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At least 1,747 records · Page 97

Pulsed laser powder bed fusion additive manufacturing of A356

Highlights: • Dense A356 specimens (98 ± 0.4%) were fabricated using a customized P-LPBF system. • Microstructure and grain morphology were examined using LOM, SEM, and EBSD. • Solidification front velocities (R) were evaluated through the KGT model. • A columnar grain structure was observed and predicted by the Hunt's criterion. - Abstract: A356 (Al7SiMg) specimens were fabricated through pulsed laser powder bed fusion (P-LPBF) additive manufacturing. Microstructural examinations and analyses were carried out through the usage of light optical microscopy (LOM), scanning electron microscopy (SEM), and electron backscatter diffraction (EBSD). The results revealed a fine cellular microstructure with the intercellular network consisting of Al cells and defined by a network of Si arms. The Al cells at the center of the melt pools and within the melt pool boundary bands were measured to be 423 ± 49 nm and 664 ± 76 nm, respectively. The presence of a fine columnar grain structure and epitaxial growth on partially melted grains was observed and explained by the KGT model and Hunt's criterion.

36 MATERIALS SCIENCE↗

Characterization of texture and grain boundary character distributions of selective laser melted Inconel 625 alloy

Highlights: • <110> texture along layer build direction was generated in as-SLMed Inconel 625. • The stress relief process dominates texture and GBCD evolution. • SLMed IN 625 alloy can be GBEed via suitable post annealing. - Abstract: Select laser melting (SLM) is one of the practical metal additive manufacturing processes to fabricate complex structures. The inhomogeneous microstructure and high residual stress are typically resulted from a non-uniform melting and rapid solidification during a SLM process, which has the significant impact on part dimensional instability, corrosion resistance, and mechanical properties. The bulk of current research is limited to the general characterization of grain size, texture, and mechanical properties. However, grain boundary character distribution (GBCD) and its relationship with texture are yet to be understood. This study has shown that the preferred <110> along building direction and <100> along laser scanning direction were produced. The high density of low angle grain boundary (LAGB) can be an indicator of residual stress levels in the as-SLMed samples. The newly-developed ∑3, ∑9 and ∑27 grain boundaries were heavily populated, and the cluster of grains interfaced by ∑3{sup n} (n = 0, 1, 2…) was introduced at the expense of LAGB only at high recrystallization annealing (1150°C or over). The research results suggest that GBCD optimization be possible in the SLMed Inconel 625 alloy via suitable post annealing, which allows improving intergranular corrosion resistance and enhancing mechanical properties.

36 MATERIALS SCIENCE↗

Defects and 3D structural inhomogeneity in electron beam additively manufactured Inconel 718

Highlights: • A protocol for 3D characterization of structure and defects in additively manufactured EBM 718 is presented. • Lack of fusion defects disrupt local microstructure, creating isolated regions of equiaxed grains. • Clustering of micron-scale nitrides is attributed to a particle rafting process. • Normalized size-number density relationship of carbides matches that of industrial ingots. • Removal of porosity via post-processing will not correct microstructural inhomogeneities created by lack of fusion defects. - Abstract: Material structure and defects created during additive manufacturing contribute to the variability in mechanical properties of these parts, limiting their use for critical applications. Three-dimensional crystallographic, structural, and chemical information in electron beam melted Inconel 718 was collected from the sub-micron to the millimeter scale using the TriBeam tomography system. The relationship of defects to the surrounding microstructure has been studied in detail. Lack of fusion defects created sharp discontinuities in the grain morphology that extended several build layers beyond the layer where the defect originated. Nitrides and carbides in the size range of 1.25 μm to 10 μm were observed throughout the volume, with pronounced nitride clustering. The similarities between solidification in additive manufacturing and traditional manufacturing processes are demonstrated by the comparable size and distribution of carbides measured for industrial-scale samples of 718. Defects created during additive manufacturing cannot be easily remedied via standard post-processing techniques, and will likely diminish the mechanical performance of additively manufactured parts.

36 MATERIALS SCIENCE↗

Effects of Sr, Ce and P on the microstructure and mechanical properties of rapidly solidified Al7Si alloys

Highlights: • Rapid solidification caused formation of nanoscaled Si particle chains. • Sr or Ce induced the columnar transition zone only at extremely high cooling rate. • Enhancement of hardness is attributed to fine dispersion of eutectic Si, grain refinement and the supersaturation of Si. • Sr or Ce caused further enhancement of hardness, attributing to Si modification. - Abstract: A series of Al7Si based alloys with trace addition of Sr, Ce or P were prepared using melt-spinning at two different high cooling rates, and the microstructure as well as the hardness of the ribbons was comprehensively studied. The results show that Sr or Ce induces the formation of columnar transition zone and modifies the morphology of eutectic Si phase from dispersed particle chains to fine fibers only at extremely high cooling rate. However, P has little effect on the microstructure of either α-Al or eutectic Si. Compared with conventional casting, the Al7Si ribbons exhibit extremely high hardness due to the fine dispersion of eutectic Si, the grain refinement and the supersaturation of Si. The hardness is further enhanced by Sr or Ce addition at extremely high cooling rate, especially for columnar and equiaxed zones, attributing to the modification effect on Si phase.

36 MATERIALS SCIENCE↗

Effects of boron addition on the morphology of silicon phases in Al-Si casting alloys

Highlights: • The influence of boron on Si phase was studied. • Boron addition reduces the length of eutectic Si plates in Al-11Si alloys. • Boron addition promotes the nucleation temperature of primary Si phases in Al-14Si alloys. • Boron addition increases the twin density in the <112>{sub Si} growth direction of eutectic Si in Al-11Si and Al-14Si alloys. - Abstract: The influence of B elements on the morphology of Si phases in Al-11Si and Al-14Si alloys has been investigated employing Optical Microscope, Scanning Electron Microscopy, Transmission Electron Microscopy and Differential Scanning Calorimetry. In Al-11Si alloy, the addition of B element not only refines the primary Al dendrites, but also reduces the length of eutectic Si plates. In Al-14Si alloys, the addition of B element promotes the nucleation temperature of primary Si phases, but shows weak influence on the nucleation temperature of eutectics. The effects of B element on the morphologies of both primary Si particle and eutectics can be attributed to the interaction between B and Si elements during the solidification process.

36 MATERIALS SCIENCE↗

Effects of Nb and Ta additions on the strength and coarsening resistance of precipitation-strengthened Al-Zr-Sc-Er-Si alloys

Highlights: • Nb and Ta micro-additions are made to a dilute Al-Er-Sc-Zr-Si alloys. • Zr-enriched primary L1{sub 2} precipitates form on solidification. • Secondary L1{sub 2} precipitates form on aging, and show improved coarsening resistance. • Nb and Ta are enriched at the secondary nanoprecipitate/matrix interface. • Micro-additions of Nb and Ta have similar effects as V, previously studied. - Abstract: A dilute Al-0.07Zr-0.02Sc-0.005Er-0.06Si (at.%) alloy was microalloyed with 0.08 at.% Nb or Ta. Atom-probe tomography reveals that, upon aging, Nb and Ta partition to the coherent L1{sub 2}-Al{sub 3}(Zr,Sc,Er) nanoprecipitates (with average concentrations of 0.2 and 0.08 at.%, respectively), with both segregating at the matrix/nanoprecipitate heterophase interface. This is consistent with the Nb- and Ta-modified alloys exhibiting, as compared to the unmodified alloy: (i) higher peak microhardness, from a higher nanoprecipitate volume fraction and/or lattice parameter mismatch; and (ii) improved aging resistance, from slower nanoprecipitate coarsening due to the small diffusivities of niobium and tantalum in aluminum. Analogous results were previously reported for a V-modified alloy.

36 MATERIALS SCIENCE↗

A comparison of Ti-6Al-4V in-situ alloying in Selective Laser Melting using simply-mixed and satellited powder blend feedstocks

Highlights: • Satelliting mixing is proposed for preparing powder feedstocks for AM. • Satelliting allows the creation of blended feedstocks of improved homogeneity. • Sample homogeneity is affected by particle size distribution and powder mixing technique. - Abstract: In-situ alloying within laser powder-bed fusion, specifically Selective Laser Melting (SLM), has been investigated for the formulation of novel alloys from elemental powders to extend the benefits offered by these technologies. Inadequate preparation of the powder feedstock prior to in-situ alloying can yield inhomogeneous microstructures, often deteriorating the mechanical performance of the deposited parts. The present work was designed to assess the use of the ‘satelliting’ method to create powder feedstocks for in-situ laser powder-bed fusion. The research was carried out on Ti-6Al-4V. Ti-6Al-4V feedstocks obtained by mixing or satelliting elemental powders were investigated and compared to a reference pre-alloyed material. The processability of the different feedstocks was assessed by comparing the microstructure of the deposits originating from the different powder blends. Results show that the powder percolation and particle size distribution of the feedstocks translate in deposited microstructures exhibiting different porosity, elemental segregation, and average grain size, revealing the impact of the powder blend characteristics on the laser energy absorbance and solidification of the alloy. This study provides fundamental insights of how to formulate powder feedstock and aims to support future research activities on the design and development of new alloys for use in powder-based additive manufacturing.

36 MATERIALS SCIENCE↗

Analyzing the microstructural evolution and hardening response of an Al-Si-Mg casting alloy with Cr addition

Highlights: • The formation of β-Al{sub 5}FeSi intermetallics was suppressed since impurity Fe has been consumed by Al{sub 13}Cr{sub 4}Si{sub 4} intermetallics; • A large number of Al{sub 13}Cr{sub 4}Si{sub 4} dispersoids were observed in Al dendrites in the as-quenched and aged alloy; • The precipitation of Cr-bearing dispersoids harden the as-quenched alloy by over 10HV; • The current thermodynamic database underestimate the solubility of Fe in Al{sub 13}Cr{sub 4}Si{sub 4} intermetallics during solidification simulation. - Abstract: Chromium is added to Al-Si based casting alloys for the mitigation of die soldering. In the present work, EBSD, EDS and TEM characterizations are combined with thermodynamic simulations to study the microstructural evolution and hardening response of an Al-Si-Mg-Cr casting alloy during heat treatments. It is shown that the Fe-containing intermetallic compounds formed in the inter-dendritic region were acicular π-Al{sub 8}(Fe, Cr)Mg{sub 3}Si{sub 6} phase and polyhedral Al-(Cr, Fe)-Si phase which is structurally similar to face-centered cubic Al{sub 13}Cr{sub 4}Si{sub 4}. The polyhedral Al-(Cr, Fe)-Si intermetallics that crystallized prior to β-Al{sub 5}FeSi consumed impurity Fe, suppressing the formation of β phase during gravity die casting process. Also, Cr-addition enables the precipitation of nano-scale Cr-bearing dispersoids in Al dendrite during solution treatment at 813 K. Hardness increment of over 10 HV can be induced by the Cr-bearing dispersoids for as-quenched alloy. Though the dispersoids have a moderate hardening effect on the as-quenched alloy, they may impair the ageing hardening response by acting as heterogeneous nucleation sites for coarse Mg-Si rods and Si particles when quenching into water at 338 K.

36 MATERIALS SCIENCE↗

Variation improvement of mechanical properties of Mg-9Al-1Zn alloy with melt conditioned high pressure die casting

Highlights: • The variation improvement of mechanical properties of AZ91D was achieved via application of high shear melt conditioning. • The elongation variation of AZ91D with MC-HPDC has a significant reduction from 31.2% for tradition HPDC to 19.7%. • High shear melt conditioning can result in grain refinement of primary α-Mg formed in both shot sleeve and die cavity. - Abstract: Melt conditioning treatment via high shearing on Mg-9Al-1Zn melt was employed to disperse the oxide inclusions, and to harness the well-dispersed particles as the effective heterogeneous nucleation sites for primary α-Mg grains during solidification in high pressure die casting. To reveal the mechanism of property improvement, Prefil pressure filtration cleanliness analyzer, field-emission scanning electron microscopy with energy dispersive X-ray spectroscopy and high-resolution transmission electron microscopy were employed in present study. The experimental results showed that the application of high shearing not only improved elongation, ultimate tensile strength and yield strength simultaneously, but also reduced the variation of the mechanical properties of Mg-9Al-1Zn alloy. The improvement was ascribed to the refinement of the primary α-Mg grains formed in both shot sleeve and die cavity, and to the reduction of porosity as well as refinement of Mg{sub 17}Al{sub 12} phases.

36 MATERIALS SCIENCE↗

In-situ microstructural observation of Ti-Cu alloys for semi-solid processing

The semi-solid processing of metallic alloys strongly depends on the microstructural features exhibited by the raw material. Consequently, many characterization techniques have been used to elucidate semi-solid microstructures. In the present work, high-temperature laser-scanning confocal microscopy (HT-LSCM) was used to characterize Ti-Cu alloys intended for thixoforming. During the reheating stage, this in-situ technique enabled us to observe the Ti-β grains formed through the reverse eutectoid transformation. Furthermore, the results showed that thermomechanical treatment was primarily responsible for breaking up the dendritic microstructure. The liquid formation and peritectic temperature were easily determined via the HT-LSCM investigation. Prior to the reverse peritectic reaction, which corresponds to the onset of equilibrium melting, we obtained experimental evidence of the melting of non-equilibrium phases that originated via segregation during solidification. Finally, it was possible to qualitatively study the coarsening mechanisms that occurred in the semi-solid state. Irrespective of the alloy composition (liquid fraction), both Ostwald ripening and coalescence occurred during the isothermal heat treatments. Based on the obtained results, HT-LCSM can be considered a valuable technique for the characterization of thixotropic alloys.

36 MATERIALS SCIENCE↗

Interaction between laser radiation and metallic powder of 316L austenitic steel during selective laser melting

Highlights: • Single and multiple tracks on a loose bulk powder substrate were generated. • Understanding of the microstructure development during SLM was achieved. • Single tracks reveal a nearly symmetrical crystallography with elongated grains. • Multiple tracks show elongated grains perpendicular to the build direction. - Abstract: During selective laser melting (SLM), a complex heat state develops that leads to a characteristic crystallography and microstructure of the processed materials. Depending on the geometry of the processed part, most scan tracks of a new layer, so-called hatches, are located above a dense substrate or already solidified structures whereas others are located above loose powder. This is, inter alia, the case for overhanging structures. Attributable to the lower thermal conductivity of loose powder, temperature gradients and cooling rates of the melt pool differentiate in these areas, resulting in a different microstructural build-up. In this work, the microstructure and the crystallographic orientation of grade 316L austenitic stainless steel processed by SLM was investigated to understand the interaction between the laser radiation and the metallic powder during SLM-processing and to investigate the remelting of a track on a previous SLM-densified track. Single and multiple tracks on a loose bulk powder substrate, as well as single tracks on a dense substrate plate, were generated. A parameter study revealed that high energy densities are necessary to build continuous tracks on a loose bulk powder substrate. In addition, the amount of adhered particles, which are sintered on the fully melted and solidified tracks, is determined in comparison to the melted powder because the sintered particles strongly influence the surface roughness. To understand the microstructure development and, particularly, the influence of adjacent hatches during SLM-processing, investigations on the resulting microstructure and crystallographic orientation of a single track and two connected multiple tracks were carried out. During SLM processing of the tracks, the substrate plate and the solidified structures influence the temperature gradient and cooling rate of the melt pool, thus directionally solidified and elongated grains occur. Furthermore, the solidification is characterized by an epitaxial growth due to a distinct thermal gradient between the melt pool and the surrounding elements.

36 MATERIALS SCIENCE↗

Scan strategies in EBM-printed IN718 and the physics of bulk 3D microstructure development

Three-dimensional (3D) characterization provides opportunities for understanding processing-structure relationships in additively manufactured (AM) materials. Bulk samples of Inconel 718 were fabricated via electron beam melting (EBM) in order to study microstructural development as a function of energy input and beam scan strategy. TriBeam tomography of bulk Inconel 718 microstructures built under steady-state growth conditions reveals the sensitivity of microstructure formation and evolution to machine process parameters. Here, samples manufactured using a narrow range of energy input per unit build area result in varied grain morphologies and crystallographic textures. Using TRUCHAS, a thermal simulation software, the thermal history of bulk scan strategies was predicted, and combined with a calibrated microstructure-processing map to accurately predict bulk grain morphologies. The solidification parameters and the 3D measured nucleation density are used to predict the transition between columnar and equiaxed grain morphologies, providing a process map to guide AM parameter choices to locally control as-printed microstructure. A two-dimensional metric for characterizing bulk grain morphology was also found to agree well with predictions from the process map calibrated by 3D data. Combined with 3D tomography and thermal modelling, the physics of structure development were understood at a new level of detail with respect to the competing processes of grain nucleation and epitaxial growth.

36 MATERIALS SCIENCE↗

Synthesis, structural characterization and Mössbauer study of LnV{sub 0.5}Fe{sub 0.5}O{sub 3} perovskites (Ln = Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho and Er)

Graphical abstract: Mössbauer spectra taken at 200 K for the Y(V{sub 0.5}Fe{sub 0.5})O{sub 3} orthoferrivanadate synthesized by arc-melting. Highlights: ► LnFe{sub 0.5}V{sub 0.5}O{sub 3} were synthesized by the first time for most of the rare-earth elements. ► These orthoferrivanadates crystallize metastably with the perovskite structure. ► Iron and vanadium are trivalent stabilized in these solid solutions. ► The Mössbauer quadrupolar splitting is correlated with the tolerance factor. ► Below 100 K, these perovskites undergo a crystallographic phase transformation. -- Abstract: Perovskites LnV{sub 0.5}Fe{sub 0.5}O{sub 3} (Ln = Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho and Er) were synthesized by rapid solidification from arc-melted samples and characterized by the study of their crystal structure and hyperfine properties. These metastable solid solutions crystallized in the Pbnm symmetry, with the iron and vanadium cations randomly distributed in the transition metal octahedral sites. Depending on the lanthanide present at the A site of the perovskite, iron is present with two valences (i.e., Fe{sup 3+} and Fe{sup 2+}). The volume of the unit cell for these perovskites increases linearly with the lanthanide ionic radius, as the perovskite approaches its ideal structure. At room temperature, the quadrupolar splitting of the trivalent paramagnetic Mössbauer component works as an indirect measurement for the Goldshmidt tolerance factor. Close to or below 100 K, these perovskites undergo a crystallographic phase transformation, probably due to orbital ordering of the V{sup 3+} cations, originating two different magnetic iron sites.

36 MATERIALS SCIENCE↗

Microstructural characterization of dendritic evolution using two-point statistics

Characterizing large four-dimensional materials datasets is difficult due to the presence of complex mi- crostructures and time-varying length scales. We showcase the use of two-point statistics as an efficient and un-biased way of extracting materials parameters from an Al-Cu alloy during solidification. The evo- lution of dendrite primary arm thickness, average secondary arm spacing, and average tip-to-tip spacing were tracked using two-point Pearson auto-correlations of scaled mean curvatures. Insights into compet- itive side-branching are also reported. We show both visually and quantitatively that most length scales change rapidly during early stages of dendritic growth, but slow as diffusion fields of dendrites overlap.

Aluminum alloys↗

The Ammonia-Hydrogen System under Pressure

Binary mixtures of hydrogen and ammonia were compressed in diamond anvil cells to 15 GPa at room temperature over a range of compositions. The phase behavior was characterized using optical microscopy, Raman spectroscopy, and synchrotron X-ray diffraction. Below 1.2 GPa we observed two-phase coexistence between liquid ammonia and fluid hydrogen phases with limited solubility of hydrogen within the ammonia-rich phase. Complete immiscibility was observed subsequent to the freezing of ammonia phase III at 1.2 GPa, although hydrogen may become metastably trapped within the disordered face-centered-cubic lattice upon rapid solidification. For all compositions studied, the phase III to phase IV transition of ammonia occurred at ~3.8 GPa and hydrogen solidified at ~5.5 GPa, transition pressures equivalent to those observed for the pure components. A P-x phase diagram for the NH 3 -H 2 system is proposed on the basis of these observations with implications for planetary ices, molecular compound formation, and possible hydrogen storage materials.

08 HYDROGEN↗

Time-Resolved SAXS/WAXS Study of the Phase Behavior and Microstructural Evolution of Drug/PEG Solid Dispersions

Simultaneous small-angle X-ray scattering/wide-angle X-ray scattering (SAXS/WAXS) was employed to elucidate the physical state and location of various small molecule drugs blended with polyethylene glycol (PEG), as well as the time dependent microstructural evolution of the systems. Samples were prepared by comelting physical mixtures of the drug and PEG, followed by solidification at 25 C. The model drugs selected encompassed a wide variety of physicochemical properties in terms of crystallization tendency and potential for interaction with PEG. It was observed that compounds which crystallized rapidly and had weak interactions with PEG tended to be excluded from the interlamellar region of the PEG matrix. In contrast, drugs which had favorable interactions with PEG were incorporated into the interlamellar regions of the polymer up until the point at which the drug crystallized whereby phase separation occurred. These factors are likely to impact the effectiveness of drug/PEG systems as drug delivery systems.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

Characterization of high-current electron beam interaction with metal targets

The process of electron beam interaction with metal targets was characterized using electrical and optical diagnostics. Electron beams with current density of 5-10 A/cm{sup 2}, electron energy up to 120 keV, pulse duration up to 200 {mu}s, and cross-sectional area of 8-30 cm{sup 2} at the target surface were generated by GESA I and GESA II facilities. Streak imaging of the target surface specular reflectivity was used to determine the onset of melting and re-solidification of the target surface. Using time- and space-resolved schlieren imaging, the evolution of surface irregularities was studied. Experimental and numerical investigations of the neutral flow evaporated from the target surface showed a neutral density of {approx}10{sup 19} cm{sup -3} in the vicinity of the target and neutral velocities up to 2 x 10{sup 5} cm/s. Framing and streak images of visible light emission were used to study the temporal evolution of the target surface plasma and vapors. Time- and space-resolved spectroscopy was applied to determine the surface plasma density and temperature, which were found to be {approx}10{sup 14} cm{sup -3} and {<=}1 eV, respectively. Because of this small plasma density, electric fields in the plasma sheath are not sufficient to cause electrohydrodynamic instability of the liquid target surface. However, hydrodynamic instabilities due to the intense neutral flow observed in experimental and numerical studies are likely to be responsible for the growth of wavelike irregularities.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗