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The Preparation Characterization and Sintering of Nanocrystalline Ceramics
(01. Izmir Institute of Technology, 1999) Çağlar, Özlem; Çiftçioğlu, Muhsin
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.
Processing and Characterization of Nanocrystalline Materials
(Izmir Institute of Technology, 2004) Genç, Gözde; Çiftçioğlu, Muhsin
Nanocrystalline materials with grain sizes under 100 nm have been counted as a very promising class of ceramic materials. The decrease in grain size imparts superior structural properties to the ceramic materials like increased fracture toughness, wear resistance and superplastic deformation at high temperatures. So, nanocrystalline ceramics can be used as structural materials in a wide range of uses covering advanced engineering applications such as aircraft and automotive technologies as well as electronics, computation and material sciences. Nanocrystalline alumina has been a popular research subject for the last decade because of the superior structural properties of alumina besides lower cost compared to other nanocrystalline materials like zirconia and titania. The raw materials are generally transitional aluminas or aluminum hydroxides such as boehmite and gibbsite all of which are widely used in industry.The main problem in nanocrystalline alumina production is to cope with agglomeration of fine powders or nano-particles in solutions due to interaction forces. Agglomeration cause nonhomogeneous microstructure with respectively larger pores which are very hard to eliminate during sintering. In this study a nanocrystalline commercial boehmite powder is used as the starting material and a homogeneous microstructure with respectively high density is aimed. Ultrasonic treatment is applied in order to reduce particle size and the stable dispersions of boehmite powder with a solid content of 30wt% was dried by spray drying. The effect of ultrasonic treatment, spray drying and compaction conditions were investigated and compared with bodies compacted from untreated powders. To see the effect of seeding on phase transformation behavior of boehmite, alpha alumina particles produced by combustion synthesis and broken into crystallites by ultrasonic treatment were used with a seed content less than 0.5%. Even that low amount of a-alumina reduced the transformation temperature by 100C but did not improve densification of alumina compacts. The homogeneity of microstructure obtained by ultrasonic treatment and granulation by spray drying yielded the highest relative densities of 65.5 % of the theoretical density. The treatment has also led more uniform microstructures compared to untreated and seeded samples during the a-phase transition which is the most important stage for densification.

Master Degree / Yüksek Lisans Tezleri

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