<Emphasis Type="Italic">In-Situ</Emphasis> Electrochemical Investigations of a Nickel-Based Alloy Subjected to Fatigue

The HASTELLOY C2000 superalloy is a commercially designed superalloy manufactured to function in reducing and oxidizing corrosive solutions. The industrial applications have tremendous potential in automotive, structural, aviation, and storage components. Although C2000 demonstrates good reducing and oxidizing traits in extremely aggressive media (which are attractive features of its chemistry), changes in the mechanical properties are believed to be insignificant due to its strong propensity to passivate under corrosive conditions. The ductility behavior and corrosion properties of C2000 are superior to those of stainless steels. The objective of the present study is to examine the corrosion-fatigue behavior of C2000 in a 3.5 wt pct sodium-chloride (NaCl) solution. C2000 submerged in 3.5 wt pct NaCl at room temperature is not susceptible to localized corrosion, such as pitting, during fatigue. At an accelerated potential of 350 mV, the current responses show an increase in the current due to slip steps emerging to the surface as a result of fatigue. The crack-initiation site and the examination of the fracture morphology are discussed. This article is based on a presentation given in the symposium entitled “Deformation and Fracture from Nano to Macro: A Symposium Honoring W.W. Gerberich’s 70th Birthday,” which occurred during the TMS Annual Meeting, March 12–16, 2006 in San Antonio, Texas and was sponsored by the Mechanical Behavior of Materials and Nanomechanical Behavior Committees of TMS.

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Slip-System-Related Dislocation Study from <Emphasis Type="Italic">In-Situ</Emphasis> Neutron Measurements

A combined experimental/computational approach is employed to study slip-system-related dislocation-substructure formation during uniaxial tension of a single-phase, face-centered-cubic (fcc), nickel-based alloy. In-situ neutron-diffraction measurements were conducted to monitor the peak-intensity, peak-position, and peak-broadening evolution during a displacement-controlled, monotonic-tension experiment at room temperature. The measured lattice-strain evolution and the macrostress/macrostrain curves were used to obtain the material parameters required for simulating the texture development by a visco-plastic self-consistent (VPSC) model. The simulated texture compared favorably with experimentally-determined texture results over a range of 0 to 30 pct engineering strain. The grain-orientation-dependent input into the Debye-intensity ring was considered. Grains favorably oriented relative to the two detector banks in the geometry of the neutron experiment were indicated. For the favorably oriented grains, the simulated slip-system activity was used to calculate the slip-system-dependent, dislocation-contrast factor. The combination of the calculated contrast factor with the experimentally-measured peak broadening allows the assessment of the parameters of the dislocation arrangement within the specifically oriented grains, which has a quantitative agreement with the transmission-electron-microscopy results. This article is based on a presentation given in the symposium entitled “Neutron and X-Ray Studies for Probing Materials Behavior,” which occurred during the TMS Spring Meeting in New Orleans, LA, March 9–13, 2008, under the auspices of the National Science Foundation, TMS, the TMS Structural Materials Division, and the TMS Advanced Characterization, Testing, and Simulation Committee.

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<Emphasis Type="Italic">In-Situ</Emphasis> Investigation of Local Boundary Migration During Recrystallization

A combination of electron channeling contrast (ECC) and electron backscatter diffraction pattern (EBSP) techniques has been used to follow in situ the migration during annealing at 323 K (50 °C) of a recrystallizing boundary through the deformed matrix of high-purity aluminum rolled to 86 pct reduction in thickness. The combination of ECC and EBSP techniques allows both detailed measurements of crystallographic orientations to be made, as well as tracking of the boundary migration with good temporal resolution. The measured boundary velocity and the local boundary morphology are analyzed based on calculations of local values for the stored energy of deformation. It is found that the migration of the investigated boundary is very complex with significant spatial and temporal variations in its movement, which cannot directly be explained by the variations in stored energies, but that these variations relate closely to local variations within the deformed microstructure ahead of the boundary, and are found related to the local spatial arrangements and misorientations of the dislocation boundaries. The results of the investigation suggest that local analysis, on the micrometer length scale, is necessary for the further understanding of recrystallization boundary migration mechanisms.     

Thermodynamics and Kinetics to Alloying Addition on <Emphasis Type="Italic">In-Situ</Emphasis> AlN/Mg Composites Synthesis <Emphasis Type="Italic">via</Emphasis> Displacement Reactions in Liquid Mg Melt

Based on the Wilson equation, extended Miedema model, and hard sphere theory, new models are developed theoretically only using the quantities of the pure component and are applied to investigate the thermodynamical and kinetic effect of alloying additions on in-situ AlN formation via displacement reaction in Mg-Al alloy melt. The results show that the alloying additions such as Si, Zn, and Cu can promote the formation of AlN in Mg-Al melt both in thermodynamics and kinetics. Meanwhile, other elements, including Mn, Nd, Ce, Ni, and La, must be matched properly in order to produce the desired reinforcement AlN in liquid Mg-Al melt.     

A Developed Method for Fabricating <Emphasis Type="Italic">In-Situ</Emphasis> TiC<Subscript><Emphasis Type="Italic">p</Emphasis></Subscript>/Mg Composites by Using Quick Preheating Treatment and Ultrasonic Vibration

Quick preheating treatment of the Al-Ti-C pellets and high-intensity ultrasonic vibration are introduced in the fabrication of in-situ TiC _p /Mg composites. Al-Ti-C pellets are preheated for about 130 seconds in the furnace at 1023 K (750 °C), in which magnesium is melted as well. In this process, plenty of heat can be accumulated due to the reactive diffusion between liquid aluminum and solid titanium in Al-Ti-C, and a small amount of Al₃Ti phase is formed as well. After adding the preheated Al-Ti-C into the molten magnesium, thermal explosion takes place in a few seconds. In the meantime, high-intensity ultrasonic vibration is applied into the melt to disperse in-situ formed TiC particles into the matrix and degas the melt as well. Microstructural characterization indicates that in-situ formed TiC particles are spherical in morphology and smaller than 2 μm in size. Furthermore, a homogeneous microstructure with low porosity of the magnesium composite is obtained due to the effect of ultrasonic vibration. A novel approach using the quick preheating treatment technique and high-intensity ultrasonic vibration to synthesize in-situ TiC _p /Mg composites is proposed in our research.     

Characterization of Damage Evolution in SiC Particle Reinforced Al Alloy Matrix Composites by <Emphasis Type=Italic>In-Situ</Emphasis> X-Ray Synchrotron Tomography

We carried out a detailed investigation of the damage behavior of SiC particle reinforced 2080 Al alloy matrix composites by in-situ X-ray synchrotron tomography. We studied the tensile damage behavior of a peak-aged aluminum matrix composite. The main damage mode was SiC particle fracture with a very small contribution from void growth. The onset of damage takes place very close to the ultimate tensile strength of the composite. Particle fracture damage is stochastic in nature and is confined to a small distance from the fracture plane. Minimal void growth is observed, primarily at pre-existing microscopic voids from processing. Microstructure-based simulations, based on two-dimensional (2-D) images from the tomography data sets, show the importance of particle distribution and morphology on the evolution of plastic strain and damage in the composite.     

<Emphasis Type="Italic">In-Situ</Emphasis> Analysis of Coarsening during Directional Solidification Experiments in High-Solute Aluminum Alloys

Coarsening within the mushy zone during continuous directional solidification experiments was studied on an Al-30 wt pct Cu alloy. High brilliance synchrotron X-radiation microscopy allowed images to be taken in-situ during solidification. Transient conditions were present during directional solidification. Under these conditions, solute-rich settling liquid flow affects the dendritic array and thus coarsening. Coarsening was studied by following the secondary dendrite arm spacing (SDAS) of a developing dendrite at different local solidification times according to the mush depth and instant interface velocity. Solute enrichment and liquid flow cause deceleration and acceleration of the solidification front, which in turn influences both the mush depth and local growth and coarsening due to variations in solutal gradients and thus local undercooling. In addition, spacing between neighboring dendrites (i.e., primary dendrite arm spacing), which determines permeability within the mushy zone, affects the development of high-order branches. This article is based on a presentation given at the International Symposium on Liquid Metal Processing and Casting (LMPC 2007), which occurred in September 2007 in Nancy, France.     

Water Network in Room-Temperature Ionic Liquid: <Emphasis Type="Italic">N,N</Emphasis>-Diethyl-<Emphasis Type="Italic">N</Emphasis>-Methyl-<Emphasis Type="Italic">N</Emphasis>-2-Methoxyethyl Ammonium Tetrafluoroborate

Crystal structures of room-temperature ionic liquid (RTIL)-H₂O mixtures are determined by the X-ray diffraction method. The RTIL is N,N-diethyl-N-methyl-N-2-methoxyethyl ammonium tetrafluoroborate, [DEME][BF₄]. At 0.9 mol pct H₂O, two kinds of superstructures occur simultaneously without a strain. Also, the volume of the unit cell is very small only at 0.9 mol pct additives. This relates to the composite domain structure, including a twin-related one, as an elastic anomaly. At other water concentrations, such an extraordinary behavior is not observable. By assuming a sublattice having an equivalent lattice constant, a water network at 1 mol pct H₂O is simulated using a Monte Carlo (MC) method. The network develops over the medium range in the simulation box.     

Precipitation in Nb-Stabilized Ferritic Stainless Steel Investigated with <Emphasis Type="Italic">in-situ</Emphasis> and <Emphasis Type="Italic">ex-situ</Emphasis> Transmission Electron Microscopy

A Nb-stabilized Fe-15Cr-0.45Nb-0.010C-0.015N ferritic stainless steel is studied with transmission electron microscopy (TEM) to investigate the morphology and kinetics of precipitation. Nb_x(C,N)_y\hbox{Nb}_{x}\hbox{(C,N)}_y and MnS precipitates are present in the steel in the initial condition. Ex-situ TEM analysis is performed on samples heat treated at 973 K, 1073 K, 1173 K, and 1273 K (700 °C, 800 °C, 900 °C, and 1000 °C). Within this temperature range, both Fe₂Nb\hbox{Fe}_2\hbox{Nb} and Fe₃Nb₃X_x\hbox{Fe}_{3}\hbox{Nb}_{3}\hbox{X}_{x} (with X = C or N) precipitates form. Fe₂\hbox{Fe}_2Nb is observed at 1073 K (800 °C).   Fe₃Nb₃X_x\;\hbox{Fe}_{3}\hbox{Nb}_{3}\hbox{X}_{x} precipitates form at the grain boundaries between 973 K and 1273 K (700 °C and 1000 °C). Up to at least 1173 K (900 °C) their fraction increases with time and temperature, but at 1273 K (1000 °C) they lose stability with respect to Nb_x(C,N)_y.\hbox{Nb}_{x}\hbox{(C,N)}_{y}. With in-situ TEM, no phase transition is observed between room temperature and 1243 K (970 °C). At 1243 K (970 °C) the precipitation of Fe₃Nb₃X_x\hbox{Fe}_{3}\hbox{Nb}_{3}\hbox{X}_{x} is observed in the neighborhood of a dissolving Nb₂\hbox{Nb}_2(C,N) precipitate. For sections of grain boundaries where no Nb_x(C,N)_y\hbox{Nb}_x\hbox{(C,N)}_y precipitates are present, Fe₃Nb₃X_x\hbox{Fe}_3\hbox{Nb}_3\hbox{X}_{x} does not form. It is concluded that the precipitation of Fe₃Nb₃X_x\hbox{Fe}_{3}\hbox{Nb}_{3}\hbox{X}_x is directly related to the dissolution of Nb₂\hbox{Nb}_2(C,N) through the redistribution of C or N.     

High-Temperature Phase Equilibria of Duplex Stainless Steels Assessed with a Novel <Emphasis Type="Italic">In-Situ</Emphasis> Neutron Scattering Approach

Duplex stainless steels are designed to solidify with ferrite as the parent phase, with subsequent austenite formation occurring in the solid state, implying that, thermodynamically, a fully ferritic range should exist at high temperatures. However, computational thermodynamic tools appear currently to overestimate the austenite stability of these systems, and contradictory data exist in the literature. In the present work, the high-temperature phase equilibria of four commercial duplex stainless steel grades, denoted 2304, 2101, 2507, and 3207, with varying alloying levels were assessed by measurements of the austenite-to-ferrite transformation at temperatures approaching 1673 K (1400 °C) using a novel in-situ neutron scattering approach. All grades became fully ferritic at some point during progressive heating. Higher austenite dissolution temperatures were measured for the higher alloyed grades, and for 3207, the temperature range for a single-phase ferritic structure approached zero. The influence of temperatures in the region of austenite dissolution was further evaluated by microstructural characterization using electron backscattered diffraction of isothermally heat-treated and quenched samples. The new experimental data are compared to thermodynamic calculations, and the precision of databases is discussed.     

History Dependence of the Microstructure on Time-Dependent Deformation During <Emphasis Type="Italic">In-Situ</Emphasis> Cooling of a Nickel-Based Single-Crystal Superalloy

Time-dependent plastic deformation through stress relaxation and creep deformation during in-situ cooling of the as-cast single-crystal superalloy CMSX-4^® has been studied via neutron diffraction, transmission electron microscopy, electro-thermal miniature testing, and analytical modeling across two temperature regimes. Between 1000 °C and 900 °C, stress relaxation prevails and gives rise to softening as evidenced by a decreased dislocation density and the presence of long segment stacking faults in γ phase. Lattice strains decrease in both the γ matrix and γ′ precipitate phases. A constitutive viscoplastic law derived from in-situ isothermal relaxation test under-estimates the equivalent plastic strain in the prediction of the stress and strain evolution during cooling in this case. It is thereby shown that the history dependence of the microstructure needs to be taken into account while deriving a constitutive law and which becomes even more relevant at high temperatures approaching the solvus. Higher temperature cooling experiments have also been carried out between 1300 °C and 1150 °C to measure the evolution of stress and plastic strain close to the γ′ solvus temperature. In-situ cooling of samples using ETMT shows that creep dominates during high-temperature deformation between 1300 °C and 1220 °C, but below a threshold temperature, typically 1220 °C work hardening begins to prevail from increasing γ′ fraction and resulting in a rapid increase in stress. The history dependence of prior accumulated deformation is also confirmed in the flow stress measurements using a single sample while cooling. The saturation stresses in the flow stress experiments show very good agreement with the stresses measured in the cooling experiments when viscoplastic deformation is dominant. This study demonstrates that experimentation during high-temperature deformation as well as the history dependence of the microstructure during cooling plays a key role in deriving an accurate viscoplastic constitutive law for the thermo-mechanical process during cooling from solidification.     

<Emphasis Type="Italic">In-Situ</Emphasis> Neutron Diffraction Studies of Micromechanical Behavior in a Friction Stir Welded AA7475-T761

An in-situ neutron diffraction technique was used to investigate the lattice strain distributions and micromechanical behavior in a friction stir welded (FSW) sheet of AA7475-T761. The neutron diffraction experiments were performed on the spectrometer for material research, STRESS-SPEC, at FRM II (Garching, Germany). The lattice strain profiles around the weld center were measured as a function of the applied strain during the tensile loading and unloading. The anisotropic elastic and plastic properties of the FSW aluminum alloy were simulated by elasto-plastic self-consistent (EPSC) model to predict the anisotropic deformation behaviors involving the grain-to-grain interactions. Material parameters used for describing the constitutive laws of each test position were determined from the measured lattice strain distributions for different diffraction hkl planes as well as the macroscopic stress-strain curve of the FSW aluminum alloy. A good agreement between experimental results and numerical simulations was obtained. The present investigations provided a reliable prediction of the anisotropic micromechanical behavior of the FSW aluminum alloy during tensile deformation.     

Orientation-Dependent Tensile Behavior of Nanolaminated Graphene-Al Composites: An <Emphasis Type="Italic">In Situ</Emphasis> Study

We conducted in situ microtension experiments in a scanning electron microscope (SEM) to study the orientation-dependent mechanical behavior of nanolaminated graphene-Al composite. We found a transition from a weak-and-brittle behavior in the isostress composite configuration to a strong-yet-ductile tensile response in the composite under isostrain condition. This is explained by the excellent load-bearing capacity of the graphene nanosheets and a crack deflection mechanism rendered by the laminate structure. These in situ measurements enabled direct observation of the deformation procedure and the exact failure mode, which highlight the importance of microstructural control in tailoring the mechanical properties of advanced metal matrix composites (MMCs).     

Estimation of the Ultimate Tensile Strength of Steel from Its <Emphasis Type="Italic">HB</Emphasis> and <Emphasis Type="Italic">HV</Emphasis> Hardness Numbers and Coercive Force

A formula is derived to accurately describe the tabulated relation between the Brinell (HB) and Vickers (HV) hardnesses of steel over the entire range of their possible variation. This formula and the formulas describing the relation between the HB hardness of chromium–molybdenum and chromium–nickel steels and their ultimate tensile strength σ_u are used to analyze the change in σ_u of 38KhNM steel upon quenching and tempering. The data that reveal a relation between σ_u of 38KhNM steel and its coercive force are obtained.     

Agglomeration of Non-metallic Inclusions at Steel/Ar Interface: <Emphasis Type="Italic">In</Emphasis>-<Emphasis Type="Italic">Situ</Emphasis> Observation Experiments and Model Validation

Better understanding of agglomeration behavior of nonmetallic inclusions in the steelmaking process is important to control the cleanliness of the steel. In this work, a revision on the Paunov simplified model has been made according to the original Kralchevsky–Paunov model. Thus, this model has been applied to quantitatively calculate the attractive capillary force on inclusions agglomerating at the liquid steel/gas interface. Moreover, the agglomeration behavior of Al₂O₃ inclusions at a low carbon steel/Ar interface has been observed in situ by high-temperature confocal laser scanning microscopy (CLSM). The velocity and acceleration of inclusions and attractive forces between Al₂O₃ inclusions of various sizes were calculated based on the CLSM video. The results calculated using the revised model offered a reasonable fit with the present experimental data for different inclusion sizes. Moreover, a quantitative comparison was made between calculations using the equivalent radius of a circle and those using the effective radius. It was found that the calculated capillary force using equivalent radius offered a better fit with the present experimental data because of the inclusion characteristics. Comparing these results with other studies in the literature allowed the authors to conclude that when applied in capillary force calculations, the equivalent radius is more suitable for inclusions with large size and irregular shape, and the effective radius is more appropriate for inclusions with small size or a large shape factor. Using this model, the effect of inclusion size on attractive capillary force has been investigated, demonstrating that larger inclusions are more strongly attracted.     

<Emphasis Type="Italic">In-Situ</Emphasis> Observation on the Diversified Morphology and Growth Behavior of Al<Subscript>3</Subscript>Ni Phase at the Liquid Al/Solid Ni Interface

The morphology and growth behavior of Al₃Ni in the liquid Al/solid Ni interface were observed through synchrotron radiation. The formation time and mechanism of Al₃Ni are connected with saturation of the molten layer. In unsaturated conditions, the growth of columnar Al₃Ni formed during solidification governed by the melting of small grains accompanied by the growth of adjacent large grains and coalescence of grains near the tips. Conversely, the scallop-type Al₃Ni formed in holding showed annexation of adjacent small grains with its morphology changing from scallop to hemisphere.     

<Emphasis Type="Italic">In-Situ</Emphasis> High-Energy X-Ray Diffuse-Scattering Study of the Phase Transition in a Ni<Subscript>2</Subscript>MnGa Ferromagnetic Shape-Memory Crystal

The full information on the changes in many crystallographic aspects, including the structural and microstructural characterizations, during the phase transformation is essential for understanding the phase transition and “memory” behavior in the ferromagnetic shape-memory alloys. In the present article, the defects-related microstructural features connected to the premartensitic and martensitic transition of a Ni₂MnGa single crystal under a uniaxial pressure of 50 MPa applied along the [110] crystallographic direction were studied by the in-situ high-energy X-ray diffuse-scattering experiments. The analysis of the characteristics of diffuse-scattering patterns around different sharp Bragg spots suggests that the influences of some defect clusters on the pressure-induced phase-transition sequences of Ni₂MnGa are significant. Our experiments show that an intermediate phase is produced during the premartensitic transition in the Ni₂MnGa single crystal, which is favorable for the nucleation of a martensitic phase. The compression stress along the [110] direction of the Heusler phase can promote the premartensitic and martensitic transition of the Ni₂MnGa single crystal. This article is based on a presentation given in the symposium entitled “Neutron and X-Ray Studies for Probing Materials Behavior,” which occurred during the TMS Spring Meeting in New Orleans, LA, March 9–13, 2008, under the auspices of the National Science Foundation, TMS, the TMS Structural Materials Division, and the TMS Advanced Characterization, Testing, and Simulation Committee.     

Mechanochemical preparation of Ni<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>Al<Subscript><Emphasis Type="Italic">y</Emphasis></Subscript>/Al<Subscript>2</Subscript>O<Subscript>3</Subscript> nanocomposites

The mechanochemical preparation of nickel aluminide/corundum (Ni _x Al _y /Al₂O₃) powder nanocomposites is shown to be possible during the mechanochemical aluminum reduction of nickel oxide at various weight proportions of the components.