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At least 1,603 records · Page 89

Precipitation hardening of laser powder bed fusion Ti-6Al-4V

Here, the laser powder bed fusion (PBF-L) additive manufacturing (AM) community has dedicated significant efforts into process optimization and control for defect-free Ti-6Al-4V. As defects become less of an issue for PBF-L Ti-6Al-4V, the processing-structure-properties (PSP) relationships between AM microstructures can now be explored to optimize mechanical properties. Lower temperature aging treatments around 550 °C in wrought Ti-6A-4V have been historically understood to precipitation harden the α phase with an ordered, hexagonal close packed (HCP) α 2 phase. The α 2 phase existed as nanoscale Ti 3 Al precipitates coherent with the parent α phase. The goal of the present investigation was to implement a vacuum heat treatment of 545 °C for 100 hours on PBF-L Ti-6Al-4V. This vacuum heat treatment took place after an initial hot isostatic pressure (HIP) treatment that decomposed the as-built, martensitic microstructure. The vacuum aging successfully produced nanoscale precipitates of α 2 phase within α-laths, confirmed via atom probe tomography (APT). Microstructural-length scale and quasi-static mechanical properties were investigated by nanoindentation and uniaxial tensile tests of miniaturized test specimens. Given the sensitivity of Ti-6Al-4V mechanical properties to small changes in chemistry, all test specimens originated from the same build. The α 2 precipitation resulted in significantly harder α-laths (≈ 2 GPa) as measured via nanoindentation, as well as a relative yield and ultimate tensile strength increase of 60 MPa and 38 MPa, respectively. Analysis of Variance (ANOVA) of the datasets revealed no statistical differences in total elongation between the HIPed and HIPed + aged specimens, indicative of the aging treatment producing a net benefit of strength with no loss in ductility.

36 MATERIALS SCIENCE↗

Final Scientific/Technical Report Rapid Design and Manufacturing of High-Performance Materials for Turbine Blades

This research demonstrated the concept of carbide precipitation-strengthened refractory high entropy alloys (RHEA). The advantage of a precipitation strengthened alloy is all phases are in thermodynamic equilibrium promoting microstructural stability, and consequently retention of properties at elevated temperatures. Additionally, as with any precipitation strengthened – or age hardened alloy, components can be heat-treated after manufacturing to manipulate the microstructure and optimize properties for performance. This is an advantage of the precipitation strengthened alloys over composites and ceramics materials, where the microstructure and properties are essentially fixed upon the initial materials manufacturing stage. High throughput (HT), multi-scale computer modeling was used to identifying novel RHEA compositions with desired characteristics needed for precipitation strengthening. The results showed that carbides precipitated and consequently, the strength of the alloys (measured in compression) increased after heat-treatment, which is the desired effect. The project also demonstrated the feasibility of producing articles from RHEA by additive manufacturing (AM).

36 MATERIALS SCIENCE↗

Rapid Design and Manufacturing of High-Performance Materials for Turbine Blades

This research demonstrated the concept of carbide precipitation-strengthened refractory high entropy alloys (RHEA). The advantage of a precipitation strengthened alloy is all phases are in thermodynamic equilibrium promoting microstructural stability, and consequently retention of properties at elevated temperatures. Additionally, as with any precipitation strengthened – or age hardened - alloy, components can be heat-treated after manufacturing to manipulate the microstructure and optimize properties for performance. This is an advantage of the precipitation strengthened alloys over composites and ceramics materials, where the microstructure and properties are essentially fixed upon the initial materials manufacturing stage. High throughput (HT), multi-scale computer modeling was used to identifying novel RHEA compositions with desired characteristics needed for precipitation strengthening. Designs were validated by producing small ingots via are melting. The results showed that carbides precipitated and consequently, the strength of the alloys (measured in compression) increased after heat-treatment, which is the desired effect. The project also demonstrated the feasibility of producing articles from RHEA by additive manufacturing (AM). Electron beam melting (EBM) and laser direct energy deposition (L-DED) additive manufacturing methods, were explored with various processing parameters were interrogated for both methods. Sound (crack-free and dense) precipitation strengthened RHEA samples were produced via EDM AM, demonstrating the feasibility of the concept.

36 MATERIALS SCIENCE↗

Report on Evolution of Inconel 718 Following HFIR Irradiation

The report presents the microstructure and mechanical properties of 3D printed Inconel 718 after irradiation in the High Flux Isotope Reactor (HFIR) at Oak Ridge National Laboratory (ORNL) to assess its potential use as a structural material. The structural components near the outlets of several proposed reactor cores will experience significant neutron fluxes and outlet coolant temperatures ranging from the hot standby temperature of 300 °C to nearly 550 °C at the center of the part. These components must support the core in appropriate loading conditions and require structural analysis at relevant temperatures. In FY21, three heat treatments were designed and conducted to simplify the microstructure and to determine how each precipitating phase contributed to the overall strength. In FY21, baseline mechanical properties were measured from uniaxial tensile tests on subsize SS-J2 specimens at room temperature and at elevated temperatures of 300, 450, and 600 °C to serve a comparison to the irradiated properties. Four capsules containing 3D printed Inconel 718 were inserted into HFIR in FY21 for a matrix of two temperatures and two doses. The lower of the two doses was available for characterization in FY22. Multiple heat treatments of Inconel 718 irradiated to nominal conditions of 2 displacements per atom (dpa) at either 300 or 600 °C were strained with uniaxial tensile tests at the Irradiated Material Examination and Testing (IMET) Facility to discern the mechanical properties. Transmission electron microscopy was performed to correlate the observed mechanical properties with nanoscale features. The initially homogenous AM718-HM increased in strength at both irradiation temperatures based on a high density of nanometer-scale radiation-induced cavities at lower temperature and nucleation and growth of γ" precipitates at higher temperatures. The precipitate-hardened AM718-HT2 showed very small differences in strength before and after irradiation: the contribution to strength from γ" precipitates was replaced with dislocation loops. Because the radioactivity of the nickel superalloys from neutron activation limited the scope of the analysis, a feasibility study examined the possibility of an ultra-miniature specimen geometry, colloquially SS-Tiny (SS-T), for mechanical property determination using the nonirradiated Inconel 718. This study found an overestimation of ductility from the SS-T geometry with yield strength and ultimate tensile strength slightly above the SS-J2 geometry: this could be contributed to a reduction in specimen thickness.

36 MATERIALS SCIENCE↗

α-Quartz Phase Stabilization, Surface Texturing, and Tunable Optical Properties of Nanocrystalline GeO 2 Films Made by Pulsed-Laser Deposition: Implications for Optical and Optoelectronic Applications

Germanium oxide (GeO 2 ) has great potential in multifunctional devices and next-generation power electronics due to its high thermal conductivity and ambipolar doping capability. However, the complexity of synthesizing the desirable polymorph with a controlled phase, surface/interface quality, microstructure, and functional properties is the main barrier to GeO 2 utilization in advanced applications. Here, in this regard, we present a method to realize the hexagonal (h) or a-quartz type GeO 2 with nano-textured surface morphology on sapphire substrates using a hybrid synthesis strategy that comprises pulsed laser deposition (PLD) and post-deposition thermal annealing. We performed a comprehensive study to investigate the effect of annealing temperature, which was varied in a wide range (600-1100 °C), on the crystal structure, phase, surface morphology, chemical stoichiometry, defect states, and optical properties of PLD-grown GeO 2 films. As-deposited GeO 2 films at 500 °C were amorphous. Upon annealing, the GeO 2 films induced an amorphous-to-crystalline phase transformation; GeO 2 films annealed at higher annealing temperatures (≥900 °C) stabilized in the hexagonal phase and demonstrated excellent crystal quality and chemical stability. Thermally activated growth process showed increased average crystallite size, which was varied in the range of 20-130 (±2) nm, while the surface roughness followed a similar trend. The spectral transmittance and band gap also increased with increasing annealing temperature. The resulting h-GeO 2 films, particularly those obtained at annealing temperatures in the 900-1100 °C range, had a higher band gap of 6.2-6.3 eV and displayed excellent optical transmittance in the visible region. Moreover, the absence of extended valence band maxima and reduced optical defect density support the quality improvement upon annealing. When considering phase-pure bulk and nanostructured GeO 2 as a possible candidate for ultra wide band gap semiconductors in cutting-edge technological applications, the results of the current work can be beneficial to realize high structural and optical quality a-quartz structured GeO 2 films.

GeO2↗

Synthesis and properties of bulk cobalt-carbide permanent magnets

Nanocrystalline bulk Co-C permanent magnets were produced by rapid hot consolidation of ball milled powder precursors. Bulk magnets with an average grain size of 20 nm and densities up to 94 percent of the theoretical density were successfully processed at pressures exceeding 1 GPa for the first time. Their microstructural and magnetic properties along with their magnetocrystalline anisotropy values are reported. Presence of iron contamination that results from the use steel milling media in milling was confirmed by elemental mapping of the bulk magnets. It is concluded that iron bonds in the form of hematite and does not adversely affect coercivity values. Here, this study shows that the Co 3 C compound does possess a sizable magnetocrystalline anisotropy, making it a suitable candidate as a rare earth free permanent magnet.

Co3 C↗

Phase stability and mechanical properties of wire + arc additively manufactured H13 tool steel at elevated temperatures

Wire + arc additive manufacturing (WAAM) is considered an innovative technology that can change the manufacturing landscape in the near future. WAAM offers the benefits of inexpensive initial system setup and a high deposition rate for fabricating medium- and large-sized parts such as die-casting tools. Here, AISI H13 tool steel, a popular die-casting tool metal, is manufactured by cold metal transfer (CMT)-based WAAM and is then comprehensively analyzed for its microstructural and mechanical properties. Location-dependent phase combinations are observed, which could be explained by nonequilibrium thermal cycles that resulted from the layer-by-layer stacking mechanism used in WAAM. In addition, remelting and reheating of the layers reduces welding anomalies (e.g., pores and voids). The metallurgical characteristics of the H13 strongly correlate with the mechanical properties. The combinations of phases at different locations of the additively manufactured part exhibit a periodic microhardness profile. Martensite, Retained Austenite, Ferrite, and Carbide phases are found in combination at different locations of the part based on the part’s temperature distribution during additive deposition. Moreover, the tensile properties at elevated temperatures (23 °C, 300 °C, and 600 °C) are comparable to those from other WAAM and additive manufacturing (AM) processes. The X-ray diffraction results verify that the microstructural stability of the fabricated parts at high temperatures would allow them to be used in high temperatures.

36 MATERIALS SCIENCE↗

Influence of energy density on the microstructure, growth orientation, and anisotropy of magnetic properties in additively manufactured Fe-3.8wt%Si transformer steels

Fe-3.8wt%Si transformer steels were processed using two different additive manufacturing (AM) techniques, laser powder bed fusion (LPBF) and directed energy deposition (DED). While the LPBF processed samples exhibited a strong <001> orientation of the BCC grains along the build axis, the DED processed samples exhibited a randomized texture along the build axis. DED processed samples showed substantially coarser columnar grains as compared to their LPBF counterparts. Here, the columnar grains exhibited a substantial number of low-angle sub-grain boundaries. All samples exhibited very good soft magnetic properties, with saturation magnetization (M s ) values ranging from 205 - 232 emu/gm, and coercivity (H c ) values ranging from 1.2 – 4.2 Oe. The Coercivity (H c ) values were significantly lower when the magnetic field was applied parallel to the build axis, as compared to being perpendicular, which can be rationalized based on the columnar nature of the grains, resulting in a higher number density of grain boundaries in case of the field applied perpendicular to the build axis.

36 MATERIALS SCIENCE↗

Thermal Expansion and Thermal Conductivity of Rare Earth Silicates

Rare earth silicates are considered promising candidate materials for environmental barrier coatings applications at elevated temperature for ceramic matrix composites. High temperature thermophysical properties are of great importance for coating system design and development. In this study, the thermal expansion and thermal conductivity of hot-pressed rare earth silicate materials were characterized at temperatures up to 1400 C. The effects of specimen porosity, composition and microstructure on the properties were also investigated. The materials processing and testing issues affecting the measurements will also be discussed.

Zhu, Dongming↗

Achieving Grain Refinement and Related Mechanical Property Improvement of an Al-Zn-Mg-Cu Alloy Through Severe Plastic Deformation

Microstructural features and mechanical properties of an Al-Zn-Mg-Cu alloy processed by equal-channel angular pressing (ECAP) have been investigated. The equivalent plastic strain obtained from the simulation agrees well with that from the analytical calculation in a way that both increase with an increase in deformation, but the strain distribution is non-uniform, appearing as a strain gradient along the norm direction. Microstructure investigation shows that grain refinement is achieved in frequency of low-angle grain boundaries fabricated by ECAP. The pole density is reduced by ECAP, during which the Brass and Goss type textures are introduced. TEM results show chain-like recrystallized grains formed at the grain boundaries and broken second-phase particles come into being due to the heavy shear force. After ECAP, the hardness and strength increase significantly while the elongation is reduced. Besides, an extreme strengthening is confirmed because of the balance between dynamic hardening and softening. The microstructure evolution mechanism is revealed in terms of grain refinement, precipitate phase breakage and texture evolution.

36 MATERIALS SCIENCE↗

Correlation of SWIR imaging with LPBF 304L stainless steel part properties

In the Laser Powder Bed Fusion (LPBF) process, the local thermal history can vary significantly over a part as the heat transfer characteristics and the laser scan path are geometry dependent. The variations introduce the potential for defects that lead to part failure, some of which are difficult to identify non-destructively with common ex-situ evaluation techniques. These defects include significant microstructural and mechanical property differences in the part interiors. In this paper, thermal features are extracted from in-situ Short-Wave Infrared (SWIR) imaging measurements to compile voxel based part representations and understand how the complexities in the thermal history affect part performance. The deviations in thermal features due to different laser processing parameters and complex scan pathing are explored. Empirical correlations are developed to map thermal features with the engineering properties (bulk yield strength, area percentage porosity, and local state) of 304L stainless steel parts manufactured by LPBF. Processing modes (insufficient melting and keyholing) are determined by mapping part property measurements with multiple thermal features. Generating the relationships between thermographic measurements and resulting SLM part properties lays the foundation for in-situ part qualification.

36 MATERIALS SCIENCE↗

Mechanical behavior of post-processed Inconel 718 manufactured through the electron beam melting process

Here, the electron beam melting (EBM) process was used to fabricate Inconel 718. The microstructure and tensile properties were characterized in both the as-fabricated and post-processed state transverse (T-orientation) and longitudinal (L-orientation) to the build direction. Post-processing involved both a hot isostatic pressing (HIP) and solution treatment and aging (STA) to homogenize the microstructure. In the as-fabricated state, EBM Inconel 718 exhibits a spatially dependent microstructure that is a function of build height. Spanning the last few layers is a cored dendritic structure comprised of the products (carbides and Laves phase) predicted under equilibrium solidification conditions. With increasing distance from the build's top surface, the cored dendritic structure becomes increasingly homogeneous with complete dissolution of the secondary dendrite arms. Further, temporal phase kinetics are observed to lead to the dissolution of the strengthening γ"γ" and precipitation of networks of fine δ needles that span the grains. Microstructurally, post-processing resulted in dissolution of the δ networks and homogeneous precipitation of γ'"γ'" throughout the height of the build. In the as-fabricated state, the monotonic tensile behavior exhibits a height sensitivity within the T-orientation at both 20 and 650 °C. Along the L-orientation, the tensile behavior exhibits strength values comparable to the reference wrought material in the fully heat-treated state. After post-processing, the yield strength, ultimate strength, and elongation at failure for the EBM Inconel 718 were observed to have beneficially increased compared to the as-fabricated material. Further, as a result of post-processing the spatial variance of the ultimate yield strength and elongation at failure within the transverse direction decreased by 4 and 3× respectively.

36 MATERIALS SCIENCE↗

Effect of aging on failure mechanism of Alloy 709 at various temperatures

Alloy 709 is a novel austenitic stainless steel with high temperature creep strength, weldability, and corrosion resistance. These properties make the material suitable for applications in the structure of next-generation nuclear power plants. Enduring high temperatures for an extended period of time in the harsh environments of a nuclear power plant results in thermal aging of the material. Therefore, it is imperative to study the effect of thermal aging on the microstructure and mechanical properties of Alloy 709 before its application in the next generation power plants. In this study, hot-processed (forged + rolled), annealed and quenched ingots of Alloy 709 are aged at 650 °C for 2000 h in air and then tested at various temperatures up to 850 °C in an in-situ heating-loading Scanning Electron Microscope (SEM) equipped with Energy Dispersive Spectroscopy (EDS) and Electron Backscatter Diffraction (EBSD). The effect of testing temperature and aging on microstructural evolutions during tensile testing of as-received and aged samples are studied. Furthermore, both as-received and aged samples displayed serrations and drop in ductility at elevated temperatures, due to the effect of dynamic strain aging (DSA). The occurrence of DSA activity was found within temperatures range of 500 °C–750 °C in as-received and 550 °C - 650 °C in aged samples. The aged samples showed less elongation accompanied by shallower dimples on the fractured surface, indicating less ductile failure mechanism compared to as-received samples. Failure mechanism observations on the fracture surface using SEM fractography are correlated to the observations made on the sample surface using in-situ SEM to achieve a complementary set of information to better understand the failure mechanism of this novel alloy.

36 MATERIALS SCIENCE↗

Effects of Laves phase particles on recovery and recrystallization behaviors of Nb-containing FeCrAl alloys

The microstructures and mechanical properties of deformed and annealed Nb-containing FeCrAl alloys were investigated. Fine dispersion of Fe 2 Nb-type Laves phase particles was observed in the bcc-Fe matrix after applying a thermomechanical treatment, especially along grain/subgrain boundaries, which effectively stabilized the recovered and recrystallized microstructures compared with the Nb-free FeCrAl alloy. The stability of recovered areas increased with Nb content up to 1 wt%. The recrystallized grain structure in Nb-containing FeCrAl alloys consisted of elongated grains along the rolling direction with a weak texture when annealed below 1100 °C. An abnormal relationship between recrystallized grain size and annealing temperature was found. Microstructural inhomogeneity in the deformed and annealed states was explained based on the Taylor factor. Annealed Nb-containing FeCrAl alloys showed a good combination of strength and ductility, which is desirable for their application as fuel cladding in light-water reactors.

36 MATERIALS SCIENCE↗

Effects of Heating and Quenching Processing Parameters on Phase Transformation of 55CrMo Steel

Microstructure and mechanical properties after induction hardening have a significant effect on the wear resistance performance and lifetime of 55CrMo steel ball screw. In the paper, the dilatometric curves were recorded at the different heating rate by a Gleeble-1500D thermo-mechanical simulator to determine the effect of heating rate on the austenitizing temperature of 55CrMo steel. Heat treatment of some specimens was performed by the Gleeble-1500D thermal simulator at the different heating temperature, holding time and cooling rate to investigate the effect of induction hardening parameters on the phase transformation, microstructure and microhardness of 55CrMo steel. Microstructure of specimen was analyzed using an optical microscope and a scanning electron microscope. Volume fraction of retained austenite was measured using an x-ray diffractometer. The mechanical properties were evaluated by a microhardness tester. The results show that the austenitizing temperature of 55CrMo steel increases with the increasing heating rate. Increasing the heating temperature, holding time and cooling rate of specimen is helpful in obtaining a uniform cryptocrystalline martensite. Volume fraction of retained austenite is less as the heating temperature is in the range of 900-950 °C. In the induction hardening of 55CrMo steel, the heating temperature should be in the range of 900-1000 °C.

36 MATERIALS SCIENCE↗