The preparation characterization and sintering of nanocrystalline ceramics

Abstract

Nanocrystalline Titania was prepared by a chemical synthesis technique commonly known as sol-gel method. In the sol gel method, Titanium (IV) Isopropoxide was mixed with Isopropanol and Nitric Acid solution in predetermined ratios. A rapid hydrolysis reaction occurs between Titanium (IV) Isopropoxide and water in the Nitric Acid solution resulting in the formation of Titan oxide (Titania). The sols were clear sols and then gelled without any change in its clarity.Nanocrystalline Titania were tried to prepare by two different techniques in this work. The first technique involved the drying of the gel and subsequent sintering of the dried gel. A number of organic additives (oxalic acid, acetic acid, polyacrylic acid and stearic acid) were mixed into the sol before gelation in order to control drying (drying control chemical addives-DCCAs). Powders was prepared from sols and gels by several processes and a solid form was obtained by dry pressing and subsequently sintered in second technique. Oxalic acid was the most efficient DCCA among the others.The dried gels and powder compacts were sintered at 650, 700, 750, 800, and 850C. The sintering behaviors of them were examined. Relative densities of the dried gels were between 79-99% depending on the sintering temperature. The green body density of the pellets were varied between 41-52%. Their relative densities after sintering were varied between 55-83% depending on the sintering temperature. The pellets were pressed at different pressures to observe the pressure effect on the densification. Increase in pressure improve the densification behavior. The best route for the nanocrystalline powder preparation was the Route 4. This powder had smaller size of agglomerate most probably the agglomerates were broken during the ultrasonic radiation.The pore size analyses showed the pore structure of the gel. The pore size of the gels are about 35 nm. FTIR Spectra gave the crystal structure of the sols gels and powders. As a result, the sintering behavior of the dried gels is better than the powder compacts. The pellets can be densified to higher densities by appropriate forming technique. Although, the dried gels have significantly high densities, the shape and the weight of the gels can not be controlled.