TiZir Titanium & Iron produces high titania slag and high purity pig iron from ilmenite in Tyssedal. The ilmenite is pelletized before smelting. Bentonite is added to the ilmenite concentrate as a binder to give the pellets strength and durability. Bentonite consists mainly of silica and alumina, which are considered as impurities in the high titania slag production. The use of organic binder has therefore been suggested as a substitute for bentonite.This work has focused on developing knowledge on the pelletization process and investigating various organic binders.Two methods of agglomeration, pelletization and briquetting, have been used in this work. Three batches of pellets have been made using a laboratory scale pelletizing drum. Two organic binders, Peridur 300 and Peridur 330, have been tested and compared to pellets made with bentonite and without binder. Seven batches of briquettes have been made using a cylindrical mold and a piston. Three organic binders, Peridur 300, calcium lignosulfonate and a nano cellulose fibre have been tested and compared to briquettes made with bentonite and without binder. The characterization included drop number test (pellets only), compression strength and thermal treatment.Briquettes were employed because using pellets yielded large deviations in the results. These deviations were believed to stem from the varying geometry of the pellets and were substantially mitigated by the use of cylindrical briquettes. It was found that Peridur 300 is a potential alternative to bentonite. The findings from thermal treatment suggest that above 500 degrees celcius sintering takes over as the dominating binding mechanism. For green strength, increasing binder viscosity has a positive effect.

This project looks at the capillary systems with salt water and oil that can be found in porous stones in oil reservoir. The interactions between the different phases and how salt concentration differences can move the oil. The first problem was to find how the water migrates from one side of an oil droplet to the other due to the concentration difference. This was discussed, but not experimentally verified. The reason for this is the high inaccuracy of the experiments and the lack of knowledge before starting. However, this project gives a lot of important knowledge about the problem, and good suggestions for improvements. It was experimentally confirmed that oil is moving due to the difference in salt concentration. From this, the diffusion coefficient was found and reported to be D = (1.08 ± 0.10) · 10−7 m2/s for glass capillary tubes of radius 0,70 mm and at 60oC, calculated from the phenomenological coefficient L that was found. It was also confirmed that the capillary force does not contribute significantly for this size of the tubes, and therefore L should be independent of the radius. The maybe most interesting result of the experiments and calculations is that the capillary force will contribute significantly to the total force and then also the movement of the oil droplet. This does not happen before the radius of the tubes where under 0,20 mm. The experiments and the estimates agreed well with the radius where the change happens.

Electro-oxidation of ethanol on smooth platinum surfaces was studied in thetemperature range 21C to 140C for 0.2 M ethanol in 0.5 M sulphuric acid.This was done by use of cyclic voltammetry and electrochemical impedancespectroscopy. In addition cyclic voltammetry with different ethanol concentrationsfrom 0.1 M to 1 M, in 0.5 M sulphuric acid was done at room temperature.Cyclic voltammetry with different ethanol concentrations showed a shift to morepositive potentials for the first oxidation peak in positive going scan as the ethanolconcentration increased. A shift to more positive potentials was also observed forthe oxidation peak in the negative scan as the concentration increased from 0.1M to 1 M. This indicates that the optimum surface condition is reached at higherpotentials for higher ethanol concentrations. This can be because ethanol andadsorbed ethanol derivatives take up more active sites at the surface, thus leavingless active sites available for adsorbed water derivatives which is necessary for theoxidation of ethanol to acetic acid and CO2.Cyclic voltammetry was done for increasing temperatures from 21C up to 140Cfor 0.2 M ethanol in 0.5 M sulphuric acid. These results showed an increasein oxidation current for all oxidation peaks as the temperature increased. Adecrease in peak potential for the first oxidation peak was observed for increasingtemperatures. This indicates that the optimum surface condition for ethanoloxidation is reached at lower potentials at higher temperatures. There was alsoseen an decrease in the apparent onset potential of the first oxidation peak as thetemperature increases. These effects can come from increased thermal activity forwater adsorption at higher temperatures. The peak potential for the oxidationpeak in negative going scan increased with increasing temperatures. This cancome from an easier reduction of platinum oxide at higher temperatures.Dynamic electrochemical impedance spectroscopy measurements was done atdifferent temperatures from 21C up to 140C for 0.2 M ethanol in 0.5 Msulphuric acid solution. The results from the measurements at 60C was fittedto electrochemical equivalent circuits. This gave indications of one kineticallysignificant surface adsorbed species in most potential regions with a notableoxidation current. This in combination with literature suggesting that acetic acidand acetaldehyde is the major products from ethanol electro-oxidation suggestthat the adsorbed intermediate is something other than CO(ads). Results fromthis work together with existing literature on ethanol oxidation was used to givea suggested simplified reaction mechanism for ethanol electro-oxidation.

Hindering the degradation of amines in the CO2-capturing process is important both for economical purposes when it comes to loss of solvent and impacts on the process, and to prevent emissions of volatile degradation compounds such as ammonia, nitrosamines and formaldehyde. To prevent the absorbent from degrading, either a non-degrading absorbent can be developed or a degradation inhibitor can be added to minimize the degradation. The degradation inhibitors tested in this thesis are meant to inhibit the oxidative degradation that mainly occurs in the absorber. The carbamate polymerization degradation due to CO2 and temperature has to be addressed on its own. The inhibitor screening apparatus was new, and a part of the assignment was testing this setup. The first experiment conducted on the inhibitor screening apparatus used a gas blend of 6% O2/2 % CO2 (N2 balance). This did not give enough degradation, which caused the need for rebuilding the rig. In the other experiments on the screening apparatus, a gas composition of 98 % O2/2 % CO2 was used to get sufficient amount of degradation for inhibitor screening. Inhibitor screening experiments were done using 150 mL of a 30 weight% (wt%) 2-aminoethanol (MEA) solution loaded with 0,4 mol CO2/mol MEA, at 55 °C with a gas flow of 10 mL/min. To test the stability of the inhibitors at higher temperature, thermal experiments with inhibitors were conducted. 7 mL solution was filled in stainless steel cylinders and heated at 135 °C, for a period of five weeks. The solution was 30 wt% MEA loaded with 0,5 mol CO2/mol MEA. Hydrazine was screened for inhibitory effect using a circulative closed loop apparatus because of the hazards related to this compound. The experiment was run with air, using a 30 wt% MEA solution loaded with 0,4 mol CO2/mol MEA, at 55 °C. Since experiments with both 6 % and 98 % oxygen were conducted, it was natural to compare the impact of oxygen concentration on the degradation products. Results indicated that 2-oxazolidinone (OZD) was preferred at the conditions with high oxygen, while N-(2-hydroxyethyl) glycine (HeGly) concentrations increased with decreasing oxygen content. The effect of metals on product composition was also investigated. The degradation compound N-(2-hydroxyethyl) imidazole (HEI) seems to be dependent on the metal concentrations, increasing in the presence of metals. For the inhibitors screened, the inhibition ranged from 23,59-67,81 %. Two compounds gave an increase in degradation. 1-hydroxyethane 1,1-diphosphonic acid (HEDP) was the only chelating agent stable at thermal conditions. The inhibitors did not appear to have a substantial effect on the carbamate polymerization. Quantification of degradation compounds in the samples was done using liquid chromatography-mass spectrometry (LC-MS) and anion chromatography-electrochemical detector (IC-EC). Amine loss and CO2-loading were determined using titration methods. Metal concentrations were determined using inductively coupled plasma-mass spectrometry (ICP-MS). Some analyses were done gravimetrically while others were done volumetrically. For comparison purposes, simple density measurements were done, and the data converted according to the amine loss in the sample.The initial intention was to use gas chromatography - mass spectrometry (GC-MS) to analyze the samples from the thermal experiments. The system was however not operable during the time available. ICP-MS analysis was not done in time for the last experiment. Ammonia analyses were not conducted in time for this thesis.

The rare earth elements are a group of 17 elements consisting of the lantahnide series, scandium and yttrium. The application with the largest rare earth consumption is the permanent rare earth magnets. The neodymium-iron-boron magnets are the strongest permanent magnetic material known and are widely used. There is a concern that there will be a shortage in Nd-Fe-B magnets in short time. This has lead to an increased interest in the recycling of the rare earth magnets in the world.This project gives a very brief introduction to the Nd-Fe-B magnets, their uses and recycling. Two types of experiments that aims at recovery of neodymium from Nd-Fe-B magnets have been performed; extraction of neodymium by the use of molten silver and extraction of neodymium by direct oxidation. In the liquid silver experiments, extraction was obtained, but the analysis gave equivocal results. In the direct oxidation experiment, the separation of an iron phase and a neodymium oxide phase failed, and the experiment was not seen as successful.Magnetic waste from WEEE Recycling was also performed, and it turned out to contain small amounts of rare earth elements.

In this project the main goal was to establish a routine for making a microfluidic flow cell (MFFC) using soft lithography methods, and test the flow cell with different electrolytes, sulphuric acid and a ruthenium red-ox couple, and eventually use the established routine to make a microfluidic fuel cell and test it. A routine was established using the negative photoresist ma-N405. The photoresist was overdeveloped to make sure an undercut profile was reached, which proved to be necessary for the subsequent metal lift-off. Titanium (10 nm) and platinum (25 nm) were vapor deposited on the glass chips, and the lift-off process was completed in a couple of days. Flow channels of two different heights (about 15 and 100 µm) were made by making an impression in PDMS. A low flow channel, height of 15 µm, showed a significant electrolyte resistance in the experimental electrochemical work, and none of the experiments gave the expected results. The electrolyte resistance was measured by electrochemical impedance spectroscopy and taken to be the value corresponding to the high frequency intersection of the real axis. In addition, this resistance was estimated from cyclic voltammetry and taken to be the reciprocal of the slope of the curve, and was found to vary between 104-107 Ω. The results from EIS and CV were compared, and they overlapped quite well. An MFFC with a channel height of 100 µm and 500 µm electrodes, resulted in a significant decrease in measured electrolyte resistance and gave improved electrochemical results. The electrolyte resistance was measured from EIS and was reduced a lot to about 300 - 10000 Ω. These results were not compared with linear regression of the linear hydrogen area since the hydrogen area was no longer linear. The cell was tested with a ruthenium red-ox couple (hexaammineruthenium(II)chloride and hexaammineruthenium(III)chloride), and an external hydrogen reference electrode placed in the outlet was found to be simpler to control than an internal reference electrode. The potential limits were -0.3 and 0.3 V vs. an external hydrogen electrode in the same electrolyte. The effect of flow rate, sweep rate and oxygen content in the electrolyte was investigated.

The goal of this work was the synthesis of a carotenoid cationic lipid for the research of carriers of nucleic acids into defective cells via transfection therapy. In the course of this project a precursor for the carotenoid cationic lipid was successfully obtained, but because of the limited time the synthesis of the carotenoid cationic lipid itself was not performed.

The possibilities for using CaNb2O6 as a photocatalyst in direct water splitting have been evaluated by investigating the electronic structure of the material. In addition the oxide was doped with nitrogen in order to modify the electronic structure and obtain visible light absorption. Experimental techniques such as electrochemical impedance spectroscopy (EIS), photocurrent, and diffuse reflectance spectroscopy (DRS) were combined with theoretical approaches to determine the bandgap, flatband potential and quasi-Fermi levels of the photocatalyst. CaNb2O6 was prepared by a sol-gel synthesis and doped with nitrogen by heat treatment of the oxide powder in an ammonia atmosphere. X-ray diffraction (XRD) confirmed phase pure orthorhombic CaNb2O6 for both pure and N-doped oxide and excluded a possible transformation of the oxide into an oxynitride. Upon illumination anodic photocurrents were observed implying that CaNb2O6 was an n-type semiconductor due to oxygen vacancies in the lattice. From the wavelength dependency of the photocurrent a direct bandgap of 3.7eV and an indirect bandgap of 3.4eV were determined for undoped CaNb2O6. Doping with nitrogen altered the optical properties of the oxide and shifted the absorption edge into the visible light region. Calculations using the density functional theory (DFT) attributed the change in absorption properties to the formation of narrow energy bands above the valence band of pure CaNb2O6. An alternative explanation could be a hybridization of N 2p and O 2p bands. Correspondingly a reduction of the bandgaps for N-doped CaNb2O6 with respect to the undoped oxide was identified. Impedance was applied to determine the flatband potential of CaNb2O6 from Mott-Schottky plots. However the obtained results seemed to be dominated by contributions from the electrode substrate. Theoretical investigations concluded that pinhole-free oxide layers creating an ohmic contact with the substrate are required in order to designate the observed impedance response to the space charge capacitance. Quasi-Fermi level measurements indicated a low photocatalytic activity of CaNb2O6 as no photocurrent could be detected. Further investigations are needed to identify the cause of the photocurrent limitations. Nevertheless probable explanations could be low conductivity in CaNb2O6, high concentrations of recombination centers or slow charge transfer kinetics. The latter was confirmed for porous oxide layers as the addition of a hole scavenger increased the measured photocurrent. Positive photocurrent transients were also observed for porous CaNb2O6 films and could be related to either the diffusion of electrons through the porous oxide layer or to a photoanodic decomposition of the photocatalyst.

A procedure for texturing of lead-free piezoelectric ceramics based on sodium potassium niobate (KNN) was investigated with respect to texturing procedure and choice of materials.Material compositions that were considered include KNN with and without addition of 0.5 mol% MnO, and KNN modified with Li and Ta (KNNLT), and Mn substituted into the A or B site of the perovskite structure. The two compositions KNN-Mn and KNNLT-Mn(A) compositions were further investigated as candidate materials for texturing.Textured samples of the two materials were made by tape casting and templated grain growth, using needle-shaped KNN particles as templates, while non-textured reference samples were made by conventional sintering of powders. Both textured and non-textured dense materials were characterized with respect to density, degree of texture and piezoelectric and dielectric properties. The non-textured materials sintered to high relative densities of 93.9 % for KNN-Mn and 96.7 % for KNNLT-Mn(A). A converse piezoelectric coefficient of over 250 pm/V was measured for non-textured KNNLT-Mn(A), and around 200 pm/V for KNN-Mn.Texturing led to a lower relative density of both compositions, 89.1 % for KNN-Mn and 92.1 % for KNNLT-Mn(A). The piezoelectric performance of KNN-Mn was not significantly affected by the texturing procedure, while the piezoelectric performance of KNNLT-Mn(A) became significantly poorer. This is due to the formation of a secondary phase in KNNLT-Mn(A) during sintering, which is probably caused by the compositional mismatch between the templates and the fine-grained matrix powder.Based on the results, and a theoretical consideration of the texturing procedure, a different choice of template particles is suggested for further work on texturing of KNN-based materials.

Silicon undergoes oxidation at room temperature, causing a formation of an oxide layer on its surface. Gaining knowledge about the oxide layer formed during ageing, is valuable with regards to production of high quality ceramics, Si3N4, especially with for the slip casting process.In this work silicon powders were exposed to humid air at different temperatures for different periods of time. From the XPS analysis, the oxygen and hydroxide content were found to be higher for powders aged at higher humidity compared to powder aged at lower humidity. This was verified by the estimated oxide thickness, which was larger for powder aged at higher humidity. No obvious difference could be observed for short and long ageing time in low humidity atmosphere. Results from Raman spectroscopy showed a more amorphous powder after storage in humid air. A clear shift and broadening of the crystalline silicon peak were observed for powders exposed to air at low and high humidity. The powders aged in humid air were further reacted with water at pH 9.4 and temperature of 60°C. The onset time for hydrogen evolution was observed to be later for samples exposed longer times to humid air. This indicates that the reactivity of the powder decreases as the oxide layer formed during ageing develops. The amount of hydrogen evolved seemed to be dependent on the hydrogen evolution time rather than the time of exposure to humid air. This was verified by the surface area, which was about the same for all samples, showing only a slightly decrease for increasing exposure time. The oxygen content measured was linearly related to the surface area for the main section of the samples. Higher hydroxide content seemed to catalyse the aqueous oxidation reacting, resulting in an earlier onset time for hydrogen evolution and a higher hydrogen flow. This was stated by a higher surface area and higher oxygen content for these samples.Powder thermally treated, at 300 °C and 900 °C, were also investigated. XPS analysis showed a thicker oxide layer for powder treated at 900 °C. No hydrogen was formed in the aqueous oxidation of powder treated at 300 °C. This was verified by a low surface area.Regarding the slip casting of silicon powders, a defect free green body can be obtained by reducing the hydrogen formation. Based on the results found, this can be obtained by the formation of a passivation oxide layer on the particle surface, formed during ageing of the powders in humid atmosphere before processing.Higher humidity and longer ageing time seems to affect the development of the oxide layer formed on the surface more than low humidity and short ageing time. To minimise the hydrogen formation, it is crucial to be able to control the hydroxide concentration in the aqueous oxidation accurately.