• Journal of the Korean Crystal Growth and Crystal Technology
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• v.27 no.2
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• pp.70-74
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• 2017

Two milling methods, dry vibration milling and wet ball milling, were used to prepare $Na_{2/3}(Ni_{1/3}Mn_{2/3})O_2$ powders as a cathode material for sodium ion batteries. The morphology and electrochemical property of the two powders with different milling processes were compared to each other. The particle size is less than $1{\mu}m$ in the dry vibration milled powder, while lots of larger particles than $1{\mu}m$ were found in the wet ball milled one. The single phase of $Na_{2/3}(Ni_{1/3}Mn_{2/3})O_2$ was obtained in the temperature range of $875{\sim}900^{\circ}C$. The discharge capacity and discharge voltage of the powder prepared by the dry process were higher than those of one prepared by the wet process.

• Proceedings of the Korean Vacuum Society Conference
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• 2012.08a
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• pp.79-79
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• 2012

A high temperature and a low temperature plasma process technologies were developed and demonstrated for synthesis, hybrid formation, surface treatment and CVD engineering of nano powder. RF thermal plasma is used for synthesis of spherical nano particles in a diameter ranged from 10 nm to 100 nm. A variety of nano particules such as Si, Ni, has been synthesized. The diameter of the nano-particles can be controlled by RF plasma power, pressure, gas flow rate and raw material feed rate. A modified RF thermal plasma also produces nano hybrid materials with graphene. Hemispherical nano-materials such as Ag, Ni, Si, SiO2, Al2O3, size ranged from 30 to 100 nm, has been grown on graphene nanoplatelet surface. The coverage ranged from 0.1 to 0.7 has been achieved uniformly over the graphene surface. Low temperature AC plasma is developed for surface modification of nano-powder. In order to have a three dimensional and lengthy plasma treatment, a spiral type of reactor has been developed. A similar plasma reactor has been modfied for nano plasma CVD process. The reactor can be heated with halogen lamp.

• Journal of Magnetics
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• v.7 no.2
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• pp.29-39
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• 2002

The initial NiCuZn synthetic ferrite were acquired from thermally decomposing the metal nitrates $Fe(NO_3)_39H_2O, Zn(NO_3)_26H_2O, Ni(NO_3)_26H_2O, and Cu(NO_3)_23H_2O$ at $150^circ{C}$ for 24 hours, and then we calcined the synthetic powder at $500^circ{C}$, pulverized each of those for 3, 6, 9, 12, and 15 hours in a steel ball mill, sintered each at $700^circ{C}$ to $1,000^circ{C}$ for 1 hour, and thus studied their microstructures and electromagnetic properties. We could make the initial specimens chemically bonded in liquidity at a low-temperature $150^circ{C}$, by using the low melting points less than $200^circ{C}$ of the metal nitrates instead of the mechanical ball-mill pulverization, then narrow a distance between the particles into a molecular one, and thus lower the reaction point of sintering by at least $200^circ{C}$ to $300^circ{C}$. Their initial permeability was 50 to 400 and their maximum magnetic induction density and coercive force, 2,400 G and 0.3 Oe to 0.5 Oe respectively, which was similar to those of NiZnCu ferrite synthesized in the conventional process. In the graph of initial permeability by frequencies, a $180^circ{C}$ rotation of the magnetic domains which appears in a broad band of micro-wave before and after the resonance frequency, could be perceived.

• Proceedings of the Korean Powder Metallurgy Institute Conference
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• 1996.11a
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• pp.6-6
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• 1996

Ceramic based nanocomposite, in which nano-sized ceramics and metals were dispersed within matrix grains and/or at grain boundaries, were successfully fabricated in the ceramic/cerarnic and ceramic/metal composite systems such as $Al_2O_3$/SiC, $Al_2O_3$/$Si_3N_4$, MgO/SiC, mullite/SiC, $Si_3N_4/SiC, $Si_3N_4$/B, $Al_2O_3$/W, $Al_2O_3$/Mo, $Al_2O_3$/Ni and $ZrO_2$/Mo systems. In these systems, the ceramiclceramic composites were fabricated from homogeneously mixed powders, powders with thin coatings of the second phases and amorphous precursor composite powders by usual powder metallurgical methods. The ceramiclmetal nanocomposites were prepared by combination of H2 reduction of metal oxides in the early stage of sinterings and usual powder metallurgical processes. The transmission electron microscopic observation for the $Al_2O_3$/SiC nanocomposite indicated that the second phases less than 70nm were mainly located within matrix grains and the larger particles were dispersed at the grain boundaries. The similar observation was also identified for other cerarnic/ceramic and ceramiclmetal nanocornposites. The striking findings in these nanocomposites were that mechanical properties were significantly improved by the nano-sized dispersion from 5 to 10 vol% even at high temperatures. For example, the improvement in hcture strength by 2 to 5 times and in creep resistance by 2 to 4 orders was observed not only for the ceramidceramic nanocomposites but also for the ceramiclmetal nanocomposites with only 5~01%se cond phase. The newly developed silicon nitride/boron nitride nanocomposites, in which nano-sized hexagonal BN particulates with low Young's modulus and fracture strength were dispersed mainly within matrix grains, gave also the strong improvement in fracture strength and thermal shock fracture resistance. In presentation, the process-rnicro/nanostructure-properties relationship will be presented in detail. The special emphasis will be placed on the understanding of the roles of nano-sized dispersions on mechanical properties.

• Journal of the Korean Ceramic Society
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• v.45 no.2
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• pp.112-118
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• 2008

To prepare the high-capacity cathode material with improved electrochemical performances, nanoparticles of $C0_3(PO_4)_2$ were coated on the powder surface of $Li[Co_{0.1}Ni_{0.15}Li_{0.2}Mn_{0.55}]O_2$, which was already synthesized by simple combustion method. The coated powders after the heat treatment at >$700^{\circ}C$ surely showed well-structured crystalline property with nanoscale surface coating layer, which was consisted of $LiCOPO_4$ phase formed from the reaction bwtween $CO_3(PO_4)_2$ and lithium impurities. In addition, cycle performance was particularly improved by the $CO_3(PO_4)_2$-coating for the cathode material for lithium rechargeable batteries.

• Bulletin of the Korean Chemical Society
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• v.30 no.11
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• pp.2584-2588
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• 2009

The effect of $LaF_3$ coating on the structural and electrochemical properties of $Li[Ni_{0.3}Co_{0.4}Mn_{0.3}]O_{2}$ cathodes was investigated using XRD, SEM, TEM, and a cycler. The coating layer consisted of nano-sized particles attached nonuniformly to the surface of pristine powder. Despite the surface coating treatment, phase difference by $LaF_3$ coating was not detected. The discharge capacities of coated electrodes were a little lower than that of pristine sample at a 1 C rate. However, as the C rate increases, the capacity retention of the coated sample becomes obviously superior to that of the pristine sample. The cyclic performances of the electrodes in the voltage range of 4.8 $\sim$ 3.0 V were also improved by the surface coating. Such enhancement is attributed to the presence of the $LaF_3$ coating layer, which effectively suppressd the reaction between electrodes and electrolytes on the surface of the $Li[Ni_{0.3}Co_{0.4}Mn_{0.3}]O_{2}$ electrode.

• Korean Journal of Metals and Materials
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• v.48 no.4
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• pp.315-319
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• 2010

In this study, the hydrogen reduction behavior of ball-milled NiO nanopowder was investigated depending on the partial pressure of water vapor. The hydrogen reduction behavior was analyzed by thermogravimetry and hygrometry under heating to 873 K in hydrogen. In order to change the partial pressure of the water vapor, the dew point of hydrogen was controlled in the range of 248 K~293 K by passing high-purity hydrogen through a saturator that contained water. Interestingly, with the increase in the dew point of the hydrogen atmosphere, the first step of the hydrogen reduction process decreased and the second step gradually increased. After the first step, a pore volume analysis revealed that the pore size distribution in the condition with a higher water vapor pressure shifted to a larger size, whereas the opposite appearedat a lower pressure. Thus, it was found that the decrease in the pore volume during the chemical reaction controlled process at a dew point of 248 K caused a reduction in retardation in the diffusion controlled process.

• Journal of the Korean Magnetics Society
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• v.9 no.2
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• pp.78-84
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• 1999

$(Ni, Zn)Fe_2O_4$ powders were prepared through self-propagating high temperature synthesis reaction and the effects of initial zinc oxide powder size and oxygen pressure on the magnetic properties of the final combustion products were studied. The ferrite powders were combustion synthesized with iron, iron oxide, nickel oxide, and zinc oxide powders under various oxygen pressures of 0.5~10 atmosphere after blended in n-hexane solution for 5 minutes with a spex mill, followed by dried at 120 $^{\circ}C$ in vacuum for 24 hours. The maximum combustion temperature and propagating rate were about 1250 $^{\circ}C$ and 9.8 mm/sec under the tap density, which were decreased with decreasing ZnO size and oxygen pressure. The final product had porous microstructure with spinel peaks in X-ray spectra. As the ZnO particle size in the reactant powders and oxygen pressure during the combustion reaction increase, coercive force, maximum magnetization, residual magnetization, squareness ratio were changed from 1324 Oe, 43.88 emu/g, 1.27 emu/g, 0.00034 emu/gOe, 37.8$^{\circ}C$ to 11.83 Oe, 68.87 emu/g, 1.23 emu/g, 0.00280 emu/gOe, 43.9 $^{\circ}C$ and 7.99 Oe, 75.84 emu/g, 0.791 emu/g, 0.001937 emu/gOe, 53.8 $^{\circ}C$ respectively. Considering the apparent activation energy changes with oxygen pressure, the combustion reaction significantly depended on initial oxygen pressure and ZnO particle size.

• Journal of Hydrogen and New Energy
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• v.35 no.3
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• pp.336-344
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• 2024

In this study, a Ni_0.9Co_0.05Mn_0.05(OH)₂ precursor used as an anode active material using a black powder leaching solution of a recycled lithium ion battery was prepared through coprecipitation synthesis with co-precipitation time, NH₄OH concentration, pH, and stirring time as variables. The characteristics of the prepared powder were analyzed by X-ray diffraction (XRD), scanning electron microscope (SEM), particle size analysis (PSA), and inductively coupled plasma optical emission spectroscopy (ICP-OES). It was confirmed that the single crystal thickness of the LiNi_1-x-yCo_xMn_yO₂ (NCM) precursor changes depending on the NH₄OH concentration and reaction pH value, and thicker single crystals are formed at 2 M NH₄OH compared to 1 M and at pH 10.8-11.8 compared to pH 11.8-12.0. NCM precursor particles increased with coprecipitation time, and it was confirmed that the 72 hours NCM precursor had the largest particle size. Through ICP-OES analysis, it was confirmed that the NCM precursor was synthesized with the target composition of Ni²⁺:Co²⁺:Mn²⁺=90:5:5.

• Korean Journal of Materials Research
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• v.14 no.4
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• pp.293-299
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• 2004

Transition metal ions doped $TiO_2$ nanostructured powders were prepared with simply heating aqueous $TiOCl_2$ solutions, contained various metal ions (Ni, Al, Fe, Zr, and Nb) of 1.47 mol% added as metal-chlorides, at $100^{\circ}C$ for 4 hrs by homogeneous precipitation process under suppressing conditions of water vaporization. The characterizations for prepared $TiO_2$ powders were carried out to observe doping of metal ions, their concentrations and microstructures using XRD, UV-VIS (DRS), XPS, SEM, TEM and ICP. Also, photo-oxidative abilities were evaluated by decomposition of 4-chlorophenol (4CP) under ultraviolet light irradiations. No secondary oxide phases were formed in all the $VTiO_2$ powders, showing doping with various transition metal ions. When adding ions ($Ni^{2+}$ or$ Al^{3+ }$ and $Zr^{4+}$ ) having valance states or ionic radii greatly different from those of $Ti^{4+}$ , the $TiO_2$ powders of mixed anatase and rutile phases were formed, whereas in the case of additions of $^Fe{3+ }$ and $Nb^{ 5+}$ as well as no addition of metal ion the powders with pure rutile phase alone were formed. Among the prepared $TiO_2$ powders, Ni$^{2+}$ doped $TiO_2$ powders, containing a small amount of anatase phase, showed excellent photo-oxidative ability in 4CP decomposition because of relative decreases in electron-hole recombination and poisoning of $TiO_2$ surface during the photoreaction.n.