Made available in DSpace on 2014-10-09T12:38:29Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:05:30Z (GMT). No. of bitstreams: 1 06049.pdf: 5680903 bytes, checksum: f40692e31a4512f59a71e08b1b4cbd33 (MD5) / Dissertacao (Mestrado) / IPEN/D / Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP

Made available in DSpace on 2014-10-09T12:54:37Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:07:21Z (GMT). No. of bitstreams: 0 / Neste trabalho, a moagem com alta energia foi utilizada para a ativação mecânica de misturas de pós de alumínio e nióbio, na proporção de 75% atômico de alumínio, para a síntese por reação de combustão do NbAl3. O objetivo foi investigar os mecanismos de ativação atuantes e a eventual preponderância de um deles. A moagem foi realizada tanto nos pós de alumínio e de nióbio separadamente (pré-ativação), como nas misturas. O processo de síntese por reação foi realizado no modo combustão simultânea, em pastilhas compactadas a partir de misturas com e sem ativação mecânica. O comportamento térmico das pastilhas foi registrado durante todo o ciclo térmico de aquecimento e, as principais características térmicas da reação de combustão, foram determinadas. O parâmetro de rede, o tamanho de cristalito e a microdeformação elástica do alumínio e do nióbio foram determinados por difratometria de raios X, mediante análise pelo método de Rietveld. A microscopia eletrônica de varredura foi utilizada para caracterização microestrutural dos pós moídos e da pastilha reagida. Constatou-se que o mecanismo preponderante de ativação mecânica é o aumento da área de interface, que ocorre durante a formação de agregados de partículas de alumínio e nióbio. A eficiência na formação de interfaces diminuiu com a utilização de nióbio pré-ativado (encruado) e com o aumento da quantidade de ácido esteárico (utilizado como agente controlador de processo durante a moagem). O efeito principal da ativação mecânica na síntese por reação de combustão foi a redução da temperatura de ignição com o aumento do tempo de moagem. A alta densidade de defeitos cristalinos, gerada durante a pré-ativação dos pós de alumínio e nióbio e na ativação mecânica das misturas, não produziu efeitos mensuráveis sobre o comportamento térmico das pastilhas. / Tese (Doutoramento) / IPEN/T / Instituto de Pesquisas Energéticas e Nucleares - IPEN/CNEN-SP

Submitted by Claudinei Pracidelli (cpracide@ipen.br) on 2015-01-21T10:18:45Z No. of bitstreams: 0 / Made available in DSpace on 2015-01-21T10:18:45Z (GMT). No. of bitstreams: 0 / Reatores PWR empregam, como combustível nuclear, pastilhas de UO2 acondicionadas em tubos de ligas de zircônio, chamados de encamisamento. Na sua fabricação são gerados cavacos de usinagem que não podem ser descartados, pois a reciclagem deste material é estratégica quanto aos aspectos de tecnologia nuclear, econômicos e ambientais. As ligas nucleares têm altíssimo custo e não são produzidas no Brasil, sendo importadas para a fabricação do combustível nuclear. Neste trabalho são abordados dois métodos para reciclar os cavacos de Zircaloy. No primeiro, os cavacos foram fundidos utilizando um forno elétrico a arco para obter lingotes. O segundo usa a técnica da metalurgia do pó, onde os cavacos foram submetidos à hidretação e o pó resultante foi moído e isostaticamente prensado e, a seguir, sinterizado a vácuo. A composição química, as fases presentes e a dureza no material foram determinadas. Os lingotes foram tratados termicamente e laminados, sendo que as microestruturas foram caracterizadas por microscopia óptica e eletrônica de varredura. Os resultados para ambos os métodos mostraram que a composição do Zircaloy reciclado cumpre as especificações químicas e apresentaram microestrutura adequada para uso nuclear. Os bons resultados do método de metalurgia do pó sugerem a possibilidade de produzir pequenas peças, como as tampas do encamisamento - end-caps, usando a sinterização no formato quase final (near net shape). / Tese (Doutorado em Tecnologia Nuclear) / IPEN/T / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

O interesse crescente no desenvolvimento de biomateriais com superfície porosa para aplicações dentárias decorre do suporte propicio ao crescimento do tecido ósseo, aumentando a adesão entre o tecido e material, favorecendo a osteointegração. O titânio pode ser considerado um ótimo material para implantes dentários, pela sua excelente biocompatibilidade, elevada resistência à corrosão e combinação de alta resistência com baixa densidade. Contudo, a alta reatividade do metal no estado líquido acaba dificultando a fabricação de implantes por fundição, sendo a metalurgia do pó composta por técnicas que permitem a obtenção de peças em temperaturas menores de processamento (estado sólido) e com módulo elástico próximo ao do tecido ósseo. O objetivo deste trabalho foi avaliar amostras porosas obtidas pela Metalurgia do Pó (MP) convencional. Inicialmente o pó de titânio comercialmente puro (Ti-cp) obtido pelo processo de hidretação-dehidretação (HDH), foi compactado em matriz uniaxial e sinterizado a vácuo em duas temperaturas,1100 e 1150°C/1h. As amostras sinterizadas foram caracterizadas quanto à densidade, porosidade, microestrutura ( microscopia óptica - MO e microscopia eletrônica de varredura - MEV), fases cristalinas (difração de raios - X - DRX), propriedades mecânicas (microdureza e ensaio de flexão em três pontos), comportamento eletroquímico (potencial de circuito aberto, espectroscopia de impedância eletroquímica e polarização anódica) e o ensaio de imersão foram empregados nas amostras obtidas por (MP) e no titânio fundido. Os resultados indicaram morfologia angular, distribuição granulométrica com média de 45 μm, além de densidade aparente e escoabilidade baixas. Foram obtidas amostras com porosidade de aproximadamente 33% e poros interligados dentro de uma faixa de tamanho de 110 140 μm. As análises por MEV e DRX das amostras sinterizadas indicaram a presença de fase α e poros. As amostras sinterizadas a 1150°C revelaram melhor comportamento mecânico em relação as amsotras sinterizadas a 1100°C. As análises eletroquímicas indicaram a elevada resistência a corrosão do titânio fundido, seguida pela amostra sinterizada 1100°C e finalmente das sinterizadas a 1150°C, quando imersas em solução da saliva artificial. O EDS foi executado para verificar a deposição de elementos na superfície. Testes de citotoxicidade demonstraram que o pó e as amostras sinterizadas não apresentaram qualquer efeito tóxico em culturas celulares. As amostras sinterizadas à 1100°C possuiam grau de porosidade e tamanho de poros que favoreceram o crescimento do tecido ósseo, além do módulo de elasticidade próximo ao tecido ósseo e foram mais resistentes a corrosão na solução simuladora. / The development of materials with a porous surface has been widely studied in the field of biomaterials, because the porous structure allows bone tissue growth, increasing the bonding since the tissue and the material, favoring osteointegration. Given the excellent biocompatibility, high corrosion resistance and combination of high strength with low density, titanium is one of the most suitable materials for dental implants. However, the high reactivity in liquid state ends up hindering their fusion. The technique of powder metallurgy (PM) is an alternative for cost reduction, allowing to obtain superior samples at lower temperatures, closer to the bone tissue in terms of elastic modulus. The objective of this study was to evaluate porous samples obtained by conventional PM. Initially the powder of commercially pure titanium (cp-Ti) was obtained by hydridedehydride (HDH) process, followed by uniaxial pressing and vacuum sintering at 1100 and 1150 °C/1h. The sintered samples were characterized - density, porosity, microstructure (SEM), crystalline phases (XRD), mechanical properties (microhardness and three point bending test), electrochemical behavior (open circuit potential, anodic polarization and electrochemical spectroscopy impedance and immersion essay) applied in porous samples and cast titanim The results indicated angular particle morphology, 45 μm average particle size distribution, low apparent density and flowability. The different processing temperatures enabled to obtain samples with approximately 33 % interconnected porosity and average pore size in 110-140μm range. SEM and XRD analysis of the sintered samples revealed the presence of α phase and pores. Samples sintered at 1150°C showed superior mechanical behavior. Electrochemical analysis (in artificial saliva solution) indicated higher corrosion resistance of cast titanium compared to porous samples . Cytotoxicity tests proved that the powder and sintered samples has no toxic effects on cell cultures. Samples sintered at 1100 °C excels in bone growth stimulation, elasticity modulus and corrosion resistance, due to superior porosity and pore size range properties, creating a material analogous to the bone.

Diploma thesis occupy with preparation of porous material from magnesium powder with a HAp admixture by cold pressing followed by spark plasma sintering (SPS). This thesis contain both preparation of bulk material, diffusion plot and charakterization of materials based on the compaction process conditions. On the basis of physical mechanical characteristics, the impact of the pressing process on the subsequent sintering and the resulting material properties are evaluated. Bulk material is characterized considering to structure and physical–mechanical properties. Properties of final metarial will serve to optimize conditions for process of bulk material preparation.

Powder metallurgy (PM) is a technology used to manufacture near net shape components for an increasing number of applications like automobile components, aircraft components, cutting tools, refractory, household appliances, etc. The general PM process comprises of Powder manufacturing/powder tailoring, Compacting, and Sintering. Based on product’s final requirements, optional secondary operations are performed. PM components for automotive application are experiencing a growth coupled with new challenges.  PM´s capability for producing complex net shaped components with desired properties has enabled it to be an alternative to other traditional manufacturing processes. Average U.S. made vehicle in 2010 contained an estimated 41.6 pounds of PM parts and in Europe, the average per vehicle PM parts in 2010 is estimated 18.5 pounds [3].  New design goals set by OEMs (original equipment manufacturers) demands for complex shaped components with high mechanical properties. Stupendous developments are done in the field of PM component manufacturing and PM raw material manufacturing, endeavoring to cater the technical and economic needs set by OEMs. Based on the application, unique powder characteristics are demanded which are in turn associated with the quality of powders produced.  Powder production for conventional PM application encompasses reduction or atomization followed by annealing. Reduced powders are called sponge iron powders, used for low density (density of PM component) application and atomized powders are used for relatively high density application. Atomization can be further classified into water atomization and gas atomization. Coarse, irregular shapes are the common features of water atomized powders and fine, spherical shapes are the common features of gas atomized powders. Water atomization is one of the prominent methods used in production of powders for conventional PM application. Oxygen content of the powders produced by water atomization plays an important role in determining it’s as sintered properties. In this work, oxide formation during various stages of water atomization and annealing were studied for iron, carbon and manganese alloy system and iron, carbon, chromium, molybdenum and manganese alloy system. Manganese content was varied (0.0%, 0.5%, 1.0%) in the above said two alloy system maintaining the same amount of other alloying constituents for comparison. Total oxygen content and oxide composition formed during processing were studied. Both alloy system showed that total oxygen content increases with increasing manganese content. The composition of oxides includes manganese, chromium and iron for Fe+C+Cr+Mo+Mn alloy system and manganese and iron for Fe+C+Mn alloy system. Key words: Powder metallurgy, Water atomization, Gas atomization, Reduced powders,  Oxygen content, Oxide composition, Annealing, Sintered properties, Iron, Chromium, Molybdenum, Manganese.

Due to growing demands for steel powder properties and continuous evolution of the powder metallurgy (PM) production it is necessary to apply new investigation technics and research applications for quality investigation of the PM products. In addition, it is important to be able to predict the probable maximum size of inclusions. The industrial scale sampling of steel was made in Höganäs AB. The three dimensional (3D) analysis of non-metallic inclusions obtained by electrolytic extraction (EE) method was applied for metal samples taken from liquid steel before water-atomization and after powder forging process. It was demonstrated that the application of the 3D analysis has a perspective and possibility to be used independently or like a reference during 2D analysis of inclusions in powder metallurgy products. The tundish samples have the maximum total number of inclusions but have smaller size of complex inclusion. The size range of inclusions in the ladle and tundish samples is between 1 and 46 μm. The main type of inclusions is spherical (Si-Ca-Al-Mg-O in composition). The powder forged samples have two main types of non-metallic particles: “gray” carbon saturated (10-250 μm) and “bright” clustered oxide particles (1-37 μm with Cr-Si-Mn-Mg-Al-O in composition). The probable maximum size of inclusions was estimated based on a new particle size distribution (PSD) and the standard extreme value distribution (EVD) methods. Both methods predicted that in 1 kg of metal the maximum size of spherical inclusions is < 15 μm in liquid steel samples and the maximum length of “bright” clustered oxide particles is < 63 μm in powder forged samples. However, the prediction of the maximum size by PSD method showed necessity of the further optimization.

M. Tech. (Department of Metallurgical Engineering, Faculty of Engineering and Technology), Vaal University of Technology. / Pure Ti, Nb, Zr, Al and V powders were used as starting materials. Ti, Ti-6Al-4V and Ti-34Nb-25Zr materials produced by SPS were compared on the basis of density, microstructure, biocompatibility, tensile strength and corrosion resistance. In this study, powder metallurgy (PM) processing route was used to fabricate the alloys. The processing route was mechanical alloying (MA) and spark plasma sintering (SPS). Commercially pure metallic powders (Ti, Nb, Zr, V and Al) of different morphological features and different formulations were prepared. Powder mixing for ternary alloys with Ti as the matrix were conducted in a turbula mixer at a speed of 49 rpm. Followed by mechanical alloying of Ti, Ti-6Al-4V and Ti-34Nb-25Zr in a high energy ball mill for 5h at 500rpm, with a ball to powder ratio of 10:1. Spark plasma sintering of Ti, Ti-6Al-4V and Ti-34Nb-25Zr biomedical alloys was conducted using a hybrid spark plasma sintering furnace at a sintering temperature, heating rate, holding time and pressure of 1200°C, 100°C/min, 10min and 50MPa, respectively. Ti-34Nb-25Zr was fabricated in two ways, fully densified and porous samples. The fully densified sample was fabricated at a sintering temperature, heating rate and holding time and pressure of 1200°C, 100°C/min, 10min and 50MPa, respectively. Whereas, porous Ti-34Nb-25Zr was fabricated using NaCl space holder at a sintering temperature, heating rate, holding time and pressure of 750°C, 50°C/min, 5min and 50MPa, respectively. This was done to compare the solid and porous alloy biocompatibility behaviour. Microstructures, elemental compositions. Phase constitution of the sintered specimens were examined using a field emission scanning electron microscope (FE-SEM) equipped with energy dispersive x-ray spectrometer (EDS) and an x-ray diffractometer (XRD). The microstructure of Ti-34Nb-25Zr had pores and precipitates of niobium. Relative density, micro-hardness, biocompatibility and corrosion test was also conducted on the metallographically polished cross sections of sintered specimens. Ti, Ti-6Al-4V and Ti-34Nb-25Zr alloys made from the irregularly shaped Ti powders and sintered on the hybrid sintering machine yielded higher densifications reaching up to 100 % relative densities. Hardness values ranging from 300-600Hv at a load of 0.5kg. The corrosion resistance of the alloys was higher in the range of 2-4 nA/cm2 exhibiting a passive behaviour in simulated body fluids, such as Hank’s, 0.9wt.% NaCl and eagles minimum essential + 10% fetal bovine serum (E-MEM+ 10% FBS). Biocompatibility tests were conducted (cytotoxicity by WST-1 with SaOS-2 human osteosarcoma cells, protein adsorption and surface wettability). Fibronectin adsorption was less for solid Ti and Ti-34Nb-25Zr (<2ng/mm) compared to Ti-34Nb-25Zr porous and Ti-6Al-4V (4 ng/mm). Albumin adsorption was the highest on Ti substrate (3 ng/mm) than on the fully densified and porous Ti-34Nb-25Zr surfaces followed by less adsorption on Ti-6Al-4V. Surface wettability of Ti and Ti-6Al-4V showed a high contact angle of between 93-98° compared to 86° for the Ti-34Nb-25Zr solid alloy, indicating that Ti-34Nb-Zr alloys exhibited hydrophilic behaviour. The surface wettability results correlated well to less fibronectin adsorption on Ti-34Nb-25Zr solid alloy and excellent adsorption for Ti-6Al-4V. Solid and porous Ti-34Nb-25Zr showed less cell proliferation (0.06 and 0.02% cell viability) which was possibly linked to fibronectin adsorption results. Biocompatibility behaviour of Ti-34Nb-25Zr solid and porous alloys was poorer than Ti (0.20% cell viability) and Ti-6Al-4V (0.23% cell viability). There was poor protein adsorption and cell proliferation on all the alloy substrates.

Thesis (MScEng) -- Stellenbosch University, 2014. / ENGLISH ABSTRACT: In this study, commercially pure titanium foam was produced using space holder powder metallurgy techniques. Titanium foam is attractive as a scaffolding material for bone replacement and implants in the body. The porous morphology of the foam promotes osteogenesis, while the mechanical behaviour of the foam is closer to that of bone, which has an elastic moduli range of 5 - 40 GPa. Titanium foam was manufactured from powder mixtures of commercially pure titanium (CPTi) powder mixed with 41.4 wt% ammonium bicarbonate (ABC) powder and 1.45 wt% polyethyl glycol (PEG) powder. In this study, two CPTi powders with different particle size distributions, < 75 μm (-200 mesh, designated TiAA) and < 200 μm (-100 mesh, designated TiG), were mixed with the space holder ABC powder, that had been sieved into specified particle size ranges. The size ranges of space holder material studied were: 0 - 710, 250 - 425, 425 - 560, and 560 - 710 μm. This allowed foams with different large or macropore distributions to be produced from the different mixtures. The mixtures were uniaxially compacted at 100 MPa into transverse rupture bars. The ABC and PEG was then removed by thermal debinding in air for 5 hours at 100 °C and 1 hour at 330 °C each, consecutively. The debound samples are then sintered under high (10-6 mbar) vacuum on yttria-stabilised zirconia substrates, heating at 5 °C/min to 1200 °C, with a 2 hour hold at temperature. The microstructures of the different foams were evaluated by examining the polished samples using light optical microscopy. Three point bend tests were conducted on the sintered bars in order to determine the flexural strength and flexural modulus of the different foams. The produced foams had a relative density range between 37.5 - 62.5 % and average macro pore size range between 300 - 500 μm. The foams were found to have an elastic modulus similar to that of bone, 2 - 7 GPa. Finally, the mechanical properties of the foams were compared to known open foam mechanical models and other research projects. It was found that: (i) changes in either metal or space holder powder influences the sintering behaviour of metal foams, (ii) sintered titanium foams with similar densities but different macro/micropore size distributions have different mechanical responses to stress and (iii) the Ashby-Gibson model, based on foam density alone, gives a rough estimate of mechanical properties for the titanium foams studied, but does not capture variations due to pore size distribution. / AFRIKAANSE OPSOMMING: In hierdie studie is kommersiële suiwer titaanskuim geproduseer met behulp van ruimtehouer poeier metallurgie tegnieke. Titaanskuim is aantreklik as 'n raamwerkmateriaal vir beenvervanging en -inplantings in die liggaam. Die poreuse morfologie van die skuim bevorder osteogenese, terwyl die meganiese gedrag van die skuim naby aan dié van been is, met ‘n elasticiteitsmodulus tussen 5 - 40 GPa. Titaanskuim is vervaardig van ‘n poeier mengsel van kommersiële suiwer titaan (CPTi) poeier gemeng met 41,4 gew% ammonium bikarbonaat (ABC) poeier en 1.45 gew% poli-etileenglikol (PEG) poeier. In hierdie studie is twee tipes CPTi poeiers met verskillende deeltjiegrootteverspreiding, < 75 μm (-200 stofdigtheid, TiAA genoem) en <200 μm (-100 stofdigtheid, TiG genoem), met die ruimtehouer ABC-poeier, wat in bepaalde deeltjiegroottereekse gesif is, gemeng. Die wisselende groottes van ruimtehouer wat bestudeer is, was: 0 - 710, 250 - 425, 425 - 560, 560 - 710 μm. Dit het die vervaardiging van skuim met verskillende groot of macroporeuse vanaf die verskillende mengsels toegelaat. Die mengsel is teen 100 MPa in een rigting gekompakteer. Die ABC en PEG is dan verwyder word deur termiese ontbinding in lug vir 5 uur by 100 °C en 1 uur by 330 °C elk, onderskeidelik. Die ontbinde monsters is dan onder hoë (10-6 mbar) leemte op yttrium-gestabiliseer zirconia-substraat, met verwarming teen 5 °C/min tot 1200 °C met 'n verdere 2 uur by 1200 °C, gesinterd. Die mikrostrukture van die verskillende skuim is geëvalueer deur gepoleerde monsters met behulp van ‘n ligmikroskopie te ondersoek . Driepunt draaitoetse is op die gesinterd stawe uitgevoer om die buigsterkte en buigmodulus van die verskillende skuime te bepaal. Die vervaardigde skuime se relatiewe digtheid het tussen 37,5 - 62,5 % gewissel en die gemiddelde makroporiegrootte tussen 300 - 500 μm gewissel. Die skuim het 'n elastisiteitsmodulus soortgelyk aan dié van been getoon, 2 – 7 GPa. Ten slotte is die meganiese eienskappe van die skuim met bekende oop skuim meganiese modelle en ander navorsingsprojekte vergelyk. Daar is bevind dat: (i) veranderinge in óf metaal of ruimtehouer poeier beïnvloed die sinteringgedrag van metaalskuime, (ii) gesinterd titaniumskuim met soortgelyke digthede, maar verskillende makro / mikroporeuse verdelings, toon verskillende meganiese reaksies op stres en die Ashby-Gibson model, gebaseer op die skuimdigtheid alleen, (iii) wat 'n rowwe skatting van die meganiese eienskappe vir die bestudeerde titaniumskuime gee, maar nie die variasies ingrootteverspreiding van porieë ondervang nie.

"The goal of heat treating manufactured steel components is to enhance the characteristics of the metal so that the components meet pre-specified quality assurance criteria. However, the heat treatment process often creates considerable distortion, dimensional change, and residual stresses in the components. These are caused mainly by thermal stresses generated by a non-uniform temperature distribution in the part, and/or by transformation stresses due to the volume mismatch between the parent phase and product phases that may form by phase transformation. With the increasing demand for tighter dimensional tolerances and better mechanical properties from heat treated components, it is important for the manufacturer to be able to predict the ability of a component to be heat treated to a desired hardness and strength without undergoing cracking, distortion, and excessive dimensional change. Several commercial softwares are available to accurately predict the heat treatment response of wrought steel components. However, these softwares cannot be used to predict the heat treatment response of steel components that are made by powder metallurgy (PM) processes since these components generally contain pores which affect the mechanical, thermal, and transformation behavior of the material. Accordingly, the primary objective of this research is to adapt commercially available simulation software, namely DANTE, so that it can accurately predict the response of PM steel components to heat treatment. Additional objectives of the research are to characterize the effect of porosity on (1) the mechanical properties, (2) the heat transfer characteristics, and (3) the kinetics of phase transformation during heat treatment of PM steels."