Master Degree / Yüksek Lisans Tezleri
Permanent URI for this collectionhttps://hdl.handle.net/11147/3008
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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 of Ultrafiltration/ Microfiltration Ceramic Composite Membranes for Biotechnology Applications(Izmir Institute of Technology, 2002) Erdem, İlker; Çiftçioğlu, MuhsinCeramic membranes possess desirable properties for industrial separation and concentration processes where extreme conditions of heat, pH, ionic strength are present. Ceramic composite membranes consisting of a support and a thin membrane layer with finer pores were prepared in this work. Ceramic supports were prepared from fine alumina and zirconia powders by dry-pressing and slipcasting.These supports were sintered in the 1100-1200°C temperature range.These supports were dip-coated with ceramic sols prepared from zirconium propoxide and aluminium isopropoxide for the preparation of thin layers with finer pores. Average particle sizes of these sols were measured as 3-7 nm for zirconia sol and 30-40 nm for alumina sol by laser scattering technique. The dipcoated membranes were calcined in the 500-600°C temperature range. The thermal characterization of membrane layers was determined with DTA/TGA. The microstructure of the ceramic composite membranes was investigated with SEM. The clean water permeability (CWP) of membranes was tested by using deionised water in a filtration set-up. Separation experiments were performed with bovine serum albumin (BSA, Stokes diameter: 7 nm) solution and whey to determine protein separation capacity of the composite membranes. The CWP of the dry pressed alumina supports heat treated at 1100°C was found to be higher than the permeability of the slip-cast zirconia supports heat treated at 1200°C. The protein retention of the slip-cast zirconia support was detected as 60% with UVVIS spectrophotmeter analysis (Abs. at 280nm). After the modification of the support with dip-coating protein retention of 96% was achieved. Then the composite membranes were used in whey protein concentration experiments. Whey, which is a complex biological liquid, containing proteins, carbohydrate, minerals, was fed to the membrane without any clarification process. The retention of whey proteins with dry-pressed alumina support modified with 1/4 diluted zirconia sol (calcination temperature: 500°C) was found to be 96% with a permeate flux of 40 Lm-2hour-1.Master Thesis The Use and Characterization of Composite Alumina-Titania Membranes for Gas Separation(Izmir Institute of Technology, 2002) Topuz, Berna; Çiftçioğlu, MuhsinThe preparation, characterization and pure gas permeation of sol-gel derived alumina and silica membranes were investigated in this work. The effects of various parameters on sol particle size and unsupported membranes pore structure were investigated by laser light scattering particle size and N2 adsorption-desorption analysis .-alumina membranes were prepared on ZrO2 supports by successive dipping into boehmite sols. Almost proportional decreases in sol particle size and membrane pore diameter were determined with increasing acid content during the boehmite sol preparation. Increasing the H+/Al3+ mole ratio from 0.1 to 0.25 caused the hydrodynamic particle size and BJH pore size to decrease from 65 to 30 nm and 3.6 to 2.9 nm, respectively. The pore size increased from 2.8 nm to 3 nm upon increasing the calcination temperature from 500 to 600oC. Unsupported membranes were heat treated in the 200 to 1200 oC range for the characterization of the phase structure. Boehmite was the dominant phase below 500 oC, gamma being the dominant phase up to 900 oC and pure .-Al2O3 phase was obtained upon heat treatment at 1200oC. Pinhole and crack free alumina membranes about 3 .m (double layer) in thickness were observed from SEM pictures with insignificant infiltration. The CO2 permeability through the double layer .-Al2O3 membrane calcined at 600 oC was about 2.25*10-7 mol/m2.s.Pa, and had a slight pressure dependence which may indicate Knudsen Diffusion and Laminar Flow as the effective transport mechanisms. Upon the calcination of a similar double layer alumina membrane at 500oC, the CO2 permeability decreased to 1.51*10-8 mol/m2.s.Pa and was independent of pressure. Silica membranes were prepared by a sol-gel technique. These sols were prepared by acid catalysed hydrolysis and condensation of tetraethylorthosilicate in the presence of a solvent. The effects of processing parameters like the acid type and amount utilized during sol preparation, sol aging, heat treatment conditions, dipping time on the membrane pore structure and the permeation of pure gases were investigated. The supported membranes were heat treated in the 50-400 oC range. The N2 and CO2 permeabilities of silica membranes varied in the 2.2 * 10-10 . 2.7 * 10-8 mol / m2.s.Pa and 1.2*10-9 . 6.95*10-8 mol / m2.s.Pa range for single layer membranes dipped for 10 seconds into the sol. The sols became viscous and gelled in 16 hours at 50 oC. The O2 permeability increased with aging time. The optimum dipping time during processing was determined to be 10 seconds. The permeabilities of these membranes increased significantly with the sol acid content. The thickness of the silica membranes were determined to be about 2.m and significant infiltration into the support was observed from the SEM pictures.