Дисертації з теми "Powder alloys"

In the present study
the effects of the powder metallurgical parameters such as the mixing method, compaction pressure, initial tungsten (W) particle size, composition, sintering temperature and sintering time on the sintering behavior of selected high density W-Ni-Cu alloys were investigated. The alloys were produced through conventional powder metallurgy route of mixing, cold compaction and sintering. The total solute (Ni-Cu) content in the produced alloys was kept constant at 10 wt%, while the copper concentration of the solutes was varied from 2.5 wt% to 10 wt%. Mainly liquid phase sintering method was applied in the production of the alloys. The results of the study were based on the density measurements, microstructural characterizations including optical and scanning electron microscopy and mechanical characterizations including hardness measurements. The results showed that the nature of the mixing method applied in the preparation of the powder mixtures has a considerable effect on the final sintered state of W-Ni-Cu alloys. Within the experimental limits of the study, the compaction v pressure and initial W particle size did not seem to affect the densification behavior. It was found that the sintering behavior of W-Ni-Cu alloys investigated in this study was essentially dominated by the Ni content in the alloy and the sintering temperature. A high degree of densification was observed in these alloys with an increase in the Ni content and sintering temperature which was suggested to be due to an increase in the solubility and diffusivity of W in the binder matrix phase with an increase in these parameters, leading to an increase in the overall sintering kinetics. Based on the results obtained in the present study, a model explaining the kinetics of the diffusional processes governing the densification and coarsening behavior of W-Ni-Cu alloys was proposed.

Additive manufacturing (AM) shows great promise for the manufacturing of next-generation engineering structures by enabling the production of engineered cellular structures, overhangs, and reducing waste. Melt-pool geometry prediction and control is critical for widespread implementation of laser powder bed processes due to speed and accuracy requirements. The process mapping approach used in previous work for different alloys and additive manufacturing processes is applied to the selective laser powder bed process for IN625 and 17-4 stainless steel alloys. The ability to predict the resulting steady state melt-pool geometry in terms of process parameters, specifically power and velocity, is explored in detail numerically and experimentally verified. A finite element model was created that simulates powder at the macro scale. This model correlates well with current experiments in showing that small amounts of powder relative to melt-pool depth have negligible effects on resulting geometry. Results indicate that the effect of powder may be negligible when comparing steady state widths of the no powder and one layer of powder cases. The work in this thesis investigates the effect of powder on the resulting steady-state melt-pool geometries for IN625 and 17-4 alloys. This analysis has been extended to the production of overhanging and cellular structures. The successful analysis will allow for better predictions and possible correction for cellular structure production issues as well as overhanging features.

In the present study, the effect of hot isostatic pressing (HIPping) variables such as HIPping temperature, HIPping cycle and powder particle size, on the microstructure and mechanical properties of HIPped samples of two Ti alloys have been assessed. Powders of the most commonly used (α + β) alloy, Ti-6Al-4V and one specific beta alloy, Ti-25V-15Cr-2Al-0.2C wt% (burn resistant titanium alloy, BuRTi) were studied. The Ti-6Al-4V powder was made by the plasma rotating electrode process (PREP). BuRTi powders, which were made both by gas atomisation and by PREP were HIPped to investigate the influence of the initial structure of the powder on the microstructure and associated mechanical properties of the HIPped alloy. The PREP Ti-6Al-4V powder was shown to be fully martensitic in the as-atomised condition. The gas-atomised and PREP powders of BuRTi showed very different as-atomised structures, but in both cases the structure was, as expected single phase beta, with the carbon retained insolution. The individual particles of gas-atomised BuRTi powder were always polycrystalline, although there was a significant scatter in grain sizes within different particles. In contrast the individual particles in the PREP powder were either coarse grained polycrystals or single crystals. These differences led to significant differences in the microstructures and properties of HIPped samples. It was found that HIPping of Ti-6Al-4V samples resulted in the formation of equiaxed regions and lath-like microstructure. The small equiaxed regions are formed by recrystallisation which occurs at original particle boundaries where most of the deformation occurs during HIPping; the lath-like microstructure is formed by simply tempering the (less deformed) original alpha prime martensite within the central part of original particles. Among the three HIPping temperatures used, samples machined from powder HIPped at 930°C exhibited a better balance of properties than those HIPped at 880°C or 1020°C. The fatigue properties of samples HIPped at 930°C, made using different HIPping procedures were compared. It was found that samples which contain the as-HIPped surface, which were made using a new HIPping procedure, have better fatigue properties than samples with as-HIPped, machined or electro-polished surfaces which were produced by conventional HIPping . The properties of optimally HIPped Ti-6Al-4V samples are as good as or better than ingot-route samples. In the case of BuRTi the original single crystals or coarse grained polycrystals in the PREP powder are retained after HIPping and limited grain growth occurs in the gas-atomised samples. The tensile strength is comparable for the gas-atomised and PREP samples, but samples tested to failure showed a significant scatter in ductility (a larger scatter in the PREP powder samples) and all fracture surfaces contained large circular fracture initiation sites, with larger sites associated with lower ductility. Initiation occurs in the centre of these circular regions in large grains or in adjacent grains which have similar orientations and the failed region expands symmetrically in powder samples where no texture is expected. The fatigue properties of the PREP samples are much lower whereas the fatigue properties of the gas atomised samples are better than those of samples from ingot route. This behaviour is associated with obvious facetted failure sites in the PREP powder samples where it is suggested that the coarser microstructure has allowed persistent slip to occur leading to localised deformation and to premature failure. These observations are discussed in terms of the potential of net shape HIPping for the production of engineering components and in this context the fact that a new HIPping schedule has been developed during this study, where the fatigue properties of samples containing an as-HIPped surface are excellent, is very significant.

Elemental W and Ni powders were mechanically alloyed in a SPEX mill with WC grinding media for durations ranging from 5 to 50 hours, then compacted samples were sintered in hydrogen to generate bulk tungsten heavy alloys with 2, 4 and 6 wt.% Ni. Evidence of a bimodal grain size distribution was seen in X-ray diffractograms of sintered samples and confirmed by scanning electron microscopy. Grain sizes in the small-grained regions ranged from 200–600 nm; those in the large-grained regions ranged from 1–2 µm. Furthermore, the volume fraction of the small-grained region increased linearly as milling time increased. A slice from a sintered sample was prepared for examination by TEM, in which particles 30–100 nm in diameter were regularly observed on the boundaries of the 200–600 nm grains. EDS point analysis showed that the particles are WC. Therefore it is concluded that heterogeneously distributed contamination from the grinding media is continually incorporated during mechanical alloying and, during sintering, inhibits grain growth through Zener pinning. Densities of sintered samples increased as milling time increased to a maximum of almost 96% of the theoretical value. Density increases with respect to milling time were initially great but diminished upon further milling. While the samples with 4 and 6 wt.% Ni both approached 96% of the theoretical density value by 50 hours of milling, densities in the samples with 2 wt.% Ni were considerably lower. Thus it appears that the Ni that becomes incorporated into the bcc W structure during mechanical alloying activates W diffusion during sintering, though there is a limit to the amount of Ni that the W structure can accommodate. This is evinced in W lattice parameter values from the as-milled powders; while the lattice parameter drops considerable from 2 to 4 wt.% Ni, the difference between 4 and 6 wt.% Ni is much smaller and the Ni content limit surely falls between the two values. Otherwise-equivalent samples with added WC powder were also produced, but did not increase the volume fraction of the small-grained region – probably because the particles remained large and were homogeneously distributed.
Ph. D.

For additive manufacturing, research has shown that the chemistry and microstructural properties of the feedstock powder can significantly affect the properties of the consolidated material. Thermal treatment and recycling parameters for powders used in both solid and liquid state processes can further affect the microstructure and properties of the consolidated parts. Understanding the powder microstructure and effects of powder pre-treatment can aid in optimizing the properties of the final consolidated part. This research proposes a method for the characterization and optimization of powder pre-processing thermal parameters using aluminum alloy powder as examples. Light microscopy, electron microscopy, and hardness were used to evaluate each condition.

A range of titanium-nickel alloys near the equiatomic composition have been processed by cold compaction and vacuum sintering. The effects of compaction pressure, sintering temperature and powder particle size on dimensional changes and densities of sintered compacts are presented. The influence of composition and heat treatment on micro hardness and transformation temperature (M_s) is described. During sintering, anisotropy of dimensional change occurs, with expansion in the radial and contraction in the axial direction of cylindrical compacts. Greater porosity is found in the sintered samples compared to that in the as-pressed condition. It is proposed that these observations are connected with the dissimilar interdiffusion rates of Ti and Ni, the segregation of powder particles in the green compacts and the occurrence of a transient liquid phase during sintering above 955°C. Subsequent hot isostatic pressing of the sintered material allows densification to near full density. The transformation temperatures and hardness of TiNi alloys containing excess amounts of nickel (> 51 at -% Ni) are sensitive to cooling rate after solid state heat treatment, which is in contrast with samples of the exact equiatomic composition. This phenomenon has been related to the decrease in the homogeneity range of TiNi compound with temperature, resulting in either the formation of second phase precipitates in the slow cooled samples or the production of a supersaturated structure in water quenched material. The pressed and sintered specimens display a well defined shape memory behaviour. The extent of shape recovery observed, following deformation and heating through the reverse transformation range, is explained in terms of the volume of pores in the sintered compacts. Ribbons of equiatomic TiNi alloy have been rapidly solidified by the chill block melt spinning technique under an argon atmosphere. The effects of rapid solidification processing and subsequent heat treatments on the transformation behaviour are presented. The crystal structures at room temperature have been analysed by X-ray powder diffraction and thin foil transmission electron microscopy. Some of the ribbons have been chopped and ball milled to produce prealloyed particulate from which compacts have been prepared by cold compaction followed by vacuum sintering. The consolidation response of the prealloyed powder is compared with that of elemental blends. The grain size of the rapidly solidified material is found to beat least an order of magnitude smaller than those observed in wrought specimens. The _s temperature of TiNi alloy is depressed by rapid solidification processing, thus allowing the R-phase to be observed in addition to the high temperature parent phase. This depression has been correlated with the fine grain structure of the spun ribbon. Sintering temperatures in excess of those employed for elemental blends are required for the prealloyed particles. This is related to the dominant effect of the alloy formation energy in elemental powders sample. However, while the volume of porosity increases with sintering temperature in elemental mixture compacts, densification takes place in the case of RS prealloyed specimens. In spite of the need for a higher sintering temperature for RS prealloyed compacts,the resulting grain size is smaller.

Titanium and its alloys have been widely used in oral implantology due to their mechanical properties, corrosion resistance and biocompatibility. However, under in vivo conditions the implants are subjected to the tribocorrosion phenomenon, which consists in the degradation mechanisms due to the combined effect of wear and corrosion. This process contributes to limiting the life span of the implant and may generate clinical problems in patients as metallic ions are released. Another cause of dental implant failure may be the loosening of the implant as metal does not promote osseointegration. The powder-metallurgy process is a promising alternative to the traditional casting fabrication process of titanium alloys for bone implants design, as the porous structure would allow the bone to grow into the pores. This would result in a better fixation of the metal implant without the need of sandblasting /acid etching the surface. The present Doctoral thesis aims at describing the corrosion and tribocorrosion behavior of titanium alloys and their degradation mechanisms when processed by powder metallurgy, as a possible alternative to standard casting for dental implant application. For this, model Ti6Al4V titanium alloy and possible substitute Ti6Al7Nb alloy, where Vanadium has been replaced by Niobium in order to avoid cytotoxicity of the resulting biomaterial, have been studied. Electrochemical and tribo-electrochemical characterization of the biomaterials have been carried out under different physico-chemical conditions with biological relevance (in artificial saliva (AS) with different fluoride content, pH and oxidising conditions) which noticeably influences the degradation mechanisms of the studied materials. A new tribocorrosion technique that allows measuring the galvanic potential and current between the wear track (anode) and the passive material (cathode) through Zero-Resistance Ammetry (ZRA) has been also used to elucidate tribocorrosion mechanisms of the model Ti6Al4V cast alloy in AS. The ZRA technique for tribocorrosion allowed predicting the real depassivated area and therefore, the deviation of the wear mechanisms from Archard wear law at Open Circuit Potential (OCP). All alloys show passivity in artificial saliva although active dissolution occurs in presence of high fluoride concentration (1000 ppm) and acidic conditions, pH 3. The degradation mechanism of sintered alloys is mainly governed by the mechanical wear in AS and only determined by the active dissolution when fluorides are added to acidified artificial saliva (pH 3). Wear was found to be governed by the prevailing oxidizing condition (simulated by changes in the electrode potential). Ti6Al4V alloy processed by powder metallurgy showed a similar tribocorrosion resistance when compared to commercially available cast alloy suggesting that powder metallurgy is a promising fabrication process for implant applications. The influence of the alloying elements, Al and Nb, on the corrosion and tribocorrosion behavior of different titanium alloys, Ti6Al7Nb, Ti7Nb and Ti6Al has been studied and in all cases, the corrosion resistance is improved when compared to pure titanium. Wear damage was found to be critically affected by the ductility of the material, thus by the alloying element. Ti6Al7Nb showed a better corrosion resistance and similar tribocorrosion behaviour when compared to Ti6Al4V. The results of this thesis have shown that Ti6Al7Nb obtained by Powder metallurgy is a promising biomedical alloy for oral implants. Wear damage of sintered Ti alloys depends on the electrochemical potential and their tribocorrosion behaviour is critically affected by a high content of fluoride found in common daily dental health care products.
El titanio y sus aleaciones han sido utilizados en implantología oral debido a sus propiedades mecánicas, resistencia a la corrosión y biocompatibilidad. Sin embargo, bajo condiciones in vivo los implantes están sometidos al fenómeno de tribocorrosión, que consiste en mecanismos de degradación debido al efecto combinado de desgaste y corrosión. Este proceso disminuye la vida útil del implante y genera problemas clínicos a medida que se liberan iones metálicos. La pérdida de fijación del implante es otra causa de fracaso del implante, por falta de osteointegración. El proceso de pulvimetalurgia es una alternativa prometedora al proceso tradicional de fabricación (colada, forja) de aleaciones de titanio para el diseño de implantes óseos, ya que la estructura porosa permitiría que el hueso crezca dentro de los poros, dando lugar a una mejor fijación del implante. La presente tesis doctoral pretende describir el comportamiento frente a la corrosión y tribocorrosión de las aleaciones de titanio y sus mecanismos de degradación cuando se procesan mediante pulvimetalurgia, como una posible alternativa a la colada estándar para la aplicación de implantes dentales. Se ha estudiado el modelo de aleación de titanio Ti6Al4V y posible sustitución por la aleación Ti6Al7Nb, donde el Vanadio ha sido sustituido por Niobio para evitar la citotoxicidad del biomaterial. La caracterización electroquímica y tribo-electroquímica de los biomateriales se ha llevado a cabo en diferentes condiciones físico-químicas con relevancia biológica (en saliva artificial (AS) con fluoruro, pH y condiciones oxidantes) que influye notablemente en los mecanismos de degradación de los materiales estudiados. También se ha utilizado una nueva técnica de tribocorrosión que permite medir el potencial galvánico y la corriente entre la pista de desgaste (ánodo) y el material pasivo (cátodo) a través de la ametría de resistencia cero (Zero-Resistence Ammetry, ZRA) para elucidar los mecanismos de tribocorrosión de la aleación de forja Ti6Al4V en AS. La técnica ZRA para tribocorrosión permitió predecir el área real despasivada y, por tanto, la desviación de los mecanismos de desgaste de la ley de desgaste de Archard en OCP. Las aleaciones muestran pasividad en AS, aunque la disolución activa se produce en presencia de alta concentración de fluoruro (1000 ppm) y condiciones ácidas, pH 3. El mecanismo de degradación de las aleaciones sinterizadas se rige principalmente por el desgaste mecánico en AS y sólo determinado por la disolución activa cuando se añaden fluoruros a la saliva artificial acidificada (pH3). Se encontró que el desgaste se rige por la condición oxidante predominante (simulada por cambios en el potencial de electrodo). La aleación Ti6Al4V procesada por pulvimetalurgia mostró una resistencia similar a la tribocorrosión cuando se comparó con la aleación forjada comercial disponible, lo que sugiere que la pulimetalurgia es un prometedor proceso de fabricación para aplicaciones de implantes. Se ha estudiado la influencia de los elementos aleantes Al y Nb sobre el comportamiento de corrosión y tribocorrosión de diferentes aleaciones de titanio Ti6Al7Nb, Ti7Nb y Ti6Al y en todos los casos la resistencia a la corrosión se mejora en comparación con el titanio puro. El daño de desgaste está afectado críticamente por la ductilidad del material, por lo tanto, por el elemento de aleación. La aleación Ti6Al7Nb mostró una mejor resistencia a la corrosión y un comportamiento similar de tribocorrosión en comparación con la aleación Ti6Al4V. Los resultados de esta tesis han demostrado que el Ti6Al7Nb obtenido por pulvimetalurgia es una prometedora aleación biomédica para implantes orales. El deterioro del desgaste de las aleaciones de Ti sinterizadas depende del potencial electroquímico y su comportamiento a tribocorrosión se ve afectado de manera crítica por un alto contenido de ion flúor
El titani i els seus aliatges s'han utilitzat en l'implantologia oral degut a les seves propietats mecàniques, resistència a la corrosió i biocompatibilitat. No obstant això, en condicions in vivo els implants són sotmesos al fenomen de tribocorrosió, que consisteix en els mecanismes de degradació causats per l'efecte combinat de desgast i corrosió. Aquest procés contribueix a limitar la vida útil de l'implant i pot generar problemes clínics com l'alliberament d'ions metàl¿lics. Una altra causa de fracàs de l'implant dental pot ser la pèrdua de fixació de l'implant, ja que el metall no promou l'osteointegració. El procés de pulvimetal¿lúrgia és una alternativa prometedora al procés tradicional de fabricació (colada i forja) d'aliatges de titani per al disseny d'implants ossis, ja que l'estructura porosa permetria que l'os creixca dins dels porus. Això donaria lloc a una millor fixació de l'implant metàl¿lic. La present tesi doctoral pretén descriure el comportament enfront de la corrosió i tribocorrosió dels aliatges de titani i els seus mecanismes de degradació quan es processen mitjançant pulverimetal¿lúrgia, com una possible alternativa a la fabricació estàndard per forja per a l'aplicació d'implants dentals. Per a això, s'ha estudiat el model d'aliatge de titani Ti6Al4V i possible substitució per l'aliatge Ti6Al7Nb, on el vanadi ha estat substituït per niobi per evitar la citotoxicitat del biomaterial resultant. La caracterització electroquímica i tribo-electroquímica dels biomaterials s'ha dut a terme en diferents condicions fisicoquímiques amb rellevància biològica (en saliva artificial (AS) amb fluorur, pH i condicions oxidants) que influix notablement en els mecanismes de degradació dels materials estudiats. També s'ha utilitzat una nova tècnica de tribocorrosió que permet mesurar el potencial galvànic i el corrent entre la pista de desgast (ànode) i el material passiu (càtode) a través de la ametria de resistència zero (Zero-Resistence Ammetry, ZRA) per elucidar els mecanismes de tribocorrosió de l'aliatge de forja Ti6Al4V en AS. La tècnica ZRA per tribocorrosió va permetre predir l'àrea real despassivada i, per tant, la desviació dels mecanismes de desgast de la llei de desgast de Archard en OCP. Tots els aliatges mostren passivitat en la saliva artificial, tot i que la dissolució activa es produix en presència d'alta concentració de fluorur (1000 ppm) i condicions àcides, pH 3. El mecanisme de degradació dels aliatges sinteritzats es regix principalment pel desgast mecànic en AS i només determinat per la dissolució activa quan s'afegixen fluorurs a la saliva artificial acidificada (pH 3). Es va trobar que el desgast es regix per la condició oxidant predominant (simulada per canvis en el potencial d'elèctrode). L'aliatge Ti6Al4V processada per pulverimetal¿lúrgia va mostrar una resistència similar a la tribocorrosió quan es va comparar amb l'aliatge forjada comercial disponible, el que suggerix que la pulverimetal¿lúrgia és un prometedor procés de fabricació per a aplicacions d'implants. S'ha estudiat la influència dels elements d'aliatge Al i Nb sobre el comportament de corrosió i tribocorrosió de diferents aliatges de titani Ti6Al7Nb, Ti7Nb i Ti6Al i en tots els casos la resistència a la corrosió es millora en comparació amb el titani pur. Es va trobar que el dany de desgast està afectat críticament per la ductilitat del material, per tant, per l'element d'aliatge. L'aliatge Ti6Al7Nb va mostrar una millor resistència a la corrosió i un comportament similar de tribocorrosió en comparació amb l'aliatge Ti6Al4V. Els resultats d'aquesta tesi han demostrat que el Ti6Al7Nb obtingut per pulverimetal¿lúrgia és un prometedor aliatge biomèdic per a implants orals. El deteriorament del desgast dels aliatges de Ti sinteritzats depèn del potencial electroquímic i el seu comportament a tribocorrosió es veu afectat de manera crí
Licausi, M. (2017). Analysis of tribocorrosion behavior of biomedical powder metallurgy titanium alloys [Tesis doctoral no publicada]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/90448
TESIS

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IPEN/T
Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP

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IPEN/T
Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP

This work details an investigation into the production of porous shape memory alloys (SMAs) via hot isostatic press (HIP) from prealloyed powders. HIPing is one of three main methods for producing porous SMAs, the other two are conventional sintering and selfpropagating hightemperature synthesis (SHS). Conventional sintering is characterized by its long processing time at near atmospheric pressure and samples made this way are limited in porosity range. The SHS method consists of preloading a chamber with elemental powders and then initiating an explosion at one end, which then propagates through the material in a very short time. HIPing provides a compromise between the two methods, requiring approximately 5 hours per cycle while operating in a very controlled environment. The HIPing method gives fine control of both temperature and pressure during the run which allows for the production of samples with varying porosity as well as for finetuning of the process for other characteristics. By starting with prealloyed powder, this study seeks to avoid the drawbacks while retaining the benefits of HIPing with elemental powders. In an extension of previous work with elemental powders, this study will apply the HIP method to a compact of prealloyed powders. It is hoped that the use of these powders will limit the formation of alternate phases as well as reducing oxidation formed during preparation. In addition, the nearspherical shape of the powders will encourage an even pore distribution. Processing techniques will be presented as well as a detailed investigation of the thermal and mechanical properties of the resulting material.

In this study, prealloyed austenitic stainless steel and premixed soft magnetic Ni-Fe permalloy compacts were consolidated through microwave and conventional sintering routes at combinations of various sintering temperatures and compaction pressures. Sintered alloys were characterized in terms of their densification, microstructural evolution as well as mechanical and magnetic properties. The effect of sintering method in terms of the applied sintering parameters on the final properties of the compacts were investigated in a comparative manner. It was determined that microwave sintered permalloys are superior compared to their conventionally sintered counterparts in densification response, microstructural characteristics such as pore shape and distribution as well as mechanical properties for both austenitic stainless steel and permalloy compacts. However, permeability of the microwave sintered permalloys was inferior to their conventionally sintered counterparts in some cases due to microstructural refinement associated with microwave sintering route.

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The microstructures of solution treated, quenched and aged A1-2.5 wt. %Li and A1-2.0 wt.%Li-2.76 wt.%Mg-1.03 wt.%Cu alloys were studied by powder X- ray diffraction. The as-quenched alloys showed extensive X-ray line broadening due to particle size effects and the intensity measurements indicated a significant amount ordering in the as-quenched state. These results were interpreted using a 'spinodal ordering' model which suggests that A1-Li-based alloys order during quenching and then spinodally decompose into regions of order and disorder so that the final microstructure comprises small ordered regions (size 40 nm) in a disordered matrix Studies on the aged A1-2.5 wt.%Li alloy indicated that after initial short-time aging, particle growth follows Ostwald ripening kinetics in agreement with previous work. Studies on the aged quaternary alloy indicated that T1 and S phases grow in this system so that precipitates are not a dominant strengthening mechanism in this alloy.

Copper (Cu) has high thermal conductivity and is thus ideal for high heat flux, thermal heat sink applications in fusion power applications. Divertor designs for future fusion power plants will expose Cu alloys to extreme thermal (>10 MW m^-2) and neutron fluxes (200 dpa) that destabilise the microstructure of Cu. To improve stability, strength and creep resistance, alloying additions are used commercially, but these compromise thermal conductivity. Dispersed oxide particles may offer the opportunity for improved mechanical stability and creep resistance even at very low volume fractions (<1%) while avoiding large reductions in thermal conductivity. However there are few studies on the processing-performance of oxide dispersion strengthened Cu alloys. In this thesis, novel oxide dispersion strengthened Cu alloys were prepared by room temperature mechanical alloying of Y₂O₃ and the mechanism of dispersion investigated. A small fraction of Y₂O₃, up to 1%, was shown to disperse effectively during mechanical alloying at room temperature in Cu. Both severe fragmentation and some local disassociation of the Y and O occurred, allowing for re-precipitation of fine nanoparticles <10 nm during consolidation and exposure to elevated temperatures. A model alloy of Cu-2 wt.% Y₂O₃ alloy had a mean oxide particle diameter of 7.1 ± 6.0 nm and a mean particle number density of 8.24 x 10²² m^-3 following consolidation. Ternary Ti additions were investigated for nanoparticle refinement and best design alloy with a composition of Cu-0.25Y₂O₃-0.25Ti was produced that had a mean nanoparticle diameter of 3.2 ± 1.5 nm and a mean particle number density of 2.36 x 10²³ m^-3 , which after thermal ageing for 545 h at 350 °C, was largely unchanged at 3.8 ± 1.7 nm, and 1.74 x 10²³ m^-3 respectively. Comparing favourably with commercial Al₂O₃ dispersion strengthened Cu, the alloy had a narrower particle size distribution and a higher particle number density. The fine dispersed oxide nanoparticles gave good grain boundary pinning, retaining an ultrafine mean grain size of 220 nm after thermal ageing. Thermal conductivity of the Ti-containing alloy was 332 ± 16W m_-1 K_-1 , and the addition of Ti increased the thermal conductivity with increasing temperature. The creep resistance was evaluated by small punch testing and in-house produced alloys outperformed commercial alloys at 350 °C. The work in this thesis indicates that mechanically alloyed Cu-Y₂O₃ or Cu-Y₂O₃-Ti alloys, with further development and evaluation, have potential as thermal heat-sink materials for fusion divertor application.

An experimental framework has been developed that allows investigation of a novel resistance bonding technique incorporating a metal powder interlayer as a means of forming sound joints between dissimilar alloys. Bonds have been produced between Ti- 6AI-4V, Inconel 718 and super CMV steel. Ti-6-4, BurTi and Inconel 718 powder interlayer layers have been trialed. The use of diffusion barrier coatings and transition layers have been explored with particular interest focussed on the effect of tantalum. These trials were then compared to analysis of corresponding bond chemistries produced by a conventional hot isostatic pressing technique. It was found that joints between Ti-6AI-4V and Inconel 718 and super CMV were prone to the formation of intermetallic films at the interface (NiTi, Ti2Ni, Fe2Ti), resulting in poor bond quality. Whilst the use of diffusion barrier layers reduced reaction zone size, tantalum layers in particular were found to severely degrade joint integrity. Bonds produced between Inconel 718 and super CMV performed more encouragingly; achieving around 70% of Inconel 718 parent metal properties in the optimum condition. Comparisons between conventional HIP procedures and resistance bonding elucidated far better powder consolidation in the former. This was shown to be due to a 'differential heating' effect under resistance heating. A quasi isostatic powder interlayer bonding technique (QUIP) has been developed that has shown to substantially improve joint integrity. This is under continuing development.

Four alloys with nominal compositions Al-8Fe-4Ni, Al-8Fe-4Ni-2,5Zr, Al-8Fe-4Ni-2.5Zr-1Mo and Al-8Fe-4Ni-2.5Zr-2V-1Mo (wt%) were produced in the form of wedge shaped ingots by chill casting in a copper mould and in powder form by high pressure gas atomisation using Helium as the atomising gas. Sub-45, sub-50 or +50-100 mum powder size fractions were canned and degassed at 573K. The first two alloys were consolidated by hot extrusion at 573K and ER=18:1 and 25:1. The third alloy could be extruded at 698K and ER=5:1 while the powders of the fourth alloy were hot pressed at 623K because of difficulties with extrusion. The microstructures at the tips of the wedge castings could be related to those of the atomised powder particles. Rapid solidification suppressed the formation of Al3Fe, Al12Mo and A111V in the tips of the wedge castings and m powder particles up to 200 mum diameter, where the microstructures consisted only of a-Al and Al9FeNi, with some week evidence for possible formation of Ll2-Al3Zr in the larger powder particles. Two types of microstructures were observed in the powder particles: Zone A, consisting of mu-Al solid solution or microcellular mu-Al+Al9FeNi eutectic structures or Zone B consisting of mu -Al+Al9FeNi dendritic structures. The transition from Zone A to Zone B microstructres shifted to smaller powder particle sizes (from 20 mum to less than 10 mum) or smaller thickness (< 300mum) of the wedge shaped ingots with increasing solute addition to the first alloy. In all cases the Al9FeNi phase formed under RS conditions had Fe/Ni=2 with solubility for the TM alloying additions. The microstructure of the extruded first alloy exhibited bands of finer and coarser structure without any remaining undeformed powder particles. The banding effect was far less pronounced m the extrusions of the second alloy, where the distribution of the Al9FeNi phase was more homogeneous but there was some evidence of non-fully deformed powder particles (< 5vol%), which were always small (< 10 mum diameter) and hard particles exhibiting the Zone A microstructure of the RS powders. In addition to mu-Al and Al9FeNi, there was a very small volume fraction of Many undeformed particles, which were associated with extended porosity, were also present in the extrusion of the third alloy but bands of finer and coarser structure were not visible. The hot pressed powders of the fourth alloy were at best partially deformed and had retained their RS microstructure with some present in the as pressed microstructure. The microstructures of the consolidated alloys were stable after heat treatment at 673K consisting of mu-Al, Al9FeNi and Ll2-Al3Zr and with the Al9FeNi phase experiencing some coarsening after 1000h, especially in the first alloy, where also the banded structure disappeared after prolonged treatment. The Zone A microstructure was significantly harder than Zone B. The additions of Zr, Mo and V resulted to increases in hardness of 20%, 60% and 110% over the first alloy in the as extruded or hot pressed conditions. After 1000h at 673K the hardness of the first alloy had dropped by 28% and 24% for the 18:1 and 25:1 extruded materials respectively, with the corresponding values for the second alloy being 17% and 11%. The hardnesses of the third and fourth alloys had dropped by about 15%. Higher tensile properties were achieved in the alloys extruded with ER=18:1. The ductilities of all alloys were poor owing to the high volume fractions of Al9FeNi. The mu-Al matrix of the first alloy extruded at ER=18:1 and 25:1 had a fibre texture with crystallographic directions parallel to the axis of the bar. The texture became stronger after heat treatment and consisted of a major fibre. Other minor components such as were also detected. Then- intensity was however fairly small when compared to . On the contrary, although the processing parameters were similar, the texture in the as-extruded bar of the second alloy (ER=18:1 and 25:1) was almost random.

In this study, nanostructured Al-Mg-Si (Al6061) alloy was prepared from elemental powders by mechanical alloying and heat treatment. 98.4% aluminum, 1% magnesium, 0.6% silicon powders were mixed and mechanically alloyed under argon atmosphere. The rotation speed of 500rpm and ball to powder ratio of 10:1 was employed. The mechanical alloyed powder was isothermally heat treated at 400 degrees Celsius for 2 h under argon atmosphere. The results showed that after 10h of milling, a solid solution of Al-Mg-Si with a grain size of ~ 40 nm was produced. The as milled and annealed powder was characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD). The microhardness values of alloy increase by increasing MA time. Mg2Si particles precipitate from solid solution during subsequent annealing. The as milled powder appeared to have good thermal stability against grain growth so that the grain size after annealing remained constant (~ 40 nm). When you are citing the document, use the following link http://essuir.sumdu.edu.ua/handle/123456789/34869

Metal alloy honeycomb structures were fabricated using a paste extrusion technique and characterized for potential application as interconnects in solid oxide fuel cells. Thermal expansion characteristics of Fe-Cr, Fe-Ni, Ni-Cr, Fe-Ni-Cr, and similar alloys containing an oxide dispersion were determined and compared with the thermal expansion behavior of yttria-stabilized zirconia (YSZ). A method was developed to calculate thermal expansion mismatch between two materials under a variety of heating and cooling conditions. It was shown that Fe 20 wt% Cr and Fe 47.5 wt% Ni alloys have low expansion mismatch with YSZ under a wide range of heating and cooling conditions. Oxidation experiments showed that Fe-Cr alloys have superior oxidation resistance in air at 700℃compared with Fe-Ni-Cr alloys with similar chromium contents. The inclusion of oxide dispersions (Y₂O₃ and CaO) into an alloy honeycomb was shown to improve oxidation resistance without affecting thermal expansion behavior. The honeycomb extrusion process provides a method by which experimental alloys can be produced and characterized rapidly to develop an alloy suitable for use as an interconnect in a solid oxide fuel cell.

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This thesis presents research on the cold gas-dynamic spray process applied to the deposition of aluminum-copper alloy coatings. Cold spray deposition is a process utilized to create corrosion protection coatings and to perform additive repair for aluminum structures. This thesis utilized a series of Al-Cu binary alloy powders, from 2–5 weight percent copper and characterized their chemistry and microstructure. The powders were deposited using the cold spray approach to study the systematic increase of the alloying agent on the deposition process and coating characteristics. Deposition efficiency, critical velocity, coating thickness, hardness, porosity, and microstructure were all characterized as functions of carrier gas pressure, carrier gas temperature and feedstock powder copper composition. This thesis has demonstrated that all of the aluminum copper powders utilized can be successfully deposited via the low-pressure cold spray process with helium as the carrier gas. The copper content of the powders has a direct effect on the volume fraction of Al2Cu intermetallics, and on the coating hardness, while having no measurable effect on critical velocity for deposition or the coating thickness per pass.

Titanium been used industrially for nearly a century. Ever since it was first reduced to its elemental form, concerted efforts have been made to improve the material and to reduce the cost of production. In this thesis, titanium is mechanically alloyed with cellulose nanocrystals followed by powder consolidation and sintering to form a solid titanium metal matrix composite. Cellulose nanocrystals (CNCs) were chosen as the particle reinforcement as they are a widely abundant and natural material. Additionally, the nanocrystals can be derived from waste materials such as pistachio shells. This offers a unique advantage to act as a green process to enhance the mechanical properties of the titanium as well as to reduce to cost of production. Vibrational milling using a SPEX 8000M mill was used to mechanically alloy titanium powder with varying concentrations of CNCs. Additionally, the milling time was varied. This process showed that varying the concentrations of CNCs between 0.5% - 2% by weight did not noticeably alter the microstructural or mechanical properties of the materials. Conversely, changing the milling time from 0.5 hours to 5 hours proved to greatly alter the microstructural and mechanical properties of the titanium matrix metal composites. Further increasing the milling time to 10 and 25 hours caused the materials to become exceedingly brittle thus, the majority of experiments focused on samples milled between 0.5 hours and 5 hours. The hardness values for the Ti-1%CNC materials increased from 325-450-600-800 for the samples milled for 0.5, 1, 2, and 5 hours respectively. The other concentrations used were found to yield similar values and trends. SEM micrographs showed that small precipitates had formed within the grains except materials milled at 5 hours, which showed the production of very coarse particles at the grain boundaries. Similarly, an attrition mill was used to mechanically alloy titanium with varying CNC concentrations. Milling time was also varied. The powders were consolidated, sintered and characterized. It was found that increasing CNC content at low milling times caused a reduction in hardness. The X-ray diffractograms also showed a trend in that the diffraction patterns shifted to the lower angle with increasing CNC concentration, thereby suggesting that the increase in CNC content facilitated the removal of oxygen atoms housed within the interstitial sites. The oxygen was observed to diffuse and precipitate platelet titanium dioxide particles. These particles were found to be located within the titanium grains and coarsened with milling time. Generally, increasing the milling time to 15 hours was found precipitate particles at the grain boundaries as well as to excessively dissolve oxygen into the titanium lattice leading to embrittlement. The materials milled for 5 hours showed the best increase in strength while maintaining good ductility.
Master of Science
Titanium has only been used industrially since the early 1940’s thanks in large to the modern advances to reduce titanium ore to its elemental state. Titanium gained much interest as a structural material because of its corrosion resistance and its exceptional strength for a lightweight metal, making the material ideal for medical and aerospace applications. Pure titanium was found to be soft and had poor wear resistance, therefore, efforts were made to create titanium alloys which mitigated these weaknesses. Often titanium is alloyed with costly and toxic elements to enhance its strength properties, making it dangerous to use in the medical field. One way to enhance the strength properties of titanium without the addition of these harmful alloying elements is to create a titanium composite by adding strong inert particles to a titanium matrix. One method to create titanium metal matrix composites is to violently mix titanium powder with the reinforcement material, through a process called mechanically alloying. Following the mixing process the powder is then compacted and heated to form a solid part through a process called sintering. While these powder processing methods are known and viable for forming titanium metal matrix composites, some of the reinforcement materials can be expensive. In this thesis, cellulose nanocrystals (CNCs) will be added as reinforcement to titanium by means of two mechanical alloying processes, vibratory milling (shaking) and attrition milling (stirring). CNCs can be derived from plant matter which is widely abundant and inexpensive. The viability of CNCs to be used as a reinforcement material, as well as the mechanical alloying processes were investigated to determine the effect on the titanium strength properties. The powder processing steps were found to cause the CNCs to react with the surrounding titanium matrix which caused beneficial oxides to form as the reinforcement materials. In general, it was found that vibratory milling caused the final titanium metal matrix composite to be hard and brittle. Attrition milling was found to be more favorable as some materials were observed to be strong yet ductile.

Nanopowders and bulk nanostructred materials have gained large interest in recent years. Bulk nanostructured materials exhibit properties that are far superior in comparison to conventional micron grained alloys. The fabrication of large scale nano-grained materials has been achieved in a two step process: (1) the production of nanostructured aluminium alloy powders and (2) the consolidation of the powder using a electromagnetic shockwave process.
The first part consists of cryo-milling; the milling of powder in an attritor filled with liquid nitrogen. This causes successive welding and fracturing events as the powder is milled, thereby creating the nano-structure. The low temperature prevents the possibility of recrystallization and grain growth. The alloy used for this work was Al 5356 (Al-5%Mg). Two different types of raw source materials were investigated: pre-alloyed powders and a mixture of aluminum with pure magnesium or an Al12Mg17 intermetallic. Experiments have been conducted in order to determine the optimum milling parameters that will simultaneously give a grain size smaller than 100 nm; equiaxed milled particles and mechanically alloyed powder (in the case of the mixture). The optimum milling parameters were established at 15 hours of milling time with a rotational speed of 300 RPM and ball to powder weight ratio of 24:1 in the case of the pre-alloyed powders. For the mixture of pure aluminum with pure magnesium the parameters were 15 hours, 300RPM and 32:1. The parameters for the mixture with the intermetallic were 18 hours, 300RPM and 32:1.
The dynamic magnetic compaction technique was done with a peak pressure of 1.1 GPa. This ultra-high strain rate process minimizes the exposure of the powders to high temperature and therefore reduces the possibility of recrystallization and grain growth. Relative densities of compacted pieces obtained ranged from 86.39% to 97.97%. However consolidation characterized by particle to particle bonding with a melted layer was not accomplished.

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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
Dissertacao (Mestrado)
IPEN/D
Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP
FAPESP:03/10049-5

The effects of mechanical alloying milling time and carbon concentration on microstructural evolution and hardness of high-carbon Fe-C alloys were investigated. Mechanical alloying and powder metallurgy methods were used to prepare the samples. Mixtures of elemental powders of iron and 1.4, 3, and 6.67 wt.% pre-milled graphite were milled in a SPEX mill with tungsten milling media for up to 100h. The milled powders were then cold-compacted and pressure-less sintered between 900°C and 1200°C for 1h and 5h followed by furnace cooling. Milled powders and sintered samples were characterized using X-ray diffraction, differential scanning calorimetry, Mossbauer spectroscopy, scanning and transmission electron microscopes. Density and micro-hardness were measured. The milled powders and sintered samples were studied as follows: In the milled powders, the formation of Fe_3 C was observed through Mossbauer spectroscopy after 5h of milling and its presence increased with milling time and carbon concentration. The particle size of the milled powders decreased and tended to become more equi-axed after 100h of milling. Micro-hardness of the milled powders drastically increased with milling time as well as carbon concentration. A DSC endothermic peak around 600°C was detected in all milled powders, and its transformation temperature decreased with milling time. In the literature, no explanation was found. In this work, this peak was found to be due to the formation of Fe_3 C phase. A DSC exothermic peak around 300°C was observed in powders milled for 5h and longer; its transformation temperature decreased with milling time. This peak was due to the recrystallization and/or recovery α-Fe and growth of Fe_3 C . In the sintered samples, almost 100% of pearlitic structure was observed in sintered samples prepared from powders milled for 0.5h. The amount of the pearlite decreased with milling time, contrary to what was found in the literature. The decrease in pearlite occurred at the same time as an increase in graphite-rich areas. With milling, carbon tended to form graphite instead of Fe_3 C. Longer milling time facilitated the nucleation of graphite during sintering. High mount of graphite-rich areas were observed in sintered samples prepared from powders milled for 40h and 100h. Nanoparticles of Fe_3 C were observed in a ferrite matrix and the graphite-rich areas in samples prepared from powders milled for 40h and 100h. Micro-hardness of the sintered samples decreased with milling time as Fe_3 C decreased. The green density of compacted milled powders decreased with milling time and the carbon concentration that affected the density of sintered samples.
Ph. D.

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Dissertação (Mestrado)
IPEN/D
Instituto de Pesquisas Energéticas e Nucleares - IPEN-CNEN/SP

In the scope of this study, TiNi foams with porosities in the range of 39-64 vol% were processed from prealloyed powders by Mg space holder technique. Porous TiNi alloys displayed homogeneously distributed spherical pores with interconnections, which is suitable for bone ingrowth. Porous Ti-50.8 at%Ni alloys were processed by sintering at 1200 °
C for 2 h to analyze the microstructure as well as mechanical behavior. SEM, TEM and XRD studies were conducted for the characterization of microstructure and phase analyses in addition to the mechanical characterization performed by monotonic and superelasticity compression tests as well as compressive fatigue tests. It was observed that stress required to trigger martensitic transformation was decreased via increasing porosity. The monotonic compression test results also indicated that altering the porosity content of TiNi foams leads to different monotonic compression behaviors. It was observed that the foams display more bulk deformation like behavior as a composite structure composed of TiNi and macropores when the porosity content was low. As the porosity content has increased, the struts became more effective and deformation proceeds by the collapse of favorable struts. On the other hand, cyclic superelasticity tests results indicated that maximum achieved and recovered strain values at the end of fifth cycle increase while the fraction of strain recovered at the end of fifth cycle decreases with decreasing porosity content. Furthermore, the fatigue lives of the processed foams were observed to vary within a band which has a width decreasing with decreasing &sigma
max / &sigma
y yielding an endurance limit ranging in between 26-89 MPa or 0.5-0.6 &sigma
y. Fractography studies on the failed foams after fatigue testing revealed that the failure occurs by the coalescence of micro-cracks initiated from pore walls leading to macro-cracks aligned at 45o with respect to the loading axis. In addition to the mentioned characterization studies, the effects of sintering temperature and time on TiNi foams with 58 vol% porosity as well as heat treatment on the microstructure and the mechanical behavior of TiNi foams with 49 vol% porosity were analyzed with SEM and compression tests. Aging of TiNi foams with 49 vol% porosity at 450 °
C for 1.5 h has shown that the presence of Ti3Ni4 precipitates improve the superelastic response.

In the present study, production of titanium and Ti6Al4V alloy foams has been investigated using powder metallurgical space holder technique in which magnesium powder were utilized to generate porosities in the range 30 to 90 vol. %. Also, sintering of titanium and Ti-6Al-4V alloy powders in loose and compacted condition at various temperatures (850-1250oC) and compaction pressures (120-1125 MPa), respectively, were investigated to elucidate the structure and mechanical properties of the porous cell walls present due to partial sintering of powders in the specimens prepared by space holder technique. In addition, microstructure and mechanical response of the porous alloys were compared with the furnace cooled bulk samples of Ti-6Al-4V-ELI alloy subsequent to betatizing. It has been observed that the magnesium also acts as a deoxidizer during foaming experiments, and its content and removal temperature is critical in determining the sample collapse. Stress-strain curves of the foams exhibited a linear elastic region
a long plateau stage
and a densification stage. Whereas, curves of loose powder sintered samples were similar to that of bulk alloy. Shearing failure in foam samples occurred as series of deformation bands formed in the direction normal to the applied load and cell collapsing occured in discrete bands. Average neck size of samples sintered in loose or compacted condition were found to be different even when they had the same porosity, and the strength was observed to change linearly with the square of neck size ratio. The relation between mechanical properties of the foam and its relative density, which is calculated considering the micro porous cell wall, was observed to obey power law. The proportionality constant and the exponent reflect the structure and properties of cell walls and edges and macro pore character.

Particulate reinforced Al alloy composites (AlMCs) are recognized as important structural materials due to their lightweight, high modulus and strength and high wear resistance. In order to understand the effect of matrix, reinforcement and secondary processing techniques on the microstructure development and mechanical properties of AlMCs produced by powder metallurgy routes, Al alloy composites reinforced with three types of reinforcements by different secondary processing techniques have been produced and examined. Fabrication of Al or 6061Al alloy based composites reinforced with nano-sized SiC particles (~500nm), micro-sized (<25µm) quasicrystalline alloy particles (hereinafter referred to as “NQX”) and micro-sized Nb particles (~130µm) has been carried out by powder metallurgy routes followed by extrusion or cold rolling. After extrusion, a homogeneous distribution of secondary particles has been obtained with rare interfacial reaction products. The 6061Al/SiC composites exhibit superior mechanical properties than either monolithic alloys or composites reinforced with micro-sized particles with retained ductility while the 6061Al/NQX and 6061Al/Nb composites show limited improvement in tensile strength mainly due to their reinforcement size and poor interfacial bonding. After cold rolling, the evolution in microstructure, texture and strength has been analysed. A typical near β fibre texture with highest intensities near Copper and Brass orientations has been developed for 6061Al/NQX and 6061Al/Nb composites. For 6061Al/SiC composites, a randomized texture with very small grains has achieved due to the presence of the non-deformable SiC particles. Mechanical property tests including microhardness, three-point bending tests and tensile tests have been carried out on cold rolled samples and the results exhibit some level of improvement when compared with as-extruded samples due to work hardening. Finally, the work moves on to the general discussion based on the previous result chapters. The microstructural development related to reinforcement, matrix and interfacial areas during extrusion and cold rolling has been summarised and the correlation between microstructure and mechanical properties has been discussed. The thesis provides a thorough understanding of AlMCs produced by powder metallurgy routes in terms of matrix, reinforcement and processing techniques. It can provide reference to the future development of AlMCs for high strength applications.

Vývoj nových materiálů pro součásti v moderních technologiích vystavené extrémním podmínkám má v současné době rostoucí význam. Děje se tak v důsledku neustále se zvyšujících požadavků průmyslových odvětví na lepší konstrukční vlastnosti nosných materiálů. Ve světle těchto faktů si tato studie klade za cíl posoudit nové složení slitin s vysokou entropií, které se vyznačují vysokým aplikačním potenciálem pro kritické aplikace. Slitiny jsou připravovány práškovou metalurgií, t.j. kombinací mechanického legování a slinování v pevné fázi. Pro účely srovnávaní vlastností jsou vybrané kompozice vyrobeny také tradičními metalurgickými metodami v roztaveném stavu, jako je vakuové indukční tavení a následné lití nebo vakuové obloukové tavení. Prášková metalurgie umožňuje postupný vývoj kompozitů s kovovou matricí (MMC) prostřednictvím přípravy oxidicky zpevněných HEA slitin. To je možné díky inherentním in-situ reakcím během procesu výroby. Když se naopak zvolí výrobní postup z taveniny, připravený kovový materiál vykazuje velké rozdíly v mikrostrukturách a souvisejících vlastnostech, v porovnání se stejným materiálem vyrobeným práškovou cestou (PM). Vyrobené práškové a tavené materiály jsou detailně charakterizovány s ohledem na komplexní vyhodnocení vlivu různých metod zpracování. Práce se zejména orientuje na mikrostrukturní charakteristiky materiálů a jejich mechanické vlastnosti, včetně vlivu tepelného zpracování na fázové transformaci a mikrostrukturní stabilitu připravených materiálů.

Manufacturing of aircraft parts is often complex and time-consuming, which has led to an increased interest in new manufacturing technologies in the Swedish industry such as additive manufacturing (AM). Additive manufacturing techniques could be a solution to meet the aircrafts’ demand since it contributes to an efficient manufacturing and allows a just-in-time production of complex metal parts in their final shape. However, the use of AM aluminum for aircraft applications is in a development phase and no surface treatment process exists. Thereby, it is of high interest to further investigate surface treatments for AM alloys. Currently at Saab AB, conventional aluminum alloys are generally anodized in tartaric sulphuric acid (TSA) to improve the corrosion resistance and adhesion properties of the metal. On the behalf of Saab AB, there is also an interest in establishing powder coating as a surface treatment. This master thesis’ purpose is to investigate the anodizing and adhesion properties for the two additive manufacturing alloys - AlSi10Mg and ScalmalloyⓇ, and compare it with the conventionally produced Al alloy 2024-T3. The anodization and the powder coating is examined by using following characterization techniques: profilometry, light microscopy, scanning electron microscopy and contact angle measurements. The results from the experimental part indicated successful anodizations for all the alloys and good adhesion properties for powder coating. This research is a first step in contributing to a better understanding of the anodic coating and adhesion properties for the AM samples ScalmalloyⓇ and AlSi10Mg

Thesis (M. S.)--Materials Science and Engineering, Georgia Institute of Technology, 2009.
Committee Chair: Cochran, Joe; Committee Member: Berczik, Doug; Committee Member: Sanders, Tom; Committee Member: Sandhage, Ken; Committee Member: Thadhani, Naresh.

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Tese (Doutoramento)
IPEN/T
Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP

Al93Fe3Cr2Nb2 (at.%) nanoquasicrystalline alloys have been shown to have the potential to push the applications of aluminium alloys to more elevated temperatures, by maintaining a high strength. They also have more thermally stable microstructures than previous nanoquasicrystalline alloys from similar systems (the most studied of which is Al93Fe3Cr2Ti2 (at.%)). Al93Fe3Cr2Nb2 (at.%) alloys have never previously been produced in samples on a scale larger than melt-spun ribbon. This study examines the production parameters of bulk nanoquasicrystalline Al-Fe-Cr-Nb alloys. Firstly an attempt was made to reduce the melting temperatures of thermally stable nanoquasicrystalline alloys through additional alloying. The melting processes of binary, ternary, quaternary and quinary nanoquasicrystalline alloys was analysed though DTA, with endothermic reactions up to 1034oC observed. Rapidly solidified Al-Fe-Cr-Nb alloys were then produced in kilogram quantities through gas atomisation at an industrial scale. The smallest atomised powder particles contained fine scale microstructures consisting of nano-scale quasicrystals embedded in an aluminium matrix. As the cooling rate of the powder particles decreased new phases, including the theta phase (Al13(Fe,Cr)2-4) and Al3Nb were produced. 0-25μm, 25-50μm and 50-75μm (diameter) size fractions of atomised powder were each consolidated through extrusion to produce nanoquasicrystalline Al-Fe-Cr-Nb bars. Composite bars of the nanoquasicrystalline alloy mixed with 10(vol.)% and 20(vol.)% pure aluminium were also produced. The consolidation of the nanoquasicrystalline atomised powders through extrusion led to precipitation of intermetallics including (Al13(Fe,Cr)2-4) and Al3Nb, particularly in the smallest powder size fractions with the most metastable microstructures. Finally the effects of the atomisation and extrusion conditions on the microstructure and its mechanical properties were studied. Improved strength, coupled with reduced ductility was observed with decreases in the elemental aluminium composition of the Al-Fe-Cr-Nb bars and the powder size fraction they were produced from. There was however improvements in toughness of the extruded composite bars, over the nanoquasicrystalline alloy bars.

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Dissertacao (Mestrado)
IPEN/D
Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

Мaгicтеpcькa диcеpтaцiя: 97 c., 8 pиc., 17 тaбл, 35 пocилaнь, додатків 1. Oб’єкт дocлiдження – теxнoлoгiчний пpoцеc вигoтoвлення пopшнiв iз cплaву A К12М2МгН. Метa poбoти – oптимiзaцiя теxнoлoгiчнoгo пpoцеcу виготовлення пopшнів iз cплaву A К12М2МгН нa бaзi AТ «Пoлтaвcький туpбoмехaнiчний зaвoд». Пpедмет дocлiдження – спосіб введення ультрадисперсних частинок нітридів і карбонітридів в металевий розплав за допомогою механічної суміші фторцирконату калію й нітриду, і сплавленої суміші фторцирконату калію, хлориду марганцю й нітриду титану. Метoди дocлiдження – у poбoтi викopиcтaнo cучacнi метoдики визнaчення влacтивocтей cплaвiв. Pезультaти дocлiджень – оптимізовано теxнoлoгiчний пpoцеc тa зaпpoпoнoвaнo теxнолoгiю oбpoблення poзплaву зa дoпo мoгoю cпocoбу введення ультpa диcпеpcниx чacтинoк нiт pидi в i кapбoнiтpид в в метaлевий poзплaв зa дoпoмoги меxaнічнoї cумiш i фторцирконату кaлiю й нiтpиду, i cплa вленoї cумiшi фтopциpкoнaту кaлiю, xлopиду мapгaнцю й нiтpиду титaну. Вивченo вплив paфiнувaльниx тa мoдифiкувaльниx елементiв на кoмплекc ливapни , меxaнiчних, екcплуaтaцiйниx влacтивocтей тa cтpуктуp у пopшневиx cплaвiв, щo дoзвoлилo oтpимaти без дефектнi виливки. Знaчущіcть poбoти – нa пiдcтaвi pезультaтiв дocлiджень зaпpoпoнoвaнo i впpoвадженo теxнoлoгiчнoлoгiчний пpoцеc oтpимaння пopшнiвi з cплaву A К12М2МгН. Гaлузі зacтocувaння – aвтoмoбiлебудiвнa пpoмиcлoвicть. Пpoгнoзнi пpипущення – зaпpoпoнoвaний теxнoлoгiчний пpoцеc вигoтoвлення пopшнiв i з cплaву A К12М2МгН мoже бути викopиcтaний в умoвax масового виpoбництвa
Master’s thesis: 97 p., 8 fig., 17 tab., 35 references , applications 1. Object of study – the technological process of manufacturing pistons from the AK12M2MgN alloy. The aim of the work – optimize the technological process of production pistons from the AK12M2MgN alloy on the basis of JSC Poltava turbomechanical plant. Subject of study – a method of introducing ultrafine particles of nitrides and carbonitrides into a metallic melt with the help of a mechanical mixture of potassium fluorocysine and nitride, and a fused mixture of potassium fluorocysine, manganese chloride and titanium nitride. Research methods – modern methods of determining the special properties of alloys are used in the work. Research results – optimize the technological process and proposed a technology for melt treatment with the method of introducing ultrafine particles of nitrides and car bonitrides into a metallic melt with the help of a mechanical mixture of potassium fluorocysine and nitride, and a fused mixture of potassium fluorocysine, manganese chloride and titanium nitride. The influence of refining and modifying elements on the complex of foundry, mechanical, operational properties and structure of piston alloys has been studied, which allowed to obtain without defective castings. Urgency of the research – based on the results of the research, the technological process of obtaining pistons from the AK12M2MnN alloy was proposed and introduced. Branch of production – automotive industry. Projected assumptions – the proposed technological process of manufacturing pistons from the AK12M2MgN alloy can be used in massive production.

19 Dec 2004.
Published through the Information Bridge: DOE Scientific and Technical Information. "IS-T 2447" Amber Lynn Genau. 12/19/2004. Report is also available in paper and microfiche from NTIS.

With a view to design processes based on gas-solid reactiontowards the production of fine-grained novel alloys andintermetallics, studies of the reduction of the mixed oxides ofFe and Mo by hydrogen towards the production of Fe-Mo alloyshave been carried out in the present work. The route offersexcellent potentials toward the bulk production of nano-grainedmaterial of tailored-composition in bulk in a green processpath. As a case study, the reduction of the mixed oxides ofiron and molybdenum were carried out from the viewpoint ofmaterials processing, chemical reaction kinetics, as well asmechanical and structural properties. The reduction kinetics ofthin layer of fine oxide particles of Fe2MoO4 was studied usingthermogravimetric technique. This technique allowed determiningreduction parameters such as temperature of reduction as wellas the activation energies for the chemical reaction as therate-controlling step. The end products were analyzed by X-raydiffraction. The reduction product was found to be reduced topure, homogeneous Fe2Mo. In order to examine the upscaling ofthe process, production of the alloy in larger amounts wascarried out in a laboratory-scale fluidized reactor and theprocess parameters were optimized. It was found that, under theconditions of the experiments, the chemical reaction was therate-controlling step. TEM, SEM and X-ray analyses of thereaction product showed the presence of a monolithicintermetallic with micro- and nanocrystalline structure. Themechanical properties of this alloy were determined.Compositions of microcrystalline Fe-Mo alloys were varied byreducing mixtures of Fe2MoO4 with MoO2 or FeO with differentFe/Mo ratios. The products after the reduction consisted of twophases, viz. intermetallic FexMoy compound and metallic Fe orMo. XRD analyses revealed that the former had microcrystallinestructure while the latter were in crystalline form. This workshows that gas-solid reaction method, together with powdermetallurgy technique is a promising process route towards theproduction of novel metallic alloys such as Fe2Mo intermetallicwith micro- and nanocrystalline grains.

Key words: nanoalloys, intermetallics, iron-molybdenumalloy, hydrogen reduction, thermogravimetry, fluidized bed,mechanical properties, structure

Thesis (Master of Sciences)--Case Western Reserve University, 2010
Department of Materials Science and Engineering Title from PDF (viewed on 2010-05-25) Includes abstract Includes bibliographical references and appendices Available online via the OhioLINK ETD Center

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Tese (Doutoramento)
IPEN/T
Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP

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IPEN/T
Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

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IPEN/T
Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

Amorphous and nanostructured Al-based alloys have attracted significant interest owing to their promising properties, including high strength combined with low density. Unfortunately, the production of these advanced materials is limited to powders or ribbons with thickness of less than 100 micrometers due to the reduced glass forming ability of the Al-based alloys. Powder metallurgy through pressure-assisted sintering is a good solution to overcome the size limitation of these materials. In this thesis, Al84Gd6Ni7Co3 glassy powders were consolidated into high-strength bulk materials by hot pressing. The sintering behavior and the microstructural evolution during hot pressing were analyzed as a function of temperature. The results reveal that, through the careful control of the sintering temperature, the combined devitrification and consolidation of the amorphous Al84Gd6Ni7Co3 powders can be achieved, leading to bulk samples with the desired hybrid microstructure and with excellent room temperature mechanical properties. Beside the sintering temperature, the microstructural state of the starting material is critical in order to obtain bulk samples with the desired microstructure and related properties. Consequently, the variation of the initial structural state of the powders as well as of their thermal stability and phase evolution during heating may be used for further tuning the mechanical performance of the hot pressed Al84Gd6Ni7Co3 samples. In order to analyze this aspect, ball milling was used to vary the crystallization behavior of the gas-atomized Al84Gd6Ni7Co3 glassy powder. The influence of milling on microstructure and thermal stability was investigated as a function of the milling time. The results show that the traces of crystalline phases present in the as-atomized powder decrease gradually with increasing the milling time. The thermal stability of the fcc-Al primary phase increases while the thermal stability of the intermetallic phases decreases with increasing milling. Moreover, significant improvement in hardness occurs after milling, which is attributed to the amorphization of the residual crystalline phases present in the as-atomized powder. These finding demonstrate that milling is an effective way to change the initial structural state of the powders and to control the thermal stability of the material. The effect of the microstructural state of the starting material on the mechanical properties of the consolidated samples was investigated in detail. For this, the milled Al84Gd6Ni7Co3 glassy powders were consolidated into bulk specimens by hot pressing. These materials exhibit superior mechanical properties than the samples produced from the as-atomized powder: record high yield strength of 1.7 GPa and fracture strength exceeding 1.8 GPa. This is combined with a plastic strain of about 4 %, Young’s modulus of 120 GPa and density of 3.75 g/cm3. A bimodal microstructure consisting of coarse grained and fine grained regions was achieved in the hot pressed samples by properly controlling the milling process. The exceptionally high strength is attributed to the increased volume fraction of the fine regions, whereas the plastic deformation is favored by the coarse regions, which are able to hinder crack propagation during loading. In addition, the fracture toughness is also improved by the existence of the coarse regions. The tribological properties of the Al84Gd6Ni7Co3 bulk samples were also evaluated. The wear resistance of the bulk samples produced from the milled powder is enhanced with respect to the specimens fabricated from the as-atomized powder, and both alloys exhibit improved wear properties compared to pure aluminum and Al88Si12. Abrasive wear is the main mechanism for these alloys. Finally, the corrosion resistance of these alloys was studied. The results indicate that the Al84Gd6Ni7Co3 bulk material produced from the as-atomized powder has better corrosion resistance than the samples obtained from the milled powder. The main corrosion behavior for these alloys is pit corrosion, intermetallic particle etchout and the corrosion of the Al-rich inter-particle areas. These results clearly demonstrate that, by the proper selection of the sintering temperature and through the appropriate choice of the initial structural state of the powders, the combined devitrification and consolidation of amorphous precursors can be successfully used to produce bulk amorphous/nanostructured Al-based materials with tunable physical and mechanical properties. This expands the known boundaries of Al alloys and offers a new route for the development of novel and innovative high-performance Al-based materials capable to meet specific requirements.