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Eingeladener Vortrag
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Experimental study on M23C6 nucleation and growth mechanisms in Ni-base superalloy single crystals
(2017)
The addition of carbon to Ni-base superalloy single crystals has been increasingly carried out to improve low angle grain boundary (LAGB) resistance and castability. Consequently, the precipitation of carbides is highly probable during long-term application of components subjected to higher temperatures (> 1000 °C). While the view on the role of carbides as strengthening or detrimental is polemical, their inevitable increased presence in carbon-doped alloys must be addressed. In the present work, the evolution of M23C6 carbides forming in the commercial grade Ni-base superalloy LEK 94 during high-temperature and low-stress creep exposure is assessed. Although carbon is not intentionally added to the LEK 94 alloy, it admits up to 0.1 at. %, which together with the high content of M23C6-forming transition metals, leads to their precipitation. The precipitation is induced here during creep experiments at 1020 °C and a nominal applied stress of 160 MPa along [001]. The correlation of precipitation and external load is carried out by evaluating the carbides in the gage section of parallel and circularly notched cylindrical samples, as well as in their heads. Characterization is made by transmission electron microscopy (TEM). Although primary MC carbides form mostly in interdendritic regions during casting, high temperature exposure induces M23C6 carbide nucleation especially in the γ phase of dendritic regions, where a stronger partitioning of refractory elements is present. The carbides have a needle shape with their main axis on 〈100〉 and a cube-on-cube orientation relationship. They present incoherent {100} facets along their elongated region and semi-coherent {111} facets at their ends. Their nucleation and growth mechanisms are discussed based on microstructural observation under different experimental conditions.
The present work describes the shear creep behavior of the superalloy LEK 94 at temperatures between 980 and 1050 °C and shear stresses between 50 and 140 MPa for loading on the macroscopic crystallographic shear system (MCSS) (011)[01-1]. The strain rate versus strain curves show short primary and extended secondary creep regimes. We find an apparent activation energy for creep of Qapp = 466 kJ/mol and a Norton-law stress exponent of n = 6. With scanning transmission electron microscopy, we characterize three material states that differ in temperature, applied stress, and accumulated strain/time. Rafting develops perpendicular to the maximum principal stress direction, gamma channels fill with dislocations, superdislocations cut gamma' particles, and dislocation networks form at gamma/gamma' interfaces. Our findings are in agreement with previous results for high-temperature and low-stress [001] and [110] tensile creep testing, and for shear creep testing of the superalloys CMSX-4 and CMSX-6 on the MCSSs (111)[01-1] and (001)[100]. The parameters that characterize the evolving gamma/gamma' microstructure and the evolving dislocation substructures depend on creep temperature, stress, strain, and time.
The realistic description of plastic deformation caused by dislocations demands the representative measurement of their features, e.g., Burgers vector, slip plane, line direction and density. In the case of bulk deformation of technical alloys, reliable data must be ensured for large regions. Nonetheless, the (thin) filiform nature of dislocations and also the heterogeneity in some microstructures additionally require flexible analysis techniques that resolve the details of their interactions. Strong and clear channeling contrasts, faint extinction contours and the absence of chromatic aberration make scanning transmission electron microscopy (STEM) an ideal imaging mode in wide and thick regions of TEM foils, as opposed to conventional (C)TEM. It is the purpose of this contribution to show how STEM can be applied for quantitative measurement of dislocation features. Furthermore, a new tool will be presented, which enables the three-dimensional (3D) reconstruction, visualization and quantification of dislocation densities and directions from stereo-pairs. The application of these techniques will be shown on a monocrystalline Ni-base superalloy, an important class of structural materials that has been implemented in the first row blades of gas turbines. The examples are extracted from specimens subjected to creep deformation at high temperature and low stress under various macroscopic deformation geometries. The spacial and angular accuracy are discussed as well as possible sources of error.
The demand for improved castability and low angle grain boundary (LAGB) resistance has led to the addition of low contents of e.g., B, Hf, Zr or C, into large industrial gas turbine components made of Ni-base superalloy single crystals (SXs). Due to the long-term application of Ni-base superalloy SX components in the temperature regime > 1000 °C, the formation of carbides is highly probable, which could jeopardize mechanical properties, such as high cycle fatigue. In the present contribution, the effect of internal and external stresses on the nucleation and growth characteristics of M23C6 carbides is investigated. Creep experiments are performed on the Ni-base superalloy SX LEK 94, which shows a low C concentration (= 0.1 at. %), at 1020 °C under parallel and circularly notched tensile specimens at a nominal stress of 160 MPa in the crystallographic direction [001]. The carbides are then characterized via scanning (S) and transmission (T) electron microscopy (EM). Nucleation is enhanced in the dendritic cores, often as coalesced colonies, extending over micrometers within M-rich (M: Cr, Re, W, Mo) γ channels. Lath shapes with facets on {100} (parallel to growth direction) and {111} are common. These facets exist since early stages (Fig.1a) and later develop misfit dislocations (Fig.1b), preserving the orientation relationship {100}γ || {100}M23C6. Fig. 1c shows a region from the creep gage, where carbides interact with superdislocations in the γ’ phase. Possible mechanisms are discussed.