SCRIPTA MATERIALIA

Estimations of the effective Young's modulus of specimens prepared by fused filament fabrication
Fang L, Yan Y, Agarwal O, Seppala JE, Migler KD, Nguyen TD and Kang SH
The elastic response of homogeneous isotropic materials is most commonly represented by their Young's modulus (E), but geometric variability associated with additive manufacturing results in materials that are neither homogeneous nor isotropic. Here we investigated methods to estimate the effective elastic modulus of samples fabricated by fused filament fabrication. We conducted finite element analysis (FEA) on printed samples based on material properties and CT-scanned geometries. The analysis revealed how the layer structure of a specimen altered the internal stress distribution and the resulting . We also investigated different empirical methods to estimate as guides. We envision the findings from our study can provide guidelines for modulus estimation of as-printed specimens, with the potential of applying to other extrusion-based additive manufacturing technologies.
Multi-scale analyses of constituent phases in a trip-assisted duplex stainless steel by electron backscatter diffraction, in situ neutron diffraction, and energy selective neutron imaging
Woo W, Kim J, Kim EY, Choi SH, Em V and Hussey DS
Micrometer to centimeter scale analyses of the crystalline phase volume fractions in a trip-assisted duplex stainless steel were performed under loading using electron backscatter diffraction (EBSD), in situ neutron diffraction, and energy selective neutron imaging (ESNI) methods. In contrast to the localized investigations of EBSD, ESNI provides macroscopic spatial distributions in a volume-averaged manner over the entire specimen with a spatial resolution of about 65 μm. The ESNI shows that the martensite is concentrated on the necking region and estimates its volume fraction of 14% at a strain of 0.2, which is comparable to the neutron diffraction result.
Precipitation and dissolution of and during heat treatment of a laser powder-bed fusion produced Ni-based superalloy
Lass EA, Stoudt MR, Katz MB and Williams ME
One drawback of the laser powder-bed fusion additive manufacturing (AM) technique is the build-up of residual stresses during processing that require a stress-relief heat treatment prior to components being removed from the build plate. Here, we demonstrate the coprecipitation of the -phase alongside the known -phase, during stress-relief annealing of AM Inconel 625 at 870 °C. The unexpected precipitation of in the AM material is attributed to the local solute enrichment to the interdendritic regions of the as-built solidification microstructure. Dissolution of the and phases is achieved after annealing for 15 min at 1150 °C.
Observation of crack growth in a polycrystalline ferroelectric by synchrotron X-ray diffraction
Huber JE, Hofmann F, Barhli S, Marrow TJ and Hildersley C
Pre-cracked samples of unpoled, polycrystalline, soft ferroelectric lead zirconate titanate were subjected to electrical and mechanical loading whilst using synchrotron X-ray diffraction to map strain-fields. Clear evidence is found of switching around the crack tip and development of a crack-wake. A -integral estimate based on strain-field data provided a sensitive measure of strain changes during loading. Electrical loading did not cause crack advance or crack-tip switching; this provides evidence for electrically permeable crack models. There was also enhancement of electrically-driven switching in the crack-wake region. The results provide improved understanding and a resource for testing fracture models in ferroelectrics.
Rafting and Elastoplastic Deformation of Superalloys Studied by Neutron Diffraction
Coakley J, Lass EA, Ma D, Frost M, Seidman DN, Dunand DC and Stone HJ
The rafting of monocrystalline Ni- and Co-based superalloys has been studied by neutron diffractometry. Lattice parameter misfit values and the difference in phase stiffnesses at room temperature, , and are presented. These microstructural parameters should assist in refining computer models that aim to predict precipitate evolution in superalloys and aid future alloy design. The nature of rafting is shown experimentally to be dependent upon the lattice parameter misfit. The yield strength of the -phase of the Co-based superalloy with a rafted microstructure occurs at , when loaded at a low strain rate.
Homogenization Kinetics of a Nickel-based Superalloy Produced by Powder Bed Fusion Laser Sintering
Zhang F, Levine LE, Allen AJ, Campbell CE, Lass EA, Cheruvathur S, Stoudt MR, Williams ME and Idell Y
Additively manufactured (AM) metal components often exhibit fine dendritic microstructures and elemental segregation due to the initial rapid solidification and subsequent melting and cooling during the build process, which without homogenization would adversely affect materials performance. In this letter, we report observation of the homogenization kinetics of an AM nickel-based superalloy using synchrotron small angle X-ray scattering. The identified kinetic time scale is in good agreement with thermodynamic diffusion simulation predictions using microstructural dimensions acquired by scanning electron microscopy. These findings could serve as a recipe for predicting, observing, and validating homogenization treatments in AM materials.
In situ observations of Berkovich indentation induced phase transitions in crystalline silicon films
Gerbig YB, Michaels CA and Cook RF
The pressure induced phase transitions of crystalline Si films were studied under a Berkovich probe using a Raman spectroscopy-enhanced instrumented indentation technique. The observations suggested strain and time as important parameters in the nucleation and growth of high-pressure phases and, in contrast to earlier reports, indicate that pressure release is not a precondition for transformation to high pressure phases.
Substrate Topography Guides Pore Morphology Evolution in Nanoporous Gold Thin Films
Chapman CA, Daggumati P, Gott SC, Rao MP and Seker E
This paper illustrates the effect of substrate topography on morphology evolution in nanoporous gold (np-Au) thin films. One micron-high silicon ridges with widths varying between 150 nm to 50 µm were fabricated and coated with 500 nm-thick np-Au films obtained by dealloying sputtered gold-silver alloy films. Analysis of scanning electron micrographs of the np-Au films following dealloying and thermal annealing revealed two distinct regimes where the ratio of film thickness to ridge width determines the morphological evolution of np-Au films.
Improved electro-mechanical performance of gold films on polyimide without adhesion layers
Putz B, Schoeppner RL, Glushko O, Bahr DF and Cordill MJ
Thin metal films on polymer substrates are of interest for flexible electronic applications and often utilize a thin interlayer to improve adhesion of metal films on flexible substrates. This work investigates the effect of a 10 nm Cr interlayer on the electro-mechanical properties of 50 nm Au films on polyimide substrates. Ex situ and in situ fragmentation experiments reveal the Cr interlayer causes brittle electro-mechanical behaviour, and thin Au films without an interlayer can support strains up to 15% without significantly degrading electrical conductivity.
Increasing the strength of nanocrystalline steels by annealing: Is segregation necessary?
Renk O, Hohenwarter A, Eder K, Kormout KS, Cairney JM and Pippan R
Hardening phenomena in nanocrystalline metals after annealing have been widely reported, and the subject of much recent debate. Solute segregation to grain boundaries and dislocation source hardening have been proposed to cause the strengthening. To shed light on the dominant mechanisms, we present results from mechanical experiments and atom probe tomography on samples with similar grain size but different amounts of solute segregation and different boundary chemistries.
Surface energies of AlN allotropes from first principles
Holec D and Mayrhofer PH
In this letter we present first-principles calculations of the surface energies of rock-salt (B1), zinc-blende (B3) and wurtzite (B4) AlN allotropes. Of several low-index facets, the highest energies are obtained for monoatomic surfaces (i.e. of only either Al or N atoms): [Formula: see text] and [Formula: see text]. The difference between Al- and N-terminated surfaces in these cases is less then 20 meV/Å. The stoichiometric facets have energies lower by 100 meV/Å or more. The obtained trends could be rationalized by a simple nearest-neighbour broken-bond model.
Size-Dependent Rupture Strain of Elastically Stretchable Metal Conductors
Graudejus O, Jia Z, Li T and Wagner S
Experiments show that the rupture strain of gold conductors on elastomers decreases as the conductors are made long and narrow. Rupture is caused by the irreversible coalescence of microcracks into one long crack. A mechanics model identifies a critical crack length ℓ(cr), above which the long crack propagates across the entire conductor width. ℓ(cr) depends on the fracture toughness of the gold film and the width of the conductor. The model provides guidance for the design of highly stretchable conductors.
Extrinsic and intrinsic fracture behavior of high pressure torsion deformed nickel
Rathmayr GB and Pippan R
Nickel discs (>99.5 wt.%) were deformed by high pressure torsion (HPT) at different temperatures (-196 °C, 25 °C, 200 °C, and 400 °C) until saturation was reached. The strength and fracture behavior of microdefect-free samples and samples with inclusions were investigated using micro and macro tensile tests, respectively. The fracture behavior is not sensitive to the HPT deformation temperature but differs significantly in the two types of sample. The ultimate tensile strength is not affected by inclusions or grain texture.
Influence of Domain Size on the Scaling Effects in Pb(Mg1/3Nb2/3)O3-PbTiO3 Ferroelectric Crystals
Lin D, Lee HJ, Zhang S, Li F, Li Z, Xu Z and Shrout TR
The property degradation observed in thin Pb(Mg(1/3)Nb(2/3))O(3)-PbTiO(3) (PMN-PT) crystals is believed to relate to large domains and subsequent clamping induced by surface-boundary. In this work, the properties were investigated as function of domain size, using controlled poling. The degraded piezoelectric and dielectric properties of thin PMN-PT were found to increase significantly, by decreasing domain size. Furthermore, the fine domain structure was found to be stable at 3kV/cm after 7.0×10(5) negative-pulse cycles, hence, enabling PMN-PT crystals for high-frequency (>20 MHz) ultrasound-transducers.
Absolute concentration of free volume-type defects in ultrafine-grained Fe prepared by high-pressure torsion
Oberdorfer B, Lorenzoni B, Unger K, Sprengel W, Zehetbauer M, Pippan R and Würschum R
A maximum excess volume ΔV/V ≈ 1.9 × 10(-3) in ultrafine-grained Fe prepared by high-pressure torsion is determined by measurements of the irreversible length change upon annealing employing a high-resolution differential dilatometer. Since dislocations and equilibrium-type grain boundaries cannot fully account for the observed released excess volume, the present study yields evidence for a high concentration of free volume-type defects inherent to nanophase materials, which is considered to be the main source of their particular properties, such as strongly enhanced diffusivities.
Fabrication of perforated sub-micron silica shells
Andreyev DS and Arriaga EA
A new synthetic approach for fabrication of perforated hollow silica morphologies using colloidal template assemblies is demonstrated. As proof-of-principle, the polystyrene/silver colloidal assemblies had chemically modified surfaces. The template dissolution resulted in the fabrication of the submicron perforated hollow silica shells. The morphologies are characterized by transmission electron microscopy, energy dispersive spectroscopy and plasmon light extinction spectrophotometry.
Transgranular Cracking in a Liquid Zn Embrittled High Strength Steel
Bhattacharya D, Cho L, Van der Aa E, Ghassemi-Armaki H, Pichler A, Findley KO and Speer JG
Intergranular Zn-assisted liquid metal embrittlement (LME) cracks have been frequently reported in steels, involving austenite grain boundary penetration of liquid Zn at high temperature. In the present study, a Zn-coated high strength steel was deformed at an intercritical temperature, and the characteristics of LME cracking were studied in a mixed microstructure composed of ferrite and austenite. Crack propagation was intergranular in austenite; in contrast, the ferrite exhibited both intergranular LME and LME. Trace analysis of the crack plane orientation was consistent with cracking along {100} cleavage planes in ferrite.