• Korean Journal of Materials Research
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• v.23 no.10
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• pp.543-549
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• 2013

The purpose of this paper was to investigate the effect of a high-energy milling (HEM) process on the particle morphology and the correlation between a thermal treatment and tetragonal/monoclinic nanostructured zirconia powders obtained by a precipitation process. To eliminate chloride residue ions from hydrous zirconia, a modified washing method was used. It was found that the used washing method was effective in removing the chloride from the precipitated gel. In order to investigate the effect of a pre-milling process on the particle morphology of the precipitate, dried $Zr(OH)_4$ was milled using a HEM machine with distilled water. The particle size of the $Zr(OH)_4$ powder exposed to HEM reduced to 100~150 nm, whereas that of fresh $Zr(OH)_4$ powder without a pre-milling process had a large and irregular size of 100 nm~1.5 ${\mu}m$. Additionally, modified heat treatment process was proposed to achieve nano-sized zirconia having a pure monoclinic phase. It was evident that two-step calcining process was effective in perfectly eliminating the tetragonal phase, having a small average particle of ~100 nm with good uniformity compared to the sample calcined by a single-step process, showing a large average particle size of ~300 nm with an irregular particle shape and a broad particle size distribution. The modified method is considered to be a promising process for nano-sized zirconia having a fully monoclinic phase.

• Korean Journal of Metals and Materials
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• v.50 no.11
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• pp.817-822
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• 2012

Nano powders of $Al_2O_3$ and $TiO_2$ compounds made by high energy ball milling were pulsed current activated sintered for studying their sintering behaviors and mechanical properties. The advantage of this process is that it allows very quick densification to near theoretical density and inhibition of grain growth. Nano-structured $Al_2TiO_5$ with small amount of $Al_2O_3$ and$TiO_2$ was formed by sintering at $1300^{\circ}C$ for 5 minute, in which average grain size was about 96 nm. Hardness and fracture toughness of the nano-structured $Al_2TiO_5$ compound with a small amount of $Al_2O_3$ and$TiO_2$ were $602kg/mm^2$ and $2.6MPa{\cdot}m^{1/2}$, respectively.

• Korean Journal of Metals and Materials
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• v.49 no.10
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• pp.818-822
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• 2011

ZnO nanorods were grown on Au-coated Si substrates by vapor phase transport (VPT) at the growth temperature of $600^{\circ}C$ using a mixture of zinc oxide and graphite powders as source material. Au thin films with the thickness of 5 nm were deposited by ion sputtering. Temperature-dependent photoluminescence (PL) was carried out to investigate the optical properties of the ZnO nanorods. Five peaks at 3.363, 3.327, 3.296, 3.228, and 3.143 eV, corresponding to the free exciton (FX), neutral donor bound exciton ($D^{\circ}X$), first order longitudinal optical phonon replica of free exciton (FX-1LO), FX-2LO, and FX-3LO emissions, were obtained at low-temperature (10 K). The intensity of these peaks decreased and their position was red shifted with the increase in the temperature. The FX emission peak energy of the ZnO nanorods exhibited an anomalous behavior (red-blue-red shift) with the increase in temperature. This is also known as an "S-shaped" emission shift. The thermal activation energy for the exciton with increasing temperature in the ZnO nanorods is found to be about 26.6 meV; the values of Varshni's empirical equation fitting parameters are = $5{\times}10^{-4}eV/K$, ${\beta}=350K$, and $E_g(0)=3.364eV$.

• Journal of Powder Materials
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• v.13 no.5 s.58
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• pp.327-335
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• 2006

In the development of new hydrogen absorbing materials for a next generation of metal hydride electrodes for rechargeable batteries, metastable Mg-Ni-based compounds find currently special attention. Amor phous-nanocrystalline $Mg_{63}Ni_{30}Y_7$ and $Mg_{50}Ni_{30}Y_{20}$ alloys were produced by mechanical alloying and melt-spinning and characterized by means of XRD, TEM and DSC. On basis of mechanically alloyed Mg-Ni-Y powders, complex hydride electrodes were fabricated and their electrochemical behaviour in 6M KOH (pH=14,8) was investigated. The electrodes made from $Mg_{63}Ni_{30}Y_7$ powders, which were prepared under use of a SPEX shaker mill, with a major fraction of nanocrystalline phase reveal a higher electrochemical activity far hydrogen reduction and a higher maximum discharge capacity (247 mAh/g) than the electrodes from alloy powder with predominantly amorphous microstructure (216 mAh/g) obtained when using a Retsch planetary ball mill at low temperatures. Those discharge capacities are higher that those fur nanocrystalline $Mg_2Ni$ electrodes. However, the cyclic stability of those alloy powder electrodes was low. Therefore, fundamental stability studies were performed on $Mg_{63}Ni_{30}Y_7$ and $Mg_{50}Ni_{30}Y_{20}$ ribbon samples in the as-quenched state and after cathodic hydrogen charging by means of anodic and cathodic polarisation measurements. Gradual oxidation and dissolution of nickel governs the anodic behaviour before a passive state is attained. A stabilizing effect of higher fractions of yttrium in the alloy on the passivation was detected. During the cathodic hydrogen charging process the alloys exhibit a change in the surface state chemistry, i.e. an enrichment of nickel-species, causing preferential oxidation and dissolution during subsequent anodization. The effect of chemical pre-treatments in 1% HF and in $10\;mg/l\;YCl_3/1%\;H_2O_2$ solution on the surface degradation processes was investigated. A HF treatment can improve their anodic passivation behavior by inhibiting a preferential nickel oxidation-dissolution at low polarisation, whereas a $YCl_3/H_2O_2$ treatment has the opposite effect. Both pre-treatment methods lead to an enhancement of cathodically induced surface degradation processes.