engleski

Synthesis of ZrTiO4 Powder from Equimolar ZrO2-TiO2 Powder Mixture by High Energy Dry Ball-Mill and Post-Anneal Processing

High-energy dry ball-milling and post-anneal processing were applied to synthesize ZrTiO4 compound oxide powder from the equimolar TiO2-ZrO2 powder mixture. X-ray diffraction technique was used to follow structural changes in the milled and the post-annealed milled samples. The milling assembly applied (vial and balls made of agate) was very efficient since in the milled samples fully amorphous structure appeared, if milling lasted long enough. In our experiments, the elapsed milling time for full amorphization was about 50 h. Contamination of samples by agate material, due to wearing-away effect, was not observed by XRD technique. In addition, more rapid preparation of the crystalline ZrTiO4 phase from the milled amorphous one was possible if the milled samples were exposed to a subsequent heat treatment. It was determined by the XRD analysis that in samples previously milled by agate assembly crystallization of amorphous ZrTiO4 phase was possible even at 650 oC, although at this temperature it was a very slow process, and a prolonged annealing time was necessery. If heat treatment of samples (milled up to 50 h) was performed at 900 oC for one hour, it caused full crystallization of amorphous into crystalline ZrTiO4 phase.

Syntheses of amorphous or crystalline ZrTiO4 phases; Equimolar ZrO2-TiO2 crystalline powder mixture; High-energy dry ball milling and post-annealing; X-ray diffraction study

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