Characterization of High-purity Niobium Structures Fabricated Using the Electron Beam Melting Process

Additive Manufacturing (AM) refers to the varied set of technologies utilized for the fabrication of complex 3D components from digital data in a layer-by-layer fashion. The use of these technologies promises to revolutionize the manufacturing industry. The electron beam melting (EBM) process has been utilized for the fabrication of fully dense near-net-shape components from various metallic materials. This process, catalogued as a powder bed fusion technology, consists of the deposition of thin layers (50 - 120µm) of metallic powder particles which are fused by the use of a high energy electron beam and has been commercialized by Swedish company Arcam AB. Superconducting radio frequency (SRF) cavities are key components that are used in linear accelerators and other light sources for studies of elemental physics. Currently, cavity fabrication is done by employing different forming processes including deep-drawing and spinning. In both of the latter techniques, a feedstock high-purity niobium sheet with a thickness ranging from 3-4 mm is mechanically deformed and shaped into the desired geometry. In this manner, half cavities are formed that are later joined by electron beam welding (EBW). The welding step causes variability in the shape of the cavity and can also introduce impurities at the surface of the weld interface. The processing route and the purity of niobium are also of utmost importance since the presence of impurities such as inclusions or defects can be detrimental for the SRF properties of cavities. The focus of this research was the use of the EBM process in the manufacture of high purity niobium parts with potential SRF applications. Reactor grade niobium was plasma atomized and used as the precursor material for fabrication using EBM. An Arcam A2 system was utilized for the fabrication. The system had all internal components of the fabrication chamber replaced and was cleaned to prevent contamination of niobium powder. A mini-vat, developed at the W.M. Keck Center for 3D Innovation was used for fabrication due to the limited amount of niobium powder available. Sifting of the material for reuse was done inside a glovebox conditioned to sustain a positive pressure using nitrogen gas and help in delaying moisture adsorption by the powder. The initial step in the research was the optimization of the fabrication parameters to obtain nearly fully dense (% Relative density \u3e 99%) components followed by the fabrication of application-specific parts to be used for measuring mechanical and physical properties. Such parts, which included a probe or antenna measuring ~85mm tall, were used in the characterization of the thermal conductivity and the residual resistivity ratio of the material; both properties are important in SRF applications. The purity of the material was monitored at different stages from the niobium stock, to the plasma atomized powder, and finally, in the EBM-fabricated parts. For the niobium stock, niobium powder, and in EBM-fabricated parts, chemical analysis was performed using ICP fusion and LECO combustion. A residual gas analyzer (RGA) was used to monitor the vacuum environment during EBM fabrication. X-ray diffraction (XRD) was also used to assess the purity of EBM-fabricated niobium. A second milestone was the characterization of the tensile properties of EBM-fabricated niobium for the first time. These properties included the average yield and ultimate tensile strengths that measured 140MPa and 255MPa respectively. Measurements of the percent elongation were done using visual feedback from a video camera. Similarly, a boundary detection algorithm was used to approximate the percent reduction in area, because only rectangular specimens were available for experimentation. The measured values averaged 34% elongation and 98% reduction in area. Microscopy was also employed to characterize the microstructure of the EBM niobium and SEM images of the fractured specimens utilized in a fractography analysis. The microstructure observed in the horizontal plane of reference was of nearly equiaxed grains with a measured size of roughly 250µm. In the vertical plane, the microstructure was of columnar grains that elongated parallel to the EBM build direction. The fractography images revealed the ductile nature of the material with the presence of micro-void coalescence in the fracture surface. The mechanical properties and microstructure of EBM-fabricated niobium were compared against those of reactor grade niobium. As will be detailed later, the reactor grade niobium had yield and ultimate tensile strengths of 135MPa and 205MPa respectively. The percent elongation was measured at 45.2% and the percent reduction in area at 97.2% for the reactor grade niobium