Effect of Layer Thickness and Heat Treatment on Microstructure and Mechanical Properties of Alloy 625 Manufactured by Electron Beam Powder Bed Fusion.

This research program investigated the effects of layer thickness (50 µm and 100 µm) on the microstructure and mechanical properties of electron beam powder bed fusion (EBPBF) additive manufacturing of Inconel 625 alloy. The as-built 50 µm and 100 µm layer thickness components were also heat treated at temperatures above 1100 °C which produced a recrystallized grain structure containing annealing twins in the 50 µm layer thickness components, and a duplex grain structure consisting of islands of very small equiaxed grains dispersed in a recrystallized, large-grain structure containing annealing twins. The heat-treated components of the microstructures and mechanical properties were compared with the as-built components in both the build direction (vertical) and perpendicular (horizontal) to the build direction. Vickers microindentation hardness (HV) values for the vertical and horizontal geometries averaged 227 and 220 for the as-built 50 µm and 100 µm layer components, respectively, and 185 and 282 for the corresponding heat-treated components. The yield stress values were 387 MPa and 365 MPa for the as-built horizontal and vertical 50 µm layer geometries, and 330 MPa and 340 MPa for the as-built 100 µm layer components. For the heat-treated 50 µm components, the yield stress values were 340 and 321 MPa for the horizontal and vertical geometries, and 581 and 489 MPa for the 100 µm layer components, respectively. The elongation for the 100 µm layer as-built horizontal components was 28% in contrast with 65% for the corresponding 100 µm heat-treated layer components, an increase of 132% for the duplex grain structure.

Investigation of Microstructure and Mechanical Properties for Ti-6Al-4V Alloy Parts Produced Using Non-Spherical Precursor Powder by Laser Powder Bed Fusion.

An unmodified, non-spherical, hydride-dehydride (HDH) Ti-6Al-4V powder having a substantial economic advantage over spherical, atomized Ti-6Al-4V alloy powder was used to fabricate a range of test components and aerospace-related products utilizing laser beam powder-bed fusion processing. The as-built products, utilizing optimized processing parameters, had a Rockwell-C scale (HRC) hardness of 44.6. Following heat treatments which included annealing at 704 °C, HIP at ~926 °C (average), and HIP + anneal, the HRC hardnesses were observed to be 43.9, 40.7, and 40.4, respectively. The corresponding tensile yield stress, UTS, and elongation for these heat treatments averaged 1.19 GPa, 1.22 GPa, 8.7%; 1.03 GPa, 1.08 GPa, 16.7%; 1.04 GPa, 1.09 GPa, 16.1%, respectively. The HIP yield strength and elongation of 1.03 GPa and 16.7% are comparable to the best commercial, wrought Ti-6Al-4V products. The corresponding HIP component microstructures consisted of elongated small grains (~125 microns diameter) containing fine, alpha/beta lamellae.

Effects of Postprocess Hot Isostatic Pressing Treatments on the Mechanical Performance of EBM Fabricated TI-6Al-2Sn-4Zr-2Mo.

An essentially fully acicular alpha-prime martensite within an equiaxed grain structure was produced in an Electron Beam Melting (EBM)-fabricated Ti-6Al-2Sn-4Zr-2Mo (Ti6242) alloy using two different Arcam EBM machines: An A2X system employing tungsten filament thermionic electron emission, and a Q20 system employing LaB6 thermionic electron emission. Post-process Hot Isostatic Pressing (HIP) treatment for 2 h at 850, 950, and 1050 °C resulted in grain refinement and equiaxed grain growth along with alpha-prime martensite decomposition to form an intragranular mixture of acicular martensite and alpha at 850 °C, and acicular alpha phase at 950 and 150 °C, often exhibiting a Widmanstätten (basketweave) structure. The corresponding tensile yield stress and ultimate tensile strength (UTS) associated with the grain growth and acicular alpha evolution decreased from ~1 and ~1.1 GPa, respectively, for the as-fabricated Ti6242 alloy to ~0.8 and 0.9 GPa, respectively, for HIP at 1050 °C. The optimum elongation of ~15-16% occurred for HIP at 850 °C; for both EBM systems. Because of the interactive role played by equiaxed grain growth and the intragrain, acicular alpha microstructures, the hardness varied only by ~7% between 41 and 38 HRC.

Interplay between cellular activity and three-dimensional scaffold-cell constructs with different foam structure processed by electron beam melting.

The cellular activity, biological response, and consequent integration of scaffold-cell construct in the physiological system are governed by the ability of cells to adhere, proliferate, and biomineralize. In this regard, we combine cellular biology and materials science and engineering to fundamentally elucidate the interplay between cellular activity and interconnected three-dimensional foamed architecture obtained by a novel process of electron beam melting and computational tools. Furthermore, the organization of key proteins, notably, actin, vinclulin, and fibronectin, involved in cellular activity and biological functions and relationship with the structure was explored. The interconnected foamed structure with ligaments was favorable to cellular activity that includes cell attachment, proliferation, and differentiation. The primary rationale for favorable modulation of cellular functions is that the foamed structure provided a channel for migration and communication between cells leading to highly mineralized extracellular matrix (ECM) by the differentiating osteoblasts. The filopodial interaction amongst cells on the ligaments was a governing factor in the secretion of ECM, with consequent influence on maturation and mineralization.

Next generation orthopaedic implants by additive manufacturing using electron beam melting.

This paper presents some examples of knee and hip implant components containing porous structures and fabricated in monolithic forms utilizing electron beam melting (EBM). In addition, utilizing stiffness or relative stiffness versus relative density design plots for open-cellular structures (mesh and foam components) of Ti-6Al-4V and Co-29Cr-6Mo alloy fabricated by EBM, it is demonstrated that stiffness-compatible implants can be fabricated for optimal stress shielding for bone regimes as well as bone cell ingrowth. Implications for the fabrication of patient-specific, monolithic, multifunctional orthopaedic implants using EBM are described along with microstructures and mechanical properties characteristic of both Ti-6Al-4V and Co-29Cr-6Mo alloy prototypes, including both solid and open-cellular prototypes manufactured by additive manufacturing (AM) using EBM.

Comparative microstructures and cytotoxicity assays for ballistic aerosols composed of micrometals and nanometals: respiratory health implications.

Aerosol particulates collected on filters from ballistic penetration and erosion events for W-Ni-Co and W-Ni-Fe kinetic energy rod projectiles penetrating steel target plates were observed to be highly cytotoxic to human epithelial A549 lung cells in culture after 48 hours of exposure. The aerosol consisted of micron-sized Fe particulates and nanoparticulate aggregates consisting of W, Ni or W, Co, and some Fe, characterized by scanning electron microscopy and transmission electron microscopy, and using energy-dispersive (X-ray) spectrometry for elemental analysis and mapping. Cytotoxic assays of manufactured micron-sized and nanosized metal particulates of W, Ni, Fe, and Co demonstrated that, consistent with many studies in the literature, only the nanoparticulate elements demonstrated measurable cytotoxicity. These results suggest the potential for very severe, short-term, human toxicity, in particular to the respiratory system on inhaling ballistic aerosols.

Evaluation of Titanium Alloys Fabricated Using Rapid Prototyping Technologies-Electron Beam Melting and Laser Beam Melting.

This study characterized properties of Ti-6Al-4V ELI (extra low interstitial, ASTM grade 23) specimens fabricated by a laser beam melting (LBM) and an electron beam melting (EBM) system for dental applications. Titanium alloy specimens were made into required size and shape for each standard test using fabrication methods. The LBM specimens were made by an LBM machine utilizing 20 µm of Ti-6Al-4V ELI powder. Ti-6Al-4V ELI specimens were also fabricated by an EBM using 40 µm of Ti-6Al-4V ELI powder (average diameter, 40 µm: Arcam ABÒ) in a vacuum. As a control, cast Ti-6Al-4V ELI specimens (Cast) were made using a centrifugal casting machine in an MgO-based mold. Also, a wrought form of Ti-6Al-4V ELI (Wrought) was used as a control. The mechanical properties, corrosion properties and grindability (wear properties) were evaluated and data was analyzed using ANOVA and a non-parametric method (α = 0.05). The strength of the LBM and wrought specimens were similar, whereas the EBM specimens were slightly lower than those two specimens. The hardness of both the LBM and EBM specimens was similar and slightly higher than that of the cast and wrought alloys. For the higher grindability speed at 1,250 m/min, the volume loss of Ti64 LBM and EBM showed no significant differences among all the fabrication methods. LBM and EBM exhibited favorable results in fabricating dental appliances with excellent properties as found for specimens made by other fabricating methods.

Open-Cellular Co-Base and Ni-Base Superalloys Fabricated by Electron Beam Melting.

Reticulated mesh samples of Co-29Cr-6Mo alloy and Ni-21Cr-9Mo-4Nb alloy (625) and stochastic foam samples of Co-29Cr-6Mo alloy fabricated by electron beam melting were characterized by optical metallography, and the dynamic stiffness (Young's modulus) was measured by resonant frequency analysis. The relative stiffness (E/Es) versus relative density (ρ/ρs) plotted on a log-log basis resulted in a fitted straight line with a slope n ≅ 2, consistent with that for ideal open cellular materials.

Microstructural and Process Characterization of Conductive Traces Printed from Ag Particulate Inks.

Conductive inks are key enablers for the use of printing techniques in the fabrication of electronic systems. Focus on the understanding of aspects controlling the electrical performance of conductive ink is paramount. A comparison was made between microparticle Ag inks and an Ag nanoparticle ink. The microstructures resulting from thermal cure processes were characterized morphologically and also in terms of their effect on the resistivity of printed traces. For microparticle inks, the variability of resistivity measurements between samples as defined by coefficient of variation (CV) was greater than 0.1 when the resistivity was 10 to 50 times that of bulk Ag. When the resistivity was lower (~1.4 times that of bulk Ag) the CV of sample sets was less than 0.1. In the case of the nanoparticle ink, resistivity was found to decrease by a factor ranging from 1.2 to 1.5 after doubling the amount of layers printed prior to curing though it was expected to remain the same. Increasing the amount of layers printed also enhanced the sintering process.

Characterization and cytotoxic assessment of ballistic aerosol particulates for tungsten alloy penetrators into steel target plates.

The nature and constituents of ballistic aerosol created by kinetic energy penetrator rods of tungsten heavy alloys (W-Fe-Ni and W-Fe-Co) perforating steel target plates was characterized by scanning and transmission electron microscopy. These aerosol regimes, which can occur in closed, armored military vehicle penetration, are of concern for potential health effects, especially as a consequence of being inhaled. In a controlled volume containing 10 equispaced steel target plates, particulates were systematically collected onto special filters. Filter collections were examined by scanning and transmission electron microscopy (SEM and TEM) which included energy-dispersive (X-ray) spectrometry (EDS). Dark-field TEM identified a significant nanoparticle concentration while EDS in the SEM identified the propensity of mass fraction particulates to consist of Fe and FeO, representing target erosion and formation of an accumulating debris field. Direct exposure of human epithelial cells (A549), a model for lung tissue, to particulates (especially nanoparticulates) collected on individual filters demonstrated induction of rapid and global cell death to the extent that production of inflammatory cytokines was entirely inhibited. These observations along with comparisons of a wide range of other nanoparticulate species exhibiting cell death in A549 culture may suggest severe human toxicity potential for inhaled ballistic aerosol, but the complexity of the aerosol (particulate) mix has not yet allowed any particular chemical composition to be identified.

Cytotoxicity and reactive oxygen species generation from aggregated carbon and carbonaceous nanoparticulate materials.

We have investigated the cytotoxicity and reactive oxygen species (ROS) generation for indoor and outdoor soots: candle, wood, diesel, tire, and natural gas burner soots--along with surrogate black carbon, various multiwall carbon nanotube aggregate materials, TiO2 (anatase) and chrysotile asbestos as reference materials. All soots were observed utilizing TEM and FESEM to be composed of aggregated, primary spherules (20-80 nm diameter) forming complex, branched fractal structures. These spherules were composed of intercalated, turbostratic arrangements of curved graphene fragments with varying concentrations ofpolycyclic aromatic hydrocarbon (PAH) isomers. In vitro cultures with an immortalized human lung epithelial carcinoma cell line (A549) treated with these materials showed decreased cell viability and variations in ROS production, with no correlations to PAH content. The data demonstrate that soots are cytotoxic and that cytotoxicity is not related to PAH content but is related to ROS generation, suggesting that soot induces cellular oxidative stress and that cell viability assays can be indicators of ROS production.

Utilization of selected area electron diffraction patterns for characterization of air submicron particulate matter collected by a thermophoretic precipitator.

A thermophoretic precipitator (TP) that uses a novelty of direct sampling of ambient air particulate matter (PM) onto transmission electron microscopy (TEM) grids was designed and utilized to determine its potential applicability for the collection and consequent qualitative analyses of representative PM in the air, especially those with aerodynamic diameter less than 1 microm (PM1.0). After a calibration process, preliminary field tests were performed under different weather conditions, locations, and time frames. TEM, selected area electron diffraction (SAED), and electron energy-dispersive X-ray spectrometry (EDS) analyses were performed on individual samples, and chemical species were analyzed. During this investigation, individual air PM with different sizes ranging from 10 microm to 10 nm for TEM analysis was collected. Two observations were made: (1) a large fraction of collected particulates were aggregates of very small particles of both organic and inorganic origin, and (2) a large fraction of the collected particulates were crystalline or polycrystalline. This study has demonstrated, by utilization of SAED patterns from TEM on air particles collected by a TP, the potential to analyze and identify individual air PM in a nanometer regime qualitatively by combining SAED and EDS data.