METALLURGICAL AND MATERIALS TRANSACTIONS A
ABSTRACTS
Volume 29A, No. 9, September 1998

This Month Featuring: Symposium on Mechanical Behavior of Bulk Nanocrystalline Solids; Transformations; Mechanical Behavior; Solidification; Materials Processing; Composite Materials. View September 1998 Contents.

SYMPOSIUM ON MECHANICAL BEHAVIOR OF BULK NANOCRYSTALLINE SOLIDS

Fabrication of Bulk Ultrafine-Grained Materials through Intense Plastic Straining
PATRICK B. BERBON, NIKOLAI K. TSENEV, RUSLAN Z. VALIEV, MINORU FURUKAWA, ZENJI HORITA, MINORU NEMOTO, and TERENCE G. LANGDON
Ultrafine grain sizes were introduced into samples of an Al-3 pct Mg solid solution alloy and a cast Al-Mg-Li-Zr alloy using the process of equal-channel angular (ECA) pressing. The Al-3 pct Mg alloy exhibited a grain size of ~0.23 µm after pressing at room temperature to a strain of ~4, but there was significant grain growth when the pressed material was heated to temperatures above ~450 K. The Al-Mg-Li-Zr alloy exhibited a grain size of ~1.2 µm, and the microstructure was heterogeneous after pressing to a strain of ~4 at 673 K and homogeneous after pressing to a strain of ~8 at 673 K with an additional strain of ~4 at 473 K. The heterogeneous material exhibited superplastic-like flow, but the homogeneous material exhibited high-strain-rate superplasticity with an elongation of >1000 pct at 623 K at a strain rate of 10-2 s-1. It is concluded that a homogeneous microstructure is required, and therefore a high pressing strain, in order to attain high-strain-rate superplasticity (HSR SP) in ultrafine-grained materials.

Microstructural Characteristics of Ultrafine-Grained Aluminum Produced Using Equal-Channel Angular Pressing
YOSHINORI IWAHASHI, MINORU FURUKAWA, ZENJI HORITA, MINORU NEMOTO, and TERENCE G. LANGDON
The shearing associated with equal-channel angular (ECA) pressing was examined using optical microscopy. Samples of pure Al with a large grain size were subjected to ECA pressing to different strains and then examined on three orthogonal planes. Samples were pressed without any rotation or with rotations of either 90 or 180 deg between each consecutive pressing. The experimental observations are compared with models which predict the shearing characteristics associated with ECA pressing under different conditions. It is demonstrated that there is good agreement, in terms of both the grain elongation and the shearing within individual grains, between the experimental results and the predictions of the models.

Microstructures and Properties of Nanocomposites Obtained through SPTS Consolidation of Powders
I.V. ALEXANDROV, Y.T. ZHU, T.C. LOWE, R.K. ISLAMGALIEV, and R.Z. VALIEV
The microstructures and properties of copper- and aluminum-based nanocomposites processed through severe plastic torsional straining (SPTS) consolidation of metallic micrometer powders and ceramic nanopowders were investigated by transmission electron microscopy (TEM), X-ray diffraction (XRD), microhardness and electrical resistivity measurements, and mechanical tests. It was shown that the SPTS consolidation of powders is an effective technique for fabricating metal-ceramic nanocomposites with a high density, ultrafine grain size, and high strength. Copper samples processed under a high pressure of 6 GPa exhibited high failure strength and strain as well as unusual strain hardening. Superplastic-like behavior was found in Al-Al2O3 nanocomposite samples.

Mechanical Behavior of a Bulk Nanostructured Iron Alloy
J.E. CARSLEY, A. FISHER, W.W. MILLIGAN, and E.C. AIFANTIS
Bulk, fully dense materials were prepared from Fe-10Cu with grain diameters between 45 nm and 1.7 µm. The materials were prepared by ball milling of powders in a glove box, followed by hot isostatic pressing (hipping) or powder forging. Larger grain sizes were obtained by thermal treatment of the consolidated powders. The bulk materials were relatively clean, with oxygen levels below 1500 wpm and other contaminants less than 0.1 at. pct. The mechanical behavior of these materials was unique. At temperatures from 77 to 470 K, the first and only mechanism of plastic deformation was intense shear banding, which was accompanied by a perfectly plastic stress-strain response (absence of strain hardening). There was a large tension-compression asymmetry in the strength, and the shear bands did not occur on the plane of maximum shear stress or the plane of zero extension. This behavior, while unusual for metals, has been observed in amorphous polymers and metallic glasses. On the other hand, the fine-grained Fe-10Cu materials behaved like coarse-grained iron in some respects, particularly by obeying the Hall-Petch equation with constants reasonably close to those of pure iron and by exhibiting low-temperature mechanical behavior which was very similar to that of steels. Transmission electron microscopy (TEM) studies found highly elongated grains within shear bands, indicating that shear banding occurred by a dislocation-based mechanism, at least at grain sizes above 100 nm. Similarities and differences between the fine-grained Fe-10Cu and metals, polymers, metallic glasses, radiation-damaged metals, and quench-damaged metals are discussed.

Effect of B on the Microstructure and Mechanical Properties of Mechanically Milled TiAl Alloys
SANG H. KIM, H.H. CHUNG, SUNG G. PYO, S.J. HWANG, and NACK J. KIM
The present study is concerned with -(Ti52Al48)100-xBx (x = 0, 0.5, 2, 5) alloys produced by mechanical milling/vacuum hot pressing (VHPing) using melt-extracted powders. Microstructure of the as-vacuum hot pressed (VHPed) alloys exhibits a duplex equiaxed microstructure of 2 and with a mean grain size of 200 nm. Besides 2 and phases, binary and 0.5 pct B alloys contain Ti2AlN and Al2O3 phases located along the grain boundaries and show appreciable coarsening in grain and dispersoid sizes during annealing treatment at 1300 °C for 5 hours. On the other hand, 2 pct B and 5 pct B alloys contain fine boride particles within the grains and show minimal coarsening during annealing. Room-temperature compressing tests of the as-VHPed alloys show low ductility, but very high yield strength > 2100 MPa. After annealing treatment, mechanically milled alloys show much higher yield strength than conventional powder metallurgy and ingot metallurgy processed alloys, with equivalent ductility to ingot metallurgy processed alloys. The 5 pct B alloy with the smallest grain size shows higher yield strength than binary alloy up to the test temperature of 700 °C. At 850 °C, 5 pct B alloy shows much lower strength than the binary alloy, indicating that the deformation of fine 5 pct B alloy is dominated by the grain boundary sliding mechanism.

Mechanical Properties, Ductility, and Grain Size of Nanocrystalline Iron Produced by Mechanical Attrition
T.R. MALOW and C.C. KOCH
The main goal of this investigation is to determine the influence of grain size on the mechanical properties and, specifically, the intrinsic ductility of nanocrystalline (nc) Fe. Ball-milled nc Fe was consolidated into compacts of near theoretical density by uniaxial warm pressing. Compaction parameters and annealing treatments resulted in a range of grain sizes for subsequent mechanical testing. The miniaturized disk bend test, hardness, and the automated ball indentation (ABI) method were used to test nanocrystal (nc) iron in compression and tension. The deformation and fracture morphologies of the tested samples were characterized by light and scanning electron microscopy. The hardness, as a function of the grain size, was described with a Hall-Petch slope, which was smaller than that in coarse-grained Fe. In tension, the material failed in a macroscopically brittle manner, while local ductility in very concentrated shear bands was observed. The compressive characteristics of the nc Fe were similar to those of a perfectly plastic material. The results are discussed in the context of the mechanical behavior of coarse-grained polycrystalline metals and alloys.

TRANSFORMATIONS

A Transmission Electron Microscope Study of 1 Pct Mn Ductile Iron with Different Austempering Treatments
M. NILI AHMADABADI
A transmission electron microscope (TEM) equipped with an energy dispersive spectroscopy (EDS) system was used to study the bainitic reaction in a conventional and a successive austempering process for 1 wt pct Mn ductile iron. In the case of conventional austempering, the specimens were full austenitized at 900 °C and then austempered at 375 °C (high austempering temperature) and 315 °C (low austempering temperature) for different periods. In the case of the successive austempering process, following austempering at 375 °C for different periods, specimens were austempered at 315 °C, and subsequently quenched in ice water. The TEM-EDS study showed that carbide precipitation in the ferritic and retained austenitic component of bainite is a function of the local concentrations of the alloying elements, austempering time, and temperature. After a short time at high austempering temperature, carbide-free bainite forms near graphite nodules. Longer austempering time or lower austempering temperature encourages carbide precipitation in the bainitic ferrite. A long austempering time at high temperature leads to decomposition of retained austenite to ferrite and carbide. A rough inspection shows that the precipitated carbides in the ferritic component of specimens austempered at low temperature lie at an angle of about 40 to 50 deg to the sheaf axis.

Static Recrystallization Kinetics with Homogeneous and Heterogeneous Nucleation Using a Cellular Automata Model
R.L. GOETZ and V. SEETHARAMAN
The kinetics of homogeneous and heterogeneous static recrystallization in a single-phase material were analyzed using two-dimensional (2-D) and three-dimensional (3-D) cellular automata (CA). A CA model was developed, which was then validated using the theory based on relationships developed by Johnson and Mehl, Avrami, and Kolmogorov (JMAK) for homogeneous site-saturated and constant-rate nucleation. The model was then modified for heterogeneous nucleation at grain boundaries, with either a fixed number of nuclei or a constant rate of nucleation. The fraction of boundary sites nucleated, for the case of fixed nucleation, varied from 0.006 to 0.28, resulting in Avrami exponents (k) ranging from 1.8 to 1.1 (site saturation). Site saturation with fixed nucleation produced a lamellar microstructure. The parameters of q and m, from Vandermeer's microstructural path method, were calculated and compared with theoretical values. Constant-rate nucleation at grain boundaries between newly recrystallized grains and the unrecrystallized matrix resulted in k values of 1. Simulated microstructures revealed that with a low nucleation rate, recrystallized grains formed in clusters, while a high nucleation rate resulted in a necklace microstructure, with kinetics similar to those observed in dynamic recrystallization (k = 1.4).

MECHANICAL BEHAVIOR

Analysis of Ridging in Aluminum Auto Body Sheet Metal
A.J. BEAUDOIN, J.D. BRYANT, and D.A. KORZEKWA
A finite-element model is presented for the analysis of surface roughening of aluminum sheet metal. A hybrid finite-element model is developed which accounts for the elasto-viscoplastic constitutive response of a single crystallographic orientation. Initialization of a finite-element mesh representing several grains is performed using data gathered through automated collection of backscattered Kikuchi diffraction data. To handle a region that contains sufficient variation (contains numerous distinct grains), the implementation is carried out using distributed computation strategies. Application is made to 6111-T4 sheet metal intended for auto body applications. The numerical simulations are complemented with mechanical testing in plane strain and biaxial stretch. Based on the simulation results, there are two conclusions that can be drawn concerning the action of surface grains deforming through crystallographic slip. One is that grains can act collectively to form localized regions of thinning. The other is that grain interactions can lead to behavior which is different from that expected if grains deform with the average (macroscale) strain. Neighbor interactions can alter the deformation from that computed using the macroscale deformation rate.

Heterogeneous Microstructures and Microtextures in Cube-Oriented Al Crystals after Channel Die Compression
QING LIU, CLAIRE MAURICE, JULIAN DRIVER, and NIELS HANSEN
Pure aluminum crystals of cube orientation have been deformed in plane-strain compression to strains of unity using a channel die. The macrostructures and microstructures were characterized in three dimensions by a range of metallographic techniques including optical, scanning, and transmission electron microscopy. Particular attention was paid to quantifying global textures and local variations in crystal orientation by means of X-ray pole figures, automatic electron back-scattered diffraction (EBSD) and semiautomatic transmission electron microscope (TEM) Kikuchi line analysis. Cube crystals are observed to break up into macroscopic deformation bands aligned along the elongation direction and strongly disorientated by rotations mostly, but not uniquely, about the transverse direction. The bands develop deformation substructures of dislocation boundaries or, in certain cases, of intersecting dislocation boundaries which have characteristic microtexture signatures of alternating lattice rotations. The transition regions between the bands are composed of equiaxed dislocation cells which accommodate continuous orientation gradients over distances of about 20 µm. Compared to the behavior of rolled Al crystals, the macroscopic bands are observed to lie in different planes, but the microscopic subdivisions and microtextures developed in the channel die and in rolling are very similar. The origins of the macroscopic and microscopic subdivisions are discussed in terms of the local deformation modes and slip amplitudes and their relation to the behavior of rolled crystals.

High-Temperature Deformation of Commercial-Purity Aluminum
E.S. PUCHI and M.H. STAIA
The stress-strain behavior of aluminum 99.5 pct (2-9) purity deformed under hot-working conditions has been found to be satisfactorily described by combining the exponential saturation equation earlier proposed by Voce and a latter model advanced by Kocks. Voce's equation describes the strain dependence of the flow stress, whereas the temperature and strain rate dependencies of both the initial flow stress and the saturation or steady-state stress are introduced by means of Kocks' model, which leads to the definition of a different temperature-compensated strain rate parameter. The basic principles of the dynamic materials model (DMM) advanced by Gegel and co-workers has been reassessed, leading to a different proposition in relation to the calculation of both the power dissipator co-content (J) and the power dissipation efficiency (), which makes use of the constitutive equation previously developed. Such concepts are later applied to the analysis of a typical industrial hot-rolling process conducted on commercial-purity aluminum. From the microstructural point of view, hot rolling of commercial-purity aluminum has been found to be conducted under conditions of relatively low power dissipation efficiency ( 0.20 to 0.25), which is likely to be associated with the predominance of dynamic recovery as the main dislocation rearrangement mechanism.

An Investigation of the Fracture and Fatigue Crack Growth Behavior of Forged Damage-Tolerant Niobium Aluminide Intermetallics
F. YE, C. MERCER, and W.O. SOBOYEJO
The results of a recent study of the effects of ternary alloying with Ti on the fatigue and fracture behavior of a new class of forged damage-tolerant niobium aluminide (Nb3Al-xTi) intermetallics are presented in this article. The alloys studied have the following nominal compositions: Nb-15Al-10Ti (10Ti alloy), Nb-15Al-25Ti (25Ti alloy), and Nb-15Al-40Ti (40Ti alloy). All compositions are quoted in atomic percentages unless stated otherwise. The 10Ti and 25Ti alloys exhibit fracture toughness levels between 10 and 20 MPa at room temperature. Fracture in these alloys occurs by brittle cleavage fracture modes. In contrast, a ductile dimpled fracture mode is observed at room-temperature for the alloy containing 40 at. pct Ti. The 40Ti alloy also exhibits exceptional combinations of room-temperature strength (695 to 904 MPa), ductility (4 to 30 pct), fracture toughness (40 to 100 MPa), and fatigue crack growth resistance (comparable to Ti-6Al-4V, monolithic Nb, and inconnel 718). The implications of the results are discussed for potential structural applications of the 40Ti alloy in the intermediate-temperature (~700 °C to 750 °C) regime.

SOLIDIFICATION

Microstructural and Compositional Transients during Accelerated Directional Solidification of Al-4.5 Wt Pct Cu
RONG-JIUNN SU, RUEL A. OVERFELT, and WARTAN A. JEMIAN
The transient behavior of mushy-zone velocities, primary dendrite arm spacings, and microsegregation effects have been investigated for an Al-4.5 wt pct Cu alloy by instantaneous velocity changes in a standard Bridgman furnace. After suddenly imposed velocity changes, the mushy-zone velocities, dendrite arm spacings, and compositions exponentially adjust to new steady-state values. Good agreement was found between the transient mushy-zone positions and velocities and predictions from the theoretical model of Saitou and Hirata. The primary dendrite arm spacings appear to adjust to changed velocity conditions about as rapidly as the mushy-zone velocity adjusts. Steady-state arm spacings agree very well with corresponding steady-state data from the literature. However, the observed composition profiles in the dendrite core and the interdendritic liquid appear to adjust more slowly than the corresponding adjustment of the mushy-zone velocity and arm spacings. Our observation of the sluggish response of the compositional profiles is consistent with an estimated Lewis number (Le = ) of 9.4 X 103 for the aluminum-copper system. The diffusivity of heat, thus, greatly exceeds the diffusivity of solute in this system. These results indicate that testing for the steady state during directional solidification experiments by looking for constant primary dendrite arm spacings can lead to errors, since the microsegregation profiles adjust more slowly than the spacings. It is suggested that constancy of composition also be tested for critical experiments investigating steady-state microsegregation effects.

Communication: Discussion of "Effect of Dendrite Arm Coarsening on Microsegregation"
T. KRAFT AND Y.A. CHANG

Authors' Reply
H. COMBEAU, J.-M. DREZET, A. MO, AND M. RAPPAZ

MATERIALS PROCESSING

Enhancement of the Mechanical Properties of a Low-Carbon, Low-Silicon Steel by Formation of a Multiphased Microstructure Containing Retained Austenite
P. JACQUES, X. CORNET, Ph. HARLET, J. LADRIÈRE, and F. DELANNAY
Dual-phase and transformation-induced plasticity (TRIP)-assisted multiphase steels are related families of high-strength formable steels exhibiting excellent mechanical characteristics. This study shows how a ferrite-bainite-martensite microstructure containing retained austenite can improve the mechanical properties of a cold-rolled low-carbon, low-silicon steel. Such a multiphased microstructure is obtained by a heat treatment involving intercritical annealing followed by a bainite transformation tempering. Depending on the heat-treatment parameters, the samples present a variety of microstructures. Due to the presence of retained austenite, some samples exhibit a TRIP effect not anticipated with such a low silicon content. A composite strengthening effect also results from the simultaneous presence of a ductile ferrite matrix with bainite and martensite as hard second phases. A true stress at maximum load of 800 MPa and a true uniform strain of 0.18 can be obtained by forming a ferrite-bainite-martensite microstructure containing up to 10 pct of retained austenite. These properties correspond to a favorable evolution of work hardening during plastic deformation.

The Sweep Constant Concept in Phase Coarsening
C.S. PANDE, R.A. MASUMURA, and S.P. MARSH
An expression for sweep constant originally introduced for grain growth is derived in terms of the parameters of the size distribution. The sweep constant is extended to the phenomenon of phase coarsening. It is shown that a relationship exists between the sweep constant, coarsening rate, and volume fraction of the particles undergoing coarsening.

Transmission Electron Microscope Specimen Preparation of Zn Powders Using the Focused Ion Beam Lift-Out Technique
B.I. PRENITZER, L.A. GIANNUZZI, K. NEWMAN, S.R. BROWN, R.B. IRWIN, T.L. SHOFNER, and F.A. STEVIE
Particles of Zn powder have been studied to show that high-quality scanning electron microscope (SEM) and transmission electron microscope (TEM) specimens can be rapidly produced from a site-specific region on a chosen particle by the focused ion beam (FIB) lift-out technique. A TEM specimen approximately 20-µm long by 5-µm wide was milled to electron transparency, extracted from the bulk particle, and micromanipulated onto a carbon coated copper mesh TEM grid. Using the FIB lift-out method, we were able to prepare a site-specific TEM specimen from a difficult material in under 3 hours. The TEM analysis of the lift-out specimen revealed a large amount of thin area free from characteristic signs of damage that may be observed as a result of conventional argon ion milling. The overall microstructure of the specimen prepared by the FIB lift-out method was consistent with samples prepared by conventional metallographic methods. A grain size of ~10 to 20 µm was observed in all specimens by both TEM and SEM analysis. Light optical microscopy revealed the presence of internal voids in ~10 to 20 pct of all particles. The SEM analysis showed the voids to extend over ~70 pct of the particle volume in some cases.

Investigation of Thermomechanical Behavior of a Work Roll and of Roll Life in Hot Strip Rolling
C.G. SUN, C.S. YUN, J.S. CHUNG, and S.M. HWANG
An integrated finite element-based model is presented for the prediction of the steady-state thermomechanical behavior of the roll-strip system and of roll life in hot strip rolling. The model is comprised of basic finite-element models, which are incorporated into an iterative-solution procedure to deal with the interdependence between the thermomechanical behavior of the strip and that of the work roll, which arises from roll-strip contact, as well as with the interdependence between the thermal and mechanical behavior. Comparison is made between the predictions and the measurements to assess solution accuracy. Then, the effect of various process parameters on the detailed aspects of thermomechanical behavior of the work roll and on roll life is investigated via a series of process simulations.

A Novel Way of Amorphous Phase Formation during Mechanical Alloying of Copper and Cadmium Powders
D.L. ZHANG and T.B. MASSALSKI
Phase formation during high-energy ball milling of copper and cadmium powders has been investigated. Both X-ray diffractometry (XRD) and differential scanning calorimetry (DSC) have been used to characterize the resulting phases. An amorphous phase forms during milling in the copper-cadmium system by a reaction between the equilibrium phase and one of the constituent metals (copper). However, the amorphous phase cannot be produced by a direct reaction between the copper and cadmium powders, nor by milling of a powder consisting of only the phase. It appears most likely that the contribution from the generated copper/ interfaces, and the accompanying increase in the total free energy, provide the additional driving force for the amorphous phase formation in this system.

COMPOSITE MATERIALS

Optimization of the Strength-Fracture Toughness Relation in Particulate-Reinforced Aluminum Composites via Control of the Matrix Microstructure
I. DUTTA, F.N. QUILES, T.R. McNELLEY, and R. NAGARAJAN
The evolution of the microstructure and mechanical properties of a 17.5 vol. pct SiC particulate-reinforced aluminum alloy 6092-matrix composite has been studied as a function of postfabrication processing and heat treatment. It is demonstrated that, by the control of particulate distribution, matrix grain, and substructure and of the matrix precipitate state, the strength-toughness combination in the composite can be optimized over a wide range of properties, without resorting to unstable, underaged (UA) matrix microstructures, which are usually deemed necessary to produce a higher fracture toughness than that displayed in the peak-aged condition. Further, it is demonstrated that, following an appropriate combination of thermomechanical processing and unconventional heat treatment, the composite may possess better stiffness, strength, and fracture toughness than a similar unreinforced alloy. In the high- and low-strength matrix microstructural conditions, the matrix grain and substructure were found to play a substantial role in determining fracture properties. However, in the intermediate-strength regime, properties appeared to be optimizable by the utilization of heat treatments only. These observations are rationalized on the basis of current understanding of the grain size dependence of fracture toughness and the detailed microstructural features resulting from thermomechanical treatments.

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