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At least 1,513 records · Page 84
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

The Application of Differential Scanning Calorimetry to Investigate Precipitation Behavior in Nickel-Base Superalloys Under Continuous Cooling and Heating Conditions

In this study, a suite of experimental tools and fast-acting, numerical-simulation techniques was used to quantify the precipitation behavior of three nickel-base superalloys: IN-100, LSHR, and 718. Experimental methods comprised differential scanning calorimetry (DSC) to establish the specific heat as a function of temperature and selected direct-resistance heating trials (using a Gleeble ® machine) to obtain samples for microstructural analysis. For the DSC experiments, each alloy was cooled at a prescribed constant rate (between 5 and 20 K/min) after an initial soak/equilibration in the high-temperature, single-phase (supersolvus) temperature regime. On-heating DSC trials beginning at ambient temperature were also performed on alloy 718 in three different starting conditions: super- δ -solvus solution treated and water quenched (denoted as ST), solution treated and aged (STA), and solution treated and overaged (STOA). DSC results, revealing the thermal signatures associated with the kinetics of precipitation of γ ' (IN-100, LSHR) or γ ' and γ " (718), were interpreted using a previously-developed fast-acting routine that treats concurrent nucleation, growth, coarsening, and dissolution. For these simulations, special attention was paid to various thermo-kinetic input parameters including equilibrium solvus-approach curves, bulk free energies of transformation, matrix-precipitate interface energies, and effective diffusivities. For the γ - γ ' superalloys (IN-100 and LSHR), estimates of precipitate volume fraction as a function of temperature from the specific-heat data revealed semi-quantitative agreement with simulation predictions. For the γ - γ '- γ " superalloy (718), simulation predictions of precipitate volume fractions were converted to specific heat as a function of temperature and showed semi-quantitative agreement with the direct measurements.

36 MATERIALS SCIENCE↗
DOE OSTI2022

A New Recycled Al–Si–Mg Alloy for Sustainable Structural Die Casting Applications

The use of secondary aluminum for structural components in the automotive industry is limited by the high Fe contents in recycled alloys which often result in the formation of brittle β-Al 5 FeSi phase which reduces the ductility of aluminum castings. In this study, a new secondary Al-Si-Mg alloy with high Fe content (about 0.44 wt.%) was developed for die casting applications. Based on thermodynamic modeling, manganese was added to obtain a designed Fe-to-Mn ratio of 2 which successfully suppressed the formation of β-Al 5 FeSi phase, by forming α-Al 15 (Fe,Mn) 3 Si 2 phase with rounded or hexagonal morphology. Additionally, a fine needle-like π-Al 8 FeMg 3 Si 2 phase was also formed within the eutectic regions. The new recycled alloy showed comparable mechanical properties in as-cast and heat treated (T5 and T6) conditions to three major primary die cast alloys (≤ 0.2 wt.% Fe) with similar composition. Ductility up to 7.4% from tensile elongation was achieved in as-cast recycled alloy due to the modification and refinement of α-Al 15 (Fe,Mn) 3 Si 2 by Mn and Sr additions. Tensile elongation was further improved to 9.1% after T6 treatment as a result of dissolution of π-Al 8 FeMg 3 Si 2 phase, defragmentation of α-Al 15 (Fe,Mn) 3 Si 2 and the spheroidization of Si phase. This new alloy provides a promising path for increasing usage of recycled aluminum with high Fe content in structural die castings for automotive and other applications.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Microstructure Evolution of a Multimodal Gamma-Prime Ni-Based Superalloy Characterized by In Situ Diffraction

The relationship between the evolution of microstructure, deformation micromechanisms and mechanical properties is difficult to establish in multimodal size distribution $_γ$$'$ superalloys, as the microstructure evolves with both temperature and time, and multiple strengthening mechanisms across each size distribution contribute to mechanical performance. In situ X-ray scattering can offer unparalleled insight regarding microstructure evolution at the temperatures and stresses of importance to gas-turbine applications; however, in situ X-ray diffraction has not been applied to the study of multimodal $_γ$$'$ distribution superalloys. Herein, lattice parameter evolution of secondary and tertiary $_γ$$'$ precipitates in a representative superalloy, Nimonic 115, is determined between 750 °C and 950 °C and correlated to room-temperature SEM and microhardness values. A large positive lattice parameter misfit of secondary $_γ$$'$ induces precipitate splitting, and the tertiary $_γ$$'$ goes into dissolution at ~ 800 °C, but with little apparent change in hardness values. The volume fraction of $_γ$$'$ decreases above 900 °C and precipitate-matrix coherency is lost, and there is a corresponding decrease in microhardness values. Importantly, the diffraction analysis demonstrates the capability to determine critical microstructural parameters of both precipitate size distributions in situ, representing an additional tool for determining microstructure-mechanical property relationships of multimodal superalloys.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Manufacturing of Dysprosium-Iron Alloys by Electrolysis in Fluoride-Based Electrolytes. Electrolysis in a Laboratory-Scale Cell

Electrolytic production of light rare earth elements and rare earth alloys with transition elements takes place in a fluoride-based electrolyte using rare earth oxides as raw material. The optimization of this method, mainly in terms of the energy efficiency and environmental impact control, is rather challenging. Anode effects, evolution of fluorine-containing compounds and side cathode reactions could largely be minimized by good control of the amount of rare earth oxide species dissolved in the fluoride-based electrolyte and their dissolution rate. The Dy{sub 2}O{sub 3} feed rate needed for stable cell operation was studied by following up the anode voltage and gas analysis. On-line analysis of the cell off-gases by FTIR showed that the electrochemical reaction for the formation of Dy-Fe alloy gives mainly CO gas and that CF{sub 4} is starting to evolve gradually at anode voltages of ca. 3.25 V. The limiting current density for the discharge of the oxide ions at the graphite anode was in the range of 0.1 to 0.18 A cm{sup −2} at dissolved Dy{sub 2}O{sub 3} contents of ca. 1 wt pct. Modeling of the laboratory cell reactor was also carried out by implementing two models, i.e., an electrical model simulating the current density distribution at the electrodes and a laminal bubbly flow model that explains the electrolyte velocity induced by gas bubble production at the anode.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Thermodynamic Study on MgO Solubility in High-Alumina-Content Slag System

In the current study, the MgO solubility in molten slag was measured to clarify the effect of basicity and Al{sub 2}O{sub 3} content on the MgO solubility equilibrating with the spinel solid phase in the CaO-SiO{sub 2}-Al{sub 2}O{sub 3} system. The MgO solubility decreased with the increasing basicity of the slag. However, the MgO solubility in the spinel equilibrium region exhibited different dependence when compared with the basicity dependence in the MgO equilibrium region. The aforementioned experimental results were quantitatively analyzed using magic-angle spinning (MAS) {sup 27}Al nuclear magnetic resonance (NMR) spectroscopy, in which the fraction of Al ions in the slag of spinel equilibrium region was changed to 4, 5, and 6. In addition, the analysis of the degree of Al avoidance modeling indicated that the change in bridging oxygen (BO) linkage species (distinguished into Al-O-Al, Si-O-Si, and Al-O-Si) was based on the Al/Si ratio change. The aforementioned change in BO linkage species led to a change in the MgO solubility with the stability of the alumina. Thus, the spinel equilibrium dissolution mechanism is discussed in detail in terms of the thermodynamic and structural influence in molten slag.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Yttria-Stabilized Zirconia Aided Electrochemical Investigation on Ferric Ions in Mixed Molten Calcium and Sodium Chlorides

Electrolytic reduction of dissolved iron oxide to metal iron in molten salts with an inert anode is an alternative short route for steelmaking without CO{sub 2} emissions. A novel and simple integrated yttria-stabilized zirconia (YSZ) cell was constructed from a YSZ tube with a closed end. The YSZ tube played multiple functions, including the container for the molten salts, the solid electrolyte membrane in the O{sup 2−}|YSZ|Pt|O{sub 2} (air) reference electrode (RE), and the solid electrolyte membrane between the working and counter electrodes (WE and CE). Electrochemical behavior of ferric ions (Fe{sup 3+}) that were formed by dissolution of 0.5 wt pct Fe{sub 2}O{sub 3} in the molten CaCl{sub 2}-NaCl eutectic mixture was investigated on a Pt WE at 1273 K by various electrochemical techniques including cyclic voltammetry, linear scan voltammetry, square wave voltammetry, chronopotentiometry, chronoamperometry, and potentiostatic electrolysis. Analysis of the mechanism of electrode reactions was further assisted by scanning electron microscopy, energy dispersive X-ray spectroscopy, and X-ray diffraction. Some electrochemical parameters were obtained, including the number of exchanged electrons and the diffusion coefficient of ferric ions in the mixed molten salts. The results from various electrochemical techniques are in good agreement with each other, and show that the electrochemical reduction of Fe{sup 3+} to Fe in the molten salt mixture could be a single three-electron transfer step and diffusion-controlled reaction that was also possibly reversible. This work may form the foundation for extraction of iron and alloys from molten salts and also provide a stable O{sup 2−}|YSZ|Pt|O{sub 2} (air) RE with wide applicability for investigation on electrochemical properties of other electroactive metal oxides in molten salts.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Zinc Removal from Basic Oxygen Steelmaking Filter Cake by Leaching with Organic Acids

The dust generated from the basic oxygen steelmaking (BOS) process is a waste material mainly containing iron that cannot be recycled owing to its high zinc content. In this study, the leaching effects of different organic acids are compared, with the aim of determining an acid that selectively leaches and removes zinc from BOS dust, so that the waste material can be recycled into ironmaking and steelmaking processes in order to substitute part of the raw materials of steelmaking. The dust used in this study was scrubbed and collected in the form of a filter cake. The acids tested were oxalic, citric, acetic, propionic, butyric, and valeric acids. Butyric acid was found to be the most effective, with a high zinc extraction level of 49.7 pct and a low iron level of only 2.5 pct. Oxalic acid was the least effective leaching reagent for both zinc and iron extractions, owing to the formation of zinc and iron oxalate precipitates following metal dissolution. The filter cake and leached residues were characterized by chemical analysis, X-ray diffraction, X-ray photoelectron spectroscopy, and scanning electron microscopy with energy dispersive spectroscpopy.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Formation Mechanisms and Leachability of Hexavalent Chromium in Cr{sub 2}O{sub 3}-Containing Refractory Castables of Electric Arc Furnace Cover

Cr (III)-containing refractories are widely used as electric-arc furnace cover because of their excellent corrosion resistance properties. However, the formation of hexavalent chromium [Cr(VI)] remains a matter of concern during the service and subsequent disposal of the spent refractories. Moreover, the Cr(VI) formation mechanism and total amount of Cr(VI) generated are not clearly understood. In this study, samples from different parts of a spent electric arc furnace cover were collected from a local integrated steel plant. The phase composition, microstructure, formation and leachability of Cr(VI) were investigated using X-ray photoelectron spectroscopy, X-ray diffraction, scanning electron microscopy with energy dispersive X-ray spectroscopy, and TRGS 613 leaching test (Technische Regeln für Gefahrstoffe-TRGS 613-October 2002)/multiple leaching tests. A Cr(VI)-containing phase namely CaCrO{sub 4} existed in the sample at a medium temperature range, while another Cr(VI)-containing phase namely hauyne (Ca{sub 4}Al{sub 6}CrO{sub 16}) and a Cr(III)-containing phase (Al{sub 2}O{sub 3}–Cr{sub 2}O{sub 3} solid solution) formed in the high temperature region. Concentrations of Cr(VI) in the leachates (as in the TRGS 613 procedure) exceeded the European permissible limit. During the leaching tests in an acid condition, Cr(VI) was reduced by Fe{sup 2+}, which was primarily derived from the dissolution of FeO in the samples, while more Cr(VI) leached out with distilled water. Formation of an Al{sub 2}O{sub 3}–Cr{sub 2}O{sub 3} solid solution can inhibit Cr(VI) generation.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Microstructural Modeling of the α + β Phase in Ti-6Al-4V: A Diffusion-Based Approach

Complex heat treatment operations and advanced manufacturing processes such as laser or electron-beam welding will see the metallic workpiece experience a considerable range of temperatures and heating/cooling rates. These intrinsic conditions will have a significant bearing upon the microstructure of the material, and in turn upon the thermo-mechanical properties. In this work, a diffusion-based approach to model the growth and shrinkage of precipitates in the alpha + beta field of the common titanium alloy Ti-6Al-4V is established. Further, the numerical model is extended using a JMA-type approach to explore the dependency of the beta-transus temperature on extremely high heating rates, whereby dissolution alone is too slow to accurately describe the alpha to beta-phase transformation. Experimental heat treatments at rates of 5, 50, and 500 °C/s were performed, and metallographic analysis of the samples was used to validate the numerical modeling framework predictions for lamellar shrinkage, while data from the literature has been used to evaluate the numerical modeling framework for the growth of equiaxed microstructures. The agreement between measurements and numerical predictions was found to be good.

36 MATERIALS SCIENCE↗
DOE OSTI2022

A Large Eddy Simulation Study of Flow Turbulence, Alumina Transport, and Bath Temperature Evolution in Conventional Aluminum-Smelting Cell Using OpenFOAM

In this study, a Large Eddy Simulation (LES) of the aluminum-smelting process is performed using OpenFOAM. To understand the coupled behavior of heat transfer, mass transfer, and flow of the smelting process, a multi-physics computational fluid dynamics (CFD) model based on the Eulerian–Eulerian multi-fluid approach is adopted. The model accounts for CO 2 bubble and magnetohydrodynamics (MHD)-driven flow, along with alumina dissolution, transport, and bath temperature evolution. The simulation predictions show small-scale turbulent vortical structures in the anode–cathode space caused by combined effect of MHD and CO 2 bubble-bath interactions and relatively large-scale asymmetric vortices in the inter-anode space caused by the CO 2 bubble-bath interactions. The vortex formation at the edges of the anodes evidently aids in transporting alumina from the central channel to the bottom of the anodes and prevents accumulation of gas bubbles in the periphery of the anode bottom. Symmetric bath cold spots are observed in the vicinity of the feeder. Cold spots are also observed in the anode–cathode distance space below the anode bottom due to the transport of undissolved solid to this region by the flow. The findings from the work are useful in developing and designing alumina-feeding strategy leading to reduced anode effects and smooth operation of the cell. The work also highlights the important flow structures in conventional aluminum-smelting cell.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Effect of Microstructural Evolution on Sagging Behavior of Cold-Rolled Aluminum Foil During the Brazing Thermal Cycle

Effect of microstructural evolution on sagging behavior of aluminum foil was investigated during the brazing thermal cycle. During the brazing thermal cycle, the sagging behavior consists of three stages: slight sagging stage, accelerative sagging stage and slow sagging stage. The sagging of cold-rolled aluminum foil mainly occurs in the accelerative sagging stage, which is governed by recovery under external stress in the sagging test. The coarse recrystallized grain is responsible for the slow sagging stage by reducing grain boundary sliding. Increasing cold-rolled reduction and addition of final annealing heat treatment can improve sagging resistance by shortening recovery process during the brazing thermal cycle. Dissolution of dispersoids has few effects on sagging deformation.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Corrosion Behavior of Carbon Steel Coated with Octadecylamine in the Secondary Circuit of a Pressurized Water Reactor

Corrosion and particle deposition in the secondary circuits of pressurized water reactors can be mitigated by alternative water chemistries featuring film-forming amines. In the present work, the corrosion of carbon steel in secondary side water with or without octadecylamine (ODA) is studied by in situ electrochemical impedance spectroscopy, combined with weight loss/gain measurements, scanning electron microscopy and glow-discharge optical emission spectroscopy. The impedance spectra are interpreted using the mixed-conduction model to extract kinetic parameters of oxide growth and metal dissolution through it. From the experimental results, it can be concluded that ODA addition reduces the corrosion rate of both fresh and pre-oxidized carbon steel in secondary circuit significantly by slowing down both interfacial reactions and transport through the oxide layer.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Microstructural and Electrochemical Evaluation of Fusion Welded Low-Nickel and 304 SS at Different Heat Input

The present research study investigates the effect of heat input using E 308 electrode (controlled by welding current, i.e., 70, 85 and 100 A) on microstructure, mechanical properties and corrosion behavior of low-nickel and 304 stainless steel (SS) weldments produced by shielded metal arc welding technique. SEM investigation shows that with the higher heat input, δ-ferrite content was reduced. Dendrite and inter-dendritic length is also reduced by lowering the heat input. For all the heat inputs, it is observed that δ-ferrite content was higher in 304 stainless steel (SS) as compared to that of low-nickel austenitic stainless steel (Cr-Mn SS). Considering the heat input for Cr-Mn SS, coarse grains were observed in the heat-affected zone region. For low heat input (LHI), tensile fracture surface has exhibited river-like pattern with dimple appearance. Corrosion studies show better pitting resistance for low heat input (LHI) samples due to higher δ-ferrite present in the weld region. Similarly, higher interphase corrosion resistance is observed in both the SS grades causing more dissolution in the LHI samples.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Heavy Deformation of Patented Near-Eutectoid Steel

Evolution of microstructure in the patented near-eutectoid steel, forged under varying situations, is critically examined in the present investigation. Steel with 0.74 wt.% carbon is isothermally annealed at 500 °C to obtain fine pearlite microstructure. Steel samples, so patented, are subjected to mechanical deformation by forging at various temperatures with different amount of thickness reduction. Microstructural analyses have revealed that mechanical deformation by forging at lower temperatures brings about partial dissolution of cementite, which is followed by the formation of ε-carbide in the microstructures. In contrast, cementite is precipitated within ferrite matrix upon warm or hot forging at higher temperatures. It is further observed that increasing deformation percent during low-temperature forging reduces interlamellar spacing of pearlite, whereas an opposite trend is noticed in case of deformation at higher temperature; moreover, deformation induced the change in interlamellar spacing and formation of fine carbide phases in microstructures has caused appreciable enhancement in hardness of the steel.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Austenitic Reversion of Cryo-rolled Ti-Stabilized Austenitic Stainless Steel: High-Resolution EBSD Investigation

In this study, AISI 321 austenitic stainless steel (ASS) was cryo-rolled and subsequently annealed at 650 and 800 °C to reverse BCC α′-martensite to FCC γ-austenite. The texture evolution associated with the reversion at the selected temperatures was investigated using high-resolution EBSD. After the reversion, TiC precipitates were observed to be more stable in 650 °C-annealed specimens than those reversed at 800 °C. {110} texture was mainly developed in specimens subjected to both annealing temperatures. However, specimens reversed at 650 °C have stronger texture than those annealed at 800 °C, even at the higher annealing time. The strong intensity of {110} texture component is attributed to the ability of AISI 321 ASS to memorize the crystallographic orientation of the deformed austenite, a phenomenon termed texture memory. The development of weaker texture in 800 °C-annealed specimens is attributed to the residual strain relief in grains, dissolution of grain boundary precipitates, and an increase in atomic migration along the grain boundaries. Based on the observed features of the reversed austenite grains and estimation from an existing model, it is suspected that the austenite reversion at 650 and 800 °C undergone diffusional and martensitic shear reversion, respectively.

36 MATERIALS SCIENCE↗
DOE OSTI2018

The Effect of Titanium Dioxide (TiO{sub 2}) Nanoparticles on Hydroxyapatite (HA)/TiO{sub 2} Composite Coating Fabricated by Electrophoretic Deposition (EPD)

Composite coatings of Hydroxyapatite (HA) with ceramics, polymers and metals are used to modify the surface structure of implants. In this research, HA/TiO{sub 2} composite coating was fabricated by electrophoretic deposition (EPD) on 316 stainless steel substrate. HA/TiO{sub 2} composite coatings with 5, 10 and 20 wt.% of TiO{sub 2}, deposited at 40 V and 90 s as an optimum condition. The samples coated at this condition led to an adherent, continuous and crack-free coating. The influence of TiO{sub 2} content was studied by performing different characterization methods such as scanning electron microscopy (SEM), energy dispersive x-ray spectroscopy (EDS), corrosion resistance in simulated body fluid (SBF), coating’s dissolution rate in physiological solution and bond strength to the substrate. The results showed that the higher amount of TiO{sub 2} in the composite coating led to increase in bond strength of coating to stainless steel substrate from 3 MPa for HA coating to 5.5 MPa for HA-20 wt.% TiO{sub 2} composite coating. In addition, it caused to reduction of corrosion current density of samples in the SBF solution from 18.92 μA/cm{sup 2} for HA coating to 6.35 μA/cm{sup 2} for HA-20 wt.% TiO{sub 2} composite coating.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Interaction Between Liquid Silver and Graphene-Coated SiC Substrate

Wettability between liquid Ag and graphene-coated SiC single crystal has been investigated by dispensed drop method at T = 970 °C under vacuum accompanied with subsecond recording of the drop/substrate images (100 frames per second) by high-speed high-resolution CCD camera. Non-contact heating method coupled with capillary purification of the Ag drop procedure has been applied. Scanning electron microscopy combined with EDS analysis and scanning probe microscopy combined with Raman spectroscopy techniques has been utilized for microstructure and surface characterization of samples before and after high-temperature wetting tests. Immediately after its detachment from the capillary, the Ag drop showed non-wetting behavior (θ > 90°) forming a high contact angle of θ = 114°. Surface characterization of the drop surface after wettability tests evidenced the presence of graphene and Si transferred from the substrate to the top of Ag drop. These findings suggest chemical interaction phenomena occurring at the interface. Locally, an intimate contact between liquid Ag and SiC substrate was allowed by the appearance of discontinuities in the graphene layer basically produced by thermomechanical stress. Local dissolution of carbon into liquid Ag and its reorganization (by segregation, nucleation and growth) as secondary graphene layer at the Ag surface was also observed.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Characterizing the Effect of Thermal Processing on Feedstock Al Alloy Powder for Additive Manufacturing Applications

Gas-atomized metallic powders are commonly used in additive manufacturing processes. Research has shown that, for certain AM techniques, the chemistry and microstructural properties of the feedstock powders significantly affect the properties of the consolidated material. Understanding the powder characteristics before use in additive manufacturing can lead to optimizing properties of additively manufactured materials as well as determining the recyclability of feedstock powders. This research studies the effect of various solution treatment processes on the characteristics and microstructural evolution of powder aluminum alloy 6061. Solution treatment times and temperatures were guided by thermodynamic and kinetic modeling. Light microscopy, scanning electron microscopy, and hardness were used to evaluate each condition in both two and three dimensions. Results indicate that the Mg{sub 2}Si present in the untreated condition dissolves after 60 min of solution treatment, while there are competing effects from the dissolution and concurrent growth of various Fe-containing phases. Additionally, it is shown that both granular and sub-granular structures exist in these rapidly solidified powders, and the sub-grains reorient themselves during solution treatment.

36 MATERIALS SCIENCE↗