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  • About
  • The Global ETD Search service is a free service for researchers to find electronic theses and dissertations. This service is provided by the Networked Digital Library of Theses and Dissertations.
    Our metadata is collected from universities around the world. If you manage a university/consortium/country archive and want to be added, details can be found on the NDLTD website.
161

Анодные материалы на основе оксидов железа для литий-ионных аккумуляторов : магистерская диссертация / Anode materials based on iron oxides for lithium-ion batteries

Кошкина, А. А., Koshkina, A. A. January 2019 (has links)
The master's thesis is devoted to establish optimal parameters produced composites of iron oxide and carbon (FeOx/C) through the physicochemical study of the samples obtained for further use as anode materials of lithium-ion batteries (LIA). This interdisciplinary work was made in the laboratory of chemistry of compounds of rare-earth elements of the The Institute of Solid State Chemistry of the Ural Branch of the Russian Academy of Sciences as well as with the use of the equipment of the Ural Center for Shared Use «Modern nanotechnologies» of Ural Federal University named after the first President of Russia B. N. Yeltsin. / Магистерская диссертация посвящена установлению оптимальных параметров получения композитов из оксида железа и углерода (FeOx/C) посредством физико-химического исследования полученных образцов для дальнейшего использования в качестве анодных материалов литий-ионных аккумуляторов (ЛИА). Данная работа носит междисциплинарный характер и была выполнена в лаборатории химии соединений редкоземельных элементов ИХТТ УрО РАН, а также с использованием оборудования УЦКП «Современные нанотехнологии» УрФУ им. Б. Н. Ельцина.
162

Dissolved Sulfide Removal by Reaction with Iron Oxides / Borttagning av löst sulfid genom reaktion med järnoxider

Stenlund, Frida January 2024 (has links)
Hydrogen sulfide is a naturally occurring compound that is very toxic, highly flammable and has a characteristic “rotten egg” smell. It can irritate eyes and airways or even cause death when highly concentrated in air. It can exist both in gaseous and aqueous form where the dissolution of hydrogen sulfide in water is highly affected by pH. There are several industries with hydrogen sulfide related problems, either for safety or economic reasons (e.g., the mining industry, pulp and paper processing, oil and gas refineries, and wastewater treatment plants). The aim was to construct and test a filter of iron oxides to treat water from dissolved hydrogen sulfide. This was done through column experiments where the columns were filled with hematite and slag from the steel industry. Both the hematite and slag columns had sulfide precipitation, evident in the black discoloration, and the sulfide concentrations drastically reduced in the outlet water compared to the inlet water, indicating that the columns worked. However, there were some signs of preferential flow. Calculations indicate that the iron in the columns would be sufficient to precipitate approximately 1138 mg L−1 H2S at a flow rate of 0.2 ml min−1 for roughly 66 days, based on mean values for the three hematite columns. This was only a small-scale column experiment, and if scaled up from 0.2 ml min−1 to 0.5 L s−1 in the field, the amount of hematite used would have to be increased by 150 000 to last the same amount of time. This method would hence be difficult to apply in the field since it would be difficult to change the filter. / Vätesulfid (H2S) är en naturligt förekommande förening som är väldigt giftig, mycket brandfarlig och har en karaktäristisk ”ruttet ägg” lukt. Det kan irritera ögon och luftvägar, samt orsaka dödsfall vid höga koncentrationer. Vätesulfid kan förekomma både som gas och upplöst i vätska, där dess vattenlöslighet påverkas kraftigt av pH. Det finns flera industrier som har problem med vätesulfid i sina verksamheter, ur ett säkerhets- och ekonomiskt perspektiv (t.ex. vattenreningsverk, gruv-, pappers-, och oljeindustrier). Syftet var att konstruera och testa ett filter på järnoxider för att rena vatten från vätesulfid. Filtret fungerar genom att vätesulfid och järnoxider reagerar för att fälla som järnsulfid och elementärt svavel. Undersökningen genomfördes som kolonnförsök där kolonnerna fylldes med hematit eller slagg från stålindustrin. Både hematit och slaggkolonnerna påvisade järnsulfidutfällning, tydliggjort på de svarta missfärgningarna, samt minskningen av sulfidkoncentrationen i utloppsvattnet jämfört med inloppsvattnet. Dessvärre uppstod problem med preferentiellt flöde. Beräkningar visar att järnet i kolonnerna skulle räcka för att fälla ca 1138 mg L−1 H2S vid ett flöde på 0,2 ml min−1 i uppskattningsvis 66 dagar, baserat på medelvärden för de tre hematitkolonnerna. Med tanke på att det här enbart är ett småskaligt experiment skulle en ökning från 0,2 ml min−1 till 0,5 L s−1 i fältskala innebära att mängden hematit skulle behöva ökas med 150 000 för att fungera lika lång tid. Den här metoden är således svår att applicera storskaligt med tanke på att det skulle bli komplicerat att byta filtret. / SULFREM
163

Effect of soil covers on coal waste dumps in KwaZulu-Natal on abiotic factors and bacteria causing acid mine drainage

Cleghorn, Charles, 1970- 03 1900 (has links)
Thesis (MSc)--Stellenbosch University, 1997. / ENGLISH ABSTRACT: The activity of iron-oxidizing bacteria, for example, Thiobacillut. ferrooxidans, in the outer layers of coal waste dumps results in the oxidation of pyrite with the formation of large volumes of acid mine drainage. The process requires atmospheric oxygen and moisture. Acid mine drainage may possibly be controlled by creating unfavourable environmental conditions in dumps for the iron-oxidizing bacteria. The present research investigated the possibility of inhibiting these bacteria and consequently acid formation in coal waste dumps by means of different dump construction techniques. Physical and chemical conditions, acid formation and populations of four groups of bacteria which might produce acid were studied in the outer layers of ten differently constructed pilot scale coal waste dumps at the Kilbarchan Mine near Newcastle, Kwazulu-Natal, from September 1993 to July 1995. Dump covers consisting of a 30-cm or 70-cm layer of Estcourt soil of low permeability covered with 70 cm or 30 cm, respectively, of more permeable Avalon soil produced anaerobic conditions in the dumps throughout most of the 22 months of the test period, as did a cover of 70 cm compacted plus 30 cm uncompacted Avalon soil alone. An uncoMpacted 30-cm or compacted 50- cm Avalon soil cover proved ineffective in causing prolonged anaerobic conditions. Uncovered dumps showed only slight reduction of oxygen in the coal waste after heavy rains. Pockets of acidity were detected on several occasions in the coal waste below the 50-cm Avalon soil layer from the time of construction and progressively increasing acidity in the uncovered dumps and the waste below the 30-cm Avalon soil cover. Iron-oxidizing bacterial populations of the T. ferrooxidans type have tended to be higher in the uncovered dumps and Avalon soil-covered dumps showing acidification than in the non-acidified dumps covered with 1 m of Avalon soil or Avalon and Estcourt soil. Associated populations of iron-oxidizing bacteria of the Metallogenium type, acidophilic and non-acidophilic thiosulphate-oxidizing bacteria were generally low in the coal waste of the dumps. Thus, five of the soil covers, all with a thickness of 1 m, but not covers with a thickness of 0.5 m or less, proved effective for almost 2 years in inhibiting the diffusion of oxygen to the underlying coal waste in the pilot scale dumps and also appeared to suppress the populations of iron-oxidizing bacteria believed to be implicated in acid formation in the coal waste. These results suggest that coal waste dumps in South Africa should be covered with soil layers of 0.5-1.0 m thick to prevent the generation of acid mine drainage. / AFRIKAANSE OPSOMMING: Die aktiwiteit van ysteroksiderende bakteriee soos Thiobacillus ferrooxidans, in die buitenste lae van steenkoolafvalhope, veroorsaak die oksidasie van piriet met die gevolg dat groot volumes suur mynafloopwater gevorm word. Hierdie proses benodig suurstof en vog. Suur mynafloopwater kan moontlik beheer word deur 'n situasie te skep waar die toestande in die hope ongunstig is vir die ysteroksiderende bakteriee. Die huidige navorsing het die moontlikheid ondersoek om hierdie bakteriee te inhibeer deur verskillende afvalhoopontwerpe op die proef te stel en sodoende suurvorming in steenkoolmynhope te beperk. Die fisiese en chemies kondisies, suurvorming en populasies van vier verskillende bakterie-groepe wat dalk by suurvorming betrokke is, is vanaf September 1993 tot Julie 1995 bestudeer in die buitenste lae van tien verskillend gekonstrueerde loodsskaalafvalhope by die Kilbarchan myn naby Newcastle in KwaZulu-Natal. Afvalhoopbedekkings bestaande uit 'n 30-cm of 70-cm Estcourt grond met 'n lae permeabiliteit bedek met'n 70-cm of 30-cm laag van meer deurlaatbare Avalon grond het anaerobe kondisies veroorsaak. Ongekompakteerde 30-cm en gekompakteerde 50-cm Avalon grondlae het egter nie bestendige anaerobe kondisies in die hope veroorsaak nie. Die onbedekte hope het aerobics gebly met slegs effense dalings van suurstofkonsentrasies gedurende en na swaar reens. Geisoleerde monsters uit die steenkoolafval onder die 50-cm Avalon grondlaag het vanaf die begin van die toetsperiode tekens van suurvorming getoon. Die onbedekte steenkoolafval en die van die sel met 'n 30-cm Avalon grondlaag het met verloop van tyd al hoe meer suur geword. Die ysteroksiderende bakterie-populasies van die T. ferrooxidans tipe het geblyk om in die onbedekte en Avalon grondbedekte hope wat tekens van suurvorming getoon het hoer te wees as in die hope wat met 'n 1-m laag Avalon grond of Avalon en Estcourt grond bedek is en geen tekens van suurvorming getoon het nie. Ysteroksiderende bakteriepopulasies van die Metallogenium tipe, nieasidofiele en asidofiele tiosulfaatoksiderende populasies was oor die algemeen laag in die steenkoolafvalhope. Vyf van die grondlae wat alma! 1 m dik was het dus geblyk om effektief te wees in die bekamping van die infiltrasie van suurstof na die onderliggende steenkoolafval in die loodskaalhope. Dit lyk asof daardie lae die ysteroksiderende populasies betrokke by suurvorming onderdruk het. Die 0.5-m grondbedekking het egter nie so 'n sterk onderdrukkende effek op die suurstofinfiltrasie of die bakteriepopulasie gehad nie. Na aanleiding van hierdie resultate blyk dit dat steenkoolafvalhope in Suid-Afrika met minstens 0.5 tot 1..0 m grond bedek moet word om effektief die probleem van suur mynafloopwater te bekamp.
164

Micro-organisms involved in iron oxidation and acid mine drainage formation in KwaZulu-Natal and their control by soil covers on coal waste dumps

Modinger, Heinrich 03 1900 (has links)
Thesis (MSc)--Stellenbosch University, 1998. / One copy microfiche. / ENGLISH ABSTRACT: The biologically catalysed oxidation of pyrite in the outer layers of coal waste dumps leads to the formation of acid mine drainage. The oxidation of pyrite to ferric iron and sulphate is a complex process involving various abiotic and biologically catalysed reactions. Pyrite is abiotically oxidized by ferric iron, with the formation of thiosulphate and ferrous iron. Thiosulphate decomposes to form various inorganic sulphur compounds. Bacterial catalysis of pyrite oxidation is achieved by iron-oxidizing bacteria oxidizing ferrous iron to ferric iron. Bacteria that oxidize sulphur compounds assist the catalysis by oxidizing thiosulphate and its decomposition products. Heterotrophic organisms may play a role by consuming organic substances inhibitory to the lithotrophic bacteria. Abiotic ecological factors, acid formation and populations of iron-oxidizing bacterial groups were studied in 10 differently constructed pilot scale coal waste dumps, as the second phase of a study which started in September 1993. Gas samples were withdrawn weekly from coal waste through permanently buried stainless steel probes, for analysis in the field using a portable oxygen/carbon dioxide meter. Samples of coal waste were extracted by auger for analysis of moisture, pH and microbial populations. The analyses of oxygen and pH can be recommended for the routine monitoring of rehabilitated waste dumps. Covers of Avalon soil 0.3 or 0.5 m thick, were not adequate to prevent acidification. Coal waste covered with 0.7 m compacted beneath 0.3 m uncompacted Avalon soil, showed a slow pH decline, but reached approximately pH 3 in 1997. Covers of compacted Estcourt soil beneath tmcompacted Avalon soil to a cover depth of 1 m were effective in preventing acidification and generally kept the coal waste anaerobic. However, all covers developed cracks during drought conditions in 1995, allowing aeration. Low pH of some samples from these dumps during 1995/1996 may have indicated the start of acidification. Bacteria oxidizing high concentrations of ferrous iron and considered to be Thiobacillus ferrooxidans, were monitored routinely, but may not have been the dominant iron-oxidizer, as population counts using media with a lower ferrous iron concentration were higher. The majority of the latter organisms could also not oxidize sulphur, hence were not T. ferrooxidans. The populations of the high ferrous iron-oxidizing bacteria were affected by pH, tending to be high in acidified and low in non-acidified coal waste. Investigations of microbial populations forming iron-oxidizing consortia in enrichment cultures from coal waste and acid drainage samples showed the presence of T. ferrooxidans, the heterotrophic bacterial genus Acidiphilium, fungi of the genus Penicillium, unidentified filamentous fungi, including Cladophialophora-like morphological types, and a yeast of the genus Dipodascus. In interaction studies, the Penicillium isolate had an inhibitory effect on T. ferrooxidans (subjected to organic compound stress), but the Cladophialophora-like fungi reduced inhibition by organics. Fungi have not previously been studied in detail as components of iron-oxidizing consortia, but the bacterial isolations agree with those elsewhere, indicating that appropriate conclusions from acid mine drainage research in other parts of the world can be applied in KwaZulu-Natal. / AFRIKAANSE OPSOMMING: Die biologies gekataliseerde oksidasie van piriet in die buitenste lae van steenkoolafvalhope lei tot die vorming van suur mynafloopwater. Die oksidasie van piriet tot ferri-yster en sulfaat is 'n komplekse proses wat abiotiese en biologies gekataliseerde reaksies insluit. Piriet word abioties deur ferri-yster geoksideer, met die vrystelling van tiosulfaat en ferro-yster. Tiosulfaat verval om verskeie anorganiese swawelverbindings te vorm. Bakteriese katalise van pirietoksidasie word deur ysteroksiderende bakteriee wat ferro-yster na ferri-yster oksideer, bewerkstellig. Bakteriee wat swawelverbindings oksideer maak 'n bydrae tot die katalise deur tiosulfaat en vervalprodukte daarvan te oksideer. Heterotrofe organismes mag ook 'n rol speel deur organiese verbindings wat die litotrofe bakteriee mag inhibeer, te verbruik. Abiotiese ekologiese faktore, suurvorming en bevolkings ysteroksiderende bakteriee is in 10 verskillend gekonstrueerde loodsskaal steenkoolafvalhope bestudeer, as die tweede fase van 'n studie wat in September 1993 begin het. Gas monsters is weekliks uit die steenkoolafval onttrek deur vlekvrye staal peilers wat permanent daarin begrawe is, en met behulp van 'n draagbare suurstoflkoolstofdioksiedanaliseerder in die veld ontleed. Monsters van die steenkoolafval is met behulp van 'n kleiboor vir die analise van vog, pH en mikrobepopulasies geneem. Die analise van suurstof en pH kan aanbeveel word vir die roetiene monitering van gerehabiliteerde afvalhope. Bedekkings van 0.3 of 0.5 m Avalongrond was nie voldoende om suurvorming te verhoed nie. Steenkoolafval wat met 0.7 m gekompakteerde en 0.3 m ongekompakteerde Avalongrond bedek is, het 'n stadige pH-daling getoon, maar het in 1997 ongeveer pH 3 bereik. Bedekkings van gekompakteerde Estcourtgrond onder ongekompakteerde A valongrond met 'n totale dikte van 1 m, was effektief in die voorkoming van suurvorming. Hulle het oor die algemeen die steenkoolafval anaerobies gehou, maar aile bedekings het tydens die droogte in 1995 krake ontwikkel, wat suurstof laat binnedring het. 'n Lae pH gedurende 1995/1996 by sommige monsters uit hierdie hope mag die begin van suurvorming aangedui het. Bakteriee wat hoe konsentrasies ferro-yster oksideer en wat as Thiobacillus ferrooxidans beskou is, was moontlik nie die dominante ysteroksideerder nie, aangesien bevolkingstellings waar 'n medium met 'n laer konsentrasie ferro-yster gebruik is, hoer bevolkings getoon het. Die meerderheid van laasgenoemde organismes kon ook nie swawel benut nie en dus nie T. ferrooxidans was nie. Die bevolkings van die hoe ferro-ysteroksiderende bakteriee is deur pH beInvloed, met 'n geneigdheid tot hoe bevolkings in suur en lae bevolkings in minder suur steenkoolafval. Ondersoeke na die rnilcrobebevollcings wat in ysteroksiderende konsortia in verryldngslculture vanaf steenkoolafval- en suur mynafloopwatermonsters voorgekom het, het die teenwoordigheid van 7'. ferrooxidans, die heterotrofe balcteriegenus Acidiphilium, fungi van die genus Penicillium, ongeIdentifiseerde fungi, insluitend Cladophialophora-agtige tipes en 'n gis van die genus Dipodascus aangetoon. By interaksiestudies het die Penicillium-isolaat 'n inhiberende effek op T ferrooxidans (onderworpe aan organiese verbindingstres) gehad, maar die Cladophialophora-agtige fungi het die inhibisie deur organiese verbindings verminder. Fungi is nog the in detail as komponente van ysteroksiderende konsortia bestudeer the, maar die isolasies van bakteried stem saam met die van elders wat aandui dat toepaslike gevolgtreldcings ten opsigte van suur mynafloopwatemavorsing vanaf ander dele van die wereld ook in KwaZulu-Natal toegepas kan word.
165

Biogeochemical Defluoridation

Evans-Tokaryk, Kerry 09 June 2011 (has links)
Fluoride in drinking water can lead to a crippling disease called fluorosis. As there is no cure for fluorosis, prevention is the only means of controlling the disease and research into fluoride remediation is critical. This work begins by providing a new approach to assessing fluoride remediation strategies using a combination of groundwater chemistry, saturation indices, and multivariate statistics based on the results of a large groundwater survey performed in a fluoride-contaminated region of India. From the Indian groundwater study, it was noted that one technique recommended for defluoridation involved using hydrous ferric oxide (HFO) as a solid phase sorbent for fluoride. This prompted investigation of bacteriogenic iron oxides (BIOS), a biogenic form of HFO, as a means of approaching bioremediation of fluoride. Batch sorption experiments at ionic strengths ranging from 0.001 to 0.1 M KNO3 and time course kinetic studies with BIOS and synthetic HFO were conducted to ascertain total sorption capacities (ST), sorption constants (Ks), and orders of reaction (n), as well as forward (kf) and reverse (kr) rate constants. Microcosm titration experiments were also conducted with BIOS and HFO in natural spring water from a groundwater discharge zone to evaluate fluoride sorption under field conditions. This thesis contributes significant, new information regarding the interaction between fluoride and BIOS, advancing knowledge of fluoride remediation and covering new ground in the uncharted field of fluoride bioremediation.
166

Multimodal characterization of superparamagnetic particles of iron oxide for inflammation imaging : application to experimental cerebral ischemia / Caractérisation multimodale des particules superparamagnétiques d'oxyde de fer pour l'imagerie de l'inflammation : application à l'ischémie cérébrale expérimentale

Marinescu, Marilena Ioana 10 January 2012 (has links)
Plusieurs études menées chez le petit animal ont montré que l'IRM réhaussé avec les nanoparticules d'oxyde de fer (USPIO) permettait de détecter la neuroinflammation. Cependant, à notre connaissance, aucune équipe n'avait à ce jour étudié le potentiel de cette approche pour le suivi d'un traitement anti-inflammatoire. Dans ce contexte, nous avons démontré la faisabilité de cette approche pour monitorer les effets de la minocycline suite à une ischémie cérébrale chez la souris. L'IRM est une technique très sensible pour la détection du fer, mais la localisation précise des USPIO tout comme leur quantification est difficile. Nous avons donc proposé de compléter l'approche IRM par une technique inédite à notre connaissance dans le domaine de l'imagerie cérébrale des USPIO : la tomographie par rayonnement Synchrotron. Nous présentons ici les tous premiers résultats montrant la faisabilité de l'approche, ainsi qu'une étude comparée de la sensibilité, des deux techniques pour la détection des USPIO dans le cerveau. Dans la première partioe de notre travail , nous apportons nos résultats concernant la biotransformation des USPIOs dans la rate de la souris dans les 40 premiers jours suivant leur injection intraveineuse obtenus en microscopie électronique par transmission (MET). / Several studies on small animals have shown that MRI enhanced with nanoparticles of iron oxide (USPIO) is able to detect the neuroinflammation. However, to our knowledge, no team had yet investigated the potential of this approach for monitoring an anti-inflammatory treatment. In this context, we have demonstrated the feasibility of this approach to monitor the effects of minocycline after cerebral ischemia in mice. MRI is a very sensitive technique for the detection of iron, but the precise location of USPIO as well as their quantification is difficult. We therefore propsed to complete the MRI approach by a new technique to our knowledge in the field of USPIO imaging in the brain : Synchrotron radiation tomography. We here present the first results showing the feasibility of this approach and a comparative study of the sensitivity of two techniques used for the detection of USPIO in the brain. In the last part of our work, we report our results on the biotransformation of USPIOs in the spleen of the mouse during the first 40 days after intravenous injection obtained by transmission electron microscopy (TEM).
167

Magnetometrické a spektrometrické analýzy polétavého prachu z lokalit s emisním znečištěním ovzduší převážně z automobilové dopravy (Pražský okruh) a z průmyslu (poblíž ostravských hutí) s využitím meteorologických dat / Magnetometrical and spectrometrical analyses of fly ashes from the areas with emissonal air pollution mainly from automobile traffic (near Prague's D0 motorway) and from industry (near Ostrava's iron-mills) with a use of meteorological data

Hrušková, Gloria January 2018 (has links)
The content of analytical part of this thesis is the study of airborne dust samples collected in places with its higher concentration: by the Prague Ring (D0 motorway) and near the Ostrava's iron-mills. In both places, automobile transportation or industrial production are the primary sources of particulate matter emissions in the air. Received samples of PM1, PM2, PM10 a TSP filters were obtained by a standard air pollution monitoring procedure. This study examines the relationship between the magnetic parameters of the samples, their level of concentration of metals frequently present in emissions from these sources, the total mass of the dust fraction in the samples and the meteorological parameters (for Ostrava samples). The magnetic properties of the filters were investigated by magnetometric analyzes using a vibration sampling magnetometer. The concentrations of the metals were monitored by X-ray fluorescence spectrometer, the weight of parts of dust filtres was measured on laboratory scales.
168

Reduction of ferric and ferrous compounds in the presence of graphite using mechanical alloying

Moloto, Ledwaba Harry 05 1900 (has links)
M.Tech. (Department of Chemistry, Faculty of Applied Sciences), Vaal University of Technology / Many oxidic iron compounds—iron oxides; oxy-hydroxides and hydroxides—not only play an important role in a variety of disciplines but also serve as a model system of reduction and catalytic reactions. There are more than 16 identifiable oxidic iron compounds. The reduction of these compounds has been investigated for centuries. Despite this, the reduction behavior of the oxides is not fully understood as yet. To date the reduction mechanism is still plagued with uncertainties and conflicting theories, partly due to the complex nature of these oxides and intermediates formed during the reduction. Thermodynamically, the reduction of iron oxide occurs in steps. For example, during the reduction of hematite (a-Fe2O3) magnetite (Fe3O4) is first formed followed by non-stoichiometric wüstite (Fe1-yO) and lastly metallic iron (a-Fe). The rate of transformation depends on the reduction conditions. Further, this reduction is accompanied by changes in the crystal structure. The reduction behavior of iron oxides using graphite under ball-milling conditions was investigated using Planetary mono mill (Fritsch Pulverisette 6), Mössbauer Spectroscopy (MS), X-ray Diffraction (XRD), Scanning electron microscopy (SEM) and Transmission Electron Microscopy (TEM). It was found that hematite transformed into magnetite, Wüstite and or cementite depending on the milling conditions. The study shows that by increasing the milling time, the rotational speed and / or the ball to powder ratio, the extent of the conversion of hematite to its reduction products increased. Further investigations are required for the elucidation of the reduction mechanism. The reaction og magnetite and graphite at different milling conditions lead to the formation of Fe2+ and Fe3+ species, the former increasing at the expense of Fe3O4. Fe3O4 completely disappeared after a BPR of 50:1 and beyond. The Fe2+ species was confirmed to be due to FeO using XRD analysis. HRSEM images Fe2O3 using scanning electron microscopy prior to and after milling at different times showed significant changes while the milling period was increased, HRSEM images showed that the once well defined hematite particles took ill-defined shapes and also became smaller in size, which was a results of the milling action that induced reaction between the two powders to form magnetite. EDX spectra at different milling times also confirmed formation of magnetite. EDX elemental analysis and quantification confirmed the elemental composition of starting material consisting mainly of iron. Similarly, HRSEM images of Fe3O4 using Scanning electron microscopy (SEM) prior to and after milling at different BPR showed significant changes when the milling period was increased. EDX spectra at different milling times also confirmed formation of partial FeO and EDX elemental analysis and quantification confirmed the elemental composition of starting material consisting mainly of iron than Fe2O3. TEM images of both Fe2O3 and Fe3O4 particles at different milling conditions displayed observable particle damages as a function of milling period.The once well - defined particles (Fe2O3 and Fe3O4 ) successively took ill – defined shapes, possibly accompanied by crystallite size reduction. MAS showed that the reactive milling of α- Fe2O3 and C resulted in reduction to Fe3O4 , FeO and or cementite depending on the milling conditions etc Time, milling speed and BPR variation which influenced the reduction. The study shows that by increasing the milling time, the rotational speed and / or the ball to powder ratio, the extent of the conversion of hematite to its reduction products increased. XRD study investigations even though were unable to detect spm species (Fe2+ and Fe3+ ) which has smaller crystallites below detection limits ,the variation in time showed an increment in the magnetite peaks accompanied by recession of hematite and graphite peaks as the milling time was increased which relates to the MAS observation.XRD also corroborated the data obtained from MAS that showed that the main constituent was magnetite and further evidence in support of the reduction of hematite to magnetite under reactive milling was obtained using XRD . Overall, the work demonstrated selective reduction of Fe2O3 to Fe3O4 and Fe3O4 to FeO by fine tuning the milling conditions. It is envisaged that the reduction of FeO to Fe and possible carburization to FexC could also be achieved.
169

Étude et analyse de couches minces par techniques multi-spectroscopiques pour une application sur une ligne de galvanisation / Study and analysis of thin layers by multi-spectroscopic techniques for an application on a galvanizing line

Ferté, Morgan 13 November 2014 (has links)
Avec l’émergence des nouveaux aciers chargés en éléments réactifs, la caractérisation des états de surface a pris une nouvelle dimension. En effet, différentes familles d’oxyde sont dommageables pour la qualité de surface de l’acier et peuvent nuire à l’application de revêtements annexes. Aussi, afin d’assurer une bonne qualité aux produits finis, le besoin de caractériser, en ligne, la surface de l’acier sur toute sa largeur est de plus en plus nécessaire. L’imagerie hyperspectrale est une technologie en plein essor qui permet à la fois la caractérisation spatiale et spectrale d’une surface. Elle n’avait cependant encore jamais été employée pour la caractérisation de couche mince dans l’industrie sidérurgique. Durant ma thèse, deux méthodologies ont ainsi été développées pour répondre à ce besoin: l’une via une mesure en réflexion spéculaire et l’autre via une mesure en émission. En complément d’un travail de synthèse d’échantillons de référence, un développement expérimental complet allant d’un banc de simulation aux traitements des données a été réalisé. Ce travail a permis de démontrer la capabilité de l’imagerie hyperspectrale pour la détection de couche mince d’oxyde sur un acier parfois à plusieurs centaines de degrés Celsius. Ces résultats encourageants ont conduit à réaliser la première implantation industrielle de cette technologie. Ce travail de thèse a permis d’étudier théoriquement et expérimentalement les phénomènes mis en jeu et de passer du concept répondant à un besoin industriel à l’implémentation en ligne d’un capteur dédié à la caractérisation d’une couche mince d’oxyde sur une surface en défilement dans des conditions industrielles / With the emergence of new steel loaded in reactive elements, the characterization of the physico-chemical properties of the surface states has taken a new dimension. Indeed, the thin films of oxide formed are damaging for the surface quality of the steel and may adversely affect the application of varied coatings. Also, to ensure a good quality on finished products, the need to characterize, online, the steel surface over its entire width is increasingly necessary. The hyperspectral imaging is an emerging technology that allows both spatial and spectral characterization of a surface. It had never been used to characterize thin layers in the steel industry. During my PhD, both methodologies have been developed to meet this need: one via a measurement in specular reflection and the other via a measurement in emission. In addition to a synthesis of reference samples, a full experimental development ranging from a simulation bench to the data processing was performed. This work has demonstrated the capability of the hyperspectral imaging to detect thin surface oxide layers on a steel surface, sometimes at several hundred degrees Celsius. These encouraging results led to the first industrial implementation of this technology. This thesis made it possible to study theoretically and experimentally the phenomena involved and to move from the concept that meets an industrial need to the implementation of an online sensor dedicated to the characterization of a thin oxide layer on a moving surface in industrial conditions
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Biogeochemical Defluoridation

Evans-Tokaryk, Kerry 09 June 2011 (has links)
Fluoride in drinking water can lead to a crippling disease called fluorosis. As there is no cure for fluorosis, prevention is the only means of controlling the disease and research into fluoride remediation is critical. This work begins by providing a new approach to assessing fluoride remediation strategies using a combination of groundwater chemistry, saturation indices, and multivariate statistics based on the results of a large groundwater survey performed in a fluoride-contaminated region of India. From the Indian groundwater study, it was noted that one technique recommended for defluoridation involved using hydrous ferric oxide (HFO) as a solid phase sorbent for fluoride. This prompted investigation of bacteriogenic iron oxides (BIOS), a biogenic form of HFO, as a means of approaching bioremediation of fluoride. Batch sorption experiments at ionic strengths ranging from 0.001 to 0.1 M KNO3 and time course kinetic studies with BIOS and synthetic HFO were conducted to ascertain total sorption capacities (ST), sorption constants (Ks), and orders of reaction (n), as well as forward (kf) and reverse (kr) rate constants. Microcosm titration experiments were also conducted with BIOS and HFO in natural spring water from a groundwater discharge zone to evaluate fluoride sorption under field conditions. This thesis contributes significant, new information regarding the interaction between fluoride and BIOS, advancing knowledge of fluoride remediation and covering new ground in the uncharted field of fluoride bioremediation.

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