The ability to make components from copper and copper alloys via additive manufacturing is spurring a range of novel applications. Although the high thermal conductivity of copper presents challenges for direct AM processes, fully dense copper components with complex geometries have been demonstrated. Of particular interest is the ability to use AM methods to fabricate internal cooling channels and mesh structures to optimize thermal management. This article describes feasibility studies to evaluate AM processing of copper parts.
Tungsten alloys are composed of tungsten microparticles embedded in a solid matrix of transition metals such as nickel, cobalt, or iron. To understand the toxicology of these alloys, male F344 rats were intramuscularly implanted with pellets of tungsten/nickel/cobalt, tungsten/nickel/iron, or pure tungsten, with tantalum pellets as a negative control. Between 6 and 12 months, aggressive rhabdomyosarcomas formed around tungsten/nickel/cobalt pellets, while those of tungsten/nickel/iron or pure tungsten did not cause cancers. Electron microscopy showed a progressive corrosion of the matrix phase of tungsten/nickel/cobalt pellets over 6 months, accompanied by high urinary concentrations of nickel and cobalt. In contrast, non-carcinogenic tungsten/nickel/iron pellets were minimally corroded and urinary metals were low; these pellets having developed a surface oxide layer in vivo that may have restricted the mobilization of carcinogenic nickel. Microarray analysis of tumors revealed large changes in gene expression compared with normal muscle, with biological processes involving the cell cycle significantly up-regulated and those involved with muscle development and differentiation significantly down-regulated. Top KEGG pathways disrupted were adherens junction, p53 signaling, and the cell cycle. Chromosomal enrichment analysis of genes showed a highly significant impact at cytoband 7q22 (chromosome 7) which included mouse double minute (MDM2) and cyclin-dependant kinase (CDK4) as well as other genes associated with human sarcomas. In conclusion, the tumorigenic potential of implanted tungsten alloys is related to mobilization of carcinogenic metals nickel and cobalt from corroding pellets, while gene expression changes in the consequent tumors are similar to radiation induced animal sarcomas as well as sporadic human sarcomas.
Pearls are composite materials of calcium carbonate polymorphs (calcite and aragonite) and organic macromolecules (polysaccharides and proteins) which contain genes and transcription factors that direct the formation of calcite and aragonite polygonal tiles, including their shape, size, and geometrical accommodation. These biologically derived instructions are transmitted from donor mussel shell mantle tissue by inserting seed grafts into freshwater production mussels. In this paper the internal and external freshwater pearl structure for the cultured triangle mussel Hyriopsis cumingii is examined by light optical microscopy, scanning electron microscopy, and x-ray diffraction. Pearl interior crystal structure evolves as mainly concentric calcite tile layers from the seed sac, with mixtures of aragonite polygonal (hexagonal-like) tiles. Within about 0.8–1 mm from the ideal (curved) pearl surface, the aragonite tiles form as continuous, overlapping layers 300–400 nm thick, with interlamellar organic material.
The layer-by-layer building of monolithic, 3D metal components from selectively melted powder layers using laser or electron beams is a novel form of 3D printing or additive manufacturing. Microstructures created in these 3D products can involve novel, directional solidification structures which can include crystallographically oriented grains containing columnar arrays of precipitates characteristic of a microstructural architecture. These microstructural architectures are advantageously rendered in 3D image constructions involving light optical microscopy and scanning and transmission electron microscopy observations. Microstructural evolution can also be effectively examined through 3D image sequences which, along with x-ray diffraction (XRD) analysis in the x-y and x-z planes, can effectively characterize related crystallographic/texture variances. This paper compares 3D microstructural architectures in Co-base and Ni-base superalloys, columnar martensitic grain structures in 17–4 PH alloy, and columnar copper oxides and dislocation arrays in copper.
The interfacial bonding between layers in ultrasonically consolidated structures is poor for some material combinations, resulting in relatively low bond strength. This makes resultant parts unsuitable for structural applications. This work discusses a study of the effects of post process heat treatment of ultrasonically consolidated commercially pure titanium and aluminum alloy 3003 dual-material systems. The lap shear strengths of as-consolidated specimens as well as heat treated ones were tested. The results show that there is significant improvement of the strengths of post processed specimens over the as-consolidated ones. The improvement is as a result of stress relieving of the strain hardened interface between the two materials and some interactions of the base materials across the interfacial boundaries at elevated temperatures, leading to stronger bonds. The study highlights the role of post process heat treatments for improving the mechanical properties of ultrasonically consolidated structures.
Microstructures and a microstructural, columnar architecture as well as mechanical behavior of as-fabricated and processed INCONEL alloy 625 components produced by additive manufacturing using electron beam melting (EBM) of prealloyed precursor powder are examined in this study. As-fabricated and hot-isostatically pressed (“hipped”) [at 1393 K (1120 °C)] cylinders examined by optical metallography (OM), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive (X-ray) spectrometry (EDS), and X-ray diffraction (XRD) exhibited an initial EBM-developed γ ″ (bct) Ni 3 Nb precipitate platelet columnar architecture within columnar [200] textured γ (fcc) Ni-Cr grains aligned in the cylinder axis, parallel to the EBM build direction. Upon annealing at 1393 K (1120 °C) (hot-isostatic press (HIP)), these precipitate columns dissolve and the columnar, γ , grains recrystallized forming generally equiaxed grains (with coherent {111} annealing twins), containing NbCr 2 laves precipitates. Microindentation hardnesses decreased from ~2.7 to ~2.2 GPa following hot-isostatic pressing (“hipping”), and the corresponding engineering (0.2 pct) offset yield stress decreased from 0.41 to 0.33 GPa, while the UTS increased from 0.75 to 0.77 GPa. However, the corresponding elongation increased from 44 to 69 pct for the hipped components.
The fabrication of Cu components by additive manufacturing using electron beam melting (EBM) from low-purity, atomized Cu powder containing a high density of Cu(2)O precipitates exhibits a novel example of precipitate dislocation architecture. Such architectures are seen by optical metallography, and scanning and transmission electron microscopy, to consist generally of equiaxed precipitate dislocation cell-like arrays (1-3 mu m) in the horizontal reference plane perpendicular to the build direction with elongated or columnar-like arrays extending from similar to 12 to >60 mu m in length and corresponding spatial dimensions of 1-3 mu m. The hardnesses for these architectures ranged from similar to HV 83 to 88, in contrast to the original Cu powder microindentation hardness of HV 72 and the commercial Cu base plate hardness of HV 57. These observations illustrate the prospect for creating some form of controlled microstructural architecture by EBM parameter alternation or optimization. (C) 2011 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
Cu reticulated mesh and stochastic open cellular foams were fabricated by additive manufacturing using electron beam melting. Fabricated densities ranged from 0.73 g/cm(3) to 6.67 g/cm3. The precursor Cu powder contained Cu2O precipitates and the fabricated components contained arrays of Cu2O precipitates and interconnected dislocation microstructures having average spacings of similar to 2 mu m, which provide hardness values similar to 75% above commercial Cu products. Plots of stiffness (Young's modulus) versus density and relative stiffness versus relative density were in very close agreement with the Gibson-Ashby model for open cellular foams. These open cellular structure components exhibit considerable potential for novel, complex, multi-functional electrical and thermal management systems, especially complex, monolithic heat exchange devices. (C) 2011 Elsevier B.V. All rights reserved.
Ti–6Al–4V open cellular foams were fabricated by additive manufacturing using electron beam melting (EBM). Foam models were developed from CT-scans of aluminum open cellular foams and embedded in CAD for EBM. These foams were fabricated with solid cell structures as well as hollow cell structures and exhibit tailorable stiffness and strength. The strength in proportion to the measured microindentation hardness is as much as 40% higher for hollow cell (wall) structures in contrast to solid, fully dense EBM fabricated components. Plots of relative stiffness versus relative density were in good agreement with the Gibson–Ashby model for open cellular foam materials. Stiffness or Young's modulus values measured using a resonant frequency-damping analysis technique were found to vary inversely with porosity especially for solid cell wall, open cellular structure foams. These foams exhibit the potential for novel biomedical, aeronautics, and automotive applications.
The microstructures and mechanical behavior of simple, as-fabricated, solid geometries (with a density of 8.4 g/cm3), as-fabricated and fabricated and annealed femoral (knee) prototypes, and reticulated mesh components (with a density of 1.5 g/cm3) all produced by additive manufacturing (AM) using electron beam melting (EBM) of Co-26Cr-6Mo-0.2C powder are examined and compared in this study. Microstructures and microstructural issues are examined by optical metallography (OM), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray spectrometry (EDS), and X-ray diffraction (XRD), while mechanical properties included selective specimen tensile testing and Vickers microindentation hardness (HV) and Rockwell C-scale hardness (HRC) measurements. Orthogonal (X-Y) melt scanning of the electron beam during AM produced unique, orthogonal and related Cr23C6 carbide (precipitate) arrays (a controlled microstructural architecture) with dimensions of ~2 μm in the build plane perpendicular to the build direction, while connected carbide columns were formed in the vertical plane, parallel to the build direction, with microindentation hardnesses ranging from 4.4 to 5.9 GPa, corresponding to a yield stress and ultimate tensile strength (UTS) of 0.51 and 1.45 GPa with elongations ranging from 1.9 to 5.3 pct. Annealing produced an equiaxed fcc grain structure with some grain boundary carbides, frequent annealing twins, and often a high density of intrinsic {111} stacking faults within the grains. The reticulated mesh strut microstructure consisted of dense carbide arrays producing an average microindentation hardness of 6.2 GPa or roughly 25 pct higher than the fully dense components.
Intermetallic, γ-TiAl, equiaxed, small-grain (∼2μm) structures with lamellar γ/α2-Ti3Al colonies with average spacing of 0.6μm have been fabricated by additive manufacturing using electron beam melting (EBM) of precursor, atomized powder. The residual microindentation (Vickers) hardness (HV) averaged 4.1GPa, corresponding to a nominal yield strength of ∼1.4GPa (∼HV/3), and a specific yield strength of 0.37GPacm3g−1 (for a density of 3.76gcm−3), in contrast to 0.27GPacm3g−1 for EBM-fabricated Ti–6Al–4V components. These results demonstrate the potential to fabricate near net shape and complex titanium aluminide products directly using EBM technology in important aerospace and automotive applications.
The microstructures and mechanical properties of rapid-layer manufactured Ti-6Al-4V specimens from precursor powder by electron beam melting (EBM) and selective laser melting (SLM) are compared with those characteristic of commercial wrought products of Ti-6Al-4V. The microstructures are characterized by optical metallography and scanning and transmission electron microscopy. The EBM built samples exhibited alpha (hcp) acicular platelet (basketweave or Widmanstatten) microstructure similar to wrought products while the SLM built samples exhibited primarily alpha' (hcp) martensitic microstructure. The EBM samples exhibited a UTS as high as 1.2 GPa and elongations in excess of 20% in contrast to the SLM samples which exhibited a UTS of 1.3 GPa and elongations of only 4%. Rockwell C-scale hardnesses ranged from 37 to 55 for the EBM samples indicative of a wide range of graded properties and complex monolithic and open (or porous) geometries which might be digitally manufactured for biomedical and aerospace applications in particular.
Carbonaceous particulate matter (PM) was collected by both thermal precipitation and glass fiber filters from specific combustion sources and examined by transmission electronmicroscopy (TEM) and field emissions canning electron microscopy (FESEM). PM from various natural as burner combustion regimes (NGPM), burning tires (TPM), a heavy duty diesel truck (DPM), wood burning (WPM), candle burning (CPM), along with commercial black carbon (BC) powder and multiwall carbon nanotube (MWCNT) aggregates material exhibited similarities in PM microstructure, and average primary spherule diameters.
In this paper we report on the collection of fine (PM1) and ultrafine (PM0.1), or nanoparticulate, carbonaceous materials using thermophoretic precipitation onto silicon monoxide/formvar-coated 3 mm grids which were examined in the transmission electron microscope (TEM). We characterize and compare diesel particulate matter (DPM), tire particulate matter (TPM), wood burning particulate matter, and other soot (or black carbons (BC)) along with carbon nanotube and related fullerene nanoparticle aggregates in the outdoor air, as well as carbon nanotube aggregates in the indoor air; and with reference to specific gas combustion sources. These TEM investigations include detailed microstructural and microdiffraction observations and comparisons as they relate to the aggregate morphologies as well as their component (primary) nanoparticles. We have also conducted both clinical surveys regarding asthma incidence and the use of gas cooking stoves as well as random surveys by zip code throughout the city of El Paso. In addition, we report on short term (2 day) and longer term (2 week) in vitro assays for black carbon and a commercial multiwall carbon nanotube aggregate sample using a murine macrophage cell line, which demonstrate significant cytotoxicity; comparable to a chrysotile asbestos nanoparticulate reference. The multi-wall carbon nanotube aggregate material is identical to those collected in the indoor and outdoor air, and may serve as a surrogate. Taken together with the plethora of toxic responses reported for DPM, these findings prompt concerns for airborne carbonaceous nanoparticulates in general. The implications of these preliminary findings and their potential health effects, as well as directions for related studies addressing these complex issues, will also be examined.
Nanotechnology and nanomaterials have become the new frontier world-wide over the past few years and prospects for the production and novel uses of large quantities of carbon nanotubes in particular are becoming an increasing reality. Correspondingly, the potential health risks for these and other nanoparticulate materials have been of considerable concern. Toxicological studies, while sparse, have been concerned with virtually uncharacterized, single wall carbon nanotubes, and the conclusions have been conflicting and uncertain. In this research we performed viability assays on a murine lung macrophage cell line to assess the comparative cytotoxicity of commercial, single wall carbon nanotubes (ropes) and two different multiwall carbon nanotube samples; utilizing chrysotile asbestos nanotubes and black carbon nanoaggregates as toxicity standards. These nanotube materials were completely characterized by transmission electron microscopy and observed to be aggregates ranging from 1 to 2 μm in mean diameter, with closed ends. The cytotoxicity data indicated a strong concentration relationship and toxicity for all the carbon nanotube materials relative to the asbestos nanotubes and black carbon. A commercial multiwall carbon nanotube aggregate exhibiting this significant cell response was observed to be identical in structure to multiwall carbon nanotube aggregates demonstrated to be ubiquitous in the environment, and especially in indoor environments, where natural gas or propane cooking stoves exist. Correspondingly, preliminary epidemiological data, although sparse, indicate a correlation between asthma incidence or classification, and exposure to gas stoves. These results suggest a number of novel epidemiological and etiological avenues for asthma triggers and related respiratory or other environmental health effects, especially since indoor number concentrations for multiwall carbon nanotube aggregates is at least 10 times the outdoor concentration, and virtually all gas combustion processes are variously effective sources. These results also raise concerns for manufactured carbon nanotube aggregates, and related fullerene nanoparticles.
Carbon nanotubes and other fullerene-related nanocrystals are ubiquitous in the atmospheric environment-both indoor and outdoor. In fact, these nanostructures have been observed even in a 10,000 year-old ice core sample, indicating their natural existence in antiquity, probably as natural gas/ methane combustion products. Similar carbon nanotubes and complex carbon nanocrystal aggregates are observed to be emitted from contemporary combustion sources such as kitchen stoves (natural gas and propane), water heater and furnace exhaust vents, natural gas-burning (electric) power plants, and industrial furnace operations, among others. These observations have been made by collecting nanoparticulates and nanocrystal aggregates on carbon/formvar and silicon monoxide/formvarcoated 3 mm grids that were examined with a transmission-electron microscope. This study begins to establish an environmental context for considering the potential impact of future nanostructured particles on human health.
Extended abstract of a paper presented at Microscopy and Microanalysis 2004 in Savannah, Georgia, USA, August 1–5, 2004.