Master Degree / Yüksek Lisans Tezleri
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Master Thesis Preparation and Rheological Characterization of Calcium Silicate/Aluminate Based Cementitious Inks(01. Izmir Institute of Technology, 2022) Keleş, Pelin; Çiftçioğlu, Muhsin; Şahin, ErdemIncreasing number of bone tissue transplant operations conducted every year has increased the use of bone grafts and bone replacement materials. The commonly employed treatment methods however have several disadvantages. Bone tissue engineering scientists has been conducting intensive research on 3D scaffolds to overcome these disadvantages. Although different materials such as hydrogels, polymers, and metals are heavily used for scaffolds the most suitable material is agreed to have a ceramic/inorganic structure since they have a similar composition to the natural bone. The perfect material for 3D scaffolds formation however has not been found due to the rheological limits of inks/suspensions used in this versatile consolidation technique. Tricalcium aluminate (C3A) and tricalcium silicate (C3S) cement powders were produced with three different marble dust sources and two different silica sources in this work. The produced powders were combined with additives such as magnesium sulfate (MgSO4), hydroxyethyl cellulose (HEC), gluconic acid (GA), polyethylene glycol (PEG), trisodium sulfate (TSC) and sodium dodecyl sulfate (SDS) for the optimization of 3D printing cementitious inks/suspensions through the investigation of their rheological properties. The optimum firing temperature for C3A powder was determined to be 1300oC with 2 hours hold period while it was found to be 1400oC for 4 hours for C3S powder preparation with rapid cooling to room temperature. The use of C3A suspensions in 3D printers necessitate the presence of 1M MgSO4 which acts as a retarder; 2% HEC and 1% PEG for increasing stability; and finally, 10% marble dust and silica. C3S suspensions should contain 1M gluconic acid, 2.5% HEC, 1% PEG, 0.1M trisodium citrate and 0.1M sodium dodecyl sulfate. Capillary rheometer results are compatible with oscillating rheometer results and have been the subject of a preliminary study for 3D printers in this thesis work.Master Thesis Processing and Characterization of Novel Graphene Containing Inks(01. Izmir Institute of Technology, 2022) Yüksel, Seda Sultan; Çiftçioğlu, Muhsin; Çiftçioğlu, MuhsinScientific and industrial community currently has an increased interest in printed electronics due to its many advantages. Metallic nanoparticles and conductive polymers are mostly used in the processing of commercial conductive inks. There is extensive research and development efforts on alternative materials as conductive fillers due to high cost, chemical instability in air and liquid media of widely used fillers. Graphene materials comprised of a single layer or multiple layers of graphene flakes have recently attracted great interest and used in applications as an excellent conductive filler due to its optical transparency, high conductivity, and flexibility. The aim of this MSc work was to prepare graphite and carbon black based conductive inks. Effects of graphite (G) to carbon black (CB) ratio and the use of exfoliation liquid on conductivity, rheology and particle size distribution were investigated for graphite containing conductive inks. Inks with the lowest resistance of 0.02 kΩ was obtained by using ball milling in N-metil-2-pirrolidon (NMP) as exfoliation liquid with the lowest particle size with an average of 18.0 µm. Inks prepared in this work showed shear thinning behavior independent of the exfoliation liquid used in their preparation. The highest thixotropy was measured in water exfoliated ink with 1801 Pa.s-1 and this dispersion had the lowest conductivity. A series of inks with different graphite to carbon black ratios were prepared under similar conditions. The lowest resistance 0.045 kΩ was determined at a graphite to carbon black ratio of 1 by using ethylene glycol as an exfoliation liquid. The use of ethylene glycol in commercial ink preparation may be advantageous due to its lower cost and environmentally friendly chemical properties. The highest degree of thixotropy and viscosity was measured in ink prepared at G/CB ratio of 0.5. This ink also had the highest resistance due to low amount of graphite compared to carbon black which indicated the critical importance of G/CB ratio.Master Thesis Rheological Behavior of Carbon Black Inks(01. Izmir Institute of Technology, 2022) Ekerler, Deniz; Çiftçioğlu, Muhsin; Çiftçioğlu, MuhsinThe printing ink industry is increasingly facing challenges in terms of high manufacturing costs and quality requirements. Rheological properties of the inks must be better understood for the development of production and application processes. Effects of pigment and dispersant content, varnish/solvent ratio, grinding medium, grinding time and storage period on rheological and printed optical properties were investigated for carbon black inks in this thesis work. The viscosity of the dispersant free ink was higher than inks with dispersant. The viscosity of the dispersant-free ink increased after three months storage whereas the viscosity of the dispersant-containing ink remained almost constant. Pigment content or V/S ratio increase resulted in higher viscosities. Grinding with 0.5 mm beads provided a finer size distribution and lower viscosities than ink ground with 0.8 mm beads. Longer grinding time increased the ink viscosities at pigment contents over 20 wt%. Thixotropy of dispersant free ink was determined to be about 12 times higher than 0.5 wt% dispersant containing ink. The thixotropy area of the 30 wt% pigment containing ink was determined to be five times higher than that of 25 wt% pigment containing ink. The thixotropy of the 25 wt% pigmented ink increased when the grinding time was changed from 30 to 60 minutes. Inks with coarser particle size distribution had higher thixotropy. Loss tangent (G''/G') at 10 Hz was used to create a correlation with color strength. Color strength of 14 out of 16 inks was determined higher with lower loss tangent values. Inks containing dispersant, higher pigment contents, varnish/solvent ratios close to one, increasing grinding time at higher pigment content increased the color strengths in printings.Master Thesis Ceramic Microfiltration Membrane Design Towards Oil Removal in Metal Industry Wastewater Streams(01. Izmir Institute of Technology, 2020) Eren, Muhammet Şakir Abdullah; Çiftçioğlu, MuhsinIncreasing water scarcity is an important threat to the whole world. The use of too much water during the production processes and the insufficient level of reuse of this water and the increasing quantities of oil containing waste generated in many industrial activities cause dangerous consequences for the environment. Highly concentrated oil-inwater emulsions are very harmful for aquatic life, soil, atmosphere and human health. Traditional treatment methods are not effective in the removal of emulsified oil droplets which have less than 20 µm of droplet size. Ceramic micro/ultrafiltration membranes have been explored and developed in recent years due to their superior advantages in oil containing water treatment/purification. The aim of this MSc study was to produce tubular ceramic supports and microfiltration membranes for the removal of oil from stable oil in water emulsions used as metal cutting fluids. The prepared metal cutting fluids were fed to the crossflow filtration system and the effects of experimental parameters such as transmembrane pressure (TMP), crossflow velocity (CFV) and oil content on membrane performance/permeate flux were investigated. The single/double layered coatings on the support surfaces were formed in the preparation of the microfiltration membranes by using stable 0.4 µm α-alumina suspensions. The 1 layer and 2 layers containing microfiltration membranes were heavily fouled and very low permeate fluxes were obtained in an hour of treatment. This was attributed to the formation of a thin oil layer on the microfiltration membrane surfaces. The reduction of the total suspended solids (TSS) and turbidity were determined as ~100 %. A stable permeate flux with a lower extent of membrane fouling and concentration polarization was obtained with 1% oil content and the support membrane and TMP=2 bars.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 Polymer-Zeolite Composite Membranes(01. Izmir Institute of Technology, 1999) Ebil, Özgenç; Çiftçioğlu, MuhsinThis thesis is on the investigation of polymer-zeolite composite membranes for gas separation and the effects of a number of parameters such as solvent and zeolite type, zeolite content, polymer/solvent ratio and preparation temperature on the microstructure of the final membrane. Although there is an increasing interest in polymeric composite membranes, most of the previous work concentrated on the synthesis and performance measurements of new membrane materials rather than the effects of different methods and parameters on processmg.In this study polymer-zeolite composite membranes were prepared by a phase inversion technique. Polysulfone, natural zeolite and synthetic zeolite 13X were used as polymer and second phases respectively. Dichloromethane and dimethylformamide were used as solvents. Four experimental sets of membranes containing the same polymer but different solvents and zeolites with increasing zeolite loadings were prepared and characterized by thermo gravimetric analysis, infrared spectroscopy, optical microscopy and scanning electron microscopy.It has been found that the types of the solvent and zeolite directly affect the final microstructure of the membranes. Solvent removal rate and distribution of zeolite particles are important and have strong effects on the mechanical performance of the membranes.Membranes prepared by using synthetic zeolite 13X and dichloromethane were determined to be the best zeolite distributions in the microstructure by optical microscopy and thermogravimetric analysis. Uniform and mechanically strong membranes with 20-60 % synthetic zeolite contents were prepared. Mechanically weak and relatively nonuniform membranes were prepared by using natural zeolite clinoptilolite. The incorporation of an ultrasonic treatment of the zeolite dispersion most likely contributed in the successful deagglomeration of the second phase in the polymer matrix.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 Preparation and Characterization of Ha Powders-Dense and Porous Ha Based Composite Materials(01. Izmir Institute of Technology, 2002) Şimşek, Deniz; Çiftçioğlu, Muhsin; Şimşek, Deniz; Çiftçioğlu, MuhsinThe synthesis of hydroxyapatite (HA) powers, whiskers and preparation of HA based ceramics have been investigated in this work. Commercial HA powders were used for comparion purposes. The powder and sintered ceramics were characterized by optical microscopy, SEM,XRD, particle size determination, dilatometry and mechanical testing.Ca-P powders were synthesized by using (NH4)2HPO4 and Ca(NO3)2. 4H2O by aprecipitation method in aqueous medium. Ca/P ratio was set to 1,5 and 1,667 that yield the mixture of Ca-P phases and HA powder respectively at pH 10, 60 C and 24hrs aging. Ca/P ratio was set to 1,667 and the effect of pH of the medium, aging temperature and aging time on the powder characteristics was investigated. pH was set to 4,6,8,9,10 and 11 while aging temperature and time kept constant at 60 C and 24 hrs.Formation of HA powder was observed over pH 8. Agglomerated Monetite-Brushite powder was obtained at pH.4. Monodispersed prismatic Brushite crystals were obtained at pH.6. Aging temperature investigation was performed at 30-90 C at pH.10 for 24 hrs aging. Increase in the aging temperature led to formation of more thermally stable HA phase. Precipitates were aged for 0, 0.5, 1, 24 and 48 hours at constant pH.10 and temperature 60 C. Thermally stable HA phase was obtained over 24hr aging. All of the oven-dried precipitates were heat treated at 400-1250 C range in order to investigate the thermal stability and phase structure development. Optimum conditions for the precipitation of thermally stable HA powder was determined as pH.10, 60 C aging temperature and 24 hrs aging time that yields equaxed HA powder with particle size about 40-60 nm.Molten salt synthesis (MSS) and hydrothermal synthesis (HDT) were used to prepare HA whiskers. XRD patterns of both whiskers have shown that HA was the dominant phase in whiskers and no other phases were detected. Hydrothermal whiskers had submicron diameters with an average aspect ratio of 20. The diameter of the MSS whiskers were in the 1-5 micron range and were mostly hexagonal with an average aspect ratio of 10.10, 20 and 30 vol% whisker containing composites were prepared. Sintering behavior and mechanical properties were investigated. 98% TD of HA ceramics (3.16 g/cm3) was obtained in the 1150-12500C range. 80-90% TD was obtained at above 1200 C for the MSS whisker composites with very little shinkages. Densities of the HDT whisker containing composites were higher than those of the MSS whisker composites. The highest hardness value was determined as 537 Hv for the HA ceramics 1250 C sintered. Hardness of the composites was lower than that of pure HA powder based ceramics due to the presence of relatively high porosity. 10vol% MSS whisker addition yields comparable compressive strength (460-470 MPa) and elastic modulus values (14-17 GPa) with that of natural bone tissues (170-193 MPa compressive strength, 14-18 GPa elastic modulus).