Master Degree / Yüksek Lisans Tezleri
Permanent URI for this collectionhttps://hdl.handle.net/11147/3008
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Master Thesis Electrocaloric Properties of the Zr-Substituted Batio3 – Na0.5bi0.5tio3 Ceramics(2023) Akkaşoğlu, Oğuz; Adem, UmutThe aim of this study is to investigate electrocaloric properties and thermodynamic behaviour, obtaining high adiabatic temperature change (ΔT) values with a broad temperature span of zirconium doped barium titanate-sodium bismuth titanate by substitution of Zr into B-site (titanium). Ceramics are synthesized in a pellet form by solid-state reactions. Chemical composition was Ba0.7Na0.15Bi0.15TixZr1-xO3 (abbreviated as BT-NBT) where x= 0.00, 0.01, 0.02, 0.03, 0.035, 0.04 and 0.05. Phase analysis was conducted by X-ray diffraction method. Microstructural analysis and average grain size determination was performed by Scanning Electron Microscopy. To understand phase transitions and physical behaviours, dielectric measurements are performed. Ferroelectric properties are investigated by using temperature dependent polarization, strain and current-electric field relationships. Electrocaloric measurements are done by using temperature dependent polarization-electric field data. Maxwell relations are used to calculate temperature dependent electrocaloric temperature change, ΔT, and from this data, temperature span, Tspan, was calculated. It was observed even though Zr substitution into the Ti-site rapidly decreases the Curie temperature and introduces relaxor ferroelectric character to the samples. However, the 1st order like nature of the ferroelectric-paraelectric phase transition at the Curie temperature and, consequently significant ΔT is maintained even for 4 % Zr substituted sample close to room temperature. Temperature span, on the other hand, has a lower value compared to previous works related to barium titanate systems. Electrocaloric efficiency is comparable to other works on Pb-free sytems and these results showed that BT-NBT systems have promising features for electrocaloric cooling technologies.Master Thesis Coating of Spinel Layers on Alumina by Electrostatic Spray Deposition (esd)(01. Izmir Institute of Technology, 2023) Demirkol, İrem; Akkurt, SedatMgAl2O4 spinel layer was coated on dense alumina pellets by advantageous ESD among the other deposition methods in terms of providing a simple, inexpensive setup and good control of the layer morphology. The main goals are successfull deposition of spinel layers on alumina pellets by ESD, to investigate the effect of ESD parameters (working distance, flow rate of precursors, applied voltage) on coating microstructure by conducting full factorial design experiments and to determine the best experimental conditions for a porous layer. Besides, MgCr2O4 layer was coated on dense alumina and MgAl2O4 layer was deposited on bisque-fired alumina pellet to extend the scope of the work. Alumina powders were compressed and sintered, respectively to obtain pellets. MgAl2O4 spinel precursor solution was sprayed on the alumina pellets by changing the parameters accordingly the full factorial design. MgAl2O4 and MgCr2O4 solutions were also sprayed on the bisque-fired and the dense alumina pellets with the parameters given the best porous layer. Elemental analysis of the residues obtained after evaporation of the solutions by energy dispersive X-ray spectroscopy (EDX), both unheated and post-heated residual powders of solutions by X-ray diffraction (XRD) and surface morphologies of coated pellets by scanning electron microscopy (SEM-EDS) were analyzed. Spinel layers on alumina pellets were successfully coated by ESD, which could provide variable surface morphologies. The optimum conditions for a porous layer were obtained as working distance of 15 mm, flow rate of 0.25 mL/h and applied voltage of 6 kV in this study. The coatings on the pellets before further heating were amorphous. Post-heating of the pellets were required to obtain crystalline spinel structure.Master Thesis Formation of Srtio3[tio2] Ceramic Composites at Low Temperatures(01. Izmir Institute of Technology, 2021) Karataş, Esin; Adem, Umut; Ahmetoğlu, Çekdar VakıfStrontium titanate ceramics are materials belonging to the perovskite material group with the formula ABO3. Strontium titanate ceramics have been a preferred material in many areas, such as the electroceramics industry, due to its high dielectric constant and high chemical stability and generally produced by manufacturing processes such as solid-state synthesis, hydrothermal method, and sol-gel. SrTiO3 ceramics have been produced in the literature with different temperatures, times, and starting materials. For ceramic products, a sintering step is required after the powder production step. Traditional sintering methods, which have been used for many years, are used to densify powders with high temperatures. Recently developed low-temperature densification methods enable the sintering process to be carried out at relatively lower temperatures. For this purpose, in this thesis, SrTiO3-TiO2 ceramic composites were produced at different reaction temperatures and times using the rHLPD method, which combines powder production and sintering steps in a single process. In the studies, the reaction temperature, time, and the effect of adding mineralizer to the prepared solution for the hydrothermal reaction on the final product were investigated. The aim of the thesis is to produce SrTiO3 from TiO2 green body using the rHLPD method. In addition, the production of SrTiO3-TiO2 ceramic composites with as high mole conversion and relative density values as possible was targeted with different parameters such as reaction temperature, reaction time, and addition of NaOH to the solution. As a result of the studies carried out with different parameters, SrTiO3-TiO2 ceramic composites with a final relative density value of approximately 81 % were produced. Consequently, in the XRD and Rietveld analysis, it was seen that the main phase was SrTiO3. In addition, there was a TiO2 phase in the structure. Finally, the SrCO3 phase was not detected in the structure.Master Thesis Preparation and Characterization of Inorganic Membranes by Using Sol-Gel Techniques(01. Izmir Institute of Technology, 2000) Yelken, Gülnihal; Çiftçioğlu, MuhsinIn this research the preparation of ceramIC membranes for gas separation applications by using sol-gel techniques were investigated. The effects of water/alkoxide ratio, H+/alkoxide ratio on the catalysis of the hydrolysis-condensation reactions and the peptization process were investigated by using N2 adsorptiondesorption isotherms, thermogravimetric analysis and FfIR (Fourier Transform Infra Red). The performance and the potential use of these materials in gas separation applications depend mainly on the ability in controlling-designing the microstructurepore network in these materials.The alumina and silica sols were prepared by using aluminium isopropoxide and tetraethylorthosilicate. Sols with different H+/ AI+3 and H20 / AI+3 ratios were prepared.These peptized clear boehmite sols were used for the preparation of unsupported Ah03 membranes at 600°C. The similar ratios were varied for the preparation of clear silica sols and these sols were further dried and heat treated at 400 C.The thermogravimetric analjsis has shown that the weights of the unsupported membranes were stable at the above temperatures. The boehmite was observed to decompose to the y-Alz03 phase at about 425°C. The FfIR analysis have proved the formation of boehmite in the sols and all the organic solvent peaks disappeared upon heat treatment.The y-Alz03 membranes all displayed Type IV isothems typical of mesoporous materials. Hysteresis loops were present in all these isotherms and fast desorption took place in the 0.4-0.6 PlPo range. The BJH pore size distributions were sharp for all the samples.The desorption pore size distributions were found to become wider at an intermediate acid content membrane which also had the lowest BET surface area. The BET particle sizes of these membranes were estimated to be in the 70-100 A0 range.The throat and pore cavity sizes of monosize sphere packings for this particle size range were observed to be in close agreement with the experimentallly determined adsorptiondesorption pore sizes.The silica samples all displayed Type I isotherms with no hysteresis typical of microporous materials. The HK (Horvoath Kawazoe) pore sizes were in the 4-5 AO range. An effect of the water content of these acid-catalyzed sols on the pore size were also detected.Master Thesis Preparation and Characterization of Whisker and Particulate Sic-Ai2 O3 Ceramic Composites(Izmir Institute of Technology, 1999) Ünver, Özlem Ebru; Çiftçioğlu, MuhsinThis work involves the preparation and the characterization of SiC particulate-Alz03 and SiC whisker- Alz03 ceramic composites. A new technique was used in order to increase the density of composite. Fine Alz03 and SiC whiskers and particulates were used as a matrix and secondary phase, respectively. Whiskers and particulate were coated with Al-S04-OH precursor by precipitation using urea. In this method, it was important to keep the alumina hydrate in the noncrystalline state at 5.5>pH>8.6. The alumina- hydrate compound was separated from SiC whiskers and particulates when the reaction was continued at high pH (pH>8.7) causing the crystallization of alumina precursor. Alumina hydrate coated SiC whiskers and particulate were used as the starting material for the preparation of SiCw/p reinforced Alz03. Die pressing was used as the most appropriate and cheapest consolidation technique of composite materials. Upon sintering Al-S04OH on the SiC transformed into Alz03 by providing empty spaces for matrix densification in the proposed technique ( shrink- fit idea). Green bodies with SiC whisker and particulate contents in the range of 10 to 40 vol.% were sintered at 14500C for 2h under atmospheric conditions. The densities of sintered composites were measured by using Archimedes method. The density of composites containing 10%, 20%, 30% and 40 vol.% coated SiC particulate and whisker composites changed from 81% to 70% of theoretical density and from 79% to 75% of theoretical density, respectively. The density of coated composites were -22% greater than that of the uncoated composites .The thermal behavior of Al-S04-OH on the SiC was characterized by using TGA, DTA. TGA curves showed that materials are hydrated and dehydroxylization was observed between -700 and 800°C. TGA and DTA curves indicated that desulfurization then occurred at about -950°C. Chemical characterization of the coated SiC whiskers and particulates were obtained by using FTIR spectrometer.The hardness of these composites were measured by usmg Vickers Microhardness Testing Device. Vickers microhardness of the 20vol.% and 30vol.% coated SiCp ,and 20vol.% and 40 vol.% SiCw-Alz03 composites were measured as 10.71, 12.94, 10.89 and 5,96 GPa, respectively and compared with the mechanical properties of the composites manufactured by the conventional methods.Master Thesis The Preparation Characterization and Sintering of Nanocrystalline Ceramics(01. Izmir Institute of Technology, 1999) Çağlar, Özlem; Çiftçioğlu, MuhsinNanocrystalline 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.Master Thesis Processing and Characterization of Nanocrystalline Materials(Izmir Institute of Technology, 2004) Genç, Gözde; Çiftçioğlu, MuhsinNanocrystalline 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 Thesis Use of Metal Templates for Microcavity Formation in Alumina(Izmir Institute of Technology, 2011) Balkan, Sırma; Akkurt, SedatAlumina ceramics with microtunnels are produced by compressing submicron sized alumina powder and Ti, Cu or stainless steel wires in a metal die before firing the compacts at 1350oC for 4 hours. Diameters of wires ranged from 50 to 125 micrometers. Copper was found to completely melt and flow away from the compact leaving no trace of copper in alumina. Stainless steel diffused out into the alumina leaving few pores behind. Titanium, on the other hand, diffused into alumina at 20 to 30micrometers/hour and left plenty of Kirkendal porosity behind. The amount of porosity could have been increased further by applying intensive milling to the powder. But no milling was done in this study and hence a complete micro-tunnel was not obtained. The Kirkendal effect was observed to be effective in producing pores in the ceramic. Densification behavior of the ceramic was also investigated with a vertical dilatometer. Densities up to 93% were achieved in the ceramics. In some tests Ti metal plates were used as diffusion couples with alumina compacts. Similar diffusion behavior was observed with plates and wires.