Additive manufacturing of superalloys offers new opportunities for alloy design but also poses significant processing difficulties. While the γ′ phase is responsible for the excellent hightemperature resistance of these alloys, it also induces cracking by precipitation hardening during manufacturing. Using small-angle X-ray scattering, we characterized the dynamic precipitation, dissolution, coarsening, and morphological evolution of the γ′ phase in situ during simulated additive manufacturing conditions. For this purpose, a CMSX-4 cylinder was subjected to cyclic heat treatment with heating and quenching rates up to 300 K/s. A specialized setup employing aluminum lenses to focus the X-ray beam was utilized to extend the q-range to small scattering vectors up to 0.035 nm-1. It was shown that the γ′ phase precipitates extremely fast without any measurable undercooling but remains below the equilibrium fraction throughout the process. Coarsening is readily measurable over timespans of only several seconds. A fraction of the γ′ phase that was dissolved during heating reprecipitated by forming new particles instead of growing on already existing precipitates. The findings provide new insight into the dynamic behavior of the γ′ phase during additive manufacturing and may prove valuable in designing new superalloys and processing strategies for additive manufacturing.
Additive manufacturing (AM) of superalloys has been attracting increasing interest. While most studies focus on the processability and mechanical properties of the finished product, it is also necessary to understand the phase transformations during the consecutive melting processes. Herein, the precipitation and dissolution of the γ′ phase in the Ni‐base superalloy CMSX‐4 in a selective laser melting process is reported. These phase transformations are studied in situ by small‐angle X‐ray scattering (SAXS) during AM. Concurrent wide‐angle X‐ray scattering (WAXS) provides information on the evolution of lattice parameters and temperature during the process. Additional thermal and thermodynamic simulations are carried out to support the experiments. The investigations are focused on the influence of different beam scanning strategies as well as the effect of laser power and scanning speed on the phase transformation dynamics. Due to the high cooling and heating rates inherent to AM, phase transformations occur far off equilibrium. Both precipitation and dissolution of γ′ phase are observed. The scan strategies are shown to have a considerable effect on the phase transformation dynamics, which exceed the impact of the beam parameters. The capability of combined SAXS and WAXS for the in situ study of phase transformations in AM processes is demonstrated.
In this work, we investigated the viability of established hot cracking models for numerically based development of crack-resistant nickel-base superalloys with a high γ′ volume fraction for additive manufacturing. Four cracking models were implemented, and one alloy designed for reduced cracking susceptibility was deduced based on each cracking criterion. The criteria were modeled using CALPHAD-based Scheil calculations. The alloys were designed using a previously developed multi-criteria optimization tool. The commercial superalloy Mar-M247 was chosen as the reference material. The alloys were fabricated by arc melting, then remelted with laser and electron beam, and the cracking was assessed. After electron beam melting, solidification cracks were more prevalent than cold cracks, and vice versa. The alloys exhibited vastly different crack densities ranging from 0 to nearly 12 mm−1. DSC measurements showed good qualitative agreement with the calculated transition temperatures. It was found that the cracking mechanisms differed strongly depending on the process temperature. A correlation analysis of the measured crack densities and the modeled cracking susceptibilities showed no clear positive correlation for any crack model, indicating that none of these models alone is sufficient to describe the cracking behavior of the alloys. One experimental alloy showed an improved cracking resistance during electron beam melting, suggesting that further development of the optimization-based alloy design approach could lead to the discovery of new crack-resistant superalloys.
The high flux combined with the high energy of the monochromatic synchrotron radiation available at modern synchrotron facilities offers vast possibilities for fundamental research on metal processing technologies. Especially in the case of laser powder bed fusion (LPBF), an additive manufacturing technology for the manufacturing of complex-shaped metallic parts, in situ methods are necessary to understand the highly dynamic thermal, mechanical, and metallurgical processes involved in the creation of the parts. At PETRA III, Deutsches Elektronen-Synchrotron, a customized LPBF system featuring all essential functions of an industrial LPBF system, is used for in situ x-ray diffraction research. Three use cases with different experimental setups and research questions are presented to demonstrate research opportunities. First, the influence of substrate pre-heating and a complex scan pattern on the strain and internal stress progression during the manufacturing of Inconel 625 parts is investigated. Second, a study on the nickel-base superalloy CMSX-4 reveals the formation and dissolution of γ′ precipitates depending on the scan pattern in different part locations. Third, phase transitions during melting and solidification of an intermetallic γ-TiAl based alloy are examined, and the advantages of using thin platelet-shaped specimens to resolve the phase components are discussed. The presented cases give an overview of in situ x-ray diffraction experiments at PETRA III for research on the LPBF technology and provide information on specific experimental procedures.
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