I detta examensarbete har undersökningar kring finfrästa ytor i härdat verktygsstål utförts i samarbete med verktygsstålsproducenten Uddeholms AB i Hagfors. Vid spånskärande bearbetning påverkas materialet ibland negativt. En försöksserie om totalt 90 finfrästa ytor i härdade varmarbetsstålen Uddeholm Orvar Supreme och Uddeholm Dievar har frästs, mätts och utvärderats för att ta reda på hur fräsprocessen inverkar på materialets egenskaper. Det visar sig att materialet påverkas olika mycket beroende på hur fräsningen utförs och med vilken typ av fräsverktyg som används. I detta arbete har endast ändradiefräsar av solid hårdmetall använts. Analysen av ytorna har gjorts med en rad mätmetoder så som optisk ytjämnhetsmätning, hårdhetsmätning med Vickersmetoden, restspänningsmätning med röntgendiffraktion och okulär inspektion av stålets mikrostruktur i ljusmikroskop. Mätningarna utfördes för att se hur materialet påverkas mekaniskt av bearbetningen.   I de mest ogynnsamma försöksfallen är den mekaniska påverkan från fräsbearbetningen av stålets ytor så stor att bearbetningen riskerar försämra tillverkade komponenters livslängd sett ur utmattningssynpunkt. Målet med arbetet är att identifiera det mest gynnsamma sätt fräsningen kan utföras på för att kunna minimera påverkan på materialets egenskaper. Detta ger möjligheten för Uddeholms AB att ge faktabaserade råd till sina kunder om vilket körsätt som ger minsta påverkan av verktygsstålet vid bearbetning. Kunderna kan nyttja då materialet till dess fulla kapacitet. / In this thesis, investigations on hardened finish milled surfaces was done in collaboration with the tool steel manufacturer Uddeholms AB in Hagfors, Sweden. The steel material is affected by machining operations, sometimes in a negative destructive manner. An experimental test series containing a total of 90 surfaces in hot work steels Uddeholm Orvar Supreme and Uddeholm Dievar were milled, measured and evaluated to clarify the milling operations effect on the steels mechanical properties. It was found that the material is affected differently according to how the milling was preformed and with which type of milling tool. In this thesis, only solid carbide end-radius milling tools were used. The surface analysis were conducted with a range of measuring techniques including optical surface roughness measurements, hardness measurements in Vickers scale, residual stress measurements with X-ray diffraction (XRD) and microstructural analysis with optical light microscope. These measurements were conducted in order to determine the milling operations mechanical affects and grade of alteration of the tool steels surfaces. In the least favorable cases, the effect from machining are so profound, that degradation of produced components can be expected in terms of fatigue wear resistance. The goal of the thesis is to identify the most favorable process parameters, in order to minimize degradation of the tooling material in customer user cases, together with the opportunity to give fact based advice to Uddeholms AB customers on the most favorable process parameters in finish milling with radius-mills of hardened hot work tool steels. In this way the customer can utilize the tooling material at its full potential.

Thermoelectric (TE) ZrNiSn samples with a half-Heusler atomic structure were synthesized by mechanical alloying (MA) and consolidation by either Spark Plasma Sintering (SPS) or hot pressing (HP). X-Ray diffraction patterns of as milled powders and consolidated samples were compared and analyzed for phase purity. Thermal conductivity, electrical conductivity and Seebeck coefficient are measured as a function of temperature in the range 300 K to 800 K and compared with measurements reported for high temperature solid state reaction synthesis of this compound. HP samples, compared to SPS samples, demonstrate increased grain growth due to longer heating times. Reduced grain size achieved by MA and SPS causes increased phonon scattering due to the increased number of grain boundaries, which lowers the thermal conductivity without doping the base system with addition phonon scattering centers. Mechanical characterization of the samples by microindentation and depth sensing indentation for hardness and elastic modulus will be discussed.

No presente trabalho quatro ligas Al-Si hipereutéticas, três das quais foram produzidas por conformação por \"spray\" e a outra por fundição, foram caracterizadas quanto a textura, dureza, microestrutura e resistência à corrosão em meio de condensado sintético automotivo (CSA). Duas das ligas conformadas por \"spray\" foram retiradas de camisas de cilindro e a outra de um pré-formado obtido em laboratório. A conformação por \"spray\" envolve a atomização de uma liga e a deposição de gotículas em um substrato, antes mesmo que todas se encontrem no estado sólido. Este processo permite a obtenção de materiais que se caracterizam por uma microestrutura livre de macrossegregações e bastante refinada, implicando melhor trabalhabilidade a quente. A caracterização da microestrutura das quatro ligas hipereutéticas revelou a presença de porosidades na liga obtida em laboratório, e microestrutura com distribuição homogênea de precipitados primários nas três ligas conformadas por \"spray\". A microestrutura de uma das ligas apresentou-se muito diferenciada, com a presença de eutético, sugerindo que esta foi fabricada por fundição. Nas camisas de cilindro foram feitas medidas de rugosidade, e em todas as ligas foram realizados ensaios de microdureza. A liga conformada por \"spray\" e obtida em laboratório foi laminada a quente e a frio. Foram realizados também estudos de textura, para tentar estabelecer uma correlação entre todas as ligas quanto ao processo de fabricação. A avaliação da textura indicou que a presença de fases de silício primário, finamente distribuídas impedem o aparecimento de texturas típicas de deformação de ligas de alumínio, mesmo após severas deformações, como as necessárias para a transformação de pré-formados em tubos que originam as camisas de cilindro. As medidas de rugosidade indicaram características próprias do acabamento superficial usado para a produção das camisas, por brunimento ou por ataque químico. Os ensaios de microdureza apresentaram variações de acordo com as rotas de fabricação sendo que a liga eutética apresentou os maiores valores de microdureza em comparação às ligas conformadas por \"spray\". Todas as ligas foram avaliadas quanto a resistência à corrosão por ensaios de espectroscopia de impedância eletroquímica em dois meios, CSA com pH 3,3 e CSA com pH 11. As quatro ligas hipereutéticas estudadas apresentaram mecanismo de corrosão similar em condensado sintético automotivo (CSA) pH 3,3. Em todas ocorreu o ataque intenso da matriz de alumínio e as partículas de silício primário atuaram como regiões catódicas. A liga 2 apresentou maior resistência à corrosão entre todas as ligas ensaiadas, tanto em CSA pH 3,3 como em pH 11. Neste último meio, uma camada de produtos de corrosão formou-se sobre todas as ligas, e os resultados indicaram mecanismos diferentes para o ataque da matriz de Al e para o crescimento da camada depositada na superfície das ligas estudadas. O ataque da matriz da liga 2 neste meio foi aparentemente mais lento do que sobre as demais ligas, com a formação de uma camada mais compacta de produtos de corrosão, estabelecendo um controle por difusão dos processos interfaciais para maiores períodos de ensaio. A camada formada sobre as demais ligas neste meio apresentou-se mais defeituosa, e nestas ocorreu também menor controle da velocidade das reações interfaciais por processos difusionais. / In the present study four hypereutectic Al-Si alloys, three produced by spray forming and one by casting, were characterized for microhardness, roughness, microstructure, texture and corrosion resistance in a synthetic automotive condensed solution (SACS). Two of the spray formed alloys tested were obtained from cylinder liners and the other was laboratory made. Spray forming involves alloy atomization and droplets deposition on a substrate, previous to the solidification of all of the droplets. This process favours the production of materials with a fine microstructure free of macrosegregation that is related to improved hot workability. The microstructure characterization of the four alloys revealed the presence of porosities in the laboratory made alloy. All the three alloys produced by spray forming showed a homogeneous distribution of primary precipitates. The microstructure of one of the alloys showed eutectic microstructure, indicating that this alloy was fabricated by casting. In the cylinder liners, the surface roughness was measured and the microhardness of all the alloys was also evaluated. Furthermore, the laboratory made alloy was hot and cold rolled. Texture determinations were carried out to investigate the correlation between the alloy type and their fabrication process. The texture investigation indicated that the fine distribution of primary silicon phase in the alloy hindered the development of texture typical of aluminium alloys deformation, even after severe mechanical work, such as those used in the conversion of pre-formed in cylinder liners. The surface roughness results indicated typical characteristics of the surface finishing used, honing or chemical etching. The microhardness results were dependent on the fabrication process used, with higher microhardness associated to the eutectic alloy comparatively to the spray formed ones. All hypereutectic alloys were tested for corrosion resistance using electrochemical impedance spectroscopy in two electrolytes, SACS with pH 3.3 and SACS with pH 11. The four tested alloys showed similar corrosion mechanisms in the acid electrolyte (SACS pH 3.3). The intense attack of the aluminium matrix occurred in ali tested alloys and the primary silicon phase was unattacked and appeared as emerging from the surface after corrosion immersion test. The primary silicon particles acted as cathodic sites. The alloy 2 showed the highest corrosion resistance among the tested alloys in both electrolytes, SACS pH 3.3 and SACS pH 11. In this last medium, a layer of corrosion products formed on all the alloys, and the results indicated different mechanisms for the aluminium matrix corrosive attack and growth of the deposited layer on the alloys surface. The kinetics of aluminium matrix attack was apparently slower in the alloy 2 than for the other alloys, resulting in the formation of a more compact layer of corrosion products, leading to diffusion controlled interfacial processes for longer test periods. The layer of corrosion products on the other three alloys (1, 3, and 4) had more defects and for these alloys diffusional controlled interfacial processes were not as significant as for alloy 2.

Cintiladores inorgânicos com tempo de decaimento de luminescência rápido, densidade alta e boa produção de luz têm sido objeto de estudos para aplicações em física nuclear, física de energias altas, tomografia nuclear e outros campos da ciência e da engenharia. Cristais de cintilação baseados em iodeto de césio (Csl) são materiais que apresentam higroscopia relativamente baixa, número atômico alto, fácil manuseio e custo baixo, características que favorecem o seu uso como detectores de radiação. Neste trabalho descreve-se a obtenção de cristais Csl puro, Csl:Br e Csl:Pb, utilizando-se a técnica de Bridgman. A concentração do elemento dopante bromo (Br) foi estudada no intervalo de 1,5x10-1 M a 10-2 M e o elemento chumbo (Pb) no intervalo de 10-2 M a 5x10-4 M. Para avaliar os cintiladores desenvolvidos foram efetuadas medidas sistemáticas de emissão de luminescência e tempo de decaimento de luminescência para a radiação gama, ensaios de transmitância óptica, ensaios de microdureza Vickers, determinações da distribuição dos dopantes ao longo dos cristais crescidos e análise da resposta dos cristais à radiação gama no intervalo de energia de 350 keV a 1330 keV e partículas alfa provenientes de fonte de 241Am com energia de 5,54 MeV. Os resultados obtidos de tempo de decaimento de luminescência para os cristais CsI:Br e CsI:Pb, no intervalo de 13 ns a 19 ns, mostraram-se promissores para medidas de alta energia. O estudo de microdureza mostrou um aumento significativo em função da concentração dos elementos dopantes, quando comparado ao cristal Csl puro, melhorando desta forma a resistência mecânica dos cristais crescidos. A validade de utilização desses cristais como sensores de radiação para medidas de radiação gama e partículas alfa, pode ser demonstrada pelos resultados da resposta à radiação. / Inorganic scintillators with fast luminescence decay time, high density and high light output have been the object of studies for application in nuclear physics, high energy physics, nuclear tomography and other fields of science and engineering. Scintillation crystals based on cesium iodide (CsI) are matters with relatively low higroscopy, high atomic number, easy handling and low cost, characteristics that favor their use as radiation detectors. In this work, the growth of pure CsI crystals, CsI:Br and CsI:Pb, using the Bridgman technique, is described. The concentration of the bromine doping element (Br) was studied in the range of 1,5x10-1 M to 10-2 M and the lead (Pb) in the range of 10-2 M to 5x10-4 M. To evaluate the scintillators developed, systematic measurements were carried out for luminescence emission and luminescence decay time for gamma radiation, optical transmittance assays, Vickers micro-hardness assays, determination of the doping elements distribution along the grown crystals and analysis of crystals response to the gamma radiation in the energy range of 350 keV to 1330 keV and alpha particles from a 241Am source, with energy of 5.54 MeV. It was obtained 13 ns to 19 ns for luminescence decay time for CsI:Br and CsI:Pb crystals. These results were very promising. The results obtained for micro-hardness showed a significant increase in function of the doping elements concentration, when compared to the pure CsI crystal, increasing consequently the mechanical resistance of the grown crystals. The validity of using these crystals as radiation sensors may be seen from the results of their response to gamma radiation and alpha particles.

This research focused on a comprehensive microstructural and mechanical property characterisation study of the Ni-Fe-Cr alloys 718 and 945X. The aim of the project was to better understand the relationship between performance and microstructure of existing (Alloy 718) and newly developed (Alloy 945X) high strength nickel alloys focusing on downhole applications. The main difference between the two alloys is that alloy 945X has lower Nb content than alloy 718, which may minimise the tendency to form delta when combined with correct processing. Previous studies have related the hydrogen embrittlement in alloy 718 with the collection of hydrogen by delta phase. Microstructural characterisation of the new alloy 945X after long term isothermal exposure up to 120 hours in the temperature range 650◦C to 900◦C was conducted with scanning electron microscopy (SEM), to generate a time-temperature-transformation (TTT) diagram. The TTT diagram was used as a road map for designing two isothermal heat treatments of alloy 945X on tensile specimens. Then, the effect of hydrogen charging on the tensile properties and microstructure of the 'as-received' and these two variant heat treatments was investigated. Fractographic analysis showed that, in the presence of hydrogen, intergranular fracture occurred for all the heat treatments, regardless the presence of delta phase at grain boundaries. There was no simple correlation between the volume fraction of delta-phase and susceptibility to hydrogen assisted embrittlement. Rather, it was demonstrated that the morphology and distribution of delta-phase along grain boundaries plays a key role and the other precipitate phases also have an influence through their effect on the ease of strain localisation. This study also examined the hydrogen embrittlement sensitivity of nickel alloy 718 given four different heat treatments to obtain various microstructural states. Each heat treatment leads to differences in the precipitate morphologies of γ', γ'' and delta phases. Material characterisation and fractography of the examined heat treatments were performed using a high resolution FEG-SEM. Three specimens of each condition were pre- charged with hydrogen and tensile properties were compared with those of non-charged specimens. It was observed that hydrogen embrittlement was associated with intergranular and transgranular microcrack formation, leading to an intergranular brittle fracture. delta phase may assist the intergranular crack propagation, and this was shown to be particularly true when this phase is coarse enough to produce crack initia- tion, but this is not the only factor determining embrittlement. Other microstructural features play a role, as does the strength of the material. Finally, the evolution of delta-(Ni3Nb) phase in alloy 718 from the early stages of precipitation, with a particular focus on identifying the grain boundary characteristics that favour precipitation of grain boundary delta phase was investigated. Results showed that delta phase was firstly formed on Σ3 boundaries after 5 hours at the examined temperature (800◦C). Increasing ageing time at 800◦C was observed to lead to an increase in size and precipitation of phases γ'-γ''-delta, an increase in fraction of the special CSL boundaries and an evolution in the morphology of twins and the growth of grains.

Cintiladores inorgânicos com tempo de decaimento de luminescência rápido, densidade alta e boa produção de luz têm sido objeto de estudos para aplicações em física nuclear, física de energias altas, tomografia nuclear e outros campos da ciência e da engenharia. Cristais de cintilação baseados em iodeto de césio (Csl) são materiais que apresentam higroscopia relativamente baixa, número atômico alto, fácil manuseio e custo baixo, características que favorecem o seu uso como detectores de radiação. Neste trabalho descreve-se a obtenção de cristais Csl puro, Csl:Br e Csl:Pb, utilizando-se a técnica de Bridgman. A concentração do elemento dopante bromo (Br) foi estudada no intervalo de 1,5x10-1 M a 10-2 M e o elemento chumbo (Pb) no intervalo de 10-2 M a 5x10-4 M. Para avaliar os cintiladores desenvolvidos foram efetuadas medidas sistemáticas de emissão de luminescência e tempo de decaimento de luminescência para a radiação gama, ensaios de transmitância óptica, ensaios de microdureza Vickers, determinações da distribuição dos dopantes ao longo dos cristais crescidos e análise da resposta dos cristais à radiação gama no intervalo de energia de 350 keV a 1330 keV e partículas alfa provenientes de fonte de 241Am com energia de 5,54 MeV. Os resultados obtidos de tempo de decaimento de luminescência para os cristais CsI:Br e CsI:Pb, no intervalo de 13 ns a 19 ns, mostraram-se promissores para medidas de alta energia. O estudo de microdureza mostrou um aumento significativo em função da concentração dos elementos dopantes, quando comparado ao cristal Csl puro, melhorando desta forma a resistência mecânica dos cristais crescidos. A validade de utilização desses cristais como sensores de radiação para medidas de radiação gama e partículas alfa, pode ser demonstrada pelos resultados da resposta à radiação. / Inorganic scintillators with fast luminescence decay time, high density and high light output have been the object of studies for application in nuclear physics, high energy physics, nuclear tomography and other fields of science and engineering. Scintillation crystals based on cesium iodide (CsI) are matters with relatively low higroscopy, high atomic number, easy handling and low cost, characteristics that favor their use as radiation detectors. In this work, the growth of pure CsI crystals, CsI:Br and CsI:Pb, using the Bridgman technique, is described. The concentration of the bromine doping element (Br) was studied in the range of 1,5x10-1 M to 10-2 M and the lead (Pb) in the range of 10-2 M to 5x10-4 M. To evaluate the scintillators developed, systematic measurements were carried out for luminescence emission and luminescence decay time for gamma radiation, optical transmittance assays, Vickers micro-hardness assays, determination of the doping elements distribution along the grown crystals and analysis of crystals response to the gamma radiation in the energy range of 350 keV to 1330 keV and alpha particles from a 241Am source, with energy of 5.54 MeV. It was obtained 13 ns to 19 ns for luminescence decay time for CsI:Br and CsI:Pb crystals. These results were very promising. The results obtained for micro-hardness showed a significant increase in function of the doping elements concentration, when compared to the pure CsI crystal, increasing consequently the mechanical resistance of the grown crystals. The validity of using these crystals as radiation sensors may be seen from the results of their response to gamma radiation and alpha particles.

Ce travail de thèse traite de la résistance au rayage des verres silico-sodo-calciques (notés SLS) en fonction de considérations environnementales, de leur composition chimique, de l'histoire du chargement, des contraintes résiduelles et de la géométrie de l'indenteur.<br />Une étude phénoménologique détaillée permet d'identifier les fissures et les régimes d'endommagement mis en œuvre pendant le rayage des verres considérés. L'influence de la composition chimique est discutée à la lumière de considérations structurales et d'observations fractographiques à l'échelle microscopique. La notion de compétition densification/cisaillement dans la déformation de ces verres semble être le paramètre clé pour comprendre leur comportement à l'indentation/rayure.<br />Un modèle mécanique a alors été envisagé pour prédire les endommagements identifiés pendant les essais expérimentaux. L'approche de Ahn* donnant une solution analytique au problème du rayage par un indenteur conique (dérivé de celui de Yoffe° pour une indentation statique) est dans cette étude généralisée. Le développement réside en deux extensions principales: i) l'extension à la géométrie de l'indenteur Vickers grâce à un modèle par éléments finis 3D de l'indentation statique par un Vickers et ii) l'extension aux verres de la famille SLS en étudiant la compétition densification/cisaillement (par des considérations expérimentales couplées à des mesures par AFM) qui contrôle principalement leur comportement à l'indentation.<br />Les résultats du modèle sont corrélés par les résultats phénoménologiques et les observations expérimentales. Le comportement à la rayure des différents verres au regard de leur caractère normal/anormal est également discriminé par le modèle.<br />_______________________<br />* Y Ahn, Deformation about sliding indentation in ceramics and its application to lapping. 1992, Perdue University: (USA).<br />° E.H. Yoffe, Elastic stress field caused by indenting brittle materials, Philosophical Magazine A, 46 (4), (1982), p. 617-628.

Scandia doped zirconia has been considered a candidate for electrolyte material in intermediate temperature Solid Oxide Fuel Cells (SOFCs) due to its high ionic conductivity, chemical stability and good electrochemical performance. The aim of this study is to determine the mechanical properties of SCZ, ie. zirconia (ZrO₂) doped with Scandia (Sc₂O₃) and small amount of ceria (CeO₂) that are important for reliability and durability of the components manufactured from SCZ. The SCZ was prepared from powder by uniaxiall cold pressing at subsequent sintering at 1550 ºC for 4 hours. The density and porosity of the sintered samples was measured following the ASTM Standard C20-00 for alcohol immersion method. A pure cubic phase of SCZ sample was identified by X-ray diffraction (XRD) at room temperature. Quantitative compositional analyses for Zr, Sc, Ce, Hf and Ti were carried out on a Cameca SX50 electron microprobe with wavelength-dispersive spectroscopy (WDS) and energy-dispersive spectroscopy (EDS). Scanning Electron Microscopy (SEM) images were acquired using both secondary electron (SE) and back-scattered electron (BSE) detectors. WDS and EDS analysis also revealed that Zr, Sc, Ce, Hf and Ti are relatively homogeneously distributed in the structure. The average grain size of sintered SCZ samples was measured to be 4 μm. Thermal expansion at different temperatures for the SCZ ceramic was determined using Thermal Mechanical Analyzer, and the instantaneous Coefficient of Thermal Expansion (CTE) was found to be 8.726х10⁻⁶ 1/°C in the in 25-400 °C temperature range. CTE increases monotonically with temperature above 400 ºC to 1.16х10⁻⁵ at 890 °C, most likely as a result of thermo-chemical expansion due to an increase in oxygen vacancy concentration. Room temperature Vickers hardens of 12.5 GPa was measured at loads of 1000 g, while indentation fracture toughness was found to vary from 2.25 to 4.29 MPa m¹⁄², depending on the methodology that was used to calculate fracture toughness from the length of the median corner cracks. Elastic moduli, namely Young and shear moduli were determined using Resonance Ultrasound Spectroscopy (RUS). It was found that elastic moduli decreases with temperature in non-linear manner, with significant drop in the 300-600 °C temperature range, the same temperature range in which loss modulus determined by Dynamic Mechanical Analyzer exhibits frequency dependant peaks. The high loss modulus and significant drop in elastic moduli in that temperature regime is attributed to the relaxation of doping cation-oxygen vacancies clusters. The flexural strength in 4-point bending was measured at room temperature, 400 °C, 600 °C and 800 °C. and the results were analyzed using Weibull statistics. It was found that flexural strength changes with temperature in a sigmoidal way, with the minimum strength at around 600 °C. Non-linear decrease in strength with temperature can be traced back to the changes in elastic moduli that are caused predominately by relaxation of oxygen vacancies.

The Pebble Bed Modular Reactor (PBMR) is one of the most technologically advanced developments in South Africa. In order to build a commercially viable demonstration power plant, all the specifically and uniquely designed equipment must first be qualified. All the prototype equipment is tested at the Helium Test Facility (HTF) at Pelindaba. One of the largest components that are tested is the Core Unloading Device (CUD). The main function of the CUD is to unload fuel from the bottom of the reactor core to enable circulation of the fuel core. The CUD housing vessel forms part of the reactor pressure boundary. Pebble-directing valves and other moving machinery are installed inside its machined inner surface. It is essential that the interior surfaces of the CUD are case hardened to provide a corrosion- and wear-resistant layer. Cold welding between the moving metal parts and the machined surface must also be prevented. Nitriding is a case hardening process that adds a hardened wear- and corrosion-resistant layer that will also prevent cold welding of the moving parts in the helium atmosphere. Only a few nitriding furnaces exist that can house a forging as large as the CUD of the PBMR. Commercial nitriding furnaces in South Africa are all too small and have limited flexibility in terms of the nitriding process. The nitriding of a vessel as large as the CUD has not yet been carried out commercially. The aim of this work was to design and develop a custom-made nitriding plant to perform the nitriding of the first PBMR/HTF CUD. Proper process control is essential to ensure that the required nitrided case has been obtained. A new concept for a gas nitriding plant was developed using the nitrided vessel interior as the nitriding process chamber. Before the commencement of detail design, a laboratory test was performed on a scale model vessel to confirm concept feasibility. The design of the plant included the mechanical design of various components essential to the nitriding process. A special stirring fan with an extended length shaft was designed, taking whirling speed into account. Considerable research was performed on the high temperature use of the various components to ensure the safe operation of the plant at temperatures of up to 600°C. Nitriding requires the use of hazardous gases such as ammonia, oxygen and nitrogen. Hydrogen is produced as a by-product and therefore safety was the most important design parameter. Thermohydraulic analyses, i.e. heat transfer and pressure drop calculations in pipes, were also performed to ensure the successful process design of the nitriding plant. The nitriding plant was subsequently constructed and operated to verify the correct design. A large amount of experimental and operating data was captured during the actual operation of the plant. This data was analysed and the thermohydraulic analyses were verified. Nitrided specimens were subjected to hardness and layer thickness tests. The measured temperature of the protruding fan shaft was within the limits predicted by Finite Element Analysis (FEA) models. Graphs of gas flow rates and other operation data confirmed the inverse proportionality between ammonia supply flow rate and measured dissociation rate. The design and operation of the nitriding plant were successful as a nitride layer thickness of 400 μm and hardness of 1 200 Vickers hardness (VHN) was achieved. This research proves that a large pressure vessel can successfully be nitrided using the vessel interior as a process chamber. / Thesis (M.Ing. (Mechanical Engineering))--North-West University, Potchefstroom Campus, 2010.

The Pebble Bed Modular Reactor (PBMR) is one of the most technologically advanced developments in South Africa. In order to build a commercially viable demonstration power plant, all the specifically and uniquely designed equipment must first be qualified. All the prototype equipment is tested at the Helium Test Facility (HTF) at Pelindaba. One of the largest components that are tested is the Core Unloading Device (CUD). The main function of the CUD is to unload fuel from the bottom of the reactor core to enable circulation of the fuel core. The CUD housing vessel forms part of the reactor pressure boundary. Pebble-directing valves and other moving machinery are installed inside its machined inner surface. It is essential that the interior surfaces of the CUD are case hardened to provide a corrosion- and wear-resistant layer. Cold welding between the moving metal parts and the machined surface must also be prevented. Nitriding is a case hardening process that adds a hardened wear- and corrosion-resistant layer that will also prevent cold welding of the moving parts in the helium atmosphere. Only a few nitriding furnaces exist that can house a forging as large as the CUD of the PBMR. Commercial nitriding furnaces in South Africa are all too small and have limited flexibility in terms of the nitriding process. The nitriding of a vessel as large as the CUD has not yet been carried out commercially. The aim of this work was to design and develop a custom-made nitriding plant to perform the nitriding of the first PBMR/HTF CUD. Proper process control is essential to ensure that the required nitrided case has been obtained. A new concept for a gas nitriding plant was developed using the nitrided vessel interior as the nitriding process chamber. Before the commencement of detail design, a laboratory test was performed on a scale model vessel to confirm concept feasibility. The design of the plant included the mechanical design of various components essential to the nitriding process. A special stirring fan with an extended length shaft was designed, taking whirling speed into account. Considerable research was performed on the high temperature use of the various components to ensure the safe operation of the plant at temperatures of up to 600°C. Nitriding requires the use of hazardous gases such as ammonia, oxygen and nitrogen. Hydrogen is produced as a by-product and therefore safety was the most important design parameter. Thermohydraulic analyses, i.e. heat transfer and pressure drop calculations in pipes, were also performed to ensure the successful process design of the nitriding plant. The nitriding plant was subsequently constructed and operated to verify the correct design. A large amount of experimental and operating data was captured during the actual operation of the plant. This data was analysed and the thermohydraulic analyses were verified. Nitrided specimens were subjected to hardness and layer thickness tests. The measured temperature of the protruding fan shaft was within the limits predicted by Finite Element Analysis (FEA) models. Graphs of gas flow rates and other operation data confirmed the inverse proportionality between ammonia supply flow rate and measured dissociation rate. The design and operation of the nitriding plant were successful as a nitride layer thickness of 400 μm and hardness of 1 200 Vickers hardness (VHN) was achieved. This research proves that a large pressure vessel can successfully be nitrided using the vessel interior as a process chamber. / Thesis (M.Ing. (Mechanical Engineering))--North-West University, Potchefstroom Campus, 2010.