Controlling microstructural evolution in metallic additive manufacturing (AM) is difficult, especially in producing refined as-built grains instead of coarse, directional grains. Traditional solutions involve adding inoculants to AM feedstocks, but titanium (Ti) alloys cannot employ this approach without producing detrimental secondary phases. Ti-Cu (Ti-copper) alloys offer a solution through constitutional supercooling and/or solid state thermal cycling under AM conditions. This work analyzes a compositionally graded directed energy deposition (DED) Ti-Cu build, single-melt laser tracks, and dilatometric heat treatments to evaluate if, when, and by what mechanism(s) microstructural refinement occurs. Refinement by inoculation of unmelted powder particles was also considered. Constitutional supercooling produced no net microstructural refinement as any equiaxed dendrites which form are remelted with new deposition. This finding agreed with solidification modeling of powder bed fusion-laser beam (PBF-LB) and DED builds. Solid state thermal cycling refined microstructures only during ex-situ dilatometric heat treatments, suggesting build parameter optimization is needed to achieve refinement in-situ. Accidental heterogeneous nucleation on unmelted Ti powder, originating from the different thermophysical properties of Ti and Cu, provided the most significant microstructural refinement. This work systematically assesses the microstructural refinement mechanisms of Ti-Cu in AM builds and offers insights into microstructural control in eutectoid alloys.
Tin-lead-antimony (50Sn–47Pb–3Sb wt.%) soldered assemblies were mechanically tested approximately 30 years after initial production and found to have solder joints of reduced strength. The microstructure of this solder alloy exhibits a ternary eutectic structure with Sn-rich, Pb-rich, and SnSb phases. Accelerated aging was performed to evaluate solder microstructural coarsening and associated strength of laboratory solder joints to correlate these properties to the “naturally aged” solder joints. Isothermal aging was conducted at room temperature, 55, 70, 100, and 135 °C and aging times that ranged from 0.1 to 365 days. The coarsening kinetics of the Pb-rich phase were determined through optical microscopy and image analysis methods established in previous studies on binary Sn–Pb solder. A kinetic equation was developed with time exponent n of 0.43 and activation energy of 24000 J/mol, suggesting grain boundary diffusion or other fast diffusion pathways controlling the microstructural evolution. Compression testing and Vickers microhardness showed significant strength loss within the first 20–30 days after soldering; then, the microstructure and mechanical properties changed more slowly over long periods of time. Further, by combining accelerated aging data and the microstructure-based kinetics, strength predictions were made that match well with the properties of the actual soldered assemblies naturally aged for 30 years. However, aging at the highest temperature of 135 °C produced anomalous behavior suggesting that extraneous aging mechanisms are active. Therefore, data obtained at this temperature or higher should not be used. Overall, the combined microstructural and mechanical property methods used in this study confirmed that the observed reduction in strength of ~ 30-year-old solder joints can be accounted for by the microstructural coarsening that takes place during long-term solid-state aging.
Tin-lead-antimony (50Sn–47Pb–3Sb wt.%) soldered assemblies were mechanically tested approximately 30 years after initial production and found to have solder joints of reduced strength. The microstructure of this solder alloy exhibits a ternary eutectic structure with Sn-rich, Pb-rich, and SnSb phases. Accelerated aging was performed to evaluate solder microstructural coarsening and associated strength of laboratory solder joints to correlate these properties to the “naturally aged” solder joints. Isothermal aging was conducted at room temperature, 55, 70, 100, and 135 °C and aging times that ranged from 0.1 to 365 days. The coarsening kinetics of the Pb-rich phase were determined through optical microscopy and image analysis methods established in previous studies on binary Sn–Pb solder. A kinetic equation was developed with time exponent n of 0.43 and activation energy of 24000 J/mol, suggesting grain boundary diffusion or other fast diffusion pathways controlling the microstructural evolution. Compression testing and Vickers microhardness showed significant strength loss within the first 20–30 days after soldering; then, the microstructure and mechanical properties changed more slowly over long periods of time. Further, by combining accelerated aging data and the microstructure-based kinetics, strength predictions were made that match well with the properties of the actual soldered assemblies naturally aged for 30 years. However, aging at the highest temperature of 135 °C produced anomalous behavior suggesting that extraneous aging mechanisms are active. Therefore, data obtained at this temperature or higher should not be used. Overall, the combined microstructural and mechanical property methods used in this study confirmed that the observed reduction in strength of ~ 30-year-old solder joints can be accounted for by the microstructural coarsening that takes place during long-term solid-state aging.
Investigations of mechanical shear driven organic film formation, or tribofilms, on catalytic metal surfaces in sliding electrical contacts date back to Hermance and Egan's seminal work on mated palladium contacts. In this report we describe investigations of tribofilm formation from outgassing epoxy vapors, consisting of multiple siloxane species, and from isolated constituent species including octamethyltrisiloxane (OMTS). Experiments performed in varying vapor concentrations of OMTS resulted in the formation of tribopolymer films with similar morphology and impact on electrical contact resistance (ECR) as previously published results of sliding electrical contacts in similar conditions submerged in higher molecular weight polymethyldisiloxane (PDMS) fluid. Infrared (IR) spectroscopy was used to confirm the characteristic signatures of siloxanes and silanes in tribopolymer deposits found in wear scars formed in OMTS. Comparisons to prior studies also showed that the films formed from outgassing epoxy vapor constituents (including OMTS and a multitude of other species) have similar characteristics to the silicon-carbon-oxygen (Si-C-O) films previously found to form in high molecular weight PDMS fluid-filled devices. Tribopolymer formation was demonstrated for a range of electrical contact alloy mated pairs (Paliney-7, Neyoro-G, NiPtRe). Experiments in increasing concentrations of OMTS vapor showed that a persistent tribofilm is rapidly formed under cyclic sliding contact shear that can interrupt electrical current, with a formation rate that increases with increasing concentration. Overall, this work demonstrates the ease with which trace organics can promote the formation of insulating tribopolymer films in electrical contacts and factors that can influence their growth.
Soft-magnetic alloys exhibit exceptional functional properties that are beneficial for a variety of electromagnetic applications. These alloys are conventionally manufactured into sheet or bar forms using well-established insgot metallurgy practices that involve hot- and cold-working steps. However, recent developments in process metallurgy have unlocked opportunities to directly produce bulk soft-magnetic alloys with improved, and often tailorable, structure–property relationships that are unachievable conventionally. The emergence of unconventional manufacturing routes for soft-magnetic alloys is largely motivated by the need to improve the energy efficiency of electromagnetic devices. In this review, literature that details emerging manufacturing approaches for soft-magnetic alloys is overviewed. This review covers (1) severe plastic deformation, (2) recent advances in melt spinning, (3) powder-based methods, and (4) additive manufacturing. These methods are discussed in comparison with conventional rolling and bar processing. Perspectives and recommended future research directions are also discussed.
A survey of cadmium plated field return hardware showed ubiquitous cadmium whisker growth. The most worn and debris-covered hardware showed the densest whisker growth. Whiskers were often found growing in agglomerates of nodules and whiskers. The hardware was rinsed with alcohol to transfer whiskers and debris from the hardware to a flat stub. Fifty whiskers were studied individually by scanning electron microscopy (SEM), including energy dispersive spectroscopy (EDS) and electron backscatter diffraction (EBSD). Most of the whiskers were single crystal, though three were found to contain grain boundaries at kinks. The whiskers ranged from 5 to 600 μm in length and 80 pct showed a <1 ¯ 2 1 ¯ 0> type growth direction. This growth direction facilitates the development of low energy side faces of the whisker, (0001) and {1010}.
The mechanical performance of an Fe-Co intermetallic alloy processed by laser powder bed fusion (L-PBF) and laser directed energy deposition (L-DED) additive manufacturing is compared. L-PBF material was characterized by high strength (500–550 MPa) and high ductility (35%) in tension, corresponding to a ~250% increase in strength and an order-of-magnitude improvement in ductility relative to conventional material. Conversely, L-DED material exhibited similarly poor tensile properties to the conventional wrought alloy, with low strength (200–300 MPa) and low ductility (0–2.7%). The disparity in properties between L-PBF and L-DED material is discussed in the context of the fundamental differences between manufacturing methods.
This study employs nonlinear ultrasonic techniques to track microstructural changes in additively manufactured metals. The second harmonic generation technique based on the transmission of Rayleigh surface waves is used to measure the acoustic nonlinearity parameter, β. Stainless steel specimens are made through three procedures: traditional wrought manufacturing, laser-powder bed fusion, and laser engineered net shaping. The β parameter is measured through successive steps of an annealing heat treatment intended to decrease dislocation density. Dislocation density is known to be sensitive to manufacturing variables. In agreement with fundamental material models for the dislocation-acoustic nonlinearity relationship in the second harmonic generation, β drops in each specimen throughout the heat treatment before recrystallization. Geometrically necessary dislocations (GNDs) are measured from electron back-scatter diffraction as a quantitative indicator of dislocations; average GND density and β are found to have a statistical correlation coefficient of 0.852 showing the sensitivity of β to dislocations in additively manufactured metals. Moreover, β shows an excellent correlation with hardness, which is a measure of the macroscopic effect of dislocations.
