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The mechanical properties of investment casted open-pore metal foams have been investigated on the example of the binary alloy Al–11Zn. The samples were subjected to different cooling conditions subsequent to casting and to different homogenization and ageing treatments. Variation in cooling was done either by quenching the mold in water or slowly cooling it in air. Homogenization and ageing varied in terms of temperature and time. The effects of the different treatments were investigated through microstructural and mechanical characterization methods. Using TEM, we found that the presence of GP zones and their morphological arrangement are the main factors dominating the mechanical performance. Micro- and nanoindentation testing of single foam struts reveal maximum hardness H when room temperature ageing was applied. Ageing at a temperature of 150 °C results in the lowest H in the present study; that is approximately 2/3 of the hardness achieved when ageing at room temperature. This can also be confirmed by the strength of non-porous bulk material obtained by tensile tests, which further show an increase in ductility up to a factor of 5 due to ageing at elevated temperatures. By compression testing of open-pore Al–11Zn foams, we notice that the presence of the microstructural effects varies in extent as a function of the strain e. At low strains, we observe differences in mechanical performance to a high extent, becoming less with increasing compaction of the samples until they behave as non-porous bulk material. Based on these findings, we deduce a strong interaction of the structural morphology of the foam and its microstructure that determines the mechanical properties dominated by strength and ductility of the base material.

The formation of dislocation substructures in up to 10 µm deep subsurface regions of two aluminium alloys, Al-5Mg and Al-11Zn, was investigated under conditions of high homologous temperature reciprocal sliding wear (HT-RSW). Under creep conditions, Al-5Mg shows a solid solution type of inverse primary creep. In contrast, Al-11Zn creeps obstacle controlled and exhibits normal primary creep. These two materials were subjected to reciprocal sliding wear at 200 and 300 °C for 100 and 1000 cycles. Flat polished disks were exposed to the 1 mm reciprocal movements of a spherical aluminium oxide counterbody under normal forces of 5 and 10 N at an oscillation frequency of 1 Hz. Using focused ion beam (FIB) micromachining thin electron transparent foils were prepared from the surface regions of the as received and worn material states. Transmission electron microscopy (TEM) was used to study the evolution of nano and micro grain sizes in the surface regions. Despite the different creep behavior, the two materials behave similar under conditions of reciprocal sliding wear. The results obtained in the present work show that subgrain sizes decrease with increasing numbers of wear cycles and increasing normal forces. Subgrain sizes also increase with increasing temperature. At 300 °C, dynamic recrystallization was observed in both Al-alloys. The results of the present work are discussed in the light of previous results reported in the literature. Areas in need of further work are highlighted.

The dependence of the microstructure on the degree of deformation in near-surface regions of a 16MnCr5 gear wheel after 2.1 × 106 loading cycles has been investigated by x-ray diffraction analysis, transmission electron microscopy, and atom probe tomography. Retained austenite and large martensite plates, along with elongated lamella-like cementite, were present in a less deformed region. Comparatively, the heavily deformed region consisted of a nanocrystalline structure with carbon segregation up to 2 at.% at grain boundaries. Spheroid-shaped cementite, formed at the grain boundaries and triple junctions of the nanosized grains, was enriched with Cr and Mn but depleted with Si. Such partitioning of Cr, Mn, and Si was not observed in the elongated cementite formed in the less deformed zone. This implies that rolling contact loading induced severe plastic deformation as well as a pronounced annealing effect in the active contact region of the toothed gear during cyclic loading.

Ni-base single-crystal turbine blades are exposed to a combination of high temperatures and high stresses during their service life in high-pressure turbines of aero engines or stationary gas turbines. This unavoidably leads to various internal microstructural changes such as rafting and the formation of cavities. This study introduces a creep-rejuvenation-creep test cycle using one miniature Ni-base single-crystal creep specimen. A novel hot isostatic press providing high quenching rates was applied to rejuvenate the damaged microstructure of the specimen after the first high-temperature creep degradation before the same specimen was repeatedly creep-tested under the same initial creep conditions. After rejuvenating, microstructural results obtained from high-resolution microscopy prove that the creep cavities were closed, dislocation densities were re-set, and the original but now slightly finer γ/γ′-microstructure was restored without any recrystallization. The subsequent creep test of the rejuvenated specimen demonstrated that the proposed rejuvenation procedure in this work is a suitable method to reproduce the initial creep behavior and to thus prolong the lifetime of an already crept Ni-base single-crystal specimen. Keywords: Creep, Creep life, γ/γ′-microstructure, Hot isostatic pressing, HIP, Pores, Rafting, Rejuvenation, Recrystallization, Single crystal superalloy

In this study a bipolar pulsed current was used for the electrochemical deposition of calcium phosphate coatings on the Nitinol superelastic alloy. The coatings were characterized using FE-SEM, XRD, FTIR, HRTEM, and gas adsorption techniques. Results show that the electrodeposited coating is a crystalline film which is composed of pure hydroxyapatite (HA) nanowalls. According to the FTIR data, the coating is free from other metastable calcium phosphate phases like octacalcium phosphate. It was shown that both monoclinic and hexagonal phases can be detected in HRTEM images and related SAED patterns. The coating, which is deposited at direct and reverse current densities of −3.0 and 0.1 mA/cm2 respectively, revealed a surface area of 38.5 m2/g and ultra-fine pores were detected in the surface of the coating plates. Study on the effect of the reverse pulse current revealed that the volume of porosity is increased by increasing in the current density of the reverse pulse. Also in this condition the resulted film was composed of nanosized HA crystals. It seems that the reverse current step can influence the porosity and the structure of the coatings by dissolution of the unstable phases which are formed during direct current step of the bipolar pulse deposition.

High-resolution characterization techniques are combined with thermodynamic calculations (CALPHAD) to rationalize microstructural features of single crystal Ni-base superalloys. Considering the chemical compositions of dendritic and interdendritic regions one can explain differences in γ′-volume fractions. Using thermodynamic calculations one can explain, why γ-nanoparticles are observed in the central regions of large cuboidal γ′-particles and why tertiary γ′-nanoparticles form in the γ-channels. The chemical compositions of the γ-channels and of the newly formed γ-particles differ because of the Gibbs–Thomson pressure which acts on the small particles. With increasing size of secondary γ′-particles, their shape changes from spherical to cuboidal. Some general thermodynamic aspects including the temperature dependencies of the Gibbs free energy G, the enthalpy H, and the entropy S and site occupancies in the ordered L12 (γ′) phase are considered. The importance of cooling rate after homogenization is discussed.

The effect of a pre-strain on the plasticity of copper single crystals subjected to in situ microshear deformation in a scanning electron microscope (SEM) is investigated. Pre-strains of 6.5 and 20% are imposed using [1 0 0] tensile testing. During tensile pre-deformation, several slip systems are activated and irregularly spaced slip bands form. A trace analysis revealed the presence of several slip bands on the tensile specimen near the grips while one family of slip bands parallel to the (1 1 1) crystallographic plane were detected in the middle of the tensile specimen. From the middle of the pre-deformed tensile specimens double microshear samples were prepared using focused ion beam (FIB) machining such that the [0 -1 -1] (1 -1 1) slip system could be directly activated. The results show how microshear behavior reacts to different levels of tensile pre-deformation. Sudden deformation events (SDEs) are observed during microshear testing. The critical stress associated with the first SDE is shown to increase with increasing pre-deformation as a result of an increasing number of slip bands introduced during pre-deformation per shear zone. The results allow also to obtain information on the interaction between dislocations activated during microshearing ([0 -1 -1] (1 -1 1)) and those which were introduced during tensile pre-deformation ([1 0 -1] (1 1 1) and [1 -1 0] (1 1 1)). When these slip systems interact glissile junctions and Lomer-Cottrell locks are likely to form. In the light of this analysis, we rationalize the occurrence of sudden deformation events based on piled up dislocation assemblies which overcome Lomer-Cottrell lock barriers.

In the present study, we systematically identify and characterize a (Nb, Mo)-rich M23C6 type of M23C6 carbide with a lattice parameter of 1.094 nm in alloy 718 for the first time using a combination of selected area electron diffraction pattern and powder X-ray diffraction analysis. The time-temperature-precipitation diagrams of the precipitates in both annealed and strained conditions are obtained by particle analysis using an automated scanning electron microscopy method. (Nb, Mo)-rich M23C6 carbides first precipitate after 24 hours at 1223 K (950 °C) annealing, while they form after 10 minutes at 1273 K (1000 °C) in the strained condition. This correlates with the excess dislocations produce during deformation.

In the present work, we use a miniature test procedure to investigate the tensile creep behaviour of the single crystal superalloy ERBO1. We test precisely oriented [0 0 1], [1 1 0] and [1 1 1] creep specimens and determine the stress and the temperature dependence of characteristic creep rates in limited stress and temperature regimes, where the stress and temperature dependence of characteristic creep rates can be well described by power law and Arrhenius type of relations, with stress exponents n and apparent activation energies Qapp. n-values increase with stress and decrease with temperature. Qapp-values, on the other hand, increase with increasing temperature and decrease with increasing stress. Creep curve shapes gradually evolve from the high temperature low stress to the low temperature high stress (LTHS) regime. This implies that there is a gradual change in elementary deformation and softening mechanisms, which is qualitatively confirmed using transmission electron microscopy. While at high tem...

Preparing a stable suspension is a main step towards the electrophoretically depositing of homogeneous and dense composite coatings on NiTi for its biomedical application. In the present study, different composite suspensions of hydroxyapatite, silicon and multi-walled carbon nano-tubes were prepared using n-butanol and triethanolamine as media and dispersing agent, respectively. Multi-walled carbon nanotubes were first functionalized in the nitric acid vapor for 15 h at 175 °C, and then mixed into suspensions. Thermal desorption spectroscopy profiles indicate the formation of functional groups on multi-walled carbon nano-tubes. An excellent suspension stability can be achieved for different amounts of triethanolamine. The amount of triethanolamine can be increased by adding a second component to a stable hydroxyapatite suspension due to an electrostatic interaction between components in suspension. The stability of composite suspension is less than that of the hydroxyapatite suspension, due to density differences, which under the gravitational force promote the demixing. The scanning electron microscopy images of the coatings surface show that more dense coatings are developed on NiTi substrate using electrophoretic deposition and sintering at 850 °C in the simultaneous presence of silicon and multi-walled carbon nanotubes in the hydroxyapatite coatings. The atomic force microscopy results of the coatings surface represent that composite coatings of hydroxyapatite-20 wt.% silicon and hydroxyapatite-20 wt.% silicon-1 wt.% multi-walled carbon nano-tubes with low zeta potential have rougher surfaces.

The present work reviews previous research on the evolution of porosity. It presents new results from a detailed study on the evolution of porosity during casting, heat treatment and creep of a single crystal Ni-base superalloy subjected to uniaxial tensile creep at 1050 °C and 160 MPa in [001] and [110] directions. A quantitative metallographic study was performed on carefully polished metallographic cross sections, monitoring sampling fields of 4500 × 1000 µm2 using the back scatter contrast of an analytical scanning electron microscope; evolutions of pore sizes and pore form factors were analyzed and all important details which were previously revealed in a synchrotron study could be reproduced. In addition, it was observed that micro cracks form at larger cast pores. They interlink and thus initiate final rupture. The [110] tensile creep tests showed lower rupture strains than the [001] experiments. In agreement with earlier work, this can be rationalized on the basis of aligned porosity along primary dendrites.

In the present work we study the formation of grooves and ledges (typical size: γ / γ ′ interfaces of single crystal Ni-base superalloys. We highlight previous work which documents the presence of such interface irregularities and shows that their number and size increases during high temperature exposure and creep. We use diffraction contrast stereo transmission electron microscopy (TEM) to provide new evidence for the presence of ledges and grooves near dislocations at γ / γ ′ interfaces after heat treatment and creep. We present a 2D model of the interfacial region which shows how dislocation stress fields alter local chemical potentials and drive diffusional fluxes which result in the formation of a groove. The results of the numerical study yield realistic groove sizes in relevant time scales. The results obtained in the present study suggest that the formation of grooves and ledges represents an elementary process which needs to be considered when rationalizing the kinetics of rafting, the directional coarsening of the γ ′ phase.

Addition of Re in nickel-based superalloys results in an increase of the creep life. However, Re is also known to segregate to the dendrite core and to promote the formation of topologically closed packed (TCP) phases. In the present work, the local segregation of Re was studied in the heat treated and creep deformed state of a nickel-based superalloy. Tensile creep deformation at 1050 °C resulted in the formation of TCP phases in the dendritic regions. Characterization using TEM confirmed the presence of μ phase that grows on {111} planes. Measurements with a nanoindenting AFM show that the μ phase is harder and shows less work hardening than both the γ and the γ ′ phases. Furthermore, in the creep deformed state the hardness of the matrix phase is very similar in the dendrite core and in interdendritic areas, although Re is still enriched in the dendrite core. It is shown that Re is consumed in the dendrite core by the TCP phases.

In the present study we investigate the creep behavior of a Ni-base single crystal superalloy. We evaluate the stress and temperature dependence of the minimum creep rate, which shows a power law type of stress dependence (characterized by a stress exponent n ) and an exponential type of temperature dependence (characterized by an apparent activation energy Q app ). Under conditions of high temperature (1323 K) and low stress (160 MPa) creep, n and Q app are determined as 5.3 and 529 kJ/mol, respectively. For lower temperatures (1123 K) and higher stresses (600 MPa) the stress exponent n is higher (8.5) while the apparent activation energy of creep is lower (382 kJ/mol). We show that there is a general trend: stress exponents n increase with increasing stress and decreasing temperature, while higher apparent activation energies are observed for lower stresses and higher temperatures. We use density functional theory (DFT) to calculate the activation energy of diffusion for Re in a binary Ni–Re alloy with low Re-concentrations. The resulting energy is almost a factor 2 smaller than the apparent activation energy of creep. We explain why it is not straightforward to rationalize the temperature dependence of creep merely on the basis of the diffusion of one alloying element. We show that the evolution of the microstructure also must be considered.

In the present work, we show how conventional and advanced mechanical, chemical, and microstructural methods can be used to characterize cast single crystal Ni-base superalloy (SX) plates across multiple length scales. Two types of microstructural heterogeneities are important, associated with the cast microstructure (dendrites (D) and interdendritic (ID) regions – large scale heterogeneity) and with the well-known g/g 0 microstructure (small scale heterogeneity). Using electron probe microanalysis(EPMA),wecanshowthatelementssuchasRe,Co,andCrpartitiontothedendriteswhileID regions contain more Al, Ta, and Ti. Analytical transmission electron microscopy and atom probe tomography (APT) show that Al, Ta, and Ti partition to the g 0 cubes while g channels show higher concentrations of Co, Cr, Re, and W. We can combine large scale (EPMA) and small-scale analytical methods (APT) to obtain reasonable estimates for g 0 volume fractions in the dendrites and in the ID regions. The chemical and mechanical properties of the SX plates studied in the present work are homogeneous, when they are determined from volumes with dimensions, which are significantly larger than the dendrite spacing. For the SX plates (140 mm � 100 mm � 20 mm) studied in the present work this holds for the average chemical composition as well as for elastic behavior and local creep properties. We highlight the potential of HRTEM and APT to contribute to a better understanding of the role of dislocations during coarsening of the g 0 phase and the effect of cooling rates after high temperature exposure on the microstructure.

The present work compares the microstructures and the creep properties of two types of single crystal Ni-base superalloy CMSX-4 materials (SXs). One was produced by conventional directional solidification Bridgman processing. The other was manufactured by selective electron beam melting (SEBM). The microstructures of the two types of materials are compared with emphasis placed on the large (dendritic/interdendritic regions) and small scale (γ-matrix/γ′-precipitates) microstructural heterogeneities, which characterize SX microstructures and their evolution during processing, heat treatment and creep. It is shown that heat treated SEBM materials have creep properties, which match or even outperform those of conventionally processed SX materials. Creep properties were assessed using a miniature creep test technique where [001] miniature tensile creep specimens were tested in the high temperature/low stress (1050 °C, 160 MPa) and in the low temperature/high stress (850 °C, 600 MPa) creep regimes. The creep behavior is interpreted based on microstructural results, which were obtained using analytical scanning and transmission electron microscopy (SEM and TEM).

In this work, the microstructures of superalloy specimens produced using selective electron beam melting additive manufacturing were characterized. The materials were produced using a CMSX-4 powder. Two selective electron beam melting processing strategies, which result in higher and lower effective cooling rates, are described. Orientation imaging microscopy, scanning transmission electron microscopy and conventional high resolution transmission electron microscopy are used to investigate the microstructures. Our results suggest that selective electron beam melting processing results in near equilibrium microstructures, as far as \(\gamma\)' volume fractions, the formation of small amounts of TCP phases and the partitioning behavior of the alloy elements are concerned. As expected, higher cooling rates result in smaller dendrite spacings, which are two orders of magnitude smaller than observed during conventional single crystal casting. During processing, columnar grains grow in directions, which are rotated with respect to each other. There are coarse \(\gamma\)/\(\gamma\)' microstructures in high angle boundary regions. Dislocation networks form low angle boundaries. A striking feature of the as processed selective electron beam melting specimens is their high dislocation density. From a fundamental point of view, this opens new possibilities for the investigation of elementary dislocation processes which accompany solidification.

We present a study on the intersublevel spacings of electrons and holes in a single layer of InAs self-assembled quantum dots. We use Fourier transform infrared transmission spectroscopy via a density chopping scheme for direct experimental observation of the intersublevel spacings of electrons without any external magnetic field. Epitaxial, complementary-doped and semi-transparent electrostatic gates are grown within the ultra high vacuum conditions of molecular beam epitaxy to voltage-tune the device, while a two dimensional electron gas (2DEG) serves as a back contact. Spacings of the hole sublevels are indirectly calculated from the photoluminescence spectrum by using a simple model given by Warburton et al [1]. Additionally, we observe that the intersubb and resonances of the 2DEG are enhanced due to the quantum dot layer on top of the device.