Effects of test temperature and grain size on the charpy impact toughness and dynamic toughness (<Emphasis Type="Italic">K</Emphasis><Subscript><Emphasis Type="Italic">ID</Emphasis></Subscript>) of polycrystalline niobium

The effects of changes in test temperature (−196 °C to 25 °C) and grain size (40 to 165 μm) on the dynamic cleavage fracture toughness (K _ID ) and Charpy impact toughness of polycrystalline niobium (Nb) have been investigated. The ductile-to-brittle transition was found to be affected by both changes in grain size and the severity of stress concentration (i.e., notch vs fatigue-precrack). In addition to conducting impact tests on notched and fatigue-precracked Charpy specimens, extensive fracture surface analyses have been performed in order to determine the location of apparent cleavage nucleation sites and to rationalize the effects of changes in microstructure and experimental variables on fracture toughness. Existing finite element analyses and the stress field distributions ahead of stress concentrators are used to compare the experimental observations with the predictions of various fracture models. The dynamic cleavage fracture toughness, K _ID , was shown to be 37±4 MPa√m and relatively independent of grain size (i.e., 40 to 105 μm) and test temperature over the range −196 °C to 25 °C.     

Rare-earth metals (REMs) in nickel aluminide-based alloys: I. Physicochemical laws of interaction in the Ni-Al-REM and Ni<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>Al<Subscript><Emphasis Type="Italic">y</Emphasis></Subscript>-REM-AE (alloying element) systems

The data on the Ni-Al-R (R = REM Sc, Y, La, lanthanides) binary and ternary systems and the interactions of three rare-earth metals (yttrium, lanthanum, cerium) with the main alloying elements (Ti (Zr, Hf), Cr (Mo, W) that are introduced into Ni₃Al-based VKNA alloys are analyzed. The binary aluminides of REMs in the Ni-Al-R ternary systems are shown to be in equilibrium with neither NiAl nor Ni₃Al. The solid solution of aluminum in RNi₅, which penetrates deep into these ternary systems, is the most stable phase in equilibrium with Ni₃Al. In the NiAl (Ni₃Al)-AE-R systems, REM precipitation (segregation) on various defects and interfaces in nickel aluminides is likely to be the most probable, and REMs are thought to interact with the most active impurities in real alloys (C, O, N), since REMs have a large atomic radius and, thus, are virtually undissolved in nickel, aluminum, and nickel aluminides.     

<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.     

<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.     

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.     

Effects of Powder Carrier on the Morphology and Compressive Strength of Iron Foams: Water <Emphasis Type="Italic">vs</Emphasis> Camphene

With its well-known popularity in structural applications, considerable attention has recently been paid to iron (Fe) and its oxides for its promising functional applications such as biodegradable implants, water-splitting electrodes, and the anode of lithium-ion batteries. For these applications, iron and its oxides can be even further utilized in the form of porous structures. In order to control the pore size, shape, and amount, we synthesized Fe foams using suspensions of micrometric Fe₂O₃ powder reduced to Fe via freeze casting in water or liquid camphene as a solvent through sublimation of either ice or camphene under 5 pct H₂/Ar gas and sintering. We then compared them and found that the resulting Fe foam using water as a solvent (p?=?71.7 pct) showed aligned lamellar macropores replicating ice dendrite colonies, while Fe foam using camphene as a solvent (p?=?68.0 pct) exhibited interconnected equiaxed macropores replicating camphene dendrites. For all directions with respect to the loading axis, the compressive behavior of the water-based Fe foam with a directional elongated wall pore structure was anisotropic (11.6?±?0.9 MPa vs 7.8?±?0.8 MPa), whereas that of the camphene-based Fe foam with a random round pore structure was nearly isotropic (12.0?±?1.1 MPa vs 11.6?±?0.4 MPa).     

<Emphasis Type="Italic">In Situ</Emphasis> Observation of the Formation and Interaction Behavior of the Oxide/Oxysulfide Inclusions on a Liquid Iron Surface

Inclusion formation and its behavior at the early stage of deoxidation and alloying operation has a considerable influence on steel cleanliness. In the present work, steel alloying, such as Mn, Al, FeSi, and FeMn additions to the liquid steel with different oxygen and sulphur content was simulated with a confocal scanning laser microscope combined with a special addition device. The inclusion formation and the inclusion interaction behavior immediately after the alloying and/or deoxidation were observed in situ. The inclusions were characterized based on both the in situ observation and the quenched sample. The effect of the sulphur and oxygen content in liquid iron, as well as that of the deoxidant type on the formation of oxides/oxysulfides is discussed taking consideration of the thermodynamics of the system. The inclusion behavior on the liquid iron surface, i.e., the interaction after its formation, the dissolution during the high temperature iso-thermal holding, and growth during the cooling was investigated. The dissolution of Mn(O,S) inclusions at 1843 K (1570 °C) was found to be driven by Mn diffusion through the inclusion/liquid iron boundary layer, and its growth during cooling was significantly affected by Marangoni flow.     

Effect of Extrusion Temperature on the Plastic Deformation of an Mg-Y-Zn Alloy Containing LPSO Phase Using <Emphasis Type="Italic">In Situ</Emphasis> Neutron Diffraction

The evolution of the internal strains during in situ tension and compression tests has been measured in an MgY₂Zn₁ alloy containing long-period stacking ordered (LPSO) phase using neutron diffraction. The alloy was extruded at two different temperatures to study the influence of the microstructure and texture of the magnesium and the LPSO phases on the deformation mechanisms. The alloy extruded at 623 K (350 °C) exhibits a strong fiber texture with the basal plane parallel to the extrusion direction due to the presence of areas of coarse non-recrystallised grains. However, at 723 K (450 °C), the magnesium phase is fully recrystallised with grains randomly oriented. On the other hand, at the two extrusion temperatures, the LPSO phase orients their basal plane parallel to the extrusion direction. Yield stress is always slightly higher in compression than in tension. Independently on the stress sign and the extrusion temperature, the beginning of plasticity is controlled by the activation of the basal slip system in the dynamic recrystallized grains. Therefore, the elongated fiber-shaped LPSO phase which behaves as the reinforcement in a metal matrix composite is responsible for this tension–compression asymmetry.     

<Emphasis Type="Italic">In Situ</Emphasis> Observation of the Precipitation,Aggregation, and Dissolution Behaviors of TiN Inclusion on the Surface of Liquid GCr15 Bearing Steel

In this study, the precipitation, aggregation, and dissolution behaviors of TiN inclusions on the surface of liquid GCr15 bearing steel have been investigated by combining the observations of confocal laser scanning microscope (CLSM) and field emission scanning electron microscope (FE-SEM) with those obtained from energy dispersive spectrometer (EDS) and theoretical analysis. The kinetic results show that the initial concentration of Ti and N are 0.0078 and 0.0049, respectively, the precipitation temperature is between 1640 K and 1680 K (1367 °C and 1407 °C), and the local cooling rate is between 0.5 and 10 K/s; TiN inclusion can precipitate only when the solid fraction is higher than 0.847 and its precipitation radius is between 1 and 6 μm. The precipitation radius of a TiN inclusion in the GCr15 bearing steel sheet can be reduced by decreasing the N content and increasing the cooling strength. The aggregation and densification of multi-particle aggregated TiN inclusions are verified by CLSM observation and theoretical analysis. The inclusions are aggregated by the cavity bridge force (CBF), and the aggregated TiN is formed by solid-phase sintering. The results of force analysis show that CBF plays a dominant role in the aggregation process of the inclusions. The atomic ratio of Ti and V obtained by EDS is 18:1, which may melt TiN and form the liquid inclusion at 1688 K (1415 °C) observed by CLSM. The theoretical analysis is conducted for the dissolution of the TiN inclusions observed by CLSM, which shows that the dissolution of the TiN inclusions is related to the size of the inclusions; the larger the size, the greater the dissolution rate. The long-strip TiN inclusion may be formed by the Ostwald ripening of two TiN inclusions. The TiN inclusions smaller than 3 μm in the GCr15 bearing steel may be formed by the dissolved Ti and N generated by the dissolution of TiN.