Submitted by Automa??o e Estat?stica (sst@bczm.ufrn.br) on 2016-01-14T18:59:50Z No. of bitstreams: 1 TatianePotiguaraOliveira_DISSERT.pdf: 4152176 bytes, checksum: 173f9461ab0652eaed0cc9d6f2283f24 (MD5) / Approved for entry into archive by Arlan Eloi Leite Silva (eloihistoriador@yahoo.com.br) on 2016-01-15T20:11:56Z (GMT) No. of bitstreams: 1 TatianePotiguaraOliveira_DISSERT.pdf: 4152176 bytes, checksum: 173f9461ab0652eaed0cc9d6f2283f24 (MD5) / Made available in DSpace on 2016-01-15T20:11:56Z (GMT). No. of bitstreams: 1 TatianePotiguaraOliveira_DISSERT.pdf: 4152176 bytes, checksum: 173f9461ab0652eaed0cc9d6f2283f24 (MD5) Previous issue date: 2014-08-01 / O comp?sito Al2O3-Cu alia a fase cer?mica da alumina, que ? extremamente dura e resistente, por?m muito fr?gil, ? fase met?lica do cobre de alta ductilidade e elevada tenacidade ? fratura. Tais caracter?sticas fazem desse material um forte candidato para aplica??o como ferramenta de corte. P?s comp?sitos Al2O3-Cu nanocristalinos e de alta homogeneidade podem ser produzidos por moagem de alta energia, assim como estruturas densas e de melhores propriedades mec?nicas podem ser obtidas por sinteriza??o com fase l?quida. Este trabalho investiga o efeito da moagem de alta energia na dispers?o das fases Al2O3 e Cu, bem como a influ?ncia do teor de Cu na forma??o das part?culas comp?sitas Al2O3-Cu. Um moinho planet?rio Pulverisatte 7 de alta energia foi usado para efetuar os experimentos de moagem. P?s de Al2O3 e Cu na propor??o de 5, 10 e 15% em massa de Cu foram colocados para moer em um recipiente com bolas de metal duro e ?lcool et?lico. Uma raz?o em massa de p? para bolas de 1:5 foi utilizada. Todos os p?s foram mo?dos at? 100 horas, e amostras de p?s foram coletadas ap?s 2, 10, 20, 50 e 70 horas de moagem. Compactos de p?s comp?sitos com forma cil?ndrica de 8 mm de di?metro foram prensados em matriz uniaxial e sinterizados em forno resistivo a 1200, 1300 e 1350 oC por 60 minutos e sob uma atmosfera de arg?nio e hidrog?nio. A taxa de aquecimento usada foi de 10 oC/min. Os p?s e as estruturas dos corpos sinterizados foram caracterizados por DRX, MEV e EDS. An?lises de TG, DSC e granulometria tamb?m foram usadas para caracterizar os p?s mo?dos, assim como, a dilatometria foi empregada para observar a contra??o dos corpos sinterizados. A densidade dos corpos verdes e sinterizados foi medida usando o m?todo geom?trico (massa/volume). Medidas de microdureza vickers com carga de 500 g durante 10 s foram efetuadas nas estruturas sinterizados. Os comp?sitos Al2O3?Cu com 5% de cobre alcan?aram densidade de 61% da densidade te?rica, e uma dureza de 129 HV quando sinterizados a 1300 oC por 1h. Diferentemente, menores densidades (59 e 51% da densidade te?rica) e durezas (110 e 105 HV) foram alcan?adas quando o teor de cobre aumento para 10 e 15%. / The Cu-Al2O3 composite ceramic combines the phase of alumina, which is extremely hard and durable, yet very brittle, to metallic copper phase high ductility and high fracture toughness. These characteristics make this material a strong candidate for use as a cutting tool. Al2O3-Cu composite powders nanocrystalline and high homogeneity can be produced by high energy milling, as well as dense and better mechanical structures can be obtained by liquid phase sintering. This work investigates the effect of high-energy milling the dispersion phase Al2O3, Cu, and the influence of the content of Cu in the formation of Cu-Al2O3 composite particles. A planetary mill Pulverisatte 7 high energy was used to perform the experiments grinding. Al2O3 powder and Cu in the proportion of 5, 10 and 15% by weight of Cu were placed in a container for grinding with balls of hard metal and ethyl alcohol. A mass ratio of balls to powder of 1:5 was used. All powders were milled to 100 hours, and powder samples were collected after 2, 10, 20, 50 and 70 hours of grinding. Composite powders with compact cylindrical shape of 8 mm diameter were pressed and sintered in uniaxial matrix resistive furnace to 1200, 1300 to 1350 ?C for 60 minutes under an atmosphere of argon and hydrogen. The heating rate used was 10?C/min. The powders and structures of the sintered bodies were characterized by XRD, SEM and EDS. Analysis TG, DSC and particle size were also used to characterize the milled powders, as well as dilatometry was used to observe the contraction of the sintered bodies. The density of the green and sintered bodies was measured using the geometric method (mass / volume). Vickers microhardness with a load of 500 g for 10 s were performed on sintered structures. The Cu-Al2O3 composite with 5% copper density reached 61% of theoretical density and a hardness of 129 HV when sintered at 1300 ? C for 1h. In contrast, lower densities (59 and 51% of the theoretical density) and hardness (110 HV and 105) were achieved when the copper content increases to 10 and 15%.

Submitted by Automa??o e Estat?stica (sst@bczm.ufrn.br) on 2017-07-03T13:37:23Z No. of bitstreams: 1 JoseLeonaldoDeSouza_DISSERT.pdf: 2323627 bytes, checksum: 0b82f3fcf1052c6990e64f3b99a70364 (MD5) / Approved for entry into archive by Arlan Eloi Leite Silva (eloihistoriador@yahoo.com.br) on 2017-07-06T16:06:51Z (GMT) No. of bitstreams: 1 JoseLeonaldoDeSouza_DISSERT.pdf: 2323627 bytes, checksum: 0b82f3fcf1052c6990e64f3b99a70364 (MD5) / Made available in DSpace on 2017-07-06T16:06:51Z (GMT). No. of bitstreams: 1 JoseLeonaldoDeSouza_DISSERT.pdf: 2323627 bytes, checksum: 0b82f3fcf1052c6990e64f3b99a70364 (MD5) Previous issue date: 2016-05-30 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior (CAPES) / Os materiais cer?micos, tais como a alumina (Al2O3) e o cobalto (Co), apresentam caracteristicas relevantes para aplica??o como ferramentas de corte, e dentre estas se destacam a elevada dureza e o alto ponto de fus?o. No entanto, a sua aplica??o ? limitada pela sua baixa tenacidade e baixa resist?ncia mec?nica. Desta forma, a fim de aumentar a tenacidade do material, mantendo-se as elevadas propriedades mec?nicas, alguns metais, como por exemplo, o cobalto (Co), t?m sido usados na tentativa de se produzir um material mais tenaz. Neste trabalho, estudouse o efeito da moagem de alta energia e da adi??o de (%p.) Co na densifica??o e microestrutura, assim como, nas propriedades mec?nicas do composto Al2O3-Co. Os p?s-particulados (Al2O3 e Co), com percentuais de 5 e 20%p. de cobalto, foram mo?dos em um moinho planet?rio durante 50 horas, e amostras de p?s foram coletadas nos intervalos de 2, 10, 15, 20, 30,40 e 50 horas. Os p?s mo?dos foram caracterizados por difra??o de raios-X (DRX), an?lises particulom?tricas, microscopia eletr?nica de varredura (MEV); e compactados em uma matriz cil?ndrica sob uma press?o uniaxial de 100 MPa. Posteriormente, os compactados a verde foram sinterizados em um forno resistivo nas temperaturas de 1200 a 1500 ?C, por 60 minutos, sob uma atmosfera de arg?nio com taxa de aquecimento de 10?C/min. Os corpos de prova sinterizados foram caracterizados por DRX, MEV e energia dispersiva (EDS). A densidade foi medida usando o m?todo geom?trico (massa/volume), e os melhores valores foram obtidos para as amostras sinterizadas a temperatura de 1500 ?C, sendo a densidade relativa igual a 78 %, seguido das sinterizadas a temperaturas de 1350?C e 1300?C, que apresentaram as respectivas densidades 68 %, e 62 %. / Ceramic materials, such as alumina (Al2O3) and cobalt (Co), present characteristics like high hardness and the high melting point for application as cutting tools. However, its application is limited because of its low toughness and low mechanical strength. Thus, in order to increase the toughness and maintaining the high mechanical properties, some metals such as cobalt (Co) have been used. In this work, the effect of the high energy milling and different amount of Co on densification, microstructure and mechanical properties of the Al2O3-Co compound were studied. The particulate powders (Al2O3 and Co), with 5 and 20 wt% of cobalt, were milled in a planetary milling for 50 hours, and powder mixture samples were collected at the intervals of 2, 10, 15, 20, 30, 40 and 50 hours. The milled powders were characterized by X-ray diffraction (XRD), particulometric analyzes, scanning electron microscopy (SEM); And compacted in a cylindrical matrix under a uniaxial pressure of 100 MPa. Subsequently, green compacts were sintered in a resistance furnace at 1200 to 1500 ?C with holding time of 60 minutes under an argon atmosphere with a heating rate of 10 ?C/min. The sintered samples were characterized by XRD, SEM and EDS. Density was measured using the geometric method (mass/volume), and the best values were obtained for the samples sintered at 1500 ?C with relative density of 78% compared with sample sintering at 1350 and 1300 ?C which presented relative densities of 68% and 62% respectively.

No description available.

MgO-C based refractory materials, often used in secondary steel making, are exposed to variouswear mechanisms in its application. The wear could be divided into oxidative, chemical andabrasive categories, all behaving differently and all being influenced by different factors. Dueto the importance of minimizing material loss and to the environmental challenges to run asustainable industry, it is of interest to gain more knowledge of the behavior of the refractorymaterial in use. The present thesis work specifically investigated slag designed of the CaOSiO2-Al2O3-MgO (CSAM) system as well as the chemical and oxidative wear mechanisms ofthree different MgO-C based refractory materials from Höganäs AB, Halmstadverken, whichcontained 5, 10 and 12 wt% carbon (labeled T05, T10 and T12). Different CSAM slags weredesigned to meet certain process criteria such as MgO and CaO saturations and wereinvestigated through thermodynamic calculations using the FactSage software and throughlaboratory scaled slag smelting experiments. The oxidation effect on the refractory material wasalso studied through pre-heating simulations in chamber furnaces, similar to the pre-heating ofa re-built ladle furnace.The thermodynamic calculations made in FactSage 7.0, using the FactPS and FToxid databases, resulted in a few different slag designs with different properties. A few different slagsfulfilled the CaO and MgO saturation limits proposed by Höganäs AB and could be consideredto test experimentally for further evaluation. The simulations also showed trends on how theliquid viscosity behaved with different slag compositions and how the solids content changedwith temperature.The oxidation experiments were performed on the different MgO-C refractory types, where thebricks with 10% carbon also contained Al2O3 antioxidants. The experiments showed that themass loss during the pre-heating is greater for refractory with higher carbon content, withexception to T10, where the mass losses were measured to 3.76 – 4.01%, 1.06 – 1.28% and6.28 – 6.33% for T05, T10 and T12 respectively. Further, the oxidation depth of each materialwas measured to 9-10 mm, 2-3 mm and 2-5 mm for the T05, T10 and T12. The experimentsalso showed that T12 refractory in particular was very susceptible to abrasive wear after beingoxidized.The slag smelting experiments were carried out through two different methods, by melting slagin MgO-C crucibles and by melting pressed slag briquettes on top of refractory bricks. Theformer tests mainly showed that the methodology was not suitable for this type of refractorymaterial due to the crucibles cracking during the experiments. The latter experiments showedsome general behaviour of the different components in the slag, where Ca, Al and Fe stayednear the surface, and Si and Mg penetrated deeper. The spinel formation at the refractory surfacewas then concluded to be the reason for Al not penetrating deeper. Further it was concludedthat no significant difference in refractory dissolution was seen between slags with- and withoutMgO, other than possibly a small increase in refractory dissolution for the latter.

The diploma thesis deals with influence of fast pressure-less sintering on the microstructure of advanced ceramic materials, namely -Al2O3 and tetragonal ZrO2 (doped by 3 mol% Y2O3) with particle sizes ranging from 60 nm to 270 nm. Fast and controlled heating rate was enabled by utilization of the special superkanthal furnace with moving sample holder. Defect-free bulk and dense samples were prepared using heating rates in order of 100-200 °C/min. Higher densities reached the samples pressed by higher pressures; the specimens with densities higher than 99 % t.d. were prepared within tens of minutes for alumina as well as for zirconia with very low thermal conductivity. Different behavior was observed only for material TZ-3Y, which exhibited core-shell structure with dense surface and porous centre after sintering at heating rates higher than 10 °C/min. It was shown in this work that such behavior was not primarily caused by the high thermal gradient resulting from high heating rates. Its creation was probably caused by chlorine impurities. The mechanism of desintering of these samples was described and eliminated by calcination of the samples at 1000 °C for 10 hours prior to fast sintering at 1500 °C, so even this material could be fast sintered up to 99.9 % theoretical density.

V předložené diplomové práci bylo studováno slinování hexagonálního Al2O3 a kubického MgAl2O4 pomocí slinovacích cyklů složených z beztlakého předslinutí metodou dvojstupňového slinování s následným doslinutím s využitím tlaku (HIPováním). Cílem bylo pokusit se snížit (při zachování vysoké dosažené hustoty) střední velikost zrn a tím zvýšit tvrdost keramiky popř. optickou transparenci. Hlavní úsilí bylo věnováno optimalizaci předslinutí pomocí různých slinovacích cyklů. Přestože bylo vyzkoušeno velké množství různých kombinací teplot a prodlev dvojstupňového slinování, nepodařilo se výrazným způsobem zvýšit výslednou tvrdost vzorků. V případě kubického MgAl2O4 bylo dosaženo hustot blížících se teoretické hustotě, což se projevilo v optické transparentnosti vzorků.

Ziel des Forschungsvorhabens war es, die Korrosionsbeständigkeit von gelöteten Metall-Keramik-Verbindungen gegenüber verschiedenen Medien mit geeigneten Untersuchungsmethoden zu bestimmen. Durch elektrochemische Messverfahren sind die Korrosionsvorgänge von metallischen Werkstoffen und ihren Fügeverbunden charakterisierbar. Es wird eine erhebliche Reduzierung der Prüfzeit gegenüber Prüfkammer- bzw. Realprüfungen erreicht. Die Auswertung der Untersuchungen ergab eine Korrelation zwischen Korrosionsbelastung und mechanischen Eigenschaften. Folgende Grundwerkstoffe und Aktivlote wurden für die Messungen verwendet: - Stähle: 1.0037, 1.4301, 1.4016 - Keramiken: Al2O3, ZrO2, SiC, Si3N4 - Lote: AgCu28-Basislot mit variierenden Titangehalten (Schwerpunkt Lot mit 3% Ti) Das Korrosionsverhalten der aktivgelöteten Metall-Keramik-Verbindungen wird entscheidend vom am stärksten korrosiv angegriffenen Teil der Probe bzw. des Bauteils bestimmt. Liegt ein chloridhaltiges Korrosionsmedium (3,5 % NaCl-Lösung) vor, dominiert der Metallpartner das Korrosionsverhalten. Die eingesetzten Stähle werden durch Lochfraß stark angegriffen. Dieser geht in flächigen Abtrag über und mit zunehmender anodischer Polarisation werden die Stähle regelrecht zerstört. In den Stählen enthaltene sulfidische Einschlüsse fördern den Korrosionsangriff. Dies wird besonders deutlich beim Stahl 1.4301, in dem sehr viele Mangansulfide zu finden sind. Die Korrosion der Lötnaht ist vergleichbar mit der des Stahles. Bei einem sulfathaltigen Korrosionsmedium (3,5 % Na2SO4-Lösung) wird zuerst die Lötnaht und dann der Stahl angegriffen. Dies wird neben der Lichtmikroskopie auch von den topographischen Messungen bestätigt. Im Falle der Verbindungen mit 1.4016 bewirken die Keramiken eine Verbreiterung des Passivbereiches im Vergleich zu Stahl, wenn auch bei höheren Stromdichten. Die Vorbelastung der Biegeproben durch anodische Polarisation bis 200 mV in 3,5 % NaCl-Lösung bewirkt die gleiche Schädigung wie die Exposition von 96 h im Salzsprühnebel gemäß DIN 50021 SS. Die Ergebnisse aus den Festigkeitsuntersuchungen an Verbindungen mit dem Stahl 1.4016 zeigen, dass gegenüber dem nichtkorrodierten Zustand die Festigkeit abnimmt. Dennoch erfolgt der Bruch in der Keramik und nicht in der Lötnaht. Mit der Bereitstellung von Stromdichte-Potential-Kurven steht ein Messverfahren zur schnellen und vergleichenden Bewertung von Metall-Keramik-Verbindungen hinsichtlich der Korrosionsanfälligkeit zur Verfügung. Die Schädigung der Verbindungen durch Korrosion bleibt im technisch beherrschbaren Bereich und steht somit dem Einsatz von Stahl als Verbindungspartner nicht entgegen.

The topic of the Ph.D. thesis was focused on the process of sintering alumina and zirconia ceramic materials with the aim to compare kinetics of sintering sub-micro and nanoparticle systems. Zirconia ceramic powders stabilized by different amount of yttria addition in the concentration range of 0 – 8 mol% were used. The different crystal structure (secured by yttria stabilization) of zirconia, as found, did not play statistically proven role in the process of zirconia sintering. The possible influence was covered by other major factors as particle size and green body structure, which does affect sintering in general. According to the Herrings law, the formula predicting sintering temperature of materials with different particle size was defined. The predicted sintering temperatures were in good correlation with the experimental data for zirconia ceramic materials prepared from both, coarser submicrometer, and also nanometer powders. In case of alumina ceramics the predicted and experimentally observed sintering temperature values did not match very well. Mainly the nanoparticle alumina materials real sintering temperature values were markedly higher than predicted. The reason was, as shown in the work, strong agglomeration of the powders and strong irregularities of particle shape. The major role of green body microstructure in the sintering process was confirmed. The final density of ceramic materials was growing in spite of sintering temperature, which was decreasing together with pore - particle size ratio (materials with similar particle size were compared). Sintering temperature was increasing together with growing size of pores trapped in the green body structure. Clear message received from the above mentioned results was the importance of elimination of stable pores with high coordination number out off the green body microstructure during shaping ceramic green parts. Same sintering kinetics model was successfully applied on the sintering process of submicro- and also nanometer zirconia ceramics. Activation energy of nanometer zirconia was notably lower in comparison to submicrometer material. For the sintering of nanoparticle zirconia was typical so called “zero stage” of sintering, clearly visible on kinetic curves. It was found out, that processes running in zirconia “green” material during zero stage of sintering are heat activated and their activation energy was determined. Pores of submicrometer zirconia were growing in an open porosity stage of sintering just a slightly (1.3 times) compared to the nanoparticle zirconia, where the growth was much higher (5.5 times of the initial pore diameter). This difference was most probably caused by preferential sintering of agglomerates within the green bodies and by particle rearrangement processes which appears in the zero stage of sintering of nanoparticular ceramics. The technology of preparation of bulk dense ytria stabilized zirconia nanomaterial with high relative density of 99.6 % t.d. and average grain size 65nm was developed within the thesis research.

Mesoporous γ-alumina is the most extensively used catalysts support in a wide range of catalytic processes. The usefulness of γ-alumina relies on its favorable combination of physical, textural, thermal, and chemical properties. Pore structure properties are among the most important properties, since high surface area and large pore volume enable higher loading of active catalytic phases, while design of pore size and pore size distribution is critical to optimize pore diffusional transport and product selectivity. In addition, accurate determination of surface area (SA), pore volume (PV) and pore size distribution (PSD) of porous supports, catalysts, and nanomaterials is vital to successful design and optimization of these materials and to the development of robust models of pore diffusional resistance and catalyst deactivation.In this dissertation, we report a simple, one-pot, solvent-deficient process to synthesize mesoporous γ-alumina without using external templates or surfactants. XRD, TEM, TGA and N2 adsorption techniques are used to characterize the morphologies and structures of the prepared alumina nanomaterials. By varying the aluminum salts or the water to aluminum molar ratio in the hydrolysis of aluminum alkoxides, γ-alumina with different morphologies and pore structures are synthesized. The obtained alumina nanomaterials have surface areas ranging from 210 m2/g to 340 m2/g, pore volumes ranging from 0.4 cm3/g to 1.7 cm3/g, and average pore widths from 4 to 18 nm. By varying the alcohols used in the rinsing and gelation of boehmite/bayerite precursors derived from a controlled hydrolysis of aluminum alkoxides, the average pore width of the γ-aluminas can be tuned from 7 to 37 nm. We also report improved calculations of PSD based on the Kelvin equation and a proposed Slit Pore Geometry model for slit-shaped mesopores of relatively large pore size (>10 nm). Two structural factors, α and β, are introduced to correct for non-ideal pore geometries. The volume density function for a log normal distribution is used to calculate the geometric mean pore diameter and standard deviation of the PSD. The Comparative Adsorption (αs) Method is also employed to independently assess mesopore surface area and volume.

Increasing productivity is a constant demand for the manufacturing industry. Low-carbon-steel is one of the most commonly used ferrous materials in the part manufacturing market. Improving productivity as well as making the process eco-friendly by implementing a dry machining condition is the essential goal of this study. Built-up-edge (BUE) is often formed in the low-carbon-steel machining process, which, results in poor surface finish and short tool life. The high-speed-machining technique can be used to reduce the BUE formation and realize an increase in productivity. Cubic boron nitride (CBN) tools are most commonly used in hard turning and cast-iron machining at high cutting speeds. There are a limited number of studies regarding low-carbon-steel machining with CBN under a high-speed and with a dry machining condition. In this study, the investigation shows the preferable type of CBN tool and the wear mechanisms involved during finish turning operations of AISI 1018 under high speed and dry machining conditions. Test results show that a low CBN content with a TiCN binder and smaller grain size offers the best tool life and surface integrity of the final part. Currently manufacturers use coated carbide tools with a recommended cutting speed of 200-300m/min with coolant to complete the finishing process for turning low carbon steel parts. In this study, by implementing CBN tools under the dry condition at 500 m/min cutting speed (speed was selected from the preliminary test performed using the uncoated CBN from 500 to 1200 m/min), the buildup edge formation has been reduced, tool life was measured to increase by 307% compared to the benchmark tool (Coated Carbide), and surface finish was measured in the range of 0.8-1.6μm Ra. / Thesis / Master of Applied Science (MASc)