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The enhanced mechanical properties of Ni-based single-crystal superalloys induced by refractory elements such as Re, Wo, Mo, etc. are essential for the manufacture of advanced aero engines' turbine blades. Whereas these elements could promote the formation of the topologically close-packed (TCP) phases, and their growth would have a deleterious effect on the creep rupture life of single-crystal superalloys. Concomitantly, the formation of the brittle phase of the internal nitrides, especially the aluminium nitride (AlN), would be detrimental to superalloys as well. Nonetheless, the formation relationship between AlN and TCP phases has maintained opaque. In this study, the relationship between the TCP phase and AlN phase was analysed by microscopic methods, such as BSE, TEM and EDS. An AlN phase located near the TCP phase in the deep surface of the superalloy was found, and its formation was suggested to be related to nitrogen penetration during the thermal exposure. This accompanying growth of the AlN phase and TCP phase in the deep surface could provide a new perspective on the formation mechanism of these brittle phases in the Ni-based single-crystal superalloys. [ABSTRACT FROM AUTHOR]

Understanding the oxidation of Ni-based single crystal (SX) superalloys is significantly important because oxidation can damage the microstructure and eventually lead to failure of the alloy. Using advanced scanning/transmission electron microscopy, oxidation effects on the microstructure of a SX superalloy during heat treatment and simulated service (stress/temperature coupling) conditions are systematically investigated in order to reveal oxide microstructures and oxidation mechanisms. Heat treatment in argon results in less weight loss, thinner γ′-free layer and fewer internal oxidation than that treated in air. But the oxide layer structures and influence depths of oxidation in both atmospheres are similar. External tensile stress not only accelerates the oxidation of alloy but also affects the oxide microstructures. Moreover, stress effects on the oxidation microstructure depend on temperature. At 750 °C, Ni–Co oxides are formed on the alloy surface, followed by the inner layer of Ni–Co–Mo–Re–W oxides at the location of original γ phase under stress free condition. As the stress increases, an oxide layer mainly containing Al, Cr, Nb, Mo and Re elements is formed between the above two oxide layers. When temperature increases to 1050 °C, as applied tensile stress increases, the thickness of oxide layer increases but the structure of oxide layer is not obviously changed. [ABSTRACT FROM AUTHOR]

To model the centrifugal loads and complex geometries experienced by turbine blades during service, the nickel-based single crystal superalloy DD6 samples with a groove structure are designed and tested under the coupling conditions of high-speed rotating of 20,000 r/min and high temperature of 980 ℃. Scanning electron microscopy and transmission electron microscopy are used to analyze the microstructural evolution of γ-γ' phases and dislocation morphologies of 400 h and 1000 h samples. The results indicate that microstructural degradation of the γ-γ' phase attributes to the larger centrifugal tensile stress S 11 in the applied physical stress compositions until deformation occurs. Our observations suggest that a/2 < 101 > -type dislocations initiate plastic deformation by slipping within the γ phase. However, their movement is constrained at the interface between the γ and γ' phases, resulting in their tendency to aggregate at this boundary. After the formation of stable interfacial dislocation networks, these dislocations then react to generate either a< 010 > -type dislocations or a/2 < 112 > -type dislocations, which cut into the γ' phase. However, under high stress conditions, the a/2 < 101 > -type dislocations are primarily cut directly in the form of dislocation pairs. • The γ-γ' phase degradation and dislocation evolution of DD6 superalloy was investigated. • Creep tests are conducted under high-speed rotating and high temperature condition. • Microstructural degradation of the γ-γ' phase attributes to the larger centrifugal tensile stress S 11. • Interfacial dislocation networks and superdislocations accelerate the separation and disappearance of the γ phase. [ABSTRACT FROM AUTHOR]

This work investigates the evolution of the crystal structure of the topologically closed packed orthorhombic P phase precipitate in a Re-containing Ni-based single crystal superalloy during thermal exposure. The P phase is formed with a thin needle morphology. The precipitate is formed from the matrix with an initial complex atomic arrangement which continues to evolve during the process of thermal exposure. Based on the experimental evidence of this study and the theoretically predicted structure reported in the literature, a mechanism of the structural transformation is proposed. The initial structure is composed of a parallelogram (P) atomic arrangement configuration, which gradually evolve into a rectangle (R) atomic arrangement configuration in the [100] P projection. In the [010] projection, the initial structure is composed of alternating rows of a larger parallelogram (P') and a larger rectangle (R') configurations, which gradually evolve into an intricate structure of P'-R' along the length [001] P direction and P'P'-R'R' along the transverse [100] P direction. The initial structure is formed for its structural similarities to the γ phase to minimize lattice mismatch. The final structure is evolved over time to conform to its thermodynamically more stable state. The structural evolution is achieved by collective atomic shuffling. These intricate atomic arrangements gives rise to the very faint and highly dense parallel striation lines along the transverse [010] P direction in [100] P view and along the length [010] P direction in [010] P view under transmission electron microscopy observation. Image, graphical abstract [ABSTRACT FROM AUTHOR]

The cyclic oxidation behavior of fourth-generation nickel-based single crystal superalloys with 2–4 wt% Mo content were studied at 900 ℃ and 1100 ℃. At 900 ℃, with the increase of Mo content, the oxide layer accumulates more growth stress, resulting in the interface between the outer oxide layer and the inner oxide layer more prone to crack initiation. At 1100 ℃, the oxidation layer accumulates more growth stress and thermal stress, so the oxidation layer occurs large scale spalling, which is more severe in 4Mo alloy. The results show that the increase of Mo content of alloy promotes the oxidation of containing W-Re alloy, which promotes the volatilization of oxides and the spalling of oxide, decreases the protection of oxide layer, and deteriorates the oxidation resistance of the alloy. • The increase of Mo content of alloy promotes the oxidation of containing W-Re alloy. • With the increase of Mo content, the volatilization of oxides and the spalling of oxide of alloy was promoted. • Mo has more severe harm to the oxidation resistance of the alloy at higher temperature. • The alloy with 2 wt% Mo addition has the highest oxidation resistance. [ABSTRACT FROM AUTHOR]

The precipitation and growth morphology of topologically close-packed (TCP) phases in a Re-containing Ni-based single crystal superalloy during thermal exposure were studied. The alloy was found to develop acicular-shaped coherent μ phase particles along <110> γ directions of the matrix after exposure at 950 °C. P phase precipitates were found to form with increased time and at higher temperatures, and in different morphologies, including acicular shaped particles along <112> γ and <110> γ directions, and plate-like particles in {110} γ planes of the matrix. The different P phase precipitates were found to have different lattice constants and different lattice correspondences with the matrix. The μ phase precipitate was also found to have different lattice correspondences with those reported in the literature. The multiplicity of lattice correspondences for the same TCP phase is attributed to the different lattice parameters, which render the precipitates to have different coherency relationships with the matrix. [ABSTRACT FROM AUTHOR]

Amorphous Al 2 O 3 coating was prepared on Ni-based single crystal superalloy via atomic layer deposition (ALD) for high temperature oxidation protection. The oxygen inward transport and outward-cation diffusion were hindered by amorphous Al 2 O 3 coating, and the coated alloy showed high oxidation resistance. The low oxygen partial pressure at the alloy/coating interface altered the alloy oxidation behavior, allowing the priority oxidation of protective Al and Cr elements. The oxidation process was controlled by the growth of Cr 2 O 3 and Al 2 O 3. The coating exhibited high spallation resistance. Degradation of the coating, the formation of NiAl 2 O 4 phase in amorphous Al 2 O 3 layer, was observed. • Amorphous Al 2 O 3 coating was proposed and prepared on Ni-based single crystal superalloy. • The amorphous Al 2 O 3 coating improved oxidation resistance and exhibited high adhesion. • The amorphous Al 2 O 3 coating altered the oxidation behavior of the alloy. • The effect mechanism of amorphous Al 2 O 3 coating on the alloy oxidation was discussed. [ABSTRACT FROM AUTHOR]

For further composition optimization, the microstructure evolution of the fourth-generation nickel-based single crystal superalloys, which contains different Co (Cobalt) additions, is studied at three thermal exposure temperatures. Based on Lifshitz, Slyozov and Wagnerz (LSW) theory and trans-interface diffusion-controlled (TIDC) theory, the effects of Co content and aging temperatures on coarsening rate of γ′ phase are investigated in detail. The results show that the diffusion coefficient of solute is accelerated, but the γ/γ′ interfacial energy decreases with the addition of Co, thus changing the coarsening rate. Furthermore, the thermodynamic equilibrium solubility difference of elements between γ′ and γ, and the segregation of elements at the γ/γ′ interface are alleviated with increase of Co, resulting in the suppression of TCP phase after long-time thermal exposure, which guides the economical design of nickel-based single crystal superalloys. • Co additions have a dual effects on microstructure evolution of the superalloys. • The effect of Co on coarsening rate of γ′ depends on temperature. • The accuracy of two coarsening prediction models is tested. [ABSTRACT FROM AUTHOR]

In this study, we investigate the movement of dislocations in Ni-based superalloys under the influence of lattice misfit stresses between the ordered γ'-cuboids and the disordered γ-matrix during thermal exposure in the absence of an applied load. This study focuses on a different condition than the conventional creep testing, and thus offers a unique opportunity to study the intrinsic behavior of the alloy. The dislocation density increases substantially with time during thermal exposure, leading to the formation of various configurations of dislocation networks on the {100} γ/γ′ interfaces, including <110> diamond-shaped, <110>/<100> mixed polygon-shaped and <100> square-shaped networks. During thermal exposure, the b = 1 2 < 110 > native dislocations first move and evolve into 60° mixed dislocations along the <110> directions on the {100} γ/γ′ interfaces, forming the <110> diamond-shaped dislocation networks. In the case of longer thermal exposures, the dislocations further evolve into pure edge dislocations along the <100> on the {100} γ/γ′ interface, leading to the evolution of the <110> diamond-shaped dislocation networks into <100> square-shaped networks, with the mixed <110>/<100> dislocation networks as an intermediate stage during the transition. These movements occur by sweep glide in the {111} planes and diagonal climb on the {100} planes for the edge and mixed dislocations and by cross-slip for the screw dislocations. The driving force for all of these movements is the interaction between the normal misfit stresses and the edge components of the Burgers vectors of the dislocations to relax the misfit stresses. An analysis based on the elastic strain energy considerations is presented to explain the driving forces for the dislocation movements. [ABSTRACT FROM AUTHOR]

Two distinct evolutionary processes of secondary γ′ precipitates in a Ni-based single crystal superalloy were revealed by means of Cs-corrected high-resolution transmission electron microscopy (HRTEM) and corresponding X-ray energy dispersive spectroscopy analyses. Upon creep testing at elevated temperatures, it was determined that large quantities of secondary γ′ precipitates were formed. The precipitates were found to select two distinctive forms and routes: one randomly dispersed in the γ matrix (2nd γ′ γ ), and the other formed at nodes of dislocation networks (2nd γ′ d ) in regular arrays. These two types of secondary γ′ precipitates exhibited different evolutionary morphologies and mechanisms. The 2nd γ′ γ precipitates progressively evolved in shape from spherical to cuboidal and then to butterfly-like shapes, and the mean size also increased gradually from 11 nm to 34 nm. The 2nd γ′ d precipitates exhibited stable cuboidal morphology and a mean size of ∼30 nm. These differences are attributable to the different element transport conditions for the two types of precipitates, i.e., an uphill diffusion for the 2nd γ′ γ precipitates and a dislocation network pipe transportation for the 2nd γ′ d precipitates. The 2nd γ′ γ precipitates show severe segregation of γ′-rich elements of Ni and Al and deficiency of γ′-poor elements of Cr compared with the 2nd γ′ d precipitates. [ABSTRACT FROM AUTHOR]

To determine the influence of Re and Ru on the phase morphologies and microstructure in Ni-based superalloys, a series of model alloys derived from the 4th generation TMS-138 superalloy have been investigated with systemically changing Re and Ru additions. All alloys are subjected to solid solution and aging treatments to achieve the typical γ/γ′ two phases microstructure. Phase transition temperatures are measured by using differential scanning calorimetry. The Re is found to increase the γ′-solvus temperature with a slope of roughly 5.4 ℃ per wt% Re in Ru-free alloys and 2.3 ℃ per wt% Re in 2Ru alloys, while the Ru exhibits much weaker effect. Microstructure and composition of the two phases are examined to understand the Re and Ru effects on γ′ size, shape, volume fraction, the elemental partition behavior, and the γ/γ′ lattice misfit. The results show that the addition of Re affects size and shape of γ′ precipitates, and also reduces γ/γ′ lattice misfit significantly. Meanwhile, Re increases partition coefficients of Cr and Ru. In comparison, the addition of Ru seems to have little effect on morphology of γ′ precipitates and the γ/γ′ lattice misfit, but Ru appears to alter partitioning behaviors of other elements. Because Re and Ru are two key elements for high generation Ni-based single crystal (SX) superalloys, this work might provide guidelines for designing next generation of SX superalloys. [Display omitted] • Re effectively increases the γ′ solvus temperature of superalloys, while Ru has slight effect on the γ′ solvus temperature. • Re addition decreases the size of γ′ phase and γ/γ′ lattice misfit, facilitating cubic precipitation of γ′ phase. • Ru addition only has little effect on the γ′ morphology and γ/γ′ lattice misfit of superalloys. • Partitioning behaviors of other alloying elements depend on the Re and Ru additions, especially Ru. [ABSTRACT FROM AUTHOR]

Although their mechanical behavior has been extensively studied, the atomic-scale deformation mechanisms of metallic nanowires (NWs) with growth twins are not completely understood. Using our own atomic-scale and dynamic mechanical testing techniques, bending experiments were conducted on single-crystalline and twin-structural Ni NWs ( D = ∼40 nm) using a high-resolution transmission electron microscope (HRTEM). Atomic-scale and time-resolved dislocation nucleation and propagation activities were captured in situ . A large number of in situ HRTEM observations indicated strong effects from the twin thickness ( TT ) on dislocation type and glide system. In thick twin lamella ( TT > ∼12 nm) and single-crystalline NWs, the plasticity was controlled by full dislocation nucleation. For NWs with twin thicknesses of ∼9 nm < TT < ∼12 nm, full and partial dislocation nucleation occurred from the free surface, and the dislocations glided on multiple systems and interacted with each other during plastic deformation. For NWs with twin thicknesses of ∼6 nm < TT < ∼9 nm, partial dislocation nucleation from the free surface and the gliding of those dislocations on the plane that intersected the twin boundaries (TBs) were the dominant plasticity events. For the NWs with twin thicknesses of ∼1 nm < TT < ∼6 nm, the plasticity was accommodated by a partial dislocation nucleation process and glide parallel to the TBs. When TT < ∼1 nm, TB migration and detwinning processes resulting from partial dislocation nucleation and glide adjacent to the TBs were frequently observed. [ABSTRACT FROM AUTHOR]

Here, we investigate a new type of kink structure that is found at γ/γ′ interfaces in nickel-based single crystal superalloys. We studied these structures at the atomic and elemental level using aberration corrected high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM). The core of the dislocation absorbs high-Z elements (i.e., Co and Re) that adopt hexagonal arrangements, and it extrudes elements (i.e., Ni and Al) that adopt face centered cubic (fcc) structures. High-Z elements (i.e., Ta and W) and Cr, which is a low-Z element, are stabilized in body centered cubic (bcc) arrangements; Cr tends to behave like Re. High-Z elements, which migrate and adopt a hexagonal structure, induce kink formation at γ/γ′ interfaces. This process must be analyzed to fully understand the kinetics and dynamics of creep in nickel-based single crystal superalloys. [ABSTRACT FROM AUTHOR]

Understanding the high-temperature initial oxidation mechanism and its dynamic processes is generally important because a small amount of initial oxidation can induce rapid corrosion and cause catastrophic failure. We reveal the mechanism of initial oxidation in a third-generation Ni-based superalloy by in situ visualizations and investigations of the nano- and atomic-scale dynamic processes from room temperature to 900 °C with a Cs-corrected environmental transmission electron microscope. The initial oxidation starts from the γ/γ′ interface at low temperatures. The high-temperature oxidation process with deficient oxygen prefers oxidation sites at the cross-junctions of the γ/γ′ interfaces. The growth rate of the oxide nanoparticles depends on the oxidation temperatures, with a low rate below 600 °C and a rapid-growth speed at temperatures higher than 700 °C. Mass transfer from the γ′ and γ phases to the γ/γ′ interface, particularly at the cross-junctions of these interfaces, is observed to cause oxide accumulation. This study provides a direct observation of the interphase, interface-junction-initiated outward oxidization including Al and Cr elements. These results shed light on the initial oxidation mechanisms of materials containing a second phase with interphase interfaces and the materials at deficient oxygen conditions as well as those with protection coating layers. [Display omitted] [ABSTRACT FROM AUTHOR]

The chemical and structural evolution within dislocation networks are investigated in a nickel-based single crystal superalloy crept under 1373K and 137MPa. The local region within dislocation networks can be divided to two separated parts: gridlines which compose the arrangements of dislocation networks and mesh regions as intervals between gridlines. With evolution of dislocation networks, precipitation of nano-sized γ′ phase (γ′ n) are observed in mesh region, while gridlines always display the FCC feature of γ phase. The formative mechanism of γ′ n is revealed as increased segregations of Cr, Co and Re along gridlines which enhance the contents of γ′-rich elements such as Al in mesh region to promote the local phase transition from FCC to highly ordered L1 2. However, growth of γ′ n requires massive diffusion of γ′-rich elements that is confined by the chemical barrier along gridlines with strong segregations of Cr, Co and Re. The mesh region of γ′ n and gridlines of γ reinforce each other forming potential γ/γ′ substructures to stabilize the dislocation networks during creep. Denser dislocation networks formed in dendrite core under larger local lattice misfit are accompanied with facilitated formation of γ/γ′ substructures which derive higher creep resistance than interdendritic region. Image, graphical abstract [ABSTRACT FROM AUTHOR]

It is important and necessary to understand the micro-mechanism of rhenium (Re) effect in the deformation process. The in-situ tensile experiments of Ni–Al and Ni–Al-Re model single crystal superalloys have been carried out in scanning electron microscope at 750 °C. It is found that Re can promote the complex stacking fault (CSF) formation, which is similar to the previous results after tensile experiments at room temperature. The micro-mechanism of Re promoting the CSF formation has been investigated by means of advanced probe-corrected scanning transmission electron microscopy and energy dispersive X-ray spectroscopy. The local high concentration of Re is observed at CSF regions after tensile experiments both at room temperature and 750 °C. The first principles calculation results further indicate that low concentration of Re increases CSF energy, while high concentration of Re decreases CSF energy, which is consistent with the experimental results. • In-situ tensile experiments of model single crystal superalloys are carried out. • Re can promote the complex stacking fault (CSF) formation. • High concentration of Re is observed in local region along CSF. • The calculation results show high concentration of Re decreases CSF energy. [ABSTRACT FROM AUTHOR]

It is known that Ni-based superalloys experience microstructural rafting during high temperature straining. This paper presents a comparative study of the different rafting models by means of finite element modeling and experimentation investigation. It was found that uniaxial elastic loading does not alter the misfit or misfit isotropy of the structure, but causes repartitioning of the misfit into elastic strains in the γ and γ' phases. This causes an elastic strain energy anisotropy and hydrostatic stress anisotropy among the vertical and horizontal γ phase channels. Both anisotropies predict a raft structure that is contrary to the experimental observation. Through a carefully designed pre-treatment at 750 °C and under a uniaxial stress of 750 MPa, an anisotropic dislocation structure was created on the {001} γ'/γ interfaces without altering the cuboidal morphology of the γ' phase. This allows the evaluation of the influence of dislocations on the rafting behavior of the alloy. It was found that rafting occurred in the pre-treated samples containing anisotropic dislocation structures during thermal exposure without applied stress, instead of isotropic corsening, and that the raft structures conform to the expectations base don the anistropic dislocation strucutres. This demonstrates that an anisotropic dislocation structure on the {001} γ'/γ interfaces is a direct cause of rafting. This is attributted to the fact that dislocations on γ'/γ interfaces help to relax the local misfit strains, causing some to expand at the expense of others. At the same time, the formation of the anisotropic dislocation structure is a direct result of the anisotropy of elastic strains induced by the applied bia stess in during the pre-treatment. These explain the complex interplay of the elastic and plastic models reported the literature. Unlabelled Image • The elastic stretching alters the partitioning of elastic strains in two phases, whereas the misfit remains unchanged. • The elastic strain energy and hydrostatic stress anisotropies are ruled out to be responsible for rafting. • The anisotropic dislocation on γ'/γ interfaces wtith γ' phase cuboid morphology unchanged were created by pre-straining. • The dislocation anisotropy is effective in causing rafting in Ni-based superalloys by causing misfit anisotropy. [ABSTRACT FROM AUTHOR]

L1 2 structured γ′ phase is the main strengthening phase of Ni-base superalloys, which contain multiple alloying elements. Locations of these elements in the lattice are crucial for understanding the mechanical/physical properties of γ′ phases. Here, we reveal the site occupancy of various elements in γ′ phases of two multi-component Ni-base single crystal superalloys by using advanced scanning transmission electron microscopy and energy disperse spectroscopy. Cr, Mo, Re, Ta, W and Ti atoms preferentially locate at Al sublattices, and Co and Ru atoms prefer Ni sublattices. Moreover, the addition of Ru does not affect the site occupancy of other alloying elements. Image 1 • EDS mapping directly shows atomic distribution of all elements in the γ′ phases. • Cr, Mo, Re, Ta, W and Ti atoms preferentially occupy Al sublattices. • Co and Ru atoms prefer Ni sublattices. • Ru has limited effect on site occupancy of other alloying elements in γ′ phase. [ABSTRACT FROM AUTHOR]

Nickel-based single crystal superalloys (Ni-SXs) are of great interests in aircraft industry due to their excellent high temperature creep strength deriving from the rigid gamma/gamma prime (γ/γ′) microstructure and the single crystal nature. The creep properties of Ni-SXs depend strongly on the degradation rate of the original rigid γ/γ′ microstructure with the dislocation movements in the microstructure. Since the applied temperature and stress strongly affect the dislocation movements, the different creep mechanisms are displayed to Ni-SXs during low temperature (∼750 °C), mid-temperature (∼950 °C) and high temperature (∼1100 °C) creep. The creep deformation during low temperature creep is mainly caused by the shearing of γ′ phase by a limited number of dislocations, while high temperature creep mainly occurs to the accumulation of creep strains with the increased dislocation activities in γ phase. To enhance the creep properties of alloy, a variety of strategies of the microstructural optimization need to be considered. One is to increase the volume fraction of γ′ phase to enhance the precipitation strengthening effects. But excessive amounts of γ′ phase are disadvantageous to low temperature strength of alloy. The coarsening of γ′ phase and the rafting process strongly correlates to dislocation movements. It is of importance to discuss the specific mechanisms of coarsening and rafting as well as their influence to the creep properties of alloy. The lattice misfit between the γ and γ′ phase plays an important role in influencing the coarsening of γ′ phase and the creep properties of alloy. A proper lattice misfit helps to form the cubic γ′ phase which is advantageous to alloy. But a too large lattice misfit can promote the coarsening of γ′ phase that damages the structural stability of alloy at high temperatures. The increased additions of refractory elements in alloy promote the formation of topologically close-packed (TCP) phase. TCP phase facilitates the nucleation and propagation of micro-cracks around it that damages the creep properties of alloy. This review aims to summarize some aspects of microstructural evolution during creep of alloy with considering their effects to creep properties. To guide the design of Ni-SXs in future, some perspectives about the microstructural optimization are properly provided. • The creep properties of Nickel-based superalloys are greatly decided by the microstructural evolution during creep. • The creep mechanisms are determined by the intrinsic dislocation activities occurred in the microstructure. • The coarsening of γ′ phase is emphasized, especially the rafting process. • Lattice misfit strongly affects the formation of dislocation networks and coarsening of γ′ phase. • The formation of TCP phase which is detrimental to creep properties need to be strictly restricted in superalloy design. [ABSTRACT FROM AUTHOR]