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Title Krug, Matthew E.
Year Microstructural Evolution and Mechanical Properties in Al-Sc Alloys With Li and Rare Earth Additions
Abbreviated Journal Book Whole
Issue 2011 Keywords
Place of Publication Language 372
Original Title Al-Sc, Al-Li, Al-Li-Sc, rare earth, LEAP, atom probe
Series Title Aluminum-scandium alloys have excellent mechanical properties at ambient and elevated temperatures due to the presence of coherent, nano-scale, L12-ordered Al3Sc precipitates. In this thesis, a variety of Al-Sc alloys with additions of Li and RE elements, primarily Yb, are studied. An addition of ytterbium reduces the cost of Al-Sc alloys by replacing some of the more-expensive Sc. Lithium is a unique alloying addition to Al-Sc alloys, because it has significant solubility in both the matrix and precipitate phases. Lithium also provides solid solution strengthening, and a large strengthening increment on aging through the formation of Al3Li precipitates. The effects of these alloying additions on Al-Sc alloys are investigated in detail, and discussed in the context of physical models linking the microstructure to measured mechanical properties. The alloys undergo a variety of aging treatments between 170 – 450 °C, producing a range of precipitate distributions. Their aging response is assessed using Vickers microhardness to monitor ambient-temperature strength, and electrical conductivity to monitor the progress of the precipitation reaction. The alloys are creep-tested in compression at 300 °C, and exhibit threshold stresses, below which no measurable creep occurs. Detailed microstructural investigations rely primarily on local electrode atom probe tomography, as well as transmission electron microscopy. The volume fractions, number densities, and chemical compositions of precipitates are measured at the nano-scale, and their size and spatial distributions are quantitatively determined. Compared to binary Al-Sc alloys, Al-Li-Sc and Al-Li-Sc-Yb alloys contain a finer distribution of Al3(Sc1-x-yLixYby) precipitates at a greater number density and volume fraction, as well as solid-solution strengthening in the Al(Li) matrix, all of which lead to a greater peak strength at ambient-temperature. Because partitioning of Li to the precipitates results in a smaller lattice parameter mismatch with the matrix, a Li addition is detrimental to the elevated temperature strength of Al-Sc alloys, but this effect is mitigated if additions of both Li and Yb are made. A model for threshold stresses at elevated temperature semi-quantitatively captures experimentally-observed trends in threshold stress data in Al-Sc-X alloys. Dislocation dynamics simulations on directly-measured precipitate arrangements lead to a rule for superposition of strength contributions from dissolved solutes, α′–Al3(Li,Sc,Yb) precipitates, and δ′–Al3Li precipitates. Series Volume
Edition Northwestern University
ISBN Ph.D. thesis Area
Serial (down) English Orig Record
no NU @ m-krug @ 11430
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Mulholland, Michael Co-precipitation Kinetic Pathways in a Blast Resistant Steel for Naval Applications Book Whole 2011 150 The nanoscale co-precipitation of Cu and M2C carbides in a high strength, low carbon quenched and tempered steel is characterized in detail along with the mechanical properties and precipitated austenite. Correlations between the nanostructure and the mechanical properties are drawn. The co-precipitation of Cu, M2C (M is any combination of Cr, Mo, or Ti), and austenite (f.c.c.) is characterized for 5 h isochronal aging times by synchrotron x-ray diffraction and 3-D atom-probe tomography for a HSLC steel, BA (BlastAlloy) 160. High number densities, ca. 1023 m-3, of co-located Cu and M2C precipitates were observed. Only small austenite volume percentages (<1.5%) were measured after aging at temperatures up to 625 °C for 5 h. Nanoscale co-precipitation is studied in detail after isothermal aging. Atom-probe tomography is utilized to quantify the co-precipitation of co-located Cu precipitates and M2C (M is any combination of Cr, Mo, Fe, or Ti) carbide strengthening precipitates. Coarsening of Cu precipitates is offset by the nucleation and growth of M2C carbide precipitate, resulting in the maintenance of a yield strength of 1047 ± 7 MPa (152 ±1 ksi) for as long as 320 h of aging time at 450 °C. Impact energies of 153 J (113 ± 6 ft-lbs) and 144 J (106 ± 2 ft-lbs) are measured at - 30 °C and – 60 °C, respectively. The co-location of Cu and M2C precipitates results in non- stationary state coarsening of the Cu precipitates. Synchrotron-source x-ray diffraction studies reveal that the measured 33% increase in impact toughness after aging for 80 h at 450 °C is due to dissolution of cementite, Fe3C, which is the source of carbon for the nucleation and growth of M2C carbide precipitates. Less than 1 volume percent austenite is observed for aging treatments at temperatures less than 600 °C, suggesting that TRIP does not play a significant role in the toughness of specimens aged at temperatures less than 600 °C. Aging treatments at temperatures greater than 600 °C produce more austenite, in the range 2-7%, but at the expense of yield strength. The differences in artifacts associated with voltage-pulsed and laser-pulsed (wavelength = 532 or 355 nm) atom-probe tomographic (APT) analyses of nanoscale precipitation in a high- strength low-carbon steel are assessed using a local-electrode atom-probe (LEAP) tomograph. It is found that the interfacial width of nanoscale Cu precipitates increases with increasing specimen apex temperatures induced by higher laser pulse-energies (0.6-2 nJ pulse-1 at a wavelength of 532 nm). This effect is probably due to surface diffusion of Cu atoms. Increasing the specimen apex temperature by using pulse energies up to 2 nJ pulse-1 at a wavelength of 532 nm is also found to increase the severity of the local magnification effect for nanoscale M2C metal carbide precipitates, which is indicated by a decrease of the local atomic density inside the carbides from 68±6 nm-3 (voltage-pulsing) to as small as 3.5±0.8 nm-3. Methods are proposed to solve these problems based on comparisons with the results obtained from voltage-pulsed APT experiments. Essentially, application of the Cu precipitate compositions and local atomic-density of M2C metal carbide precipitates measured by voltage-pulsed APT to 532 or 355 nm wavelength laser-pulsed data permits correct quantification of precipitation. Based on detailed three-dimensional (3-D) local-electrode atom-probe (LEAP) tomographic measurements of the properties of Cu and M2C precipitates, the yield strength of a high-toughness secondary-hardening steel, BA160, as a function of aging time is predicted using a newly developed 3-D yield strength model. Contributions from each strengthening constituent are evaluated with the model and superposition laws are applied to add each contribution. Prediction of the yield strength entirely based on 3-D microstructural information is thus achieved. The accuracy of the prediction depends on the superposition laws and the LEAP tomographic measurements, especially the mean radius and volume fraction of M2C precipitates. Northwestern University Ph.D. thesis Evanston, IL English no NU @ karnesky @ 11305
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Booth-Morrison, Christopher Nanoscale Studies of the Early Stages of Phase Separation in Model Ni-Al-Cr Superalloys Journal Article 2009 Ph.D. Thesis 196 Ph.D. thesis no NU @ c-booth @ 10592
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Kolli, R. Prakash Kinetics of nanoscale Cu-rich precipitates in a multicomponent concentrated steel Book Whole 2007 320 Kinetics; Cu; precipitate; steel The kinetics of nanoscale Cu-rich precipitates of multicomponent concentrated steels has been investigated utilizing primarily APT and supplemented with a synchrotron radiation experiment, first-principles calculations, Thermo-Calc study, and CTEM (at the longest aging time). Results on mechanical properties and microstructure at a greater length scale are also presented. The studied steels, NUCu-170 and NUCu-140-x, are HSLC steels, and are primarily strengthened by nanoscale Cu-rich precipitates. NUCu-170 contains 1.82 at. % Cu, whereas NUCu-140-x contains nominally ca. 1.15 at. % Cu. This study focused on a 900 °C solutionizing treatment followed by isothermal aging at 500 °C between 0.25 and 1024 h for NUCu-170 and NUCu-140-1, and aging at 550 °C between 0.25 and 4 h for NUCu-140-3. In addition, a double aging treatment of 550 °C aging followed by 200 °C for 2 h was investigated for NUCu-140-3. Ph.D. thesis Northwestern University no NU @ m-krug @ 10472
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Karnesky, Richard A. Mechanical Properties and Microstructure of Al–Sc with Rare-Earth Element or Al[sub:2]O[sub:3] Additions Book Whole 2007 258 Al-Sc Aluminum alloys strengthened with coherent (L1[sub:2]), nanosize Al[sub:3]Sc precipitates are structural materials that have outstanding strength at ambient and elevated temperatures. They are creep resistant at 300 °C and exhibit a threshold stress, below which creep is not measurable. Introducing ternary alloying additions, such as rare-earth elements (RE=Y, Dy, Er), that segregate within Al[sub:3]Sc precipitates improves this creep resistance by increasing the lattice parameter misfit of precipitates with Al. In this thesis, Al–600 Sc–200 RE and Al–900 Sc–300 Er (at. ppm) are studied. These elements are an order of magnitude less expensive than Sc, so reduce alloy costs. As an alternative or supplement to ternary additions, submicron (incoherent) Al[sub:2]O[sub:3] dispersoids impart additional strengthening. The dispersion-strengthened cast alloys, DSC–Al–1100 Sc and DSC–Al–800 Sc–300 Zr, studied in this thesis contain 30 vol.% Al[sub:2]O[sub:3]. In this thesis, the temporal evolution of Al–Sc–RE and DSC–Al–Sc(–Zr) alloys are measured using Local-Electrode Atom-Probe (LEAP) tomography, conventional transmission electron microscopy, and electrical conductivity. These techniques measure the changes in precipitate number density, size, volume fraction, chemical composition, and interprecipitate distance and are compared to models. They are also employed to measure the diffusivity and solid solubility of Er in Al in Al–300 Er, Al–450 Er, and Al–600 Er. The mechanical behavior (microhardness, yield, and creep) of the alloys is studied at 25, 300, and 350 °C. The effect of Al[sub:3](Sc[sub:1-x]Er[sub:x]) precipitate size and interprecipitate distance is studied by varying isochronal and isothermal aging treatments. Various models and simulations are compared to experimental data. At ambient temperatures, very small Al[sub:3](Sc[sub:1-x]M[sub:x]) precipitates contribute to order strengthening and larger (unshearable) precipitates are bypassed by dislocations through Orowan bowing. Dislocation dynamics simulations allow both processes to operate in a glide plane, where precipitate distributions may be gathered directly or be informed by LEAP tomography data. At elevated temperatures, the lattice parameter and modulus mismatches of Al[sub:3](Sc[sub:1-x]M[sub:x]) oppose both dislocation climb over Al[sub:3](Sc[sub:1-x]M[sub:x]) and dislocation detachment from Al[sub:2]O[sub:3]. Northwestern University Ph.D. thesis Evanston, IL English no NU @ karnesky @ 10000
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van Dalen, Marsha E. Microstructure and Creep Properties of Al-Sc Alloys Micro-alloyed with Lanthanides (Yb or Gd) and Transition Metals (Ti or Zr) Book Whole 2007 289 Al-Sc This thesis examines the effects of micro-alloying additions to Al-Sc alloys on the microstructure, coarsening resistance and creep properties. The overarching goal of this research is to develop castable, creep-resistant aluminum alloys which can be used at temperatures in excess of 300°C. Successful high-temperature application of aluminum based alloys offers a lower cost and lower weight alternative to other materials commonly used at high temperatures, including titanium- and nickel-based alloys. To this end, this aims to improve the properties of the Al alloys by adding various alloying elements in small quantities, on the order of several hundred atomic parts per million, to aluminum. The thesis begins by focusing on additions of Ti to Al-Sc. Ti is a slow diffuser in Al [1], and it will be shown that it improves the coarsening kinetics of the precipitate phase at 300°C. Since these alloys are coarsening resistant, it is found that they can be aged and crept at temperatures of up to 425°C. The properties displayed are similar to those of Al-Sc-Zr alloys studied previously [2, 3]. The examination of Ti additions is followed by a study of the additions of lanthanide elements. These elements are of interest since they are known to increase the lattice parameter of the precipitate phase [4-8], which could potentially lead to improved creep resistance [9]. Initially, binary Al-Yb alloys are studied to obtain some fundamental knowledge of the behavior of Yb in Al. Subsequent additions of Yb to Al-Sc result in improved creep resistance. A similar improved creep resistance is observed for additions of Gd to Al-Sc. Finally, this dissertation concludes with the study of Al-Sc-Yb-Zr alloys. Since the goal of this research is to obtain a creep-resistant as well as coarsening resistant alloy, both a slow diffusing element (Zr) and an element which improves the creep resistance (Yb) are added. The quaternary alloys are found to maintain the creep resistance and coarsening resistance of the Al- Sc-Yb and Al-Sc-Zr alloys, respectively, which points to opportunities for future research in this area. Northwestern University Ph.D. thesis no NU @ karnesky @ 9848
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Amouyal, Yaron Thermodynamics and kinetics of grain boundaries in ultra fine grained copper produced by severe plastic deformation Book Whole 2007 148 Reducing the average grain size of polycrystalline metals and alloys is a traditional way of increasing their strength. Moreover, many other attractive properties can be achieved by reducing average grain size: low-temperature superplasticity, improved magnetic properties, and homogeneity of physical properties. The recently developed technique of Equal Channel Angular Pressing (ECAP) allowed a breakthrough in decreasing the grain size of bulk materials to the sub-micrometer level. Its main principle is pressing a metal billet through an angular channel, a process that involves extremely large shear deformations forming dislocation cell structure at submicron scale. Subsequent pressings result in the formation of ultra-fine grains (UFG) with high-angle grain boundaries (GBs). Many unusual properties of materials produced by ECAP are attributed to nonequilibrium grain boundaries. These GBs are expected to exhibit higher values of energy, higher amplitude of strain fields, larger free volume, and higher diffusivity than their relaxed counterparts. Although the concept of non-equilibrium state of GBs is theoretically well established, its experimental foundation is still controversial. The aim of the present study is, therefore, providing an adequate experimental proof for the concept of non-equilibrium GBs by measurements of GB diffusivity and energy in copper and copper alloys subjected to ECAP. The diffusion of 63Ni radiotracer in Cu and Cu-Zr alloy was studied using the serial-sectioning method. The diffusion annealings were performed in the temperature range 150 °C – 350 °C for annealing times when volume diffusion is frozen and only short-circuit diffusion occurs. The microstructure studies by Transmission Electron Microscopy (TEM), Atomic Force Microscopy (AFM), and Focused Ion Beam (FIB) microscopy indicated that alloying with Zr is essential for stabilizing the ECAP-processed alloys against grain growth and recrystallization. In all samples studied the experimentally-acquired diffusion profiles exhibited two distinct slopes, which are associated with "slow"- and "fast" diffusion paths. The former is very close to that of relaxed GBs in coarse-grained Cu. Based on the analysis of the activity profiles, we proposed a hierarchical microstructure model of the UFG Cu-Zr alloy studied. In this model, a cellular skeleton of "fast" GBs with the characteristic cell size in the micrometer range is embedded in a network of "slow" GBs formed by sub-micrometer grains. This model allowed a quantitative processing of the measured activity profiles. The Arrhenius parameters of the GB diffusivities for the "slow" and "fast" GBs were determined, indicating a 3-4 orders of magnitude difference in respective pre-exponential factors. The measured radiotracer penetration profiles in pure ECAP-ed Cu exhibited a bimodal shape similar to that observed in the Cu-Zr alloy. In contrast to the Cu-Zr alloy, the pure Cu exhibited recrystallization during all thermal annealings. The explicit expression describing the kinetics of recrystallization in ECAP-ed Cu was obtained. A model that considers diffusion in UFG polycrystal undergoing recrystallization was developed. Its main assumption is that diffusion flux is allowed in the UFG phase only, while the recrystallizing grains "freeze" the concentration of solutes existing in the UFG matrix before it was consumed by recrystallizing grain. Application of this model enabled us deriving the slow-diffusion coefficients from the experimentally measured penetration profiles. The Arrhenius parameters of the GB diffusivities for the "slow" and "fast" GBs were determined, indicating about 3 orders of magnitude difference in respective pre-exponential factors. The relative energies of GBs in ultrafine grain copper obtained by ECAP were determined using the thermal grooving technique. The dihedral angles at the roots of GB grooves formed after annealings at 400 °C for 15 min and at 800 °C for 2h were determined with the aid of AFM. The average relative GB energies in the ECAP-ed samples annealed at 400 and 800 °C are 0.48 ± 0.11 and 0.27 ± 0.07 , respectively. Theoretical estimates of the relaxation time of non-equilibrium GBs indicated that little relaxation should occur after annealing at 400 °C, while full relaxation is expected after annealing at 800 °C. It was shown that the measured difference in GB energies can be correlated with the presence of two types of GBs in the same sample exhibiting very different diffusivities. We associated the fast-diffusion paths with unusually high GB diffusivities, and the high-energy GBs observed by AFM with the non-equilibrium GBs that were formed during ECAP. The volume fraction of such boundaries is small and they are separated by an extensive network of normal (i.e. exhibiting usual GB diffusivities and energies characteristic for annealed coarse grain polycrystals) GBs. These findings provide a solid experimental foundation for the concept of non-equilibrium GBs. Senate of the Technion – Israel Institute of Technology Ph.D. thesis no NU @ karnesky @ 9840
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Brothers, Alan Harold Processing and Properties of Advanced Metallic Foams Book Whole 2006 251 Since the development of the first aluminum foams in the middle of the 20th century [178], great advances have been made in the processing and fundamental understanding of metallic foams. As a result of these advances, metallic foams are now penetrating a number of applications where their unique suite of properties makes them superior to solid materials, such as lightweight structures, packaging and impact protection, and filtration and catalysis [3]. The purpose of this work is to extend the use of metallic foams in such applications by expanding their processing to include more sophisticated base alloys and architectures. The first four chapters discuss replacement of conventional crystalline metal foams with ones made from high-strength, low-melting amorphous metals, a substitution that offers potential for achieving mechanical properties superior to those of the best crystalline metal foams, without sacrificing the simplicity of processing methods made for low-melting crystalline alloys. Three different amorphous metal foams are developed in these chapters, and their structures and properties characterized. It is shown for the first time that amorphous metal foams, due to stabilization of shear bands during bending of their small strut-like features, are capable of compressive ductility comparable to that of ductile crystalline metal foams. A two-fold improvement 4 in mechanical energy absorption relative to crystalline aluminum foams is shown experimentally to result from this stabilization. The last two chapters discuss modifications in foam processing that are designed to introduce controllable and continuous gradients in local foam density, which should improve mass efficiency by mimicking the optimized structures found in natural cellular materials [64], as well as facilitate the bonding and joining of foams with solid materials in higher-order structures. Two new processing methods are developed, one based on replication of nonuniformly-compressed polymer precursors, and the other based on nonuniform chemical milling of uniform foams, and each method is demonstrated through the production of low-density aluminum foams having simple model density gradients. Northwestern University Ph.D. thesis no NU @ karnesky @ 1933
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Knipling, Keith E Development of a Nanoscale Precipitation-Strengthened Creep-Resistant Aluminum Alloy Containing Trialuminide Precipitates Book Whole 2006 230 Al-Zr This research is toward developing a castable and heat-treatable precipitation-strengthened aluminum alloy exhibiting coarsening- and creep resistance at temperatures exceeding 400°C. Criteria for selecting alloying elements capable of producing such an alloy are established. Those systems forming Al3M trialuminide compounds with a cubic L12 crystal structure are favored, and based on a review of the existing literature, these are assessed in terms of solid-solubility and diffusivity in &#945;-Al (satisfying the need for slow coarsening kinetics), and castability (which is discussed based on the binary phase diagrams). The first Group 3 element, Sc, and the second Group 4 element, Zr, are shown to be most promising. These expectations are confirmed by an initial study on the Al-Ti system, which demonstrates that conventionally-solidified alloys are not capable of precipitation strengthening. The Al-Zr system, by contrast, exhibits precipitation of nanometer-scale Al3Zr (L12) producing pronounced precipitation hardening when aged at 375, 400, or 425°C. The Al3Zr precipitates are coarsening resistant and have the metastable L12 structure up to 500°C, a result of very sluggish diffusion of Zr in &#945;-Al. Ternary additions of Ti are also investigated, forming Al3(Zr,Ti) (L12) precipitates with a reduced lattice parameter mismatch with &#945;-Al, potentially improving the coarsening resistance. The composition of Al3(Zr,Ti) precipitates formed at 375 or 425°C are measured directly using 3-D atom-probe tomography. At these temperatures, the Zr:Ti atomic ratio in the precipitates is about 10 and 5, respectively, indicating that most of the available Ti fails to partition to the Al3(Zr,Ti) phase. This is consistent with prior studies on Al-Sc alloys, where the slower-diffusing ternary solute species make up a small fraction of the Al3Sc-based precipitates. Despite the confirmed presence of Ti, Al3(Zr,Ti) precipitates exhibit no improvement in terms of coarsening resistance compared to binary Al3Zr. Mechanical properties of the Al-Zr and Al-Zr-Ti alloys are investigated utilizing Vickers microhardness and creep. The alloys deformed by creep at 300&#8722;400°C exhibit a dislocation climb-controlled threshold stress, ca. 6&#8722;12 MPa. The binary Al-Zr and ternary Al-Zr-Ti alloys behave similarly under ambient- and high temperature loading, consistent with the similar microstructures of the two alloys. Ph.D. thesis Northwestern University no NU @ keith.knipling @ 1785
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Gerstl, Stephan S. A. Three-Dimensional Nanometer Scale Analyses of Precipitate Structures and Local Compositions in TiAl Engineering Alloys Book Whole 2006 231 Titanium aluminide (TiAl) alloys are among the fastest developing class of materials for use in high temperature structural applications. Their low density and high strength make them excellent candidates for both engine and airframe applications. Creep properties of TiAl alloys, however, have been a limiting factor in applying the material to a larger commercial market. In this research, nanometer scale compositional and structural analyses of several TiAl alloys, ranging from model Ti-Al-C ternary alloys to putative commercial alloys with 10 components are investigated utilizing threedimensional atom probe (3DAP) and transmission electron microscopies. Nanometer sized borides, silicides, and carbide precipitates are involved in strengthening TiAl alloys, however, chemical partitioning measurements reveal oxygen concentrations up to 14 at. % within the precipitate phases, resulting in the realization of oxycarbide formation contributing to the precipitation strengthening of TiAl alloys. iv The local compositions of lamellar microstructures and a variety of precipitates in the TiAl system, including boride, silicide, binary carbides, and intermetallic carbides are investigated. Chemical partitioning of the microalloying elements between the a2/g lamellar phases, and the precipitate/g–matrix phases are determined. Both W and Hf have been shown to exhibit a near interfacial excess of 0.26 and 0.35 atoms nm-2 respectively within ca. 7 nm of lamellar interfaces in a complex TiAl alloy. In the case of needle-shaped perovskite Ti3AlC carbide precipitates, periodic domain boundaries are observed 5.3±0.8 nm apart along their growth axis parallel to the TiAl[001] crystallographic direction with concomitant composition variations after 24 hrs. at 800°C. Northwestern University Ph.D. thesis no NU @ karnesky @ 803
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