precursors synthesized by coprecipitation reaction have a spherical morphology with a size larger than 10 ㎛. Spherical precursors in the several micrometer range are difficult to obtain due to the limited coprecipitation reaction time, and can lead to vigorous collisions between the precursor particles. In this study, spherical and small-sized Ni(OH)₂ precursors were synthesized using a new synthesis method instead of the conventional precipitation method. The highest capacity, 170 mAh g^-1, could be achieved in the temperature range of 730~760 ℃. The improved capacity was confirmed to be due to the higher quality of the layered structure.

• Journal of the Korean Ceramic Society
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• v.43 no.7 s.290
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• pp.402-407
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• 2006

NiO/YSZ(70 wt%NiO) composite powders were prepared by ball-milling of 8YSZ and NiO precursors, dried and then followed by calcination. The approach was to combine acidic $Ni(NO_3)_2{\cdot}6H_2O$ and basic $2NiCO_3{\cdot}3Ni(OH)_2{\cdot}4H_2O$ via acid-base reaction as a mixed NiO precursor. Their effects were studied in the aspects of DSC, microstructure, porosity, and electrical conductivity. Ni/YSZ composite of 1N9C (1 mole NiO from the nitrate and 9 moles of NiO from the carbonate) was prepared by consolidation at $1400^{\circ}C$ for 3 h, and then followed by reduction at $1000^{\circ}C$ for 3 h under flowing of 6% $H_2/N_2$. It showed a homogeneous microstructure with ${\sim}20%$ porosity and 1880 S/cm at $1000^{\circ}C$.

• Journal of Powder Materials
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• v.23 no.4
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• pp.287-296
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• 2016

$Ni_{1/3}Co_{1/3}Mn_{1/3}(OH)_2$ powders have been synthesized in a continuously stirred tank reactor via a co-precipitation reaction between aqueous metal sulfates and NaOH using $NH_4OH$ as a chelating agent. The co-precipitation temperature is varied in the range of $30-80^{\circ}C$. Calcination of the prepared precursors with $Li_2CO_3$ for 8 h at $1000^{\circ}C$ in air results in Li $Ni_{1/3}Co_{1/3}Mn_{1/3}O_2$ 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 $80^{\circ}C$ 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 $80^{\circ}C$ are inferior to those at $50^{\circ}C$. It is concluded that the optimum co-precipitation temperature is around $50^{\circ}C$.

• Journal of the Korean Electrochemical Society
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• v.16 no.4
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• pp.191-197
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• 2013

The one of the cathode material, $Li(Ni_{0.5}Co_{0.2}Mn_{0.3})O_2$, was synthesized by the precursor, $Ni_{0.5}Co_{0.2}Mn_{0.3}(OH)_2$, from the co-precipitation method and the morphologies of the primary particle of precursors were flake and needle-shape by controlling the precipitation parameters. Identical powder properties, such as particle size, tap density, chemical composition, were obtained by same process of lithiation and heat-treatment. The relation between electrochemical performances of $Li(Ni_{0.5}Co_{0.2}Mn_{0.3})O_2$ and the primary particle morphology of precursors was analyzed by SEM, XRD and EELS. In the $Li(Ni_{0.5}Co_{0.2}Mn_{0.3})O_2$ cathode from the needle-shape precursor, the primary particle size was smaller than that from flake-shape precursor and high Li concentration at grain edge comparing grain center. The cycle and rate performances of the cathode from needle-shape precursor shows superior to those from flake-shape precursor, which might be attributed to low charge-transfer resistance by impedance measurement.

• Journal of Sensor Science and Technology
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• v.23 no.3
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• pp.211-215
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• 2014

The Pt-, Ni- and Cr-decorated tubular $SnO_2$ nanofibers for gas sensors were prepared by the electrospinning of polyvinylpyrrolidone (PVP) nanofibers containing Pt, Ni, and Cr precursors, the sputtering of $SnO_2$ on the electrospun PVP nanofibers, and the removal of sacrificial PVP parts by heat treatment at $600^{\circ}C$ for 2 h. Pt-decorated tubular $SnO_2$ nanofibers showed high response ($R_a/R_g=210.5$, $R_g$: resistance in gas, $R_a$: resistance in air) to 5 ppm $C_2H_5OH$ at $350^{\circ}C$ with negligible cross-responses to other interference gases (5 ppm trimethylamine, $NH_3$, HCHO, p-xylene, toluene and benzene). Cr-decorated tubular $SnO_2$nanofibers showed the selective detection of p-xylene at $400^{\circ}C$. In contrast, no significant selectivity to a specific gas was found in Ni-decorated tubular $SnO_2$ nanofibers. The selective and sensitive detection of gases using Pt-decorated and Cr-decorated tubular $SnO_2$ nanofibers were discussed in relation to the catalytic promotion of gas sensing reaction.

• Korean Journal of Materials Research
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• v.26 no.11
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• pp.649-655
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• 2016

Ni nanoparticles (NPs)-graphitic carbon nanofiber (GCNF) composites were fabricated using an electrospinning method. The amounts of Ni precursor used as catalyst for the catalytic graphitization were controlled at 0, 2, 5, and 8 wt% to improve the photovoltaic performances of the nanoparticles and make them suitable for use as counter electrodes for dye-sensitized solar cells (DSSCs). As a result, Ni NPs-GCNF composites that were fabricated with 8 wt% Ni precursors showed a high circuit voltage (0.73 V), high photocurrent density ($14.26mA/cm^2$), and superb power-conversion efficiency (6.72%) when compared to those characteristics of other samples. These performance improvements can be attributed to the reduced charge transport resistance that results from the synergetic effect of the superior catalytic activity of Ni NPs and the efficient charge transfer due to the formation of GCNF with high electrical conductivity. Thus, Ni NPs-GCNF composites may be used as promising counter electrodes in DSSCs.

• Journal of the Microelectronics and Packaging Society
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• v.22 no.3
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• pp.45-50
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• 2015

The goal of this research is the create novel magnets with no rare-earth contents, with larger energy product by comparison with currently used ferrites. For this purpose we developed nano-sized hard-type/soft-type composite ferrite in which high remanent magnetization (Mr) and high coercivity (Hc). Nano-sized Ba-ferrite, Ni-Zn ferrite and $BaFe_{12}O_{19}/Ni_{0.5}Zn_{0.5}Fe_2O_4$ composite ferrites were prepared by sol-gel combustion method by use of glicine-nitrate and citric acid. Nanocomposite ferrites were calcined at temperature range $700-900^{\circ}C$ for 1h. According to the X-ray diffraction patterns and FT-IR spectra, single phase of NiZn-ferrite and Ba-ferrite were detected and hard/soft nanocomposite ferrite was indicated to the coexistence of the magnetoplumbite-structural $BaFe_{12}O_{19}$ and spinel-structural $Ni_{0.5}Zn_{0.5}Fe_2O_4$ that agreed with the standard JCPDS 10-0325 data. The particle size of nanocomposite turn out to be less than 120 nm. The nanocomposite ferrite shows a single-phase magnetization behavior, implying that the hard magnetic phase and soft magnetic phase were well exchange-coupled. The specific saturation magnetization ($M_s$) of the nanocomposite ferrite is located between hard ($BaFe_{12}O_{19}$) and soft ferrite($Ni_{0.5}Zn_{0.5}Fe_2O_4$). The remanence (Mr) of nanocomposite ferrite is much higher than that of the individual $BaFe_{12}O_{19}$ and $Ni_{0.5}Zn_{0.5}Fe_2O_4$ ferrite, and $(BH)_{max}$ is increased slightly.

• Journal of the Korean Electrochemical Society
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• v.8 no.1
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• pp.42-46
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• 2005

It has been known that the synthesis of the cathode materials for the lithium rechargeable batteries by the sol-gel process has many advantages over the conventional solid-state method. It has been, however, a continuing issue that new additional steps should be introduced to commercialize this process. In this work, spray drying was introduced to the existing sol-gel process as a continuous mass production method of the pre-heat treatment precursor materials. The precursors of $LiCoO_2$ and $LiNi_{0.8}Co_{0.2}O_2$ were continuously produced through spray drying from the solution containing stoichiometric amount of lithium, cobalt, and nickel sources as well as a chelating agent. The process variables, such as pH of the starting solution, spray drying conditions, and calcination conditions were optimized. The XRD pattern for the synthesized material indicated a good crystallinity with a layered structure.

• Resources Recycling
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• v.28 no.5
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• pp.60-67
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• 2019

A valuable metal recovery from waste resources such as spent rechargeable secondary batteries is of critical issues because of a sharp increase in the amount of waste resources. In this context, it is necessary to research not only recycling waste lithium-ion batteries (LIBs), but also reusing valuable metals (e.g., Li, Co, Ni, Mn etc.) recovered from waste LIBs. In particular, the lithium hydroxide ($LiOH{\cdot}xH_2O$), which is of precursors that can be prepared by the recovery of Li in waste LIBs, can be reused as a catalyst, a carbon dioxide absorbent, and again as a precursor for cathode materials of LIB. However, most studies of recycling the waste LIBs have been focused on the preparation of lithium carbonate with a recovery of Li. Herein, we show the preparation of high purity lithium hydroxide powder along with the precipitation process, and the systematic study to find an optimum condition is also carried out. The lithium carbonate, which is recovered from waste LIBs, was used as starting materials for synthesis of lithium hydroxide. The optimum precipitation conditions for the preparation of LiOH were found as follows: based on stirring, reaction temperature $90^{\circ}C$, reaction time 3 hr, precursor ratio 1:1. To synthesize uniform and high purity lithium hydroxide, 2-step precipitation process was additionally performed, and consequently, high purity $LiOH{\cdot}xH_2O$ powder was obtained.