M. A. Kirk

Argonne National Laboratory, Lemont, Illinois, United States

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Publications (219)284.07 Total impact

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    ABSTRACT: We report here the microstructural changes occurring in the zirconium alloy Excel (Zr-3.5 wt% Sn-0.8Nb-0.8Mo-0.2Fe) during heavy ion irradiation. In situ irradiation experiments were conducted at reactor operating temperatures on two Zr Excel alloy microstructures with different states of alloying elements, with the states achieved by different solution heat treatments. In the first case, the alloying elements were mostly concentrated in the beta (β) phase, whereas, in the second case, large Zr3(Mo,Nb,Fe)4 secondary phase precipitates (SPPs) were grown in the alpha (α) phase by long term aging. The heavy ion induced damage and resultant compositional changes were examined using transmission electron microscopy (TEM) in combination with scanning transmission electron microscope (STEM)-energy dispersive x-ray spectroscopy (EDS) mapping. Significant differences were seen in microstructural evolution between the two different microstructures that were irradiated under similar conditions. Nucleation and growth of -component loops and their dependence on the alloying elements are a major focus of the current investigation. It was observed that the -component loops nucleate readily at 100, 300, and 400 °C after a threshold incubation dose (TID), which varies with irradiation temperature and the state of alloying elements. It was found that the TID for the formation of -component loops increases with decrease in irradiation temperature. Alloying elements that are present in the form of SPPs increase the TID compared to when they are in the β phase solid solution. Dose and temperature dependence of loop size and density are presented. Radiation induced redistribution and clustering of alloying elements (Sn, Mo, and Fe) have been observed and related to the formation of -component loops. It has been shown that at the higher temperature tests, irradiation induced dissolution of precipitates occurs whereas irradiation induced amorphization occurs at 100 °C. Furthermore, dose and temperature seem to be the main factors governing the dissolution of SPPs and redistribution of alloying elements, which in turn controls the nucleation and growth of -component loops. The correlation between the microstructural evolution and microchemistry has been found by EDS and is discussed in detail.
    Journal of Materials Research 05/2015; 30. DOI:10.1557/jmr.2015.89 · 1.82 Impact Factor
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    ABSTRACT: Material performance in extreme radiation environments is central to the design of future nuclear reactors. Radiation induces significant damage in the form of dislocation loops and voids in irradiated materials, and continuous radiation often leads to void growth and subsequent void swelling in metals with low stacking fault energy. Here we show that by using in situ heavy ion irradiation in a transmission electron microscope, pre-introduced nanovoids in nanotwinned Cu efficiently absorb radiation-induced defects accompanied by gradual elimination of nanovoids, enhancing radiation tolerance of Cu. In situ studies and atomistic simulations reveal that such remarkable self-healing capability stems from high density of coherent and incoherent twin boundaries that rapidly capture and transport point defects and dislocation loops to nanovoids, which act as storage bins for interstitial loops. This study describes a counterintuitive yet significant concept: deliberate introduction of nanovoids in conjunction with nanotwins enables unprecedented damage tolerance in metallic materials.
    Nature Communications 04/2015; 6:7036. DOI:10.1038/ncomms8036 · 10.74 Impact Factor
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    ABSTRACT: Using in-situ transmission electron microscopy, we have directly observed nano-scale defects formed in ultra-high purity tungsten by low-dose high energy self-ion irradiation at 30K. At cryogenic temperature lattice defects have reduced mobility, so these microscope observations offer a window on the initial, primary damage caused by individual collision cascade events. Electron microscope images provide direct evidence for a power-law size distribution of nano-scale defects formed in high-energy cascades, with an upper size limit independent of the incident ion energy, as predicted by Sand et al. [Eur. Phys. Lett., 103:46003, (2013)]. Furthermore, the analysis of pair distribution functions of defects observed in the micrographs shows significant intra-cascade spatial correlations consistent with strong elastic interaction between the defects.
    EPL (Europhysics Letters) 03/2015; 110(3). DOI:10.1209/0295-5075/110/36001 · 2.27 Impact Factor
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    Marquis Kirk, Xiaoou Yi, Michael Jenkins
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    ABSTRACT: We describe aspects of transmission electron microscopy (TEM) technique to image and quantify the defect state following neutron or ion irradiation with an emphasis on experimental considerations. After outlining various neutron and ion irradiation scenarios, including some sample preparation suggestions, we discuss methods to measure defect densities, size distributions, structures, and interstitial or vacancy nature. The importance of the image simulations of Zhou is suggested for guidance to the most accurate quantification of the defect state. It is hoped that the usefulness of the present paper will be greatest for those experiments that compare defect states in materials after different irradiation conditions, or especially those studies designed to benchmark advanced computer model simulations of defect production and evolution. The successful simulation of the defect state in bulk samples neutron irradiated to high dose at high temperature is a goal to which the suggestions in this paper can contribute.
    Journal of Materials Research 02/2015; DOI:10.1557/jmr.2015.19 · 1.82 Impact Factor
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    ABSTRACT: In situ and ex situ transmission electron microscopy observation of small Kr bubbles in both single-crystal and polycrystalline UO2 were conducted to understand the inert gas bubble behavior in oxide nuclear fuel. The bubble size and volume swelling are shown as weak functions of ion dose but strongly depend on the temperature. The Kr bubble formation at room temperature was observed for the first time. The depth profiles of implanted Kr determined by atom probe tomography are in good agreement with the calculated profiles by SRIM, but the measured concentration of Kr is about 1/4 of the calculated concentration. This difference is mainly due to low solubility of Kr in UO2 matrix and high release of Kr from sample surface under irradiation.
    Journal of Nuclear Materials 01/2015; 456:125–132. DOI:10.1016/j.jnucmat.2014.09.026 · 2.02 Impact Factor
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    ABSTRACT: In situ transmission electron microscopy observation of polycrystalline UO2 (with average grain size of about 5 µm) irradiated with Kr ions at 600°C and 800°C was conducted to understand the radiation-induced dislocation evolution under the influence of grain boundaries. The dislocation evolution in the grain interior of polycrystalline UO2 was similar under Kr irradiation at different ion energies and temperatures. As expected, it was characterized by the nucleation and growth of dislocation loops at low irradiation doses, followed by transformation to extended dislocation lines and tangles at high doses. For the first time, a dislocation-denuded zone was observed near a grain boundary in the 1-MeV Kr-irradiated UO2 sample at 800°C. The denuded zone in the vicinity of grain boundary was not found when the irradiation temperature was at 600°C. The suppression of dislocation loop formation near the boundary is likely due to the enhanced interstitial diffusion toward grain boundary at the high temperature.
    JOM: the journal of the Minerals, Metals & Materials Society 10/2014; DOI:10.1007/s11837-014-1186-6 · 1.40 Impact Factor
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    ABSTRACT: Oxide dispersion strengthened ferritic alloys have superior radiation tolerance and thus become appealing candidates as fuel cladding materials for next generation nuclear reactors. In this study we constructed a model system, Fe/Y2O3 nanolayers with individual layer thicknesses of 10 and 50 nm, in order to understand their radiation response and corresponding damage mitigation mechanisms. These nanolayers were subjected to in situ Kr ion irradiation at room temperature up to similar to 8 displacements-per-atom. As-deposited Y2O3 layers had primarily amorphous structure. Radiation induced prominent nanocrystallization and grain growth in 50 nm thick Y2O3 layers. Conversely, little crystallization occurred in 10 nm thick Y2O3 layers implying size dependent enhancement of radiation tolerance. In situ video also captured grain growth in both Fe and Y2O3 and outstanding morphological stability of layer interfaces against Kr ion irradiation.
    Journal of Nuclear Materials 09/2014; 452(1-3). DOI:10.1016/j.jnucmat.2014.05.046 · 2.02 Impact Factor
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    Materials Research Letters 08/2014; 3(1):35-42. DOI:10.1080/21663831.2014.951494
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    ABSTRACT: In situ Transmission Electron Microscopy was conducted for single crystal UO2 to understand the microstructure evolution during 300 keV Xe irradiation at room temperature. The dislocation microstructure evolution was shown to occur as nucleation and growth of dislocation loops at low irradiation doses, followed by transformation to extended dislocation segments and tangles at higher doses. Xe bubbles with dimensions of 1–2 nm were observed after room-temperature irradiation. Electron Energy Loss Spectroscopy indicated that UO2 remained stoichiometric under room temperature Xe irradiation.
    Nuclear Instruments and Methods in Physics Research Section B Beam Interactions with Materials and Atoms 07/2014; 330:55–60. DOI:10.1016/j.nimb.2014.03.018 · 1.19 Impact Factor
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    ABSTRACT: Oxide Dispersion Strengthened (ODS) reduced activation ferritic steels are promising candidate materials for structural components of both nuclear fission and fusion reactors. However, when irradiated with energetic particles, they may suffer changes on their microstructures that degrade their mechanical performance. In-situ transmission electron microscopy studies on ion-irradiated ODS steels can give remarkable insights into fundamental aspects of radiation damage allowing dynamic observations of defect formation, mobilities, and interactions during irradiation. In this investigation, a commercially available PM2000 ODS steel was in-situ irradiated with 150 KeV Fe+ at room temperature and 700°C. These experiments showed that the oxide nanoparticles in these steels remain stable up to the higher irradiation dose (~ 1.5 dpa), and that these particles seem to be effective sinks for irradiation induced defects.
    Journal of Physics Conference Series 06/2014; 522(1):012032. DOI:10.1088/1742-6596/522/1/012032
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    ABSTRACT: Phase stability of Ni3(Al, Ti) precipitates in Inconel X-750 under cascade damage was studied using heavy ion irradiation with transmission electron microscope (TEM) in situ observations. From 333 K to 673 K (60 °C to 400 °C), ordered Ni3(Al, Ti) precipitates became completely disordered at low irradiation dose of 0.06 displacement per atom (dpa). At higher dose, a trend of precipitate dissolution occurring under disordered state was observed, which is due to the ballistic mixing effect by irradiation. However, at temperatures greater than 773 K (500 °C), the precipitates stayed ordered up to 5.4 dpa, supporting the view that irradiation-induced disordering/dissolution and thermal recovery reach a balance between 673 K and 773 K (400 °C and 500 °C). Effects of Ti/Al ratio and irradiation dose rate are also discussed.
    Metallurgical and Materials Transactions A 04/2014; 45a(6). DOI:10.1007/s11661-014-2309-y · 1.73 Impact Factor
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    ABSTRACT: In order to understand radiation damage in the nickel based superalloy Inconel X-750 in thermal reactors, where (n, α) transmutation reaction also occurred in addition to fast neutron induced atomic displacement, heavy ion (1 MeV Kr2+) irradiation with pre-injected helium was performed under in-situ observations of an intermediate voltage electron microscope at Argonne National Laboratory. By comparing to our previous studies using 1 MeV Kr2+ irradiation solely, the pre-injected helium was found to be essential in cavity nucleation. Cavities started to be visible after Kr2+ irradiation to 2.7 dpa at ≥200 °C in samples containing 200 appm, 1000 appm, and 5000 appm helium, respectively, but not at lower temperatures. The cavity growth was observed during the continuous irradiation. Cavity formation appeared along with a reduced number density of stacking fault tetrahedra, vacancy type defects. With higher pre-injected helium amount, a higher density of smaller cavities was observed. This is considered to be the result of local trapping effect of helium which disperses vacancies. The average cavity size increases with increasing irradiation temperatures; the density reduced; and the distribution of cavities became heterogeneous at elevated temperatures. In contrast to previous characterization of in-reactor neutron irradiated Inconel X-750, no obvious cavity sink to grain boundaries and phase boundaries was found even at high doses and elevated temperatures. MC-type carbides were observed as strong sources for agglomeration of cavities due to their enhanced trapping strength of helium and vacancies.
    Journal of Applied Physics 03/2014; 115(10):103508-103508-8. DOI:10.1063/1.4867637 · 2.19 Impact Factor
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    ABSTRACT: In the current investigation, TEM in-situ heavy ion (1MeV Kr2þ) irradiation with helium pre-injected at elevated temperature (400 �C) was conducted to simulate in-reactor neutron irradiation induced damage in CANDU spacer material Inconel X-750, in an effort to understand the effects of helium on irradiation induced cavity microstructures. Three different quantities of helium, 400 appm, 1000 appm, and 5000 appm, were pre-injected directly into TEM foils at 400 �C. The samples containing helium were then irradiated in-situ with 1MeV Kr2þ at 400 �C to a final dose of 5.4 dpa (displacement per atom). Cavities were formed from the helium injection solely and the cavity density and size increased with increasing helium dosage. In contrast to previous heavy ion irradiations with cold pre-injected helium, heterogeneous nucleation of cavities was observed. During the ensuing heavy ion irradiation, dynamical observation showed noticeable size increase in cavities which nucleated close to the grain boundaries. A “bubble-void” transformation was observed after Kr2þ irradiation to high dose (5.4 dpa) in samples containing 1000 appm and 5000 appm helium. Cavity distribution was found to be consistent with in-reactor neutron irradiation induced cavity microstructures. This implies that the distribution of helium is greatly dependent on the injection temperature, and helium pre-injection at high temperature is preferred for simulating the migration of the transmutation produced helium.
    Journal of Applied Physics 03/2014; 115(10). DOI:10.1063/1.4867638 · 2.19 Impact Factor
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    D R Mason, X Yi, M A Kirk, S L Dudarev
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    ABSTRACT: Using _in situ_ transmission electron microscopy (TEM), we have observed nanometre scale dislocation loops formed when an ultra-high-purity tungsten foil is irradiated with a very low fluence of self-ions. Analysis of the TEM images has revealed the largest loops to be predominantly of prismatic 1/2<111> type and of vacancy character. The formation of such dislocation loops is surprising since isolated loops are expected to be highly mobile, and should escape from the foil. In this work we show that the observed size and number density of loops can be explained by the fact that the loops are _not_ isolated - the loops formed in close proximity in the cascades interact with each other and with vacancy clusters, also formed in cascades, through long-range elastic fields, which prevent the escape of loops from the foil. We find that experimental observations are well reproduced by object Kinetic Monte Carlo simulations of evolution of cascades _only_ if elastic interaction between the loops is taken into account. Our analysis highlights the profound effect of elastic interaction between defects on the microstructural evolution of irradiated materials.
    Journal of Physics Condensed Matter 02/2014; 26(37). DOI:10.1088/0953-8984/26/37/375701 · 2.22 Impact Factor
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    ABSTRACT: Heavy ion irradiation induced damage in Inconel X-750 at low temperatures (60–400 °C) has been reported in our previous study. In the current investigation, the microstructure evolution and phase change during heavy (1 MeV Kr2+) irradiation at elevated temperatures (500 °C and 600 °C) were characterized under in situ observation of intermediate voltage electron microscope (IVEM) at Argonne National Laboratory. For each temperature, defect analyses using the weak beam dark field method were carried out at several doses, up to 5.4 dpa. Small defects (<5 nm) yielded from high temperature irradiation comprise mainly stacking fault tetrahedras (SFTs), small ⅓ 〈1 1 1〉 and ½ 〈1 1 0〉 type dislocation loops. Large interstitial Frank loops were observed and a clear characteristic for growth of loops was video-captured. Unfaulting of interstitial Frank loops was observed. The number density of the defects saturated at a relatively low dose of 0.68 dpa. No obvious change of defect fraction was found with increasing dose, but more complex dislocation structures formed at higher doses. In contrast to low temperature irradiation, the primary strengthening phase γ′ was found to be stable during irradiation at temperatures >500 °C and was not disordered up to 5.4 dpa. No cavities were observed after the irradiation even at 600 °C.
    Journal of Nuclear Materials 02/2014; 445(s 1–3):227–234. DOI:10.1016/j.jnucmat.2013.11.008 · 2.02 Impact Factor
  • D. Kaoumi, J. Adamson, M. Kirk
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    ABSTRACT: Ferritic/martensitic steels are candidate materials for structural and cladding components designed for Generation IV reactors because of their superior resistance to radiation damage at the high operating temperatures envisioned in these reactors. To enable the development and optimization of such advanced alloys for in-reactor use, a fundamental understanding of radiation damage accumulation in materials is required. In this work, two model F/M steels (12Cr model alloy and 9Cr model alloy) were irradiated with 1 MeV Kr ions at 50 K, 180 K, 298 K, 473 K and 573 K in situ in a TEM. The microstructure evolution under irradiation was followed and characterized at successive doses in terms of irradiation-induced defect formation and evolution, defect density, size distribution and interaction with the as-fabricated microstructure (e.g. dislocation networks, lath boundaries) using weak-beam dark-field imaging. The effect of the irradiation temperature on the defect kinetics is assessed at doses up to 2 dpa.
    Journal of Nuclear Materials 02/2014; 445(s 1–3):12–19. DOI:10.1016/j.jnucmat.2013.10.047 · 2.02 Impact Factor

Publication Stats

3k Citations
284.07 Total Impact Points

Institutions

  • 1974–2015
    • Argonne National Laboratory
      • Division of Materials Science
      Lemont, Illinois, United States
  • 1993–2014
    • University of Oxford
      • Department of Materials
      Oxford, England, United Kingdom
  • 1998
    • University of Vienna
      Wien, Vienna, Austria
  • 1991
    • Iowa State University
      Ames, Iowa, United States
  • 1990–1991
    • University of Illinois, Urbana-Champaign
      • Department of Materials Science and Engineering
      Urbana, Illinois, United States