Nanotechnology offers significant opportunities in providing solutions to existing engineering problems as well as breakthroughs in new fields of science and technology. In order to fully realize benefits from such initiatives, nanomanufacturing methods must be developed to integrate enabling constructs into commercial mainstream. Even though significant advances have been made, widespread industrialization in many areas remains limited. Manufacturing methods, therefore, must continually be developed to bridge gaps between nanoscience discovery and commercialization. A promising technology for integration of top-down nanomanufacturing yet to receive full industrialization is equal channel angular pressing, a process transforming metallic materials into nanostructured or ultraine grained materials with significantly improved performance characteristics. To bridge the gap between process potential and actual manufacturing output, a prototype top-down nanomanufacturing system identified as indexing equal channel angular pressing (IX-ECAP) was developed. The unit was designed to capitalize on opportunities of transforming spent or scrap engineering elements into key engineering commodities. A manufacturing system was constructed to impose severe plastic deformation via simple shear in an equal channel angular pressing die on 1100 and 4043 aluminum welding rods. 1/4 fraction factorial split-plot experiments assessed significance of five predictors on the response, microhardness, for the 4043 alloy. Predictor variables included temperature, number of passes, pressing speed, back pressure, and vibration. Main effects were studied employing a resolution III design. Multiple linear regression was used for model development. Initial studies were performed using continuous processing followed by contingency designs involving discrete variable length work pieces. IX-ECAP offered a viable solution in severe plastic deformation processing. Discrete variable length work piece pressing proved very successful. With three passes through the system, 4043 processed material experienced an 88.88% increase in microhardness, 203.4% increase in converted yield strength, and a 98.5% reduction in theoretical final grain size to 103 nanometers using the Hall-Petch relation. The process factor, number of passes, was statistically significant at the 95% confidence level; whereas, temperature was significant at the 90% confidence level. Limitations of system components precluded completion of studies involving continuous pressing. Proposed system redesigns, however, will ensure mainstream commercialization of continuous length work piece processing.

Equal-channel angular pressing (ECAP) is one of the severe plastic deformation (SPD) to produce ultra-fine grain (UFG) material, and its principle and microstructural developments. The majority of papers on SPD materials have been devoted to the face centered cubic (FCC) structure materials such as Al, Cu and Ni. The UFG of high alloy ECAP processing has been difficult up to now, but we were successful in this study. Fe-20%Cr steel with extremely low C and N has different slip behavior from the FCC. The mechanical properties and corrosion resistance were investigated in term microstructural evolution during ECAP processing. / 博士(工学) / Doctor of Philosophy in Engineering / 同志社大学 / Doshisha University

Serious issues including solidification porosity, columnar grains, and large grain sizes are common during fusion-based metal additive manufacturing due to the inherent melting and solidification that occurs during printing. In recent years, a high-temperature, rapid plastic deformation technique called additive friction stir deposition (AFSD) has shown great promise in overcoming these issues. Because the deposited material stays in the solid state during printing, there are no melting and solidification events and the process can result in as-printed material that is fully-dense with equiaxed, fine grains. As AFSD is an emerging process, developing an understanding of the synergy between material deformation and the resultant microstructure evolution, especially the strain magnitude, its influence on dynamic microstructure evolution, and material flow details, is imperative for the full implementation of AFSD. Therefore, the purpose of this work is to investigate the severe plastic deformation in AFSD through complementary studies on the concurrent evolution of shape and microstructure during the deposition of dissimilar aluminum alloys. In this work, we systematically study (1) the entire deposition via dissimilar cladding along with (2) specific volumes within the deposited layer via embedded tracers printed at varied processing parameters. X-ray computed tomography and electron backscatter diffraction are employed to visualize the complex shape of the deposits and understand the microstructure progression. Investigation of dissimilar cladding of homogeneous AA2024 feed-rods onto an AA6061 substrate establishes a working understanding of the mechanisms related to material flow and microstructure evolution across the whole deposit (macroscopic shape evolution) as well as at the interface between the deposit and the substrate. Variations in tooling and rotation rate affect the interfacial features, average grain size, and depth of microstructural influence. The non-planar and asymmetric nature of AFSD on the macro-scale is revealed and a maximum boundary of deposited material is established which gives a frame of reference for the next material flow study within the deposition zone. An understanding of the mesoscopic morphological evolution and concurrent dynamic microstructure evolution of representative volumes within the deposition zone is determined by comparing depositions of hybrid feed-rods (AA6061 matrix containing an embedded tracer of AA2024). Samples were printed with and without an in-plane velocity to compare initial material feeding to steady-state deposition. Variations in initial tracer location and tool rotation rate/in-plane velocity pairs affect the final morphology, intensity of mixing, and microstructure of the deposited tracer material. The tracer material undergoes drastic mesoscopic shape evolution from millimeter-scale cylinders to long, curved micro-ribbons. There is simultaneous grain refinement in AA2024 via geometric dynamic recrystallization during initial material feeding, after which the grain size remains relatively constant at a steady-state size. The lower bound of strain is estimated based on extrusion, torsion, and shear-thinning factors. The step-by-step mesoscopic deformation and microstructure evolution is further elucidated by characterizing depositions of hybrid feed-rods with a series of embedded tracers. The AFSD tooling is stopped quickly at the end of the deposition with a quench applied to "freeze" the sample. X-ray computed tomography reveals multiple intermediate morphologies including the progression from a cylinder to a tight spiral, to a flattened spiral shape, and to a thin disc. EBSD mapping shows that a refined microstructure is formed soon after the material leaves to tool head with areas off the centerline reaching a fully recrystallized state more quickly. The findings from this work summarize the current understanding of the link between material deformation and microstructure evolution in AFSD. Hopefully these first fundamental studies on the co-evolution of material flow and grain structure during AFSD can inspire future work, especially in the area of heterogeneous multi-material printing. / Doctor of Philosophy / Additive friction stir deposition (AFSD) is a new metal 3D printing process that uses friction to heat up and deposit materials rather than using a laser to melt the material into place. This is beneficial since it avoids problems that come from melting and solidification (e.g., porosity, hot cracking, residual stresses, columnar grains). Since AFSD is such a new technology, an understanding of some of the fundamental processing science is needed in order to predict and control the performance of the resultant parts. This is because the processing of a material affects its structure (at multiple scales, for example macro-, micro-, atomic) which then affects the properties a material will exhibit which, finally, dictates the performance of the overall part. Therefore, the purpose of this work is to explore how the feed material is transformed and deposited into the final layer after printing and to link the original processing conditions to the resultant structure. To investigate the interface between the deposited layer and the substrate, we use a simple feed-rod of one aluminum alloy (AA2024) and deposit it onto a substrate of another aluminum alloy (AA6061). To look at just one small volume within the deposited layer, we use a hybrid feed-rod that is mostly AA6061 except for small cylinders of AA2024 that are placed either in the center or on the edge of the feed-rod so that we can track the AA2024. Printing these feed-rods under different processing conditions will help us understand the connection between processing and structure. Using a characterization technique called X-ray computed tomography we can visualize a 3D representation of the final position for the AA2024 material. In order to evaluate the structure on the micro-scale, a characterization technique called electron backscatter diffraction is used to show the individual grains of our metal. The main contributions of this work are as follows: 1) a lower bound of strain is estimated for AFSD, 2) various intermediate deformation steps are captured for the tracer cylinders including a progression from cylinder to multiple spiral shapes to a thin disc to long ribbons, 3) these deformation steps are linked to different microstructures, and 4) changing the tool geometry and other processing parameters significantly alters the range of shapes and microstructures developed in the deposited material. These findings bring us closer to a fully controllable system as well as sparking some interesting areas for future research because of the complex shapes we observed. These results could lead to the customization and optimization of 3D spirals, ribbons, etc. designed for a certain application.

<p>Predstavljena je nova metoda intenzivne plastične deformacije &ndash; višefazno sabijanje V-alatom. Koristeći ovu metodu, sabijanjem u osamnaest faza, unapređene su mehaničke osobine niskougljeničnog čelika Č.1221 &ndash; tvrdoća, čvrstoća i deformabilnost. Za ispitivanje mikrostrukture korišćeni su svetlosni, skening i transmisioni mikroskop. Prosečna veličina kristalnog zrna početnog materijala od 19 mikrometara je smanjena na 250 nanometara nakon dvanaest faza sabijanja. Nakon osamnaest faza sabijanja na čelu uzorka ostvarena je ukupna deformacija u iznosu od 3,38.</p> / <p>A new severe plastic deformation method has been presented - multistage upsetting by V-shape dies. By using this method, in eighteen upsetting stages, mechanical propreties (hardness, strenght and formability) of C15E low carbon steel has been improved. For microstructure analysis light, scanning and transmission microscopes have been employed. Initial average grain size of 19 &mu;m has been reduced to 250 nm after twelve upsetting stages. After eighteen upsetting stages, total effective deformation at the sample forehead of 3,38 has been obtained.</p>

The aim of this thesis work is to design and manufacture a Dissimilar Channel Angular Pressing (DCAP) system for severe plastic deformation of aluminum alloy sheets in order to obtain ultra-fine grained structure. First, a DCAP system was designed by Finite Element Analysis and constructed after various optimization trials. Next, 6061-T0 aluminum alloy plates were severely deformed by various DCAP passes through the system. The samples were characterized by metallography, X-ray diffraction, tension and hardness tests. It has been observed that the yield strength was improved about 100 % after 2 DCAP passes, and 45 nm sub-grain size was obtained.

A study was carried out on the selection of processing condition that would yield Mg-Ti with most favourable hydrogenation properties. Processing routes under consideration were / mechanical milling under inert atmosphere, reactive milling i.e. milling under hydrogen atmosphere, ECAP (equal channel angular pressing) and thermal plasma synthesis. Structure resulting from each of these processing routes was characterized with respect to size reduction, coherently diffracting volume and the distribution of Ti catalyst. Mechanical milling yielded a particulate structure made up of large Mg agglomerates with embedded Ti fragments with a uniform distribution. Mg agglomerates have sizes larger than 100 &micro / m which arises as a result of a balance between cold welding process and ductile fracture. Repeated folding of Mg particles entraps Ti fragments inside the Mg agglomerates resulting in a very uniform distribution. Coherently diffracting volumes measured by X-ray Rietveld analysis have small sizes ca. 26 nm which implies that the agglomerates typically comprise 1011 crystallites. Mechanical milling under hydrogen, i.e. reactive milling, led to drastic reduction in particle size. Mg and Ti convert to MgH2 and TiH2 which are milled efficiently due to their brittleness resulting in particle sizes of sub-micron range. Hydrogenation experiments carried out on Mg-10 vol % Ti milled under argon yields enthalpy and entropy values of -76.74 kJ/mol-H2 and -138.64 J/K.mol-H2 for absorption and 66.54 kJ/mol H2 and 120.12 J/K.mol H2 for desorption, respectively. For 1 bar of hydrogen pressure, this corresponds to a hydrogen release temperature of 280 &deg / C. This value is not far off the lowest desorption temperature reported for powder processed Mg based alloys. ECAP processing is a bulk process where the powders, consolidated in the first pass, have limited contact with atmosphere. This process which can be repeated many times lead to structural evolution similar to that of milling, but for efficient mixing of phases it was necessary to employ multi-pass deformation. An advantage of ECAP deformation is strain hardening of the consolidated powders which has improved milling ability. Based on this, a new route was proposed for the processing of ductile hydrogen storage alloys. This involves several passes of ECAP deformation carried out in open atmosphere and a final milling operation of short duration under inert atmosphere. The plasma processing yields Mg particles of extremely small size. Evaporation of Mg-Ti powder mixture and the subsequent condensation process yield Mg particles which are less than 100 nm. Ti particles, under the current experimental condition used, have irregular size distribution but some could be quite small, i.e. in the order of a few tens of nanometers. Of the four processing routes, it was concluded that both reactive milling and thermal plasma processing are well suited for the production of hydrogen storage alloys. Reactive milling yield particles in submicron range and plasma processing seems to be capable of yielding nanosize Mg particles which, potentially, could be decorated with even smaller Ti particles.

As ligas à base de níquel de alta resistência são utilizadas em uma infinidade de sistemas avançados, onde baixo peso e sistemas de transmissão mecânica de alta densidade de energia são necessários. Componentes, tais como, engrenagens, rolamentos e eixos poderiam ser consideravelmente menor e mais durável se uma grande melhoria em propriedades mecânicas de ligas à base de níquel for alcançada. Um refinamento significativo no tamanho de grão (incluindo nível nano) é um método promissor para a obtenção de melhorias fundamentais nas propriedades mecânicas. O tamanho de grão é conhecido por ter um efeito significativo sobre o comportamento mecânico dos materiais. Um dos métodos mais favoráveis de alcançar refinamento de grão extremo é submetendo os materiais à deformação plástica intensa. As principais variáveis microestruturais nas superligas são a quantidade de precipitados e sua morfologia, o tamanho e a forma do grão e a distribuição de carbonetos (Cr7C3 e Cr23C6) que poderão reduzir propriedades mecânicas da liga. Neste trabalho é apresentada análise por microscopia óptica e eletrônica de transmissão e também os dados de dureza após deformação plástica intensa (tensão de cisalhamento puro) e alguns tratamentos térmicos. / High strength nickel based alloys are used in a multitude of advanced systems where lightweight, high power density mechanical power transmission systems are required. Components such as gears, bearings and shafts could be made significantly smaller and more durable if a major improvement in nickel based alloy mechanical properties could be achieved. A significant refinement in grain size (includes nano level) is thought to be a promising method for achieving fundamental improvements in mechanical properties. Grain size is known to have a significant effect on the mechanical behavior of materials. One of the most favorable methods of achieving extreme grain refinement is by subjecting the materials to severe plastic deformation. The principal microstructural variations in superalloys are the precipitation amount and morphology, grain size and the distribution of carbide precipitation (Cr7C3 and Cr23C6) that could reduce the mechanical properties of the alloys. This work shows optical and transmission electron microscopy analysis and also hardness data after severe plastic deformation (pure shear stress) and some thermal treatments.

As ligas à base de níquel de alta resistência são utilizadas em uma infinidade de sistemas avançados, onde baixo peso e sistemas de transmissão mecânica de alta densidade de energia são necessários. Componentes, tais como, engrenagens, rolamentos e eixos poderiam ser consideravelmente menor e mais durável se uma grande melhoria em propriedades mecânicas de ligas à base de níquel for alcançada. Um refinamento significativo no tamanho de grão (incluindo nível nano) é um método promissor para a obtenção de melhorias fundamentais nas propriedades mecânicas. O tamanho de grão é conhecido por ter um efeito significativo sobre o comportamento mecânico dos materiais. Um dos métodos mais favoráveis de alcançar refinamento de grão extremo é submetendo os materiais à deformação plástica intensa. As principais variáveis microestruturais nas superligas são a quantidade de precipitados e sua morfologia, o tamanho e a forma do grão e a distribuição de carbonetos (Cr7C3 e Cr23C6) que poderão reduzir propriedades mecânicas da liga. Neste trabalho é apresentada análise por microscopia óptica e eletrônica de transmissão e também os dados de dureza após deformação plástica intensa (tensão de cisalhamento puro) e alguns tratamentos térmicos. / High strength nickel based alloys are used in a multitude of advanced systems where lightweight, high power density mechanical power transmission systems are required. Components such as gears, bearings and shafts could be made significantly smaller and more durable if a major improvement in nickel based alloy mechanical properties could be achieved. A significant refinement in grain size (includes nano level) is thought to be a promising method for achieving fundamental improvements in mechanical properties. Grain size is known to have a significant effect on the mechanical behavior of materials. One of the most favorable methods of achieving extreme grain refinement is by subjecting the materials to severe plastic deformation. The principal microstructural variations in superalloys are the precipitation amount and morphology, grain size and the distribution of carbide precipitation (Cr7C3 and Cr23C6) that could reduce the mechanical properties of the alloys. This work shows optical and transmission electron microscopy analysis and also hardness data after severe plastic deformation (pure shear stress) and some thermal treatments.

Da in der Natur die Festigkeit der Stoffe bzw. Werkstoffe mit deren Massendichte korreliert [1], bieten sich dem Werkstoffingenieur zwei Möglichkeiten das genannte Ziel zu erreichen: Entweder er reduziert die effektive Dichte bereits sehr fester Werkstoffe durch konstruktive bzw. geometrische Optimierungen, oder es gelingt sehr leichte Werkstoffe mit deutlich gesteigerter Festigkeit herzustellen. Die erstgenannte Verfahrensweise stellt zu großen Teilen ein konstruktives bzw. fertigungstechnisches Problem dar. Von werkstoffwissenschaftlichem Interesse ist deshalb nur die zweite Möglichkeit. Dabei sollen sämtliche derzeit bekannte festigkeitssteigernde Faktoren und möglicherweise auch deren Synergien genutzt werden um einen hochfesten Leichtbauwerkstoff herzustellen. Dazu muss gleichzeitig ein neuartiges Hochumformverfahren für Leichtmetallverbundwerkstoffe erarbeitet werden, das diesen Anforderungen entspricht und eine dafür geeignete Werkstoffkombination gefunden werden. Konventionelle Verfahren zur Hochumformung erlauben häufig nur unter erheblichem Mehraufwand die Verarbeitung von Verbundwerkstoffen, weshalb die Hochumformung von Leichtmetallverbundwerkstoffen zur Festigkeitssteigerung in der Literatur praktisch keine Rolle spielt. Deshalb soll in dieser Arbeit das Umformverfahren Rundkneten zur Anwendung kommen, das die Hochumformung auch sehr heterogener Werkstoffe erlaubt. Darüber hinaus wird eine zusätzliche positive Wirkung auf die Festigkeit durch eingebaute Grenzflächen auf den Gesamtverbund erwartet. Wie sich im Laufe der Arbeit heraus stellte, eignet sich das verwendete Verfahren nicht ausschließlich zur Festigkeitssteigerung von Verbundwerkstoffen. Durch die sehr regelmäßige und fraktale Anordnung der Komponenten im Gesamtverbund ergaben sich auch einige Anknüpfungspunkte, die weit über die Eignung im Sinne eines Leichtbauwerkstoffes hinaus gehen. Aus diesem Grund liegt der Schwerpunkt der Arbeit zwar auf der mechanischen Charakterisierung der hergestellten Verbunde, in Kapitel 6 werden aber auch weitere Nutzungsmöglichkeiten diskutiert. Die gewählte Materialkombination Titan-Aluminium ist als Beispiel zu verstehen. Prinzipiell ist das vorgestellte Verfahren auf viele weitere Materialkombinationen anwendbar, solange grundlegende umformtechnische Regeln beachtet werden. [1] Ashby, M. F.: Materials Selection in Mechanical Design. Heidelberg: Spektrum Akademischer Verlag, 2006. 648 S.

Submitted by Aelson Maciera (aelsoncm@terra.com.br) on 2017-08-16T19:31:06Z No. of bitstreams: 1 DissDAGP.pdf: 24957220 bytes, checksum: d8c9cd6b22c7e40f1a1f5c7c88deb93a (MD5) / Approved for entry into archive by Ronildo Prado (bco.producao.intelectual@gmail.com) on 2018-01-30T16:50:04Z (GMT) No. of bitstreams: 1 DissDAGP.pdf: 24957220 bytes, checksum: d8c9cd6b22c7e40f1a1f5c7c88deb93a (MD5) / Approved for entry into archive by Ronildo Prado (bco.producao.intelectual@gmail.com) on 2018-01-30T16:50:13Z (GMT) No. of bitstreams: 1 DissDAGP.pdf: 24957220 bytes, checksum: d8c9cd6b22c7e40f1a1f5c7c88deb93a (MD5) / Made available in DSpace on 2018-01-30T16:57:24Z (GMT). No. of bitstreams: 1 DissDAGP.pdf: 24957220 bytes, checksum: d8c9cd6b22c7e40f1a1f5c7c88deb93a (MD5) Previous issue date: 2017-03-03 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES) / Biomedical devices currently in use (prostheses, implants) have satisfactory performance in many cases. However, sometimes the body reacts to the device insertion and may lead to its rapid replacement. Some of these disadvantages can be solved by the use of titanium and its alloys, due to their excellent combination of corrosion resistance, wear resistance and biocompatibility compared to other competing biomaterials. This work presents the possibility of obtaining near β titanium alloy with ultrafine grains produced by severe plastic deformation. For this, the Ti-13Nb-13Zr alloy was processed by high-pressure torsion processing method. Samples were processed with different loads and number of turns. The samples were evaluated by Vickers microhardness. As-received and deformed samples were analyzed through X-Ray diffraction. The microstructures were observed by optical microscopy and scanning electron microscope and the microtexture and phase mappings of the material evaluated through the ASTAR equipment in the transmission electron microscope. After characterization, it was observed that there is a refinement of the microstructure and increase of the microhardness of the Ti-13Nb-13Zr alloy deformed by HPT. Due to the superior microhardness of the deformed material and the results of phase transformations indicate a potential application as nanostructured biomaterial. / Os dispositivos biomédicos utilizados atualmente (próteses, implantes) possuem desempenho satisfatório em muitos casos. No entanto, às vezes, o corpo reage à inserção destes dispositivos exigindo a sua rápida substituição. Algumas destas desvantagens podem ser resolvidas pelo uso de titânio e suas ligas, devido à sua excelente combinação de resistência à corrosão, resistência ao desgaste e biocompatibilidade em comparação com outros biomateriais concorrentes. Este trabalho apresenta a possibilidade de obtenção de liga de titânio quase β com grãos ultrafinos produzidos por deformação plástica severa para três diferentes condições iniciais de microestrutura. Para isso, a liga Ti-13Nb-13Zr foi processada pelo método de processamento de torção sob alta pressão (High-Pressure Torsion - HPT). As amostras foram processadas com diferentes cargas e número de voltas e avaliadas por meio de microdureza Vickers. Amostras como recebidas e deformadas foram analisadas através de difração de raios X. As microestruturas foram observadas por meio de microscopia óptica e eletrônica de varredura. A microtextura e mapeamentos de fase do material foram avaliados através do equipamento ASTAR no microscópio eletrônico de transmissão. Após a caracterização, foi observado que existe um refinamento da microestrutura e aumento da microdureza da liga Ti-13Nb-13Zr deformada por HPT. A microdureza superior do material deformado e os resultados de transformações de fase apontam para uma potencial aplicação como biomaterial nanoestruturado.