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 μm. 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.

Half-Heusler alloys are a potential thermoelectric material for use in high-temperature applications. In an attempt to produce half-Heusler thermoelectric materials with fine microstructures, TiCoSb was synthesized by the mechanical alloying of stoichiometric elemental powder compositions and then consolidated by vacuum hot pressing. The phase transformations during the mechanical alloying and hot consolidation process were investigated using XRD and SEM. A single-phase, half- Heusler allow was successfully produced by the mechanical alloying process, but a minor portion of the second phase of the CoSb formation was observed after the vacuum hot pressing. The thermoelectric properties as a function of the temperature were evaluated for the hot-pressed specimens. The Seebeck coefficients in the test range showed negative values, representing n-type conductivity, and the absolute value was found to be relatively low due to the existence of the second phase. It is shown that the electrical conductivity is relatively high and that the thermal conductivities are compatibly low in MA TiCoSb. The maximum ZT value was found to be relatively low in the test temperature range, possibly due to the lower Seebeck coefficient. The Hall mobility value appeared to be quite low, leading to the lower value of Seebeck coefficient. Thus, it is likely that the single phase produced by mechanical alloying process will show much higher ZT values after an excess Ti addition. It is also believed that further property enhancement can be obtained if appropriate dopants are selectively introduced into this MA TiCoSb System.

기계적 합금화 공정을 이용하여 열전재료FeSi2분말을 제조하여 열간압축법을 사용하여 성형하였다. 열간압축 성형된 FeSi2는 열전특성을 나타내는 β-FeSi2 상 및 상변태가 완료되지 않은 α-Fe2Si5와 ε-FeSi의 혼합상으로 이루어져 있음이 확인되었다. 열전재료로의 β-FeSi2 상변태 유도를 위해 항온열처리를 행하여 상변태 조건을 조사하였다. SEM, TEM, XRD, DTA 등을 이용하여 상변태 거동을 분석한 결과, 830˚C에서 24시간 진공 항온열처리 후 단상의 β-FeSi2 상을 얻을 수 있었다. 항온열처리 전의 열간압축 성형체와 상변태가 완료된 β-FeSi2의 기계적 성질과 열전 특성을 측정하여 비교 분석하였다.