Ti has received considerable attention for aerospace, vehicle, and semiconductor industry applications because of its acid-resistant nature, low density, and high mechanical strength. A common precursor used for preparing Ti materials is TiCl4. To prepare high-purity TiCl4, a process based on the removal of VOCl3 has been widely applied. However, VOCl3 removal by distillation and condensation is difficult because of the similar physical properties of TiCl4 and VOCl3. To circumvent this problem, in this study, we have developed a process for VOCl3 removal using Cu powder and mineral oil as purifying agents. The effects of reaction time and temperature, and ratio of purifying agents on the VOCl3 removal efficiency are investigated by chemical and structural measurements. Clear TiCl4 is obtained after the removal of VOCl3. Notably, complete removal of VOCl3 is achieved with 2.0 wt% of mineral oil. Moreover, the refined TiCl4 is used as a precursor for the synthesis of Ti powder. Ti powder is fabricated by a thermal reduction process at 1,100oC using an H2-Ar gas mixture. The average size of the Ti powder particles is in the range of 1-3 μm.

공침법으로 제조된 비정질 PbTiO3전구체의 결정화거동과 구조적 변화를 XRD, 라만스펙트럼, TEM, RDF등으로 조사하였다. 전구체는 이온안정제로 H2O2혹은 NH4NO3를 사용하여 제조된 질산납과 사염화티탄의 혼합수용액으로부터 45˚C, pH 9에서 제조되었다. 이온안정제로 H2O2를 사용한 경우보다 NH4NO3를 사용하여 제조된 공침물이 더 낮은 온도에서 결정화가 시작되며 결정화의 활성화에너지도 더 작은 값을 가진다. 비정질의 공침물은 transient phase를 거쳐 결정 PbTiO3로 변태된다. 비정질 상태의 평균 원자거리는 열처리온도의 증가에 따라 감소한다.

We investigated the effects of leaching concentration (0.1 ~ 1.0 M) and time (1 ~ 120 min) on the phosphorus recovery from ash and dried sewage sludge produced by titanium tetrachloride (TiCl4) flocculation by acidic (H2SO4 and HCl) or alkaline (KOH and NaOH) leaching. The extraction efficiencies of dried sludge were 2.7 ~ 12.6% for H2SO4, 2.5 ~ 10.5% for HCl, 3.6 ~ 9.6% for KOH, and 7.1 ~ 9.9% for NaOH with 1 M, and the maximum efficiency was obtained within 45 min. The maximum %P extracted of sludge ash was 83.1 for H2SO4, 80.2 for HCl, 51.2 for KOH, and 51.2 for NaOH with 1 M, obtained within 45 min. The rate constants (min−1) for the leaching of P from sludge ash were found to be 1.199 for H2SO4, 1.026 for HCl, 0.264 for KOH, and 0.622 for NaOH. The P leaching increased with the increase in leaching concentration, and the maximum leaching for ash was obtained within 0.3 M, regardless of acidic or alkaline leaching. The overall results indicate that the ash of TiCl4 flocculated sewage sludge can be treated with H2SO4 to efficiently recover P.