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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]

• β-NiAl phase precipitates in a novel high Ru-containing Ni-SC. • Ru element is found to be obviously biased in β-NiAl phase. • The partition of Ru assists nucleation of β-NiAl phase during solidification. • Studies based on the solidification path of experimental alloy were carried out. The precipitation of β-NiAl phase in a high Ru-containing Ni-based single crystal superalloys was investigated. The β-NiAl phase is mainly distributed in the interdendritic region of the as-cast structure. And it was found parts of Ru elements were polarized in β-NiAl phase as the existence of strong bonds between Ru atoms and Al atoms. In addition, the solidification path of the experimental alloy passes through the region of the L → L 1 + γ → L 2 + γ + β-NiAl → L 3 + γ + β-NiAl + precipitated γ′ → γ + β-NiAl + precipitated γ′ + γ/γ′ eutectics. It provides experimental data and theoretical guidance for the composition design of the novel Ru-containing high-generation Ni-SCs. [ABSTRACT FROM AUTHOR]

The important factors limiting the fourth-generation Ni-based single-crystal superalloys (Ni-SXs) are the increases in cost and density. A cheaper and lighter potential alternative element of Ru, Co's comprehensive effects were studied. The effects of Co and inhomogeneity between dendrite core (DC) and interdendritic region (ID) on creep performance at 1100 °C and 137 MPa in a 4th generation Ni-SXs were systematically investigated. The results show that the Ni-SXs with 9 wt% Co has the longest creep lifetime. Co additions alleviate the overall element segregations between DC and ID, especially Re, Cr, and W. And reverse partitioning behavior of Co also changes the partitioning ratio of elements between γ and γ′ phases, resulting in the inhibition of TCP phases precipitation for most creep time to avoid excessive consumption of solid solution strengthening elements and local stress concentration. The decrease of the lattice constant of γ reduces lattice misfit between γ and γ′ with the addition of Co, leading to the enlargement of dislocation network spacing and less resistance for movement or shearing of dislocation. The decrease of γ′ solvus temperature with Co addition promotes the dissolution of γ′ at high working temperature, resulting in severe topological inversion of γ/γ′ microstructures at ID. In addition, the main creep cracks of all Ni-SXs appear at ID, so the inhomogeneity between DC and ID is concerned. • The precipitation of TCP phases are inhibited with Co addition, which is a basis of low-cost and low-density alloy design. • The comprehensive effects of Co on high temperature creep properties are investigated and an optimal Co content exists. • The increase of Co affected the γ′ phase content, lattice mismatch, element distribution and TCP phase. • The effect of Co on microstructures evolution varies at different creep stages. • The inhomogeneity between dendrite core and interdendritic region causes creep cracks originate from interdendritic region. [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]

[Display omitted] • The thermodynamic and dynamic factors influencing the nucleation and growth of topologically close-packed (TCP) phases are summarized in detail. • The possible mechanism of the interface structure affecting TCP phase growth is discussed. • The corresponding research directions of TCP phase precipitation and alloy design are proposed. The nucleation and growth of topologically close-packed (TCP) phases in Ni-based single crystal superalloys (SCs) are controlled by composition, temperature, time, interface structure and stress. The formation of TCP phases causes detrimental effects on the mechanical properties of SCs. Therefore, it is crucial to study the formation mechanism and control factors of TCP phases to develop new-generation Ni-based SCs. Different alloying elements influence the TCP phase nucleation by adjusting the chemical driving force. The interface structure determined by interface energy and strain energy mainly affects the growth mechanism and morphology of the TCP phase. Various temperature determines the driving force for TCP nucleation and diffusion rates of elements during TCP phase growth. Holding time is also crucial to the growth and evolution of TCP phases. Applied stress also has an impact on the precipitation of TCP phases. Evolution between different types of TCP phases depends on the temperature, composition and crystal structure of TCP phases. TCP phases damage the mechanical properties mainly by causing stress concentration and weak interface strength. The review aims to establish a link among TCP phase formation, alloy design and microstructure from the macroscopic view to the microscopic view, providing some perspectives for future research. [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]

This work investigates the effect of Ru on the solution heat treatment window of the Ni-based single crystal superalloy. The addition of the Ru influences the solidification microstructure and widens the window. The solidification process is established to occur in the sequence of γ (dendrite) → γ + γ' grid eutectic (inter-dendrite) → γ + γ' lamella eutectic (inter-dendrite) → γ' (inter-dendrite). This is followed by the γ → γ + γ' decomposition of the γ dendrite into the common channel-cuboid structure upon cooling. The solvus of γ' and the solidus of the alloy define the window. In alloys containing inter-dendrite eutectic, the window is in principle zero. In this case, only the dynamic window created by homogenization diffusion may allow heat treatment. Adding Ru decreases the elements' partition ratios between the dendrite core and dendrite edge regions. It also promotes the enrichment of Re at the γ/γ' phase interfaces, which helps to refine the γ + γ' channel-cuboid structure and reduce the differences in both the size and volume fraction of the γ' phase between dendrite core and dendrite edge. Ru is found to inhibit the formation of (Ta, X)C carbide. These help widen the solution treatment temperature window of the Ni-based single crystal alloy. [Display omitted] • The solidification of the Ni-based single crystal superalloy is established. • The addition of the Ru can widen the solution heat treatment window. • The metallurgical principle behind the window of solution heat treatment is explained. • The effect of Ru on the window and the microstructure in cross-scale is clarified. [ABSTRACT FROM AUTHOR]

As the blade material of engine, nickel-base single crystal superalloy has been subjected to complex service environment such as high temperature and alternating load for a long time. In this work, the mechanism of fatigue microcrack initiation and propagation in a nickel-based single crystal at 950 °C and 1050 °C was studied by using the in-situ scanning electron microscope high temperature fatigue test system. At 950 °C, the alloy deformation was controlled by slip and the crack shear γ/γ' phase cracking, showing Stage I mode. At 1050 °C, the alloy crack tearing occurred at the γ phase parallel to the loading direction and γ/γ' interface perpendicular to the loading direction and presents a Stage II mode perpendicular to the loading axis, then changes into Stage I in the accelerating stage. The deformation mechanism of fatigue cracking at two temperatures was compared. Besides, the influence of the microstructure defects on the fatigue crack behavior was discussed. The results show that the propagation of the microcrack below 100 μm shows evident fluctuations, which is closely related to the microstructure and the development stage of the fatigue crack. • The fatigue crack behavior of a nickel-base single crystal superalloy was investigated by in-situ SEM at 950 °C and 1050 °C. • The microscopic deformation mechanism of fatigue cracking at 950 °C and 1050 °C was revealed. • The effect of microstructure defects on the initiation and propagation behavior of fatigue cracks was discussed. [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]

The oxidation behavior of a fourth-generation nickel-based single crystal superalloy with different heat treatments were studied at 1100 °C in air. The specimens were divided into three groups, one as-cast group, and two heat-treated groups: solution treated and fully heat treated. The elemental distribution is mainly affected by the solution temperature, the higher the solution temperature, the more uniform the distribution of elements. Heat treatment can effectively reduce the difference in oxidation behavior between dendritic region and interdendritic region. However, due to the inability to form a continuous Al 2 O 3 layer, the oxidation resistance of heat-treated specimens degrades. • The elements distribution will affect the oxidation behavior of superalloys. • The Al content of the region will affect the morphology of the internal Al 2 O 3 layer. • Heat treatment can reduce the oxidation difference between dendritic region and interdendritic region. • After heat treatment, the alloy is more prone to large-scale oxide spalling. [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]

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]

[Display omitted] • Co alleviates large-scale heterogeneity of multiple microstructures of the alloys. • Co significantly reduces the partitioning coefficient of γ forming elements, which alleviates small-scale heterogeneity. • Co additions suppress TCP precipitation and increase microstructure stability. The effects of Co on multi-scale elemental distributions were studied in an advanced Ru-containing Ni-based single crystal superalloys. Two types scales of microstructural heterogeneities, the large-scale dendritic segregations and small-scale elemental partitions between γ/γ' phase were compared in as-cast, heat-treated and thermal-exposed alloys. The elemental homogeneities on both large and small scale were shown to be enhanced with Co additions, giving rise to the restricted precipitation of TCP phase. It is thus expected the potential role of Co to replace part of Ru in advanced superalloys. [ABSTRACT FROM AUTHOR]

The plastic deformation behavior of three various orientation specimens of a nickel-based single-crystal (SX) superalloy were investigated by in-situ electron back-scattered diffraction (EBSD) at room temperature. Tensile properties, slip morphology, the evolution of Schmid factor, lattice rotation, and local strain were thoroughly discussed. In [1 1 13] specimen, the interaction of multi slip behavior induced local strain concentration, which restricted the plasticity but enhanced the strain hardening. Due to the single slip behavior, lower tensile strength and higher elongation were discovered in [9 1 7] and [2 1 3] specimens. Furthermore, during the plastic deformation of [1 1 13] specimen, lattice rotation is confined around [0 0 1] pole and shows a dispersive distribution, which is triggered by the multi slip behavior. A modified Sachs model considering multi slip behavior has been developed to predict the lattice rotation, this model is also applicable to severely deformed grains in polycrystalline materials. [ABSTRACT FROM AUTHOR]

The structural and mechanical response of pure body-centered cubic (BCC) Nb under shock loading were systematically studied. Shock-induced orthorhombic (α") martensitic transformations were observed in single crystals Nb with different orientations, in which dense lenticular α" martensite variants distribute uniformly along different directions by forming a hierarchical structure. Neighbouring martensite variants share a {111}<110> α" twinning relationship between each other, and high-density dislocations are found distributing along the α"/BCC(β) interface. The formation of α" martensite was dominated by a mechanism of collinear shuffling of alternating {110} β planes along with <1 1 ¯ 0> β direction by a displacement δ. The collision between martensite variants along different direction induce abundant microcracks, with BCC-to-ω and BCC-to-FCC phase transformations occurring at the crack tips. These findings not only provide the experimental evidence of shock-induced α" martensitic transformation in pure BCC metals, but also link the microstructure interaction of materials to their macroscopic shock failure directly, which may have a broad impact on the study of shock deformation in different materials. [ABSTRACT FROM AUTHOR]

Creep properties of a 4th generation nickel-based single crystal superalloy (Ni-SX) are investigated at 1150 °C and 1100 °C. Fracture mechanism is revealed as competitive microcrack initiation induced by topologically close-packed (TCP) phase formation and creep inconsistency on dendritic structures showing the strong temperature-and-time dependent relations. At 1150 °C, alloy displays the high nucleation rate of TCP phases. Dense TCP particles dissolve the surrounding γ/γ' microstructures forming large depleted zone where is easily stress-concentrated. Dislocations are found to emit from the interface between TCP and depleted zone that promotes dislocation shearing and microcrack initiation in the large depleted zone, as well as the fracture of alloy. On contrary, alloy crept at 1100 °C suffers to relatively restricted TCP nucleation. But the longer creep time gives to larger size of TCP precipitates. Compared to alloy crept at 1150 °C, the depleted zone is much smaller that is not prone for stress concentration. For this creep inconsistency induced by dendritic segregation plays the main role in determining the creep properties. The larger local strain rate forms microcracks primarily in interdendritic region causing the final fracture. • Creep behaviors of a new 4th generation Ni-SX are compared at 1150 °C and 1100 °C. • Temperature-and-time dependent TCP precipitation and creep inconsistency affect the creep. • Depending on temperature, the two factors display competitive behaviors. • Higher temperature of 1150 °C enlarges the influence of TCP precipitation. • Creep inconsistency on dendritic structures dominants the creep at 1100 °C. [ABSTRACT FROM AUTHOR]