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  • 1.
    Bentzel, Grady W.
    et al.
    Drexel University, PA 19104 USA.
    Naguib, Michael
    Drexel University, PA 19104 USA.
    Lane, Nina J.
    Drexel University, PA 19104 USA.
    Vogel, Sven C.
    Los Alamos National Lab, NM 87545 USA.
    Presser, Volker
    Drexel University, PA 19104 USA.
    Dubois, Sylvain
    University of Poitiers, France.
    Lu, Jun
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
    Hultman, Lars
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
    Barsoum, Michel W.
    Drexel University, PA 19104 USA.
    Caspi, Elad N.
    Drexel University, PA 19104 USA; Nucl Research Centre Negev, Israel.
    High-Temperature Neutron Diffraction, Raman Spectroscopy, and First-Principles Calculations of Ti3SnC2 and Ti2SnC2016In: Journal of The American Ceramic Society, ISSN 0002-7820, E-ISSN 1551-2916, Vol. 99, no 7, p. 2233-2242Article in journal (Refereed)
    Abstract [en]

    Herein, we report-for the first time-on the additive-free bulk synthesis of Ti3SnC2. A detailed experimental study of the structure of the latter together with a secondary phase, Ti2SnC, is presented through the use of X-ray diffraction (XRD), and high-resolution transmission microscopy (HRTEM). A previous sample of Ti3SnC2, made using Fe as an additive and Ti2SnC as a secondary phase, was studied by high-temperature neutron diffraction (HTND) and XRD. The room-temperature crystallographic parameters of the two MAX phases in the two samples are quite similar. Based on Rietveld analysis of the HTND data, the average linear thermal expansion coefficients of Ti3SnC2 in the a and c directions were found to be 8.5 (2).10(-6) K-1 and 8.9 (1) . 10(-6) K-1, respectively. The respective values for the Ti2SnC phase are 10.1 (3) . 10(-6) K-1 and 10.8 (6) . 10(-6) K-1. Unlike other MAX phases, the atomic displacement parameters of the Sn atoms in Ti3SnC2 are comparable to those of the Ti and C atoms. When the predictions of the atomic displacement parameters obtained from density functional theory are compared to the experimental results, good quantitative agreement is found for the Sn atoms. In the case of the Ti and C atoms, the agreement is more qualitative. We also used first principles to calculate the elastic properties of both Ti2SnC and Ti3SnC2 and their Raman active modes. The latter are compared to experiment and the agreement was found to be good.

  • 2.
    Lane, Nina J
    et al.
    Drexel University, USA .
    Naguib, Michael
    Drexel University,USA .
    Lu, Jun
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Eklund, Per
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Hultman, Lars
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Barsoum, Michel W
    Drexel University, USA .
    Comment on "Ti5Al2C3: A New Ternary Carbide Belonging to MAX Phases in the Ti-Al-C System"2012In: Journal of The American Ceramic Society, ISSN 0002-7820, E-ISSN 1551-2916, Vol. 95, no 10, p. 3352-3354Article in journal (Refereed)
    Abstract [en]

    n/a

  • 3.
    Mouzon, Johanne
    et al.
    Luleå University of Technology.
    Lindbäck, Ture
    Luleå University of Technology.
    Odén, Magnus
    Luleå University of Technology.
    Influence of Agglomeration on the Transparency of Yttria Ceramics2008In: Journal of The American Ceramic Society, ISSN 0002-7820, E-ISSN 1551-2916, Vol. 10, no 91, p. 3380-3387Article in journal (Refereed)
    Abstract [en]

     In this work, five yttria powders with slightly different states of agglomeration, inherited from various procedures of dewatering the same precursor, were densified by a combination of vacuum sintering followed by hot isostatic pressing (HIP). In order to relate the densification behavior of each powder to its state of agglomeration, all powders were characterized by tap density measurements, X-ray diffraction, nitrogen adsorption, and laser scattering, while the microstructures of the corresponding densified samples were studied by optical and scanning electron microscopy. The five yttria powders produced sintered samples that differed remarkably from each other in terms of transparency. These discrepancies were related to the degree of fineness in the powders at two different levels. At the level of primary particles, fine and weakly agglomerated powder was very sinterable, causing abnormal grain growth to occur only in the very late stage of sintering. However, the resulting entrapped pores and reduction due to vacuum sintering were responsible for poor optical properties. At the agglomerate level, a bimodal size distribution was identified for all powders. For powders showing severe agglomeration of the primary particles, increasing the relative content of the smaller size population of agglomerates was found to trigger abnormal grain-growth earlier during presintering. This was attributed to the density around large agglomerates exceeding a critical threshold in the green bodies. Finally, transparency was achieved in samples for which presintering was stopped before grain growth became abnormal. This confirmed that the key to successfully obtaining transparency was to keep porosity intergranular, which could be removed subsequently by HIP treatment.

  • 4.
    Mouzon, Johanne
    et al.
    Luleå University of Technology.
    Odén, Magnus
    Luleå University of Technology.
    Tillement, Olivier
    Universite´ C. Bernard Lyon I.
    Jorand, Yves
    GEMPPM, INSA Lyon.
    Effect of drying and dewatering on yttria precursors with transient morphology2006In: Journal of The American Ceramic Society, ISSN 0002-7820, E-ISSN 1551-2916, Vol. 89, no 10, p. 3094-3100Article in journal (Refereed)
    Abstract [en]

    The influence of drying and dewatering of a yttrium hydroxynitrate precursor with transient morphology was investigated. The ability of this precursor to form soft agglomerated nanoparticles after calcination is dependent on the dewatering method. Freeze drying leads to finer particles than other dewatering methods that involve removal of the solvent from its liquid state. As water is directly removed by sublimation during freeze drying, this method inhibits the formation of solid bridges between hydroxynitrate platelets. These bridges, which form with the other dewatering methods, destabilize the spheroidization process of the platelets during subsequent firing at high temperatures.

  • 5.
    Naguib, Michael
    et al.
    Drexel University.
    Presser, Volker
    Drexel University.
    Tallman, Darin
    Drexel University.
    Lu, Jun
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Hultman, Lars
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Gogotsi, Yury
    Drexel University.
    Barsoum, Michel W
    Drexel University.
    On the Topotactic Transformation of Ti2AlC into a Ti-C-O-F Cubic Phase by Heating in Molten Lithium Fluoride in Air2011In: Journal of The American Ceramic Society, ISSN 0002-7820, E-ISSN 1551-2916, Vol. 94, no 12, p. 4556-4561Article in journal (Refereed)
    Abstract [en]

    Herein we report on the formation of a TiCOF phase via the topotactic transformation of Ti2AlC by immersion in molten lithium fluoride, LiF, at 900 degrees C in air for 2 h. The Al diffuses out of the structure and reacts with LiF to form Li3AlF6. X-ray diffraction, Raman spectroscopy, optical, scanning and transmission electron microscopy, with energy-dispersive spectroscopy, showed the selective etching of Al from the structure and the formation of a cubic, rock-salt, TiCOF phase. The transformation is topotaxial, involves de-twinning of the hexagonal Ti2AlC structure and results in domains that are of the order of 10 nm. The reaction rate is significantly higher when the reaction is carried out in air than when it is carried out in vacuum.

  • 6.
    Nordberg, Lars-Olov
    et al.
    Stockholm University.
    Käll, Per-Olov
    Linköping University, Department of Physics, Chemistry and Biology. Linköping University, The Institute of Technology.
    Nygren, Mats
    Dept. Physical, Inorganic and Structural Chemistry, Stockholm University.
    Shen, Zhijian
    Dept. Physical, Inorganic and Structural Chemistry, Stockholm University.
    Stability and oxidation properties of RE–α-Sialon ceramics (RE = Y, Nd, Sm, Yb)1998In: Journal of The American Ceramic Society, ISSN 0002-7820, E-ISSN 1551-2916, Vol. 81, no 6, p. 1461-1470Article in journal (Refereed)
    Abstract [en]

    Oxidation studies of hot-pressed RE–α-sialons, REx-Si12−4.5xAl4.5xO1.5xN16−1.5x (with x = 0.40 for RE = Nd, Sm,Yb; and x = 0.48 for RE = Y) were carried out in oxygen in a TG apparatus for ca. 20 h. Very good oxidation resistance was found for the Yb-doped samples, with parabolic rateconstants Kp ≈ 0.09 × 10−6–3 × 10−6 mg2 cm−4 s−1 in the temperature range 1250–1350°C. The promising performance of this material was corroborated by long-term oxidation experiments (5 days) in air at 1350°C. Although the oxidation kinetics can be described by simple equations related to the parabolic rate law (e.g., the arctan equation, ΔW/Ao = α·arctan(bt)½+ct½), the oxidation process in these materials is likely to be complex. The significantly lower oxidation resistance of the RE = Nd, Sm doped α-sialons, especially at higher temperatures, is related to the formation of melilite, RE2Si3−yAlyO3+yN4−y (y ≈ 1), in these systems. The melilite phase is also responsible for the thermal instability of the Nd– and Sm–α-sialons.

  • 7.
    Persson, Jeanette
    et al.
    Stockholm University.
    Käll, Per-Olov
    Stockholm University.
    Nygren, Mats
    Stockholm University.
    Interpretation of the Parabolic and Non-Parabolic Oxidation Behaviour of Silicon Oxynitride1992In: Journal of The American Ceramic Society, ISSN 0002-7820, E-ISSN 1551-2916, Vol. 75, no 12, p. 3377-3384Article in journal (Refereed)
    Abstract [en]

    The oxidation process of Si2N2O, prepared by a hot isostatic pressing technique, has been studied by the thermogravimetric method. The oxidation has been performed in oxygen for 20 h in the temperature range 1300° to 1600°C, producing oxide scales of amorphous SiO2 and α-cristobalite. The weight gain for T 1350°C does not begin to follow a parabolic rate law, until a certain time, t0. The A0 parameter in the parabolic rate law, (Δw/A0)2=Kpt+B, represents the cross section area, A, through which the oxygen diffuses; in the derivation of this law A is assumed to be constant during the experiment. If crystallization occurs during the oxidation process, A will decrease with time. A function, A(t), describing the time dependence, has been developed and incorporated into the parabolic rate law, yielding a new rate law, which reads ΔW/A0=a arctan √bt+ct. This new rate law is valid in the time interval t < t0, whereas, for t > t0, the oxidation process follows the equation (Δw/A0)2=K°pt+B0. The relation of the latter equation to the common parabolic rate law is described. All of the oxidation curves are described by these equations. The activation energy of the oxygen diffusion (and of the oxidation (Kp)) is found to be 245 ± 25 kJ/mol, which is consistent with literature values reported for oxygen diffusion.

  • 8.
    Ramasamy, Madhumidha
    et al.
    Forschungszentrum Julich GmbH, Julich, Germany.
    Baumann, Stefan
    Forschungszentrum Julich GmbH, Julich, Germany.
    Palisaitis, Justinas
    Forschungszentrum Julich GmbH, Julich, Germany.
    Schulze-Kuppers, Falk
    Forschungszentrum Julich GmbH, Julich, Germany.
    Balaguer, Maria
    Forschungszentrum Julich GmbH, Julich, Germany.
    Kim, Daejin
    Forschungszentrum Julich GmbH, Julich, Germany.
    Meulenberg, Wilhelm A.
    Forschungszentrum Julich GmbH, Julich, Germany.
    Mayer, Jochim
    Forschungszentrum Julich GmbH, Julich, Germany.
    Bhave, Ramesh
    Oak Ridge National Laboratory.
    Guillon, Olivier
    Forschungszentrum Julich GmbH, Julich, Germany.
    Bram, Martin
    Forschungszentrum Julich GmbH, Julich, Germany.
    Influence of Microstructure and Surface Activation of Dual-Phase Membrane Ce0.8Gd0.2O2−δ–FeCo2O4 on Oxygen Permeation2016In: Journal of The American Ceramic Society, ISSN 0002-7820, E-ISSN 1551-2916, Vol. 99, no 1, p. 349-355Article in journal (Refereed)
    Abstract [en]

    Dual-phase oxygen transport membranes are fast-growing research interest for application in oxyfuel combustion process. One such potential candidate is CGO-FCO (60 wt% Ce0.8Gd0.2O2−δ–40 wt% FeCo2O4) identified to provide good oxygen permeation flux with substantial stability in harsh atmosphere. Dense CGO-FCO membranes of 1 mm thickness were fabricated by sintering dry pellets pressed from powders synthesized by one-pot method (modified Pechini process) at 1200°C for 10 h. Microstructure analysis indicates presence of a third orthorhombic perovskite phase in the sintered composite. It was also identified that the spinel phase tends to form an oxygen deficient phase at the grain boundary of spinel and CGO phases. Surface exchange limitation of the membranes was overcome by La0.6Sr0.4Co0.2Fe0.8O3−δ (LSCF) porous layer coating over the composite. The oxygen permeation flux of the CGO-FCO screen printed with a porous layer of 10 μm thick LSCF is 0.11 mL/cm2 per minute at 850°C with argon as sweep and air as feed gas at the rates of 50 and 250 mL/min.

  • 9.
    Spencer, C B
    et al.
    Drexel University.
    Cordoba Gallego, Jose Manuel
    Linköping University, Department of Physics, Chemistry and Biology, Nanostructured Materials . Linköping University, The Institute of Technology.
    Obando, N
    Texas A&M University.
    Sakulich, A
    Drexel University.
    Radovic, M
    Texas A&M University.
    Odén, Magnus
    Linköping University, Department of Physics, Chemistry and Biology, Nanostructured Materials . Linköping University, The Institute of Technology.
    Hultman, Lars
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Barsoum, M W
    Drexel University.
    Phase Evaluation in Al(2)O(3) Fiber-Reinforced Ti(2)AlC During Sintering in the 1300 degrees C-1500 degrees C Temperature Range2011In: Journal of The American Ceramic Society, ISSN 0002-7820, E-ISSN 1551-2916, Vol. 94, no 10, p. 3327-3334Article in journal (Refereed)
    Abstract [en]

    In this article, the reactivity of Ti(2)AlC powders, with 3 and 10 mu m alumina, Al(2)O(3), fibers during pressure-assisted sintering is explored. Samples were fabricated by hot-isostatic-pressing (HIPed) or hot-pressing (HPed), and characterized by X-ray diffraction, differential thermal analysis, and electron microscopy-both scanning and transmission-equipped with energy dispersive X-ray spectroscopes. Samples prepared at 1300 degrees C were fully dense, with no apparent reaction between fiber and matrix. In samples HPed to 1500 degrees C, even pure Ti(2)AlC powders dissociated to Ti(3)AlC(2) according to: 2 Ti(2)AlC = Ti(3)AlC(2) + TiAl(x) (l) + (1-x) Al (l/v), with x andlt; 1. More severe Al loss results in the formation of TiC(y). The presence of the Al(2)O(3) fibers delayed densification enough to allow most of the Al and some of the Ti to escape into the vacuum of the hot press or react with the encapsulating glass during HIPing a resulting in a more intensive dissociation of the Ti(2)AlC. Although, in principle Ti(2)AlC can be reinforced with Al(2)O(3) fibers, the processing/use temperature will have to be kept below 1500 degrees C, as, at that temperature the fibers, used here, sinter together.

  • 10.
    Yang, Jian
    et al.
    Drexel University, PA 19104 USA; Drexel University, PA 19104 USA; Nanjing Technical University, Peoples R China.
    Naguib, Michael
    Oak Ridge National Lab, TN 37381 USA.
    Ghidiu, Michael
    Drexel University, PA 19104 USA;.
    Pan, Li-Mei
    Nanjing Technical University, Peoples R China.
    Gu, Jian
    Nanjing Technical University, Peoples R China.
    Nanda, Jagjit
    Oak Ridge National Lab, TN 37381 USA.
    Halim, Joseph
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering. Drexel University, PA 19104 USA; Drexel University, PA 19104 USA.
    Gogotsi, Yury
    Drexel University, PA 19104 USA; Drexel University, PA 19104 USA.
    Barsoum, Michel W.
    Drexel University, PA 19104 USA; Drexel University, PA 19104 USA.
    Two-Dimensional Nb-Based M4C3 Solid Solutions (MXenes)2016In: Journal of The American Ceramic Society, ISSN 0002-7820, E-ISSN 1551-2916, Vol. 99, no 2, p. 660-666Article in journal (Refereed)
    Abstract [en]

    Herein, two new two-dimensional Nb4C3-based solid solutions (MXenes), (Nb-0.8,Ti-0.2)(4)C3Tx and (Nb-0.8,Zr-0.2)(4)C3Tx (where T is a surface termination) were synthesizedas confirmed by X-ray diffractionfrom their corresponding MAX phase precursors (Nb-0.8,Ti-0.2)(4)AlC3 and (Nb-0.8,Zr-0.2)(4)AlC3. This is the first report on a Zr-containing MXene. Intercalation of Li ions into these two compositions, and Nb4C3Tx was studied to determine the potential of those materials for energy storage applications. Lithiation and delithiation peaks at 2.26 and 2.35 V, respectively, appeared in the case of Nb4C3Tx, but were not present in Nb2CTx. After 20 cycles at a rate of C/4, the specific capacities of (Nb-0.8,Ti-0.2)(4)C3Tx and (Nb-0.8,Zr-0.2)(4)C3Tx were 158 and 132 mAh/g, respectively, both slightly lower than the capacity of Nb4C3Tx.

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