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Title Kolli, R. Prakash
Year Kinetics of nanoscale Cu-rich precipitates in a multicomponent concentrated steel
Abbreviated Journal Book Whole
Issue 2007 Keywords (down)
Place of Publication Language 320
Original Title Kinetics; Cu; precipitate; steel
Series Title 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. Series Volume
ISBN Ph.D. thesis Area Northwestern University
Serial Orig Record
no NU @ m-krug @ 10472
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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 α-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 α-Al. Ternary additions of Ti are also investigated, forming Al3(Zr,Ti) (L12) precipitates with a reduced lattice parameter mismatch with α-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 300−400°C exhibit a dislocation climb-controlled threshold stress, ca. 6−12 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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Krug, Matthew E. Microstructural Evolution and Mechanical Properties in Al-Sc Alloys With Li and Rare Earth Additions Book Whole 2011 372 Al-Sc, Al-Li, Al-Li-Sc, rare earth, LEAP, atom probe 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. Northwestern University Ph.D. thesis English no NU @ m-krug @ 11430
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Fuller, Christian B. Temporal Evolution of the Microstructures of Al(Sc,Zr) Alloys and Their Influences on Mechanical Properties Book Whole 2003 179 Al-Sc Al(Sc) alloys represent a new class of potential alloys for aerospace and automotive applications. These alloys have superior mechanical properties due to the presence of fine, coherent, unshearable Al3Sc precipitates, which form upon the decomposition of an supersaturated Al(Sc) solid-solution. Additions of Zr to Al(Sc) are found to improve alloy strength and coarsening resistance, but the operating mechanisms are not well understood. In this thesis, the relationships between the mechanical and microstructural properties of Al(Sc,Zr) alloy are presented. Three-dimensional atom probe microscopy (3DAP) and conventional and high-resolution transmission electron microscopies (CTEM and HREM) are utilized to study the temporal evolution of Al3Sc1-xZrx (L12 structure) precipitates in dilute Al(Sc,Zr) alloys (precipitate volume fractions < 1%) aged between 300 and 375°C. Concentration profiles, obtained with 3DAP, show Sc and Zr to partition to Al3Sc1-xZrx precipitates, and Zr to segregate near the Al/Al3Sc1-xZrx interface. CTEM and 3DAP are utilized to determine the temporal evolution of Al(Sc,Zr) alloys, which is discussed employing diffusion-limited coarsening theories. Zirconium additions are found to retard the precipitate coarsening kinetics and stabilize precipitate morphologies. Mechanical properties of Al(Sc,Zr) alloys are investigated utilizing Vicker’s microhardness and creep. Deformation at ambient-temperature is explained by classic precipitation-strengthening mechanisms, where a transition between precipitate shearing and Orowan looping is calculated to occur at an average precipitate radius, <r>, of 2-3 nm. Al(Sc,Zr) alloys deformed by creep at 300°C are found to exhibit a climb controlled threshold stress, which is shown to increase with <r>, in agreement with previous results in Al(Sc) alloys and a previous general climb model considering the interaction between dislocations and coherent misfitting precipitates. Finally, the effect of various heat-treatments upon the microstructure and mechanical properties of a rolled 5754 aluminum alloy modified with 0.23 wt.% Sc and 0.22 wt. % Zr are investigated. The presence of the Al3Sc1-xZrx precipitates is found to improve the alloy strength, by pinning subgrain and grain boundaries, as shown by hardness, tensile, and fatigue measurements. Northwestern University Ph.D. thesis no NU @ karnesky @ 147
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Marquis, Emmanuelle A. Microstructural Evolution and Strengthening Mechanisms in Al-Sc and Al-Mg-Sc Alloys Book Whole 2002 223 Al-Sc Al-Sc alloys are potential candidates for structural industrial applications because of their excellent mechanical properties due to the presence of small, coherent Al3Sc (L12 structure) precipitates that are formed during aging. Additional Mg alloying not only enhances the mechanical properties by solid-solution hardening but also provides corrosion resistance and better weldability. Understanding and controlling the microstructure, i.e. the temporal evolution of the Al3Sc precipitate morphologies and the effects of other alloying elements such as Mg, are critical for optimizing mechanical properties. First, this research aims at describing the microstructural evolution of the Al3Sc precipitates during aging using transmission electron microscopies. The effects of Mg additions on precipitation are described using high-resolution transmission electron microscopy observations and three-dimensional atom-probe microscopy analyses.Results on Mg segregation, on the nanoscale level, at the coherent Al / Al3Sc interface are presented. A second goal of this research is to understand the precipitation-strengthening parameters controlling optimal yield strength at room temperature and creep resistance at elevated temperature (0.6 Tm), the effects of precipitate size and volume fraction upon yield and creep strengths of dilute Al-Sc and Al-Mg-Sc alloys are studied. Room temperature strength is described in terms of precipitate shearing and Orowan dislocation looping. Creep threshold stresses are found to be about ten times lower than the yield stresses at 300°C, indicative of a climb-controlled bypass mechanism, which is modeled by extending existing dislocation-particle interaction models. Northwestern University Ph.D. thesis no NU @ karnesky @ 151
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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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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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Yoon, Kevin Eylhan Temporal Evolution of the Chemistry and Nanostructure of Multicomponent Model Ni-Based Superalloys Book Whole 2004 189 Ni-based superalloys are critical materials in the aerospace industry because of their excellent balance of mechanical properties including the elevated-temperature strength, which is a result of the dual-phase microstructure, consisting of the Ni-rich [gamma]-matrix (FCC) and [gamma]'-precipitates (L1[sub:2] structure). It is critical to understand the effects of each alloying element on the microstructure of Ni-based superalloys in order to further improve the mechanical properties, which are direct consequences of the microstructure. Nanoscale chemistry, nanostructure, and temporal evolution of several Ni-based superalloys, ranging from a simple model Ni-Cr-Al ternary alloy to a complex commercial superalloy, René N6, have been investigated utilizing three-dimensional atom probe (3DAP) microscopy and conventional transmission electron microscopy (CTEM). First, this research demonstrates the power of 3DAP microscopy, which can analyze the chemistry of the complex commercial superalloy, René N6, with nine elements. Concentration profiles and proximity histogram were obtained displaying the partitioning behavior of all alloying elements and especially Re interfacial segregation at the [gamma]/[gamma]' interface. Next, a model Ni-based superalloy, Ni-Cr-Al alloy, was studied as a reference for the study of a more complex quaternary alloy, Ni-Cr-Al-Re alloy. The temporal evolution of chemistry and nanostructure of the alloy are determined employing 3DAP microscopy. The coarsening kinetics of the [gamma]'-precipitates is examined and compared with theory, which is in partial agreement. A new coarsening mechanism has been suggested which explains the difference between the experimental results and the theoretical predictions. In addition, experimental results are also compared with the results of kinetic Monte Carlo (KMC) simulations. Finally, the effects of a Re addition on the temporal evolution of chemistry and microstructure of the Ni-Cr-Al alloy and coarsening kinetics of the [gamma]'-precipitates have been investigated employing 3DAP microscopy and CTEM. The Re addition stabilizes the spheroidal morphology of the [gamma]'-precipitates for extended aging times and retards the coarsening kinetics without any Re interfacial segregation. The coarsening kinetics is also compared with the theory. Northwestern University Ph.D. thesis no NU @ karnesky @ 15
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Sudbrack, Chantal K. Decomposition Behavior in Model Ni-Al-Cr-X Superalloys: Temporal Evolution and Compositional Pathways on a Nanoscale Book Whole 2004 209 In model Ni-Al-Cr-X superalloys, the compositional pathways and temporal evolution of coherent [gamma]' (L1[sub:2])-precipitation from an isothermally aged solid-solution, [gamma] (FCC), is investigated at: (i) 600°C, to study nucleation, growth, and coarsening; and (ii) 800°C, to study the influence of W on coarsening of a Ni-Al-Cr alloy. In the quenched Ni-5.2 Al-14.2 Cr at.% alloy, radial distribution functions establish Ni3(Al,Cr)-type short-range ordering that extends 0.6 nm and is Cr depleted. Phase separation at 600°C occurs by nucleation and growth, and the [gamma]'-precipitates’ morphology is a mixture of isolated spheroids and spheroids in various stages of coalescence. Sub-nanometer scale compositional profiles across the [gamma]/[gamma]' interfaces reveal: (i) transient chemical gradients of Al depletion and Cr enrichment adjacent to the precipitates; (ii) trapped Cr atoms in the growing precipitates; (iii) the interfacial width is component dependent; and (iv) increased Al solubility in the [gamma]'-precipitates resulting from capillarity. For a quasi-steady state, the governing power-law time dependencies during coarsening are compared to extant models and discussed in light of recent KMC simulations performed at Northwestern. Independent of the solute diffusivities, the [gamma]/[gamma]' interfacial free-energy is determined from coarsening data to be 22 to 23 mJ m[super:-2]. In Ni-9.8 Al-8.3 Cr at.% and Ni-9.7 Al-8.5 Cr at.%, spheroidal precipitates (5-15 nm diameter) form during quenching. Initially, chemical gradients exist in the [gamma]'-precipitates, however, they disappear after 1 h. After 16 h aging at 800°C, the precipitates have a cuboidal morphology and align along the elastically soft <100>-type directions. Particle size distributions and spatial pair correlation functions evolve temporally, and are discussed in context of the morphological development of the [gamma]'-precipitates. The coarsening kinetics of the mean radius and interfacial area per unit volume obey t1/3 and t–1/3 law, where the addition of W decreases the coarsening rate by a third. The slower kinetics are attributed to W’s influence on elemental partitioning, which leads to stronger partitioning of Al to the [gamma]'-phase and Cr to the &#947;-phase, and to its smaller diffusivity. Finally, an inflection-point method for determining reproducible phase compositions from three-dimensional atom-probe data is described, which is important for determining partitioning ratios. Northwestern University Ph.D. thesis I want to bring to your attention a mistake in my thesis with respect to the units on the compositional rate constant, kappa, which was a caught in the review process of recent submission of mine to Acta Mater. Kappa is obtained by fitting experimental data of the supersaturation del C of a particular phase, to: delC = C(t)- C(eqm)= kappa * t^(-1/3) so the units of kappa are at.% s^(1/3) NOT at.% s^(-1/3). Please make note of this. In my thesis, it applies to Figures: 4.1 (page 89), 4.2 (page 90), 4.3 (page 94) and Table 4.1 (page 95). no NU @ karnesky @ 16
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Sebastian, Jason T. Nanoscale Studies of Segregation at Ceramic/Metal Interfaces Book Whole 2004 250 Three-dimensional atom-probe (3DAP) microscopy has been applied to the study of segregation at ceramic/metal interfaces. In particular, the proximity histogram (proxigram) method has been implemented to extract the relative Gibbsian interfacial excess of solute from the 3DAP reconstructions directly, without recourse to external standards. Four systems have been studied—the MgO/Cu(X) (X = Ag or Sb) systems, the CdO/Ag(Au) system, and the MnO/Ag(Sb) system. For all four systems, the relative Gibbsian interfacial excess of solute at the ceramic/metal interface is determined, and trends in this value for the different systems are discussed. The observed trends for segregation imply that the driving force for solute segregation at these ceramic/metal interfaces is not due solely to a release of elastic energy associated with the segregating solute atoms. In the case of the MnO/Ag(Sb) system, the nanoscale temporal evolution of the oxide MnO precipitates as a function of specimen heat treatment is discussed. The observations have important implications for understanding the earliest stages of nucleation and growth of metal oxide precipitates created by internal oxidation. Northwestern University Ph.D. thesis no NU @ karnesky @ 148
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