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Ilmenit se v naravi pojavlja kot akcesorni mineral v mnogih kamninah. Ker je zelo obstojen, se v procesih preperevanja pod vplivom vode in vetra kopiči v obliki težkih peskov, ki predstavljajo najpomembnejšo ekonomsko surovino za pridobivanje titana. Namen magistrske naloge je bil pokazati, da lahko naravne ilmenitne težke peske, ki so ekološko sprejemljivi ter na voljo v velikih količinah, uporabimo tudi za alternativne namene, na primer za pripravo keramike za termoelektrične aplikacije. V magistrski nalogi sem kot vhodni material uporabila ilmenitni pesek, ki ga v Cinkarni Celje uporabljajo za pridobivanje titanovega dioksida. Pesek sem najprej oksidirala pri temperaturah 600–800 °C in s tem sprožila nastanek rutilnih lamel. Peske sem sintrala v inertni atmosferi po dveh postopkih: s konvencionalnim sintranjem (na 1200 °C) ter s sintranjem v pulznem toku (SPS na 1100 °C). Na oba načina sem pripravila gosto keramiko. Prahove in sintrano keramiko sem analizirala z lasersko granulometrijo, TG, XRD, SEM/EDXS, MS, določila sem tudi gostoto sintranih vzorcev. V zadnjem koraku smo izmerili termoelektrične lastnosti sintranih vzorcev. Rezultati so pokazali, da so vzorci po sintranju sestavljeni iz matrice s sestavo psevdobrookit–feropsevdobrookit. Vzorci, ki so bili pripravljeni iz predoksidiranih prahov so vsebovali še vključke rutila. Konvencionalno sintrani vzorci so bili nekoliko bolj porozni in so imeli nižjo gostoto, kot vzorci pripravljeni po postopku SPS. Povprečna velikost zrn je pri vzorcih sintranih po SPS postopku manjša kot pri konvencionalno sintranih vzorcih. Meritve termoelektričnih lastnosti so pokazale, da imajo tako konvencionalno sintrani, kot tudi vzorci sintrani po SPS postopku nizko toplotno prevodnost, relativno visok Seebeckov koeficient ter nizko električno prevodnost, kar bi bilo potrebno izboljšati. Rezultati so pokazali, da so naravni ilmenitni peski primerni za pripravo funkcionalne keramike. Ilmenite is the most common accessory mineral in many rocks. During weathering, the primary rocks disintegrate and the ilmenite grains accumulate to heavy mineral fractions also known as heavy mineral sands. These sands today represent the main source of titanium. The aim of my master thesis was to show that natural ilmenite-rich heavy sands can also be used for advanced applications such as preparation of functional ceramics with thermoelectric properties. In my experimental work, I used ilmenite-rich sand provided by Cinkarna Celje as the starting powder. The starting (as received) powder was pre-oxidized at 600, 700 and up to 800 °C to trigger exsolution of rutile lamellae in ilmenite grains. The as-received powder and the pre-oxidized powders were sintered in an inert atmosphere using two procedures: pressureless conventional sintering (at 1200 °C) and pressure-assisted pulsed flow sintering (SPS at 1100°C). The powders were analyzed by laser granulometry, TG, XRD, SEM/EDXS and MS, we also determined absolute density of the sintered samples. In the last step, thermoelectric properties of the sintered samples were measured. The results have shown that all sintered samples consist of a matrix with the composition on the pseudobrookite–ferropseudobrookite tie-line, whereas the samples prepared from pre-oxidized powders contained rutile inclusions. The conventionally sintered samples were slightly more porous and had a lower density than the samples prepared by SPS. The average grain size was significantly smaller for the SPS sintered samples than for the conventionally sintered samples. Measurements of thermoelectric properties showed that both the conventionally sintered and SPS sintered samples have promising thermoelectric properties and show low thermal conductivity, relatively high Seebeck coefficient, but low electrical conductivity, which should be improved in the future. In my thesis, I have shown that natural ilmenite powder has great potential for the production of advanced functional ceramics. |
