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This study explores the influence of thermo-mechanical behavior and microstructure on recovery and recrystallization in single-crystal superalloys during casting and subsequent solution heat treatment, using miniature testing. Here, the temporal evolution of resistance was measured using in situ electrothermal mechanical testing (ETMT) to track the process of recovery and recrystallization (RX). It was found that recrystallization is dominant only when recovery is incomplete and is dependent on both the history dependence of the strain path as well as the magnitude of the accumulated plastic strain. A precursor to recrystallization is the occurrence of subgrains and deformation twins on the sample surface, where a characteristic butterfly-type morphology of γ′ precipitates is always observed in highly strained regions. The migration of RX grain boundaries is accompanied by the elimination of lattice curvature associated with the density of geometrically necessary dislocations. Homogenized samples provide the most reliable results, while interpreting resistivity changes with recovery and recrystallization is more challenging when inhomogeneity (microsegregation, local variation of mechanical properties) in as-cast material prevails. [ABSTRACT FROM AUTHOR]

A suite of experimental tools and fast-acting, numerical-simulation techniques was used to quantify the precipitation behavior of three nickel-base superalloys: IN-100, LSHR, and 718. Experimental methods comprised differential scanning calorimetry (DSC) to establish the specific heat as a function of temperature and selected direct-resistance heating trials (using a Gleeble® machine) to obtain samples for microstructural analysis. For the DSC experiments, each alloy was cooled at a prescribed constant rate (between 5 and 20 K/min) after an initial soak/equilibration in the high-temperature, single-phase (supersolvus) temperature regime. On-heating DSC trials beginning at ambient temperature were also performed on alloy 718 in three different starting conditions: super-δ-solvus solution treated and water quenched (denoted as ST), solution treated and aged (STA), and solution treated and overaged (STOA). DSC results, revealing the thermal signatures associated with the kinetics of precipitation of γ′ (IN-100, LSHR) or γ′ and γ″ (718), were interpreted using a previously-developed fast-acting routine that treats concurrent nucleation, growth, coarsening, and dissolution. For these simulations, special attention was paid to various thermo-kinetic input parameters including equilibrium solvus-approach curves, bulk free energies of transformation, matrix-precipitate interface energies, and effective diffusivities. For the γ-γ′ superalloys (IN-100 and LSHR), estimates of precipitate volume fraction as a function of temperature from the specific-heat data revealed semi-quantitative agreement with simulation predictions. For the γ-γ′-γ″ superalloy (718), simulation predictions of precipitate volume fractions were converted to specific heat as a function of temperature and showed semi-quantitative agreement with the direct measurements. [ABSTRACT FROM AUTHOR]

Two in-situ test techniques were used to obtain insight into the isothermal precipitation kinetics of γ″ and γ′ in superalloy 718. The first method consisted of measurements of Young's modulus using a dynamic-resonance method (DRM), and the other comprised determination of the evolution of the lattice parameter of the γ-matrix phase via neutron diffraction. For both techniques, solution-treated-and-water-quenched samples were heated to a nominal test temperature of 923 K, 953 K, 1013 K, or 1053 K and held for a time of ~ 5 to 50 hours, at the end of which a near-steady condition in terms of an apparently-constant modulus/lattice parameter had been achieved. The observations from each test technique suggested sequential periods of rapid initial increase in volume fraction followed by a gradually-decreasing rate of change. The data were converted to transformed fraction as a function of time and interpreted in terms of phenomenological (JMAK) and mechanistic (nucleation-and-growth) models. From the former approach, Avrami exponents which decreased from approximately unity at the lower two temperatures to ~ 0.5 at the highest temperature, were deduced. The transformed fraction-versus-time behaviors were well replicated using fast-acting numerical simulations based on the mechanistic model. These simulations highlighted the competition between nucleation and growth in determining overall transformation kinetics. [ABSTRACT FROM AUTHOR]

A fast-acting, mean-field method for simulating precipitation of the γ′′ and γ′ phases during aging of superalloy 718 following super-delta-solvus solution treatment was formulated and validated using observations in the literature. The approach assumed classical (homogeneous) nucleation and diffusion-controlled growth (N&G) of disk/ellipsoidal-shaped-γ′′ and spherical-γ′ particles. For the γ′′ precipitates in particular, the evolution equations for both nucleation and growth incorporated corrections for the non-spherical shape, assuming a fixed aspect ratio. In addition, special attention was paid to the choice of input material properties for simulations. These parameters included the bulk free energies of transformation, particle-matrix (misfit) elastic strain energy (for γ′′), effective diffusivities, and the γ′′–γ and γ′–γ interface energies. The applicability of the diffusivities and interface energies chosen for the N&G simulations was established by their consistency in replicating previously measured rate constants for the diffusion-controlled coarsening of both γ′′ and γ′. The N&G formulation was discretized to obtain numerical (spreadsheet) solutions via the Kampmann–Wagner approach. Simulation results for the temporal evolution of volume fraction and average size of the precipitates showed good agreement with experimental measurements. The sensitivity of model predictions to various input parameters was also quantified. [ABSTRACT FROM AUTHOR]

Misfit stresses in the γ″-strengthened Ni-base superalloy Inconel 718 were calculated from the measured constrained misfit strain using Eshelby's inclusion method. The constrained misfit strains of the γ″ precipitates were measured using neutron diffraction at various temperatures with the aid of the stress-induced variant selection method. Eshelby tensor was calculated using the expressions for the case of anisotropic matrix given by Mura. Results show the presence of significant compressive misfit stresses in the γ″ precipitates with an anisotropic distribution, namely 3.0 GPa along the habit plane and 1.7 GPa along the plane normal direction at room temperature, and 2.0 and 1.2 GPa at 664 °C. The decrease in misfit stresses was due to the decrease in stiffness and the different coefficients of thermal expansion of the γ and γ″ phases. The average internal stresses in the γ matrix due to lattice misfit were found to be ~ 329 MPa at room temperature and ~ 186 MPa at 664 °C in tension. The possibility of relieving such high levels of misfit stresses in precipitates by loss of coherency during continued growth of precipitates is also discussed. [ABSTRACT FROM AUTHOR]

Polycrystalline Ni-base superalloy Inconel 718 derives the strengthening mainly from Ni3Nb γ″ phase. To investigate the evolution of lattice spacing of γ″ precipitates, in situ neutron diffraction experiments were performed during aging heat treatment of two Inconel 718 bar samples at 780 °C for 8 hours. One sample was aged with a negligible applied stress (5 MPa) and the other with an applied tensile stress of 300 MPa. The diffraction data demonstrate three stages of lattice spacing evolution due to compositional and morphological changes during aging. (1) Stage I, the γ lattice spacing decreases isotropically in the first hour of aging as the composition changes. (2) Stage II, the γ lattice spacing decreases and the γ″ lattice spacing increases between 1 and 5 hours of aging, at this stage compositional change on the lattice evolution weakens with aging time and the morphological change becomes comparable. (3) Stage III, as aging proceeds, compositional change is negligible, while morphological change is dominant; the γ lattice spacing decreases in the longitudinal direction but increases in the transverse direction; in contrast, the converse occurs in γ″ lattice spacing evolution. [ABSTRACT FROM AUTHOR]

The geometrical factor in freckle formation has rarely been taken into account. In this work, freckle formation in superalloy components is examined. It is found that freckle formation is subject to the effects of the edge and curvature. In polygonal casting sections, freckles are formed preferably on the convex edges. In the components with a curved contour, freckles are exclusively formed on the outward-curving surface having positive curvature. [ABSTRACT FROM AUTHOR]

Vaporization and its associated surface defect formation have become one of the most important challenges in manufacturing single-crystal components. During the kinetic-influenced casting and solution heat treatment of Ni-base superalloys, elements undergo processes of vaporization and deposition causing unpredictable defects. To quantitatively examine the vaporization phenomenon, partial vapor pressures of Ni, Al and Cr in Ni-base alloys were measured in the γ phase over the temperature range of 1473 K to 1650 K using Knudsen effusion mass spectrometry. Experimental results showed that the partial pressure of Al is about two orders of magnitude lower than that of Ni and five times lower than that of Cr, revealing that the vaporization of Al is almost negligible compared with those of Ni and Cr at solution heat treatment temperatures. Variation of partial pressures during homogenization of the as-cast Ni-base alloys was measured in long-term isothermal experiments at 1573 K. It was found that Cr vapor pressure decreases by a factor of two in the first 20 hours whereas the Ni and Al remain nearly constant. [ABSTRACT FROM AUTHOR]

γ″ diffraction peaks are hard to discern in neutron/X-ray diffraction patterns, hindering studies on the γ″-strengthened superalloys using in-situ diffraction. In this study, we propose a variant selection method to increase the intensity of γ″ peaks and to facilitate accurate fitting. The specific variants of γ″ are controlled by applying a 300 MPa tensile stress during aging at 790 °C for 5 hours. The interaction energy between the applied stress and the transformation strain of each γ″ variant differs, leading to an increase in the amount of the variants with a greater energy reduction at the expense of other variants. The enhanced variants result in greater γ″ peak intensities in neutron diffraction patterns, allowing both the Pawley refinement and single peak fitting to be performed. Lattice parameters of γ″ and γ phases, and lattice misfit between the two phases and volume fraction of γ″ are acquired. The uncertainties associated with the fitting maintain an acceptable level corresponding to 150 microstrains. The proposed variant selection method shows potential for studying the role of γ″ phase in Ni-base superalloys. [ABSTRACT FROM AUTHOR]

The evolution of eutectic morphologies following primary solidification has been studied in the refractory metal aluminide (Ta-Al-Fe, Nb-Al-Co, and Nb-Al-Fe) ternary systems. The undercooling accompanying solid growth, as related to the extended solute solubility in the primary and secondary phases can be used to account for the evolution of phase morphologies during ternary eutectic solidification. For small undercooling, the conditions of interfacial equilibrium remain valid, while in the case of significant undercooling when nucleation constraints occur, there is a departure from equilibrium leading to unexpected phases. In Ta-Al-Fe, an extended solubility of Fe in σ was observed, which was consistent with the formation of a halo of μ phase on primary σ. In Nb-Al-Co, a halo of C14 is formed on primary CoAl, but very limited vice versa. However, in the absence of a solidus projection it was not possible to definitively determine the extended solute solubility in the primary phase. In Nb-Al-Fe when nucleation constraints arise, the inability to initiate coupled growth of NbAl3 + C14 leads to the occurrence of a two-phase halo of C14 + Nb2Al, indicating a large undercooling and departure from equilibrium. [ABSTRACT FROM AUTHOR]

A three-stage mechanistic model for solidification cracking during TIG welding of steel is proposed from in situ synchrotron X-ray imaging of solidification cracking and subsequent analysis of fracture surfaces. Stage 1—Nucleation of inter-granular hot cracks: cracks nucleate inter-granularly in sub-surface where maximum volumetric strain is localized and volume fraction of liquid is less than 0.1; the crack nuclei occur at solute-enriched liquid pockets which remain trapped in increasingly impermeable semi-solid skeleton. Stage 2—Coalescence of cracks via inter-granular fracture: as the applied strain increases, cracks coalesce through inter-granular fracture; the coalescence path is preferential to the direction of the heat source and propagates through the grain boundaries to solidifying dendrites. Stage 3—Propagation through inter-dendritic hot tearing: inter-dendritic hot tearing occurs along the boundaries between solidifying columnar dendrites with higher liquid fraction. It is recommended that future solidification cracking criterion shall be based on the application of multiphase mechanics and fracture mechanics to the failure of semi-solid materials. [ABSTRACT FROM AUTHOR]

An analysis of the microstructure of the interdendritic regions in an as-cast third generation single-crystal nickel-base superalloy CMSX-10K has been carried out using automated serial sectioning with sequential focused ion beam (FIB) milling and image capture of the secondary electron image in a combined FIB–scanning electron microscope (SEM). Two interdendritic morphologies with vastly different γ/ γ′ spacing were identified; these are (1) fine γ/ γ′ morphology and (2) coarse cellular γ′ separated by narrow γ channels. The FIB results indicate that following primary solidification ( L → γ), solidification of the interdendritic region commences in areas that show the fine γ/ γ′ morphology, (1) on the γ dendrite lobe. This is followed by a gradual transition to growth of the coarse cellular γ/ γ′ channel structure, (2) which occur up to the termination of the solidification process. [ABSTRACT FROM AUTHOR]

A comparison has been made between the amount of microsegregation predicted by a numerical model and that found experimentally in Al-Cu alloys varying in composition between 1 and 8 wt pct Cu. A depleted region was predicted and observed experimentally near the Al2Cu. The depleted region was formed below the eutectic temperature and had a significant effect on the ordered composition-fraction plots, particularly for high alloy compositions. Although the fit between experiment and theory was reasonably good, it was concluded that it was necessary to propose that local equilibrium was not maintained between the phases in the solid-state reactions. [ABSTRACT FROM AUTHOR]