Sub-micrometer ultra fine CeO2-ZrO2 mixed oxides have been prepared by milling solid cerium carbonate and zirconium oxy-chloride with ammonia and followed by filtering, drying and calcining procedures. The effects of Ce/Zr molar ratio, milling time and calcining temperature on the phase composition, particle size and morphology, surface charge, as well as the polishing property were investigated. The results show that the mixed oxide calcined at 1 000 ℃ is composed of cubic ceria doped with zirconium and tetragonal zirconia doped with cerium, and the phase composition varies with calcination temperature and the Ce/Zr molar ratio. The monoclinic zirconia is observed when decreasing calcination temperature and shortening milling time, demonstrating that milling and calcining can force the phase transformation from monoclinic zirconia to cerium stabilized tetragonal zirconia and zirconium doped cubic ceria solid solutions. The removal rate for the optical glass polishing varies with Ce/Zr molar ratio. A synergetic polishing effect is found when Ce/Zr molar ratio below 4, and the optimal Ce/Zr molar ratio is 1∶1. At the same time, the cubic ceria content, density, particle size and surface charge all increase when calcination temperature increasing from 800 ℃ to 1 100 ℃. However, the particle morphology changes from disperse quasi-sphere to irregular aggregation and the maximal removal rate for optical glass polishing lies at 1 000 ℃.These facts show that the polishing property of the synthesized ceria-zirconia mixed oxide is affected by the particle physical characteristics comprehensively.
Crystalline neodymium carbonates were prepared by treating the amorphous precipitate formed from the reaction between neodymium chloride and ammonium bicarbonate under hydrothermal condition. Their composition, morphology and crystal phase were identified by means of elemental analysis, SEM and XRD. It was found that Nd2(CO3)3·2.5H2O with tengerite-type structure and sheet morphology was obtained when the feed molar ratio(FMR=n(NH4)2CO3/ NdCl3)was 2 or 1.8 and hydrothermally treated at 150 ℃ for 12h. However, orthogonal NdOHCO3 particles agglomerated with long rod crystals were formed when lowering FMR to 1.5 under the same hydrothermal condition. Phase transformation from tengerite-type Nd2(CO3)3·2.5H2O to orthogonal NdOHCO3 was occurred when increasing hydrothermal temperature or prolonging hydrothermal time, which is beneficial to the preparation of neodymium hydroxyl-carbonate with neodymium oxide content higher than 70%.
