Thèses sur le sujet « Accumulative roll bonding »

Multilayered aluminium alloy composites were produced by accumulative roll bonding (ARB) to very high strain to generate sheet materials consisting of either 32 or 64 alternating layers of Al and Al-0.3w.%Sc alloy. Based on the starting heat treatment condition of the Al(Sc) alloy and the roll bonding temperature, several different Al/Al(Sc) combinations were produced: (i) SSSS-ARB (Al(Sc) in the supersaturated condition; Tdef = 200 ???C; 32 layers); (ii) Aged-ARB (Al(Sc) in the artificially aged condition; Tdef = 200 ???C; 32 layers), and (iii) SSSS-ARB-HT (Al(Sc) in the SSSS condition; Tdef = 350 ???C; 64 layers). Regardless of the roll bonding conditions, Al(Sc) in the form of a dispersion of ultrafine Al3Sc particles strongly impedes structural changes during thermomechanical processing whereas Al readily undergoes extensive dynamic and static restoration. The major aim of the thesis is to understand the effect of initial microstructure and processing conditions on microstructural development in these multilayered Al/Al(Sc) composites. The microstructures were investigated mainly by backscatter electron (BSE) and ion channeling contrast (ICC) imaging in the DualBeam Platform and transmission electron microscopy (TEM) whereas the crystallographic nature of the microstructures were investigated by electron backscatter diffraction (EBSD) and the various diffraction techniques available in the TEM. The mechanical properties of the materials were investigated by hardness and tensile testing. The deformation microstructure and texture of these two alloy combinations were strongly influenced by both the initial heat treatment condition of the Al(Sc) alloy whereby large-scale shear bands are generated during rolling when a dispersion of fine Al3Sc particles is present in the Al(Sc) layers. The deformation mechanism of both SSSS-ARB and Aged-ARB was strongly controlled by the relative hardening behaviour of adjacent layers. In Aged-ARB, a higher magnitude of in-plane shear stress, exceeding the flow stress of Al(Sc), was operative at the interfaces between layers; this was shown to cause the shear banding in this material. All materials were annealed for up to 6h at 350 ??C. This extended annealing generated alternating layers of coarse grains (Al layers) and a recovered substructure (Al(Sc) layers) with the substantial waviness of the layers in both Aged-ARB and SSSS-ARB-HT being inherited from the as-deformed material. While the Al(Sc) layers remain unrecrystallized in all materials due to particle pinning effects, the Al layers underwent continuous and discontinuous recrystallization after low and high temperature roll bonding, respectively. Shear banding in Aged-ARB also resulted in a reduction in intensity of the rolling texture components and had a randomizing effect on the recrystallization texture of the Al layers. The Al/A(Sc) multilayered composites were found to conform to the classic inverse strength/ductility relationship and no significant improvement in ductility (for a given strength) was evident. The barriers to achieving an excellent combination of ductility and strength (i.e. toughness) in these materials were identified to be delamination of the layers, which can be largely reduced (or eliminated) by careful control of starting materials (heat treatment condition and thickness) as well as the processing parameters during ARB.

Magnesium alloys are widely used in engineering applications, including aerospace and automobile industries, due to their desirable properties, such as lower density, high damping capacity, relatively high thermal conductivity, good machinability, and recyclability. Researchers have, therefore, been developing new magnesium materials. However, mechanical and corrosion properties are still limiting many commercial applications of magnesium alloys. In this Ph.D. thesis research, I developed Mg-Ti composite materials to offer some solutions to further improve the mechanical behavior of magnesium, such as titanium-magnesium (Ti-Mg) claddings, Mg-Ti multilayers, and Ti particle enforced Mg alloys. Low cost manufacturing processes, such as hot roll-bonding (RB) and accumulative roll-bonding (ARB) techniques, were used to produce Mg-Ti composites and sheets. The microstructural evolution and mechanical properties of composites were investigated using optical microscopy (OM), X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), electron backscatter diffraction (EBSD), nanoindentation, and tensile tests. In the first part of this study, I investigated the bonding strength of the AZ31/Ti to understand the mechanical properties of Mg/Ti composites. Using a single pass RB process, I fabricated AZ31/Ti multilayers with the thickness reduction in a range of 25% to 55%. The hot-rolled AZ31/Ti multilayers were heat-treated at 400 °C for 6, 12, and 24 hours, respectively, in an argon atmosphere. Tensile-shear tests were designed to measure the bonding strength between AZ31/Ti multilayers. Furthermore, the experimental results revealed good bonding of the AZ31/Ti multilayers without forming any intermetallic compounds in the as-rolled and heat-treated AZ31/Ti multilayers. The good bonding between Ti and AZ31 is the result of diffusion bonding whose thickness increases with increasing heat-treatment time and thickness reduction. The shear strength of the Ti/AZ31 multilayer increases with increasing bonding layer thickness. In the second part of this study, I characterized the microstructure and texture of three-layered Ti/AZ31/Ti clad sheets which were produced by single-pass hot rolling with a reduction of thickness 38% (sheet I) and 50% (sheet II). The AZ31 layer in sheets I and II exhibited shear bands and tensile twins {1012}⟨1001⟩ . The shear bands acted as local strain concentration areas which led to failure of the clad sheets with limited elongation. Heat treatment caused changes in the microstructure and mechanical properties of clad sheets due to static recrystallization (SRX) on twins and shear bands in the AZ31 layer. Recrystallized grains usually randomize the texture which causes weaken the strong deformed (0001) basal texture. Twins served as nucleation sites for grain growth during SRX. Tensile tests at room temperature showed significantly improved ductility of the clad sheets after heat treatment at 400°C for 12h. The results showed that the mechanical properties of clad sheets II are better than clad sheet I: The clad sheet II shows elongation 13% and 35% along the rolling direction (RD) for as-rolled and annealed clad sheet, respectively whereas the clad sheet I shows elongation 10% and 22% along RD for as-rolled and annealed clad sheet, respectively. In the final part of this study, I examined the effects of dispersed pure titanium particles (150 mesh) with 0, 2.3, 3.5, 4.9, and 8.6 wt. % on the microstructure and mechanical properties of AZ31-Mg alloy matrix. Mg-Ti composites were processed through three accumulative roll bonding (ARB) steps using thickness reductions of 50% in each pass followed by heat treatment at 400 °C for 12 h in an argon atmosphere. ARB is an efficient process to fabricate Mg-Ti composites. Mechanical properties of Mg- 0Ti and Mg-2.3Ti composite were enhanced by ~ 8% and 13 % in yield strength and ~ 30% and 32 % in ultimate tensile strength, respectively. Meanwhile, the elongation of the composites were decreased by 63% and 70%, respectively. After heat treatment, the results showed a decrease in yield strength and increase in elongation to fracture. The mechanical properties of the Mg-0 and Mg-2.3Ti composite were enhanced: ultimate tensile strength by 9% and 7%, and elongation by 40% and 67%, while the yield strength was decreased by 28% and 36% compared with the initial AZ31. Enhancements of strength and ductility were the results of two mechanisms: a random matrix texture by ARB and ductile titanium particle dispersion.

Ein Verbundwerkstoff aus Titan und Aluminium kann mittels akkumulativem Walzplattieren hergestellt werden. Dabei wird die Dehngrenze angehoben, wenn die Titanlagen nicht abschnüren, sondern laminar bleiben. Die Herstellung eines laminaren Ti/Al-Verbundwerkstoffes ist neu gegenüber den bisherigen Studien. Diese Dissertation beschreibt die Hindernisse und Lösungen, die aus metallphysikalischer Überlegung entstanden und praktisch umgesetzt worden sind. Bei der starken Umformung je ARB-Zyklus neigt das Titan bereits beim zweiten Walzen zur Bildung von Einschnürungen. Das kann durch eine Verringerung der Dickenreduktion je Zyklus sowie durch eine Erhöhung der Verfestigungsrate unterdrückt oder verzögert werden. Walzen mit unterschiedlich großen Ober- und Unterwalzen führt im Vergleich zum symmetrischen Walzen bei gleicher Dickenreduktion zu verstärktem Einschnüren der Titanlagen. Da der Prozess jedoch eine Verringerung der Dickenreduktion erlaubt, ermöglicht er die Zahl der Einschnürungen bei gegenüber dem Quartowalzen gleicher Geschwindigkeit zu verringern. Die spezifische Festigkeit erreicht hierbei einen Wert von auf dem Niveau hochfester Stähle.

O presente trabalho teve como objetivo a caracterização mecânica, microestrutural e inspeção fratográfica do compósito de matriz de alumínio Al-1100 reforçado com partículas de carbeto de silício-SiC (40 μm) fabricados por meio de laminação acumulativa (ARB- do inglês Accumulative Roll Bonding), assim como, para efeito comparativo, foram estudados o Al-1100 processado por ARB sem adição de partículas e Al-1100 como recebido. Ensaio de desgaste microadesivo com esfera fixa e ensaio de tração unidirecional quase estático que foram realizados em amostras sem entalhes e em amostras contendo diferentes geometrias de entalhe. Microscopia óptica, microscopia eletrônica de varredura nos modos: elétrons secundários, elétrons retroespalhados, espectroscopia de energia dispersiva por raios-X e difração de elétrons retroespalhados, difração de raios-X e microtomografia computadorizada foram utilizados para caracterizar as amostras. Os resultados obtidos mostraram êxito da incorporação de partículas de SiC na matriz de Alumínio por meio do processo ARB. Houve ganhos relevantes na resistência máxima à tração, na rigidez e na deformação máxima no momento da ruptura, devido à incorporação de SiCp. Essas propriedades foram bastante influenciadas na presença de concentradores de tensão (entalhes). A resistência ao desgaste do compósito foi excepcionalmente incrementada comparativamente aos demais materiais. Todos os resultados foram corroborados pelas análises microetrutural e fratográficas.
The present study aims to characterize mechanical, microstructural and through fractographic inspection laminates Al-1100 aluminum matrix composite reinforced with silicon carbide particles, SiCp (40 μm), manufactured by accumulative roll bonding (ARB), as well as, for comparative effect, were studied Al-1100 processed by ARB without the addition of particles and Al-1100 received. Micro-adhesive wear test with fixed ball and test almost static unidirectional traction were performed on samples without scoring, and in samples containing different geometries notches. Optical microscopy, scanning electron microscopy modes: secondary electrons, backscattered electrons, energy dispersive X-ray and electron backscatter diffraction, X-ray diffraction and computed microtomography, these were used to characterize the samples. The results indicated successful incorporation of SiC particles in the aluminum matrix by ARB process. There have been significant gains in maximum tensile strength, stiffness and maximum deformation at the time of rupture, due to incorporation of SiCp. These properties were strongly influenced in the presence of stress concentrators (notches). The resistance of the composite wear was exceptionally increased compared to Al-1100 ARB. All results were corroborated by microstructural and fractographics analysis.

Le multi-colaminage est connu pour pouvoir créer des composites ayant une résistance mécanique améliorée et coupler les bonnes propriétés des deux métaux utilisés. L’étude s’est focalisée sur l’élaboration à froid et à chaud de deux composites fonctionnels à base d’aluminium : Al6061/ Al5754 et Al6061/Acier IF. Sur le premier composite, une comparaison a été faite entre le procédé classique et le multi-colaminage croisé, où la direction de laminage est tournée de 90° entre chaque passe. Ce dernier s’est avéré plus apte à hyperdéformer et donc à améliorer la résistance mécanique à température ambiante alors qu’une élaboration à chaud limite cette augmentation par rapport au procédé classique. Au niveau de l’architecture des composites, une réalisation à l’ambiante strictionne puis fractionne la phase dure occasionnant une chute de la résistance mécanique pour le second composite, tandis qu’une réalisation en température conserve la stratification et permet la disparition des interfaces pour le premier composite et l’apparition d’intermétalliques pour le second. Enfin, le composite Al6061/Al5754 s’est montré apte à résister à la fissuration à chaud tandis que le composite Al6061/Acier IF est capable de blinder magnétiquement
The Accumulative Roll Bonding (ARB), consisting in a repetition of roll bonding, is known as a suitable process to work out composite with tailored properties and higher mechanical strength. The present study aimed to develop two functional composites at room and hot temperatures: AA6061/AA5754 and AA6061/IF steel. The first one was developed with both ARB and Cross-ARB (CARB). The Cross-ARB changes the rolling direction by 90° between each pass. As a result, the second process showed higher strength at room temperature. A hotter temperature of process prevented a further enhancement of the strength. According to the temperature of the process, different architectures were obtained. Indeed, ARB at room temperature led to the necking then to the fragmentation of the hard phase and, as a consequence to the collapse of the strength of the composite AA6061/IF steel. The temperature preserved the stratification in the AA6061/AA5754 composite but favored the appearance of intermetallic phase in the AA6061/ IF steel composite. Eventually, the first composite was able to resist to the hot cracking while the second showed magnetic shielding effectiveness

Accumulative roll bonding was adapted to fabricate a carbon nanotube reinforced aluminum matrix composite. The microstructure was investigated by transmission electron microscopy, and it was confirmed that the nanotubes were embedded into the metal matrix while maintaining their multiwalled structure. Measurements revealed that the as-received carbon nanotubes had a bimodal diameter size distribution, while only nanotubes with diameters >30 nm and more than 30 walls were retained during four consecutive rolling operations at 50% reduction. The elastic deflection and vibration damping properties of the laminated composite were investigated by cantilever bending test and by impulse excitation method in samples with different concentrations of carbon nanotubes. Measurements by both methods revealed that a 0.23wt% concentration of nanotubes increased the elastic modulus according to the rule of mixtures and the damping behavior of the composites increased by the addition of nanotubes up to 0.1wt%.
Materials Engineering

碩士
國立東華大學
材料科學與工程學系
102
Magnesium-Lithium alloy is a candidate material for aerospace application. However, this alloy bears the poor corrosion resistance, moreover it cannot be strengthened by the solid solution and precipitation hardening. Therefore, the multilayer composite structures of AA1050 and Mg-9Li-1Zn (LZ91) were produced by using the accumulative roll bonding (ARB) at 473K. The grain refining strengthening and composite strengthening are expected, and the merits of magnesium and aluminum composite are displayed. The results show the grain size of LZ91 alloy could be refined via multi-cycles of ARB process, and mechanical properties of Al/LZ91could be improved consequently. The more number of ARB cycles, the finer of gain size of LZ91. Besides, annealing process was adopted for improving the bonding of interface. According to the EDS results, compound was found in the LZ91/Al interface during annealing at 573K, and interface became brittle. The compound was identified as Al3Mg2 from the XRD spectrum. Also, TEM observation showed that the Al3Mg2 and a little amount of Al12Mg17 compounds were found in the interface.

The improvement in mechanical strength offered by ultra fine- (UF) and nanocrystalline (NC) sized grains is very attractive for potential applications of structural metals. Accumulative Roll-Bonding (ARB) is one of the promising new techniques for producing bulk UF grained metals. There are numerous reports on the monotonic mechanical behavior of various ARBed metals, however there are few, if any, on the cyclic deformation behavior of such metals. The primary objective of this study is to investigate the cyclic deformation behaviour and the related micro-mechanisms of ARBed metals from a fundamental perspective. To achieve this, the microstructure and the deformation behavior of commercial purity aluminum, OFHC copper, and DLP copper after ARB processing have been systematically characterized. The as-ARBed microstructure is found to be composite natured, with constituents of different grain sizes. The three constituents are: (i)UF grained matrix, (ii)NC primary discontinuities, and (iii)conventional sized pre-existing coarse grains. Due to this composite nature, three different cyclic strain accommodation mechanisms were found in the ARBed OFHC copper: (i)conventional dislocation patterns in the large grains, (ii)reactivation of pre-existing shear bands, and (iii)stress/strain driven grain coarsening at sites of strain localization. The order of activation of the mechanisms can be described with a composite approach based on activation energy. The occurrence of grain coarsening is the major contributor to the cyclic softening response observed in OFHC copper. Conversely, the lesser extent of cyclic softening in the other two metals is likely due to the higher microstructure stability of the initial as-ARBed materials. The microstructure stability is believed to be the primary influencing factor for the extent of grain coarsening and cyclic softening. The applied cyclic plastic strain is a secondary influencing factor, although this is generally overshadowed by the limitation of grain coarsening due to the short cyclic lifespan of these metals. The occurrences of shear banding and grain coarsening reported in the present ARBed metals are similarly reported for UF grained metals from other processes, e.g. ECAPed metals. Thus, its relationship to the cyclic deformation response and governing factors are believed to be applicable for UF grained metals in general.

Accumulative Roll Bonding (ARB) was used to fabricate Graphene Oxide-reinforced Al-matrix composites, benefiting from a grain refinement effect of the metal-lic matrix. Graphene Oxide reinforcement was suspended in a stabilized aqueous solution and applied, prior to each ARB cycle, through airgun spraying, in order to obtain a ho-mogeneous distribution. Concentrations of 0.5, 2.5 and 10 mg/ml (graphene ox-ide/millipore water) were used. For each concentration, samples produced have under-gone up to 5 rolling cycles. Optical and electron scanning microscopies were used for microstructural char-acterization of the rolled composites which revealed a non-homogenous deformation of the layers across the composite’s thickness. Although not desired but expected, Alumin-ium oxide formation occurred where the reinforcement was applied. Although the presence of graphene-oxide promoted an increase in the micro-hardness, higher values were obtained with its lowest concentration for the same num-ber of ARB cycles. The number of ARB cycles and the direction of the tested sections also influenced the microhardness results since the 5-cycle samples and the rolling di-rection sections for all the samples achieved higher hardness results. Graphene Oxide revealed to be a major contributor to the increase of stiffness during bending of the test-ed samples. The ARB processed samples revealed a decrease on the electrical conductivity when compared with the annealed Aluminium, since the Graphene Oxide and Alumini-um oxide have insulator properties. The contribution of the reinforcement to this de-crease was only noticeable when using higher concentrations, since the sample with less concentration of the applied Graphene Oxide revealed slightly better results than the sample without any reinforcement.

The main focus of this thesis is the characterization of defects and microstructure in high-energy ball milled magnesium hydride powder and magnesium-based multilayered composites. Enhancement in kinetics of hydrogen cycling in magnesium can be achieved by applying severe plastic deformation. A literature survey reveals that, due to extreme instability of -MgH2 in transmission electron microscope (TEM), the physical parameters that researchers have studied are limited to particle size and grain size. By utilizing a cryogenic TEM sample holder, we extended the stability time of the hydride phase during TEM characterization. Milling for only 30 minutes resulted in a significant enhancement in desorption kinetics. A subsequent annealing cycle under pressurized hydrogen reverted the kinetics to its initial sluggish state. Cryo-TEM analysis of the milled hydride revealed that mechanical milling induces deformation twinning in the hydride microstructure. Milling did not alter the thermodynamics of desorption. Twins can enhance the kinetics by acting as preferential locations for the heterogeneous nucleation of metallic magnesium. We also looked at the phase transformation characteristics of desorption in MgH2. By using energy-filtered TEM, we investigated the morphology of the phases in a partially desorbed state. Our observations prove that desorption phase transformation in MgH2 is of nucleation and growth type, with a substantial energy barrier for nucleation. This is contrary to the generally assumed core-shell structure in most of the simulation models for this system. We also tested the hydrogen storage cycling behavior of bulk centimeter-scale Mg-Ti and Mg-SS multilayer composites synthesized by accumulative roll-bonding. Addition of either phase (Ti or SS) allows the reversible hydrogen sorption at 350C, whereas identically roll-bonded pure magnesium cannot be absorbed. In the composites the first cycle of absorption (also called activation) kinetics improve with increased number of fold and roll (FR) operations. With increasing FR operations the distribution of the Ti phase is progressively refined, and the shape of the absorption curve no longer remains sigmoidal. Up to a point, increasing the loading amount of the second phase also accelerates the kinetics. Microscopy analysis performed on 1-2 wt.% hydrogen absorbed composites demonstrates that MgH2 formed exclusively on various heterogeneous nucleation sites. During activation, MgH2 nucleation occurred at the Mg-hard phase interfaces. On the subsequent absorption cycles, heterogeneous nucleation primarily occurred in the vicinity of internal free surfaces such as cracks.
Materials Engineering

Ein Verbundwerkstoff aus Titan und Aluminium kann mittels akkumulativem Walzplattieren hergestellt werden. Dabei wird die Dehngrenze angehoben, wenn die Titanlagen nicht abschnüren, sondern laminar bleiben. Die Herstellung eines laminaren Ti/Al-Verbundwerkstoffes ist neu gegenüber den bisherigen Studien. Diese Dissertation beschreibt die Hindernisse und Lösungen, die aus metallphysikalischer Überlegung entstanden und praktisch umgesetzt worden sind. Bei der starken Umformung je ARB-Zyklus neigt das Titan bereits beim zweiten Walzen zur Bildung von Einschnürungen. Das kann durch eine Verringerung der Dickenreduktion je Zyklus sowie durch eine Erhöhung der Verfestigungsrate unterdrückt oder verzögert werden. Walzen mit unterschiedlich großen Ober- und Unterwalzen führt im Vergleich zum symmetrischen Walzen bei gleicher Dickenreduktion zu verstärktem Einschnüren der Titanlagen. Da der Prozess jedoch eine Verringerung der Dickenreduktion erlaubt, ermöglicht er die Zahl der Einschnürungen bei gegenüber dem Quartowalzen gleicher Geschwindigkeit zu verringern. Die spezifische Festigkeit erreicht hierbei einen Wert von auf dem Niveau hochfester Stähle.:1. Einleitung - hochfeste, verformbare und leichte Halbzeuge für ressourcenschonende Mobilität 2 2. Zielstellung - hochfeste Leichtmetall-Verbundbleche mit feinlamellaren Strukturen und geringer Korngröße 4 3. Grundlagen 7 3.1. Härtungsmechanismen 7 3.2. Ultrafeinkörnige Werkstoffe und Werkstoffkonzepte für den Leichtbau 10 3.3. Akkumulatives Walzplattieren 15 3.4. Titan/Aluminium-Verbundmaterialien durch ARB 18 3.5. Prinzip und Anwendung von Differential speed rolling 21 4. Methoden 24 4.1. Walzen und Akkumulatives Walzplattieren 24 4.2. DSR - Scherwalzen 27 4.3. Metallographische Probenpräparation 29 4.4. Elektronenmikroskopie, EBSD und Korngrößenbestimmung 32 4.5. Zugversuche 34 4.6. Härtemessungen 36 5. Akkumulatives Walzplattieren 38 5.1. Einfluss von Walzenparametern 38 5.1.1.Walzgut- und Walzenvorheizung 38 5.1.2. Zwischenglühung 45 5.1.3. Walzgeschwindigkeit 60 5.1.4. Mechanische Spannung durch Haspelzug 64 5.1.5. Vergleich von Triowalzen und Quartowalzen 70 5.2. Parametersatz und Vergleich des Verbundes mit EinzelmaterialBlechen 77 5.3. Nachwalzen 80 6. DSR / Walzen mit verschiedenen Geschwindigkeiten der Arbeitswalzen 84 6.1. Ermittlung der Scherung beim Walzen mit verschiedenen Geschwindigkeiten der Arbeitswalzen in Abhängigkeit der vorherigen ARB-Zyklen 84 6.2. Entwicklung des Gefüges in homogenen Metallen und Verbundmetallen 88 7. Abschließende Diskussion und Ausblick 100 8. Zusammenfassung 106 9. Literatur 108

M. Tech. (Mechanical Engineering, Faculty of Engineering and Technology): Vaal University of Technology
Presently there exist a lot of controversies about the mechanical properties of nanomaterials. Several convincing reasons and justifications have been put forward for the controversies. Some of the reasons are varying processing routes, varying ways of defining equations, varying grain sizes, varying internal constituent structures, varying techniques of imposing strain on the specimen etc. It is therefore necessary for scientists, engineers and technologists to come up with a clearer way of defining and dealing with nanomaterials’ mechanical properties. The parameters of the internal constituent structures of nanomaterials are random in nature with random spatial patterns. So they can best be studied using random processes, specifically as stochastic processes. In this dissertation the tools of stochastic processes have been used as they offer a better approach to understand and analyse random processes. This research adopts the approach of ascertaining the correct mathematical models to be used for experimentation and modelling. After a thorough literature survey it was observed that size and temperature are two important parameters that must be considered in selecting the relevant mathematical definitions for nanomaterials’ mechanical properties. Temperature has a vital role to play during grain refinement since all severe plastic deformation involves thermomechanical processes. The second task performed in this research is to develop the mathematical formulations based on the experimental observation of 2-D grains and 3-D grains deformed by Accumulative Roll-Bonding and Equal Channel Angular Pressing. The experimental observations revealed that grains deformed by Accumulative Roll-Bonding and Equal Channel Angular Pressing are elongated when observed from the rolling direction, and transverse direction, and equiaxed when observed from the normal direction. In this dissertation, the different experimental observations for the grain size variants during grain refinement were established for 2-D and 3-D grains. This led to the development of a stochastic model of grain-elongation for 2-D and 3-D grains. The third task was experimentations and validation of proposed models. Accumulative Roll-Bonding, Equal Channel Angular Pressing and mechanical testing (tensile test) experiments were performed. The effect of size on elongation and material properties were studied to validate the developed models since size has a major effect on material’s properties. The fourth task was obtaining results and discussion of theoretical developed models and experimental results. The following facts were experimentally observed and also revealed by the models. Different approaches of measuring grain size reveal different strains that cannot be directly obtained from plots of the corresponding grain sizes. Grain elongation evolved as small values for larger grains, but became larger for smaller grains. Material properties increased with elongation reaching a maximum and started decreasing as is evident in the Hall-Petch to the Reverse Hall-Petch Relationship. This was alluded to the fact that extreme plastic straining led to distorted structures where grain boundaries and curvatures were in “non-equilibrium” states. Overall, this dissertation contributed new knowledge to the body of knowledge of nanomaterials’ mechanical properties in a number of ways. The major contributions to the body of knowledge by his study can be summarized as follows: (1) The study has contributed in developing a model of elongation for 2-D grain and 3-D grains. It has been generally reported by researchers that materials deformed by Accumulative Roll-Bonding and Equal Channel Angular Pressing are generally elongated but none of these researchers have developed a model of elongation. Elongation revealed more information about “size” during grain refinement. (2) The Transmission Electron Microscopy revealed the grain shape in three directions. The rolling direction or sliding direction, the normal direction and the transverse direction. Most developed models ignored the different approaches of measuring nanomaterials’ mechanical properties. Most existing models dealt only with the equivalent radius measurement during grain refinement. In this dissertation, the different approaches of measuring nanomaterials’ mechanical properties have been considered in the developed models. From this dissertation an accurate correlation can be made from microscopy results and theoretical results. (3) This research has shown that most of the published results on nanomaterials’ mechanical properties may be correct although controversies exist when comparing the different results. This research has also shown that researchers might have considered different approaches to measure nanomaterials’ mechanical properties. The reason for different results is due to different approaches of measuring nanomaterials’ mechanical properties as revealed in this research. Since different approaches of measuring nanomaterials’ mechanical properties led to different obtained results, this justify that most published results of nanomaterials’ mechanical properties may be correct. This dissertation revealed more properties of nanomaterials that are ignored by the models that considered only the equivalent length. (4) This research has contributed to the understanding of nanomaterials controversies when comparing results from different researchers.

博士
國立中山大學
材料科學研究所
92
The amorphous alloys have attracted great attention due to their characteristics and future potential. This research is intended to synthesis new amorphous alloy with high glass forming ability as well as low density. The addition of lighter-weight elements such as Al, Ti, Zr, Ni and Cu are tried. The selected vitrification methods in this study are solid-state accumulated roll bonding (ARB) and arc-melting of multi-element alloys. Although the procedures of solid-state reaction are more complicated than that of casting, the influence of cooling rate on amorphization process is not important. Various Zr based binary, ternary, and pentanary alloys are synthesized by the ARB method. Besides, two pentanary alloys are also developed by arc melting method for the properties comparison with those made by ARB. The evolutions of hardness, strain accumulation, the enhanced diffusion, nanocrystalline phase size, amorphous volume fraction, elastic modulus, and relative energy states in various Zr based alloy systems during ARB are characterized and analyzed by transmission electron microscopy (TEM), in correlation with X-ray diffraction results. It appears that compatible initial foil hardness would be most beneficial to the nanocrystallization and amorphization processes during the room temperature ARB; the influence would overwhelm the atomic size effect (i.e., the anti-Hume-Rothery rule) applicable for solidification processing such as drop casting or melt spinning. Meanwhile, the estimated diffusion rates during ARB are higher by several orders of magnitude than the lattice diffusion in bulk materials and the hardness is seen to increase with increasing ARB cycles. The last stage for the nanocrystalline phase to suddenly transform into the amorphous state is examined, coupled with thermodynamic analysis. From the experimental observations and interfacial energy calculations for multilayered films, it is demonstrated that the rapid increase of interfacial free energy of the nanocrystalline phases with increasing ARB cycles appears to be a determining role in enhancing amorphization process. The local spatial distributions of the nanocrystalline and amorphous phases are seen under TEM to be non-uniform, varying significantly in size and quantity in different regions. The diffraction spots and rings in the TEM diffraction patterns are still originated from the pure elements, meaning that the nanocrystalline phases are those unmixed hard particles left from the previous severe deformation and diffusion processes. A critical size of the nanocrystalline phases around 3 nm is consistently observed in all binary, ternary, and pentanary Zr-X based alloys, below the critical size a sudden transformation from the nanocrystalline to amorphous state would occur. Finally, the hardness and Young’s modulus of the nanocrystalline and amorphous materials are estimated based on the microhardness results. On the other hand, a pentanary alloy (according to the composition of the synthesized ARB specimens) is also made by the arc melting method for comparison. The sharp peaks are still observed in XRD pattern of the as-melted alloys. Hence, the melt spinning method is followed. A nearly completely amorphous state is obtained in the melt spun alloy. The hardness readings of the prepared alloys are all significantly higher than those typically for metallic alloys. Moreover, the resulting Zr based amorphous alloys made by ARB possess glass transition and crystallization temperatures similar to those processed by melt spinning or drop casting.