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  • 1.
    Eklund, Per
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Beckers, Manfred
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Frodelius, Jenny
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Högberg, Hans
    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.
    Magnetron sputtering of Ti3SiC2 thin films from a Ti3SiC2 compound target2007In: Journal of Vacuum Science & Technology. A. Vacuum, Surfaces, and Films, ISSN 0734-2101, E-ISSN 1520-8559, Vol. 25, no 5, p. 1381-1388Article in journal (Refereed)
    Abstract [en]

    Ti3 Si C2 thin films were synthesized by magnetron sputtering from Ti3 Si C2 and Ti targets. Sputtering from a Ti3 Si C2 target alone resulted in films with a C content of ∼50 at. % or more, due to gas-phase scattering processes and differences in angular and energy distributions between species ejected from the target. Addition of Ti to the deposition flux from a Ti3 Si C2 target is shown to bind the excess C in Ti Cx intergrown with Ti3 Si C2 and Ti4 Si C3. Additionally, a substoichiometric Ti Cx buffer layer is shown to serve as a C sink and enable the growth of Ti3 Si C2.

  • 2.
    Eklund, Per
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Frodelius, Jenny
    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.
    Lu, Jun
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Magnfält, Daniel
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
    Epitaxial growth of gamma-Al2O3 on Ti2AlC(0001) by reactive high-power impulse magnetron sputtering2014In: AIP Advances, ISSN 2158-3226, E-ISSN 2158-3226, Vol. 4, no 1, p. 017138-Article in journal (Refereed)
    Abstract [en]

    Al2O3 was deposited by reactive high-power impulse magnetron sputtering at 600 degrees C onto pre-deposited Ti2AlC(0001) thin films on alpha-Al2O3(0001) substrates. The Al2O3 was deposited to a thickness of 65 nm and formed an adherent layer of epitaxial gamma-Al2O3(111) as shown by transmission electron microscopy. The demonstration of epitaxial growth of gamma-Al2O3 on Ti2AlC (0001) open prospects for growth of crystalline alumina as protective coatings on Ti2AlC and related nanolaminated materials. The crystallographic orientation relationships are gamma-Al2O3(111)//Ti2AlC(0001) (out-of-plane) and gamma-Al2O3(2 (2) over bar0)//Ti2AlC(11 (2) over bar0) (in-plane) as determined by electron diffraction. Annealing in vacuum at 900 degrees C resulted in partial decomposition of the Ti2AlC by depletion of Al and diffusion into and through the gamma-Al2O3 layer.

  • 3.
    Eklund, Per
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Murugaiah, Anand
    Department of Materials Science and Engineering, Drexel University, Philadelphia, USA.
    Emmerlich, Jens
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Czigany, Zsolt
    Research Institute for Technical Physics and Materials Science, Hungarian Academy of Sciences, Budapest, Hungary.
    Frodelius, Jenny
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Barsoum, Michel W.
    Department of Materials Science and Engineering, Drexel University, Philadelphia, USA.
    Högberg, Hans
    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.
    Homoepitaxial growth of Ti-Si-C MAX-phase thin films on bulk Ti3SiC2 substrates2007In: Journal of Crystal Growth, ISSN 0022-0248, E-ISSN 1873-5002, Vol. 304, no 1, p. 264-269Article in journal (Refereed)
    Abstract [en]

    Ti3SiC2 films were grown on polycrystalline Ti3SiC2 bulk substrates using DC magnetron sputtering. The crystallographic orientation of the film grains is shown to be determined by the respective substrate-grain orientation through homoepitaxial MAX-phase growth. For a film composition close to Ti:Si:C=3:1:2, the films predominantly consist of MAX phases, both Ti3SiC2 and the metastable Ti4SiC3. Lower Si content resulted in growth of TiC with Ti3SiC2 as a minority phase. Thus, MAX-phase heterostructures with preferred crystallographic relationships can also be realized.

  • 4.
    Frodelius, Jenny
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Characterization of Ti2AlC coatings deposited with High Velocity Oxy-Fuel and Magnetron Sputtering Techniques2008Licentiate thesis, comprehensive summary (Other academic)
    Abstract [en]

    This Thesis presents two different deposition techniques for the synthesis of Ti2AlC coatings. First, I have fabricated Ti2AlC coatings by high velocity oxy-fuel (HVOF) spraying. Analysis with scanning electron microscopy (SEM) show dense coatings with thicknesses of ~150 µm when spraying with a MAXTHAL 211TM Ti2AlC powder of size ~38 µm in an H2/O2 gas flow. The films showed good adhesion to stainless steel substrates as determined by bending tests and the hardness was 3-5 GPa. X-ray diffraction (XRD) detected minority phases of Ti3AlC2, TiC, and AlxTiy alloys. The use of a larger powder size of 56 µm resulted in an increased amount of cracks and delaminations in the coatings. This was explained by less melted material, which is needed as a binding material. Second, magnetron sputtering of thin films was performed with a MAXTHAL 211TM Ti2AlC compound target. Depositions were made at substrate temperatures between ambient and 1000 °C. Elastic recoil detection analysis (ERDA) shows that the films exhibit a C composition between 42 and 52 at% which differs from the nominal composition of 25 at% for the Ti2AlC-target. The Al content, in turn, depends on the substrate temperature as Al is likely to start to evaporate around 700 °C. Co-sputtering with Ti target at a temperature of 700 °C, however, yielded Ti2AlC films with only minority contents of TiC. Thus, the addition of Ti is suggested to have two beneficial roles of balancing out excess of C and to retain Al by providing for more stoichiometric Ti2AlC synthesis conditions. Transmission electron microscopy and X-ray pole figures show that the Ti2AlC grains grow in two preferred orientations; epitaxial Ti2AlC (0001) // Al2O3 (0001) and with 37° tilted basal planes of Ti2AlC (101̅7) // Al2O3 (0001).

    List of papers
    1. Ti2AlC coatings deposited by High Velocity Oxy-Fuel spraying
    Open this publication in new window or tab >>Ti2AlC coatings deposited by High Velocity Oxy-Fuel spraying
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    2008 (English)In: Surface and Coatings Technology, ISSN 0257-8972, Vol. 202, no 24, p. 5976-5981Article in journal (Refereed) Published
    Abstract [en]

    High Velocity Oxy-Fuel has been utilized to spray coatings from Ti2AlC (MAXTHAL 211®) powders. X-ray diffraction showed that the coatings consist predominantly of Ti2AlC with inclusions of the phases Ti3AlC2, TiC, and Al–Ti alloys. The fraction of Ti2AlC in coatings sprayed with a powder size of 38 μm was found to increase with decreasing power of the spraying flame as controlled by the total gas flow of H2 and O2. A more coarse powder (56 μm) is less sensitive to the total gas flow and retains higher volume fraction of MAX-phase in the coatings, however, at the expense of increasing porosity. X-ray pole figure measurements showed a preferred crystal orientation in the coatings with the Ti2AlC (000l) planes aligned to the substrate surface. Bending tests show a good adhesion to stainless steel substrates and indentation yields a hardness of 3–5 GPa for the coatings sprayed with a powder size of 38 μm.

    Place, publisher, year, edition, pages
    Elsevier, 2008
    Keywords
    MAX-phase, High Velocity Oxy-Fuel (HVOF), Phase transitions, X-ray diffraction, Scanning electron microscopy (SEM)
    National Category
    Engineering and Technology
    Identifiers
    urn:nbn:se:liu:diva-13102 (URN)10.1016/j.surfcoat.2008.06.184 (DOI)
    Available from: 2008-04-01 Created: 2008-04-01 Last updated: 2016-08-31
    2. Direct current magnetron sputtering from a Ti2AlC target
    Open this publication in new window or tab >>Direct current magnetron sputtering from a Ti2AlC target
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    Manuscript (Other academic)
    Identifiers
    urn:nbn:se:liu:diva-13103 (URN)
    Available from: 2008-04-01 Created: 2008-04-01 Last updated: 2010-01-13
  • 5.
    Frodelius, Jenny
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Thick and Thin Ti2AlC Coatings2010Doctoral thesis, comprehensive summary (Other academic)
    Abstract [en]

    This Thesis explores the deposition techniques of magnetron sputtering and high velocity oxy-fuel (HVOF) spraying for Ti2AlC as a promising high-temperature material. Magnetron sputtering aims at producing thin (≤1 μm) Ti2AlC films of high crystal quality for use as a model system in understanding the material’s basic properties. HVOF is a new method for deposition of thick (≥200 μm) coatings by spraying Ti2AlC powder, with the aim of transferring the good bulk properties to coatings. The oxidation behavior of Ti2AlC coatings has been investigated for temperatures up to 1200 °C in air. As-deposited Ti2AlC(0001) thin films decompose into TiC during vacuum annealing at 700 °C by out-diffusion of Al as shown by x-ray diffraction analysis. The release of Al starts already at 500 °C in ambient air as driven by aluminum oxide formation on the film surface where the oxide initially forms clusters as observed by electron microscopy. While sputtering from a Ti2AlC target is simpler than by using different elemental targets, the resulting film composition differs from the target stoichiometry. This is due to differences in energy and angular distribution of the sputtered species and evaporation of Al at substrate temperatures above 700 °C. The composition can be compensated for by adding Ti to bind the Al and obtain phase-pure Ti2AlC coatings. For HVOF, I demonstrate how the total gas flow of a H2/O2 mixture (441-953 liter/min) and the powder grain size (30-56 μm) determine the thickness, density, and microstructure of the coatings. High gas flow and small grain size yield thick coatings of 210 μm with a low porosity of 2-8 % and a tensile stress of ≥80 MPa. A fraction of the Ti2AlC powder decomposes during spraying into TiC, Ti3AlC2, and Ti-Al alloys. The coatings also contain as much as 25 at.% O since the powder partly oxidizes during the spraying process. Increasing the powder size and decreasing the total gas flow yield a higher amount of Ti2AlC, but produces thinner coatings with lower cohesion. Post-annealing of the coatings at 900 °C in vacuum increases the Ti2AlC content due to a reversible phase transformation of the as-sprayed material. The high oxygen content, however, hinders the coating to completely transform into Ti2AlC and deteriorates its oxidation resistance. The work thus offers insights to the key parameters for optimizing Ti2AlC coating processing.

    List of papers
    1. Ti2AlC coatings deposited by High Velocity Oxy-Fuel spraying
    Open this publication in new window or tab >>Ti2AlC coatings deposited by High Velocity Oxy-Fuel spraying
    Show others...
    2008 (English)In: Surface and Coatings Technology, ISSN 0257-8972, Vol. 202, no 24, p. 5976-5981Article in journal (Refereed) Published
    Abstract [en]

    High Velocity Oxy-Fuel has been utilized to spray coatings from Ti2AlC (MAXTHAL 211®) powders. X-ray diffraction showed that the coatings consist predominantly of Ti2AlC with inclusions of the phases Ti3AlC2, TiC, and Al–Ti alloys. The fraction of Ti2AlC in coatings sprayed with a powder size of 38 μm was found to increase with decreasing power of the spraying flame as controlled by the total gas flow of H2 and O2. A more coarse powder (56 μm) is less sensitive to the total gas flow and retains higher volume fraction of MAX-phase in the coatings, however, at the expense of increasing porosity. X-ray pole figure measurements showed a preferred crystal orientation in the coatings with the Ti2AlC (000l) planes aligned to the substrate surface. Bending tests show a good adhesion to stainless steel substrates and indentation yields a hardness of 3–5 GPa for the coatings sprayed with a powder size of 38 μm.

    Place, publisher, year, edition, pages
    Elsevier, 2008
    Keywords
    MAX-phase, High Velocity Oxy-Fuel (HVOF), Phase transitions, X-ray diffraction, Scanning electron microscopy (SEM)
    National Category
    Engineering and Technology
    Identifiers
    urn:nbn:se:liu:diva-13102 (URN)10.1016/j.surfcoat.2008.06.184 (DOI)
    Available from: 2008-04-01 Created: 2008-04-01 Last updated: 2016-08-31
    2. Microstructure of high velocity oxy-fuel sprayed Ti2AlC coatings
    Open this publication in new window or tab >>Microstructure of high velocity oxy-fuel sprayed Ti2AlC coatings
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    2010 (English)In: Journal of Materials Science, ISSN 0022-2461, E-ISSN 1573-4803, Vol. 45, no 10, p. 2760-2769Article in journal (Refereed) Published
    Abstract [en]

    The microstructure formation and phase transformations in Ti2AlC-rich coatings deposited by High Velocity Oxy-fuel spraying of Maxthal 211(A (R)) powders is presented. High resolution electron microscopy analysis, using both scanning and transmission electron microscopy with energy dispersive spectrometry and energy filtering, combined with X-ray diffraction reveals that the coatings consist of Ti2AlC grains surrounded by regions of very small TiC grains embedded in Ti (x) Al (y) . The composition of the Ti (x) Al (y) depends on its surrounding and varies with size and distribution of the adjacent TiC grains. Impact of spray parameters on coating microstructure is also discussed. Two spray parameters were varied; powder size distribution and flame power. They were found to greatly affect the coating microstructure. Increasing powder size and decreasing flame power increase the amount of Ti2AlC, but produces thinner coatings with lower cohesion. Larger powder size will also decrease oxygen incorporation.

    Place, publisher, year, edition, pages
    Springer, 2010
    National Category
    Engineering and Technology
    Identifiers
    urn:nbn:se:liu:diva-54608 (URN)10.1007/s10853-010-4263-4 (DOI)000275457100029 ()
    Available from: 2010-03-26 Created: 2010-03-26 Last updated: 2017-12-12
    3. Annealing of thermally sprayed Ti2AlC coatings
    Open this publication in new window or tab >>Annealing of thermally sprayed Ti2AlC coatings
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    2011 (English)In: INTERNATIONAL JOURNAL OF APPLIED CERAMIC TECHNOLOGY, ISSN 1546-542X, Vol. 8, no 1, p. 74-84Article in journal (Refereed) Published
    Abstract [en]

    Phase transformations during annealing of coatings sprayed with the High Velocity Oxy-Fuel technique using Ti2AlC powder have been investigated by in-situ x-ray diffraction. The asdeposited coatings, consisting of Ti2AlC, Ti3AlC2, TiC, Ti-Al, and oxides, are stable up to 500 °C. Ti3AlC2 forms above 550 °C and Ti2AlC forms above 700 °C by intercalation of Al into TiCx. For temperatures between 900 and 1100 °C, Ti3AlC2 and Ti2AlC decompose by losing Al to the surrounding matrix resulting in TiCx, and Al2O3. The thermal expansion coefficient between ambient and 700°C is 11.9·10-6 K-1. The thermal diffusivity at room temperature is 1.9·10-6 m2/s.

    Place, publisher, year, edition, pages
    Blackwell, 2011
    National Category
    Natural Sciences
    Identifiers
    urn:nbn:se:liu:diva-57516 (URN)10.1111/j.1744-7402.2010.02569.x (DOI)000285968600009 ()
    Available from: 2010-06-22 Created: 2010-06-22 Last updated: 2016-08-31
    4. Oxidation of Ti2AlC bulk and spray deposited coatings
    Open this publication in new window or tab >>Oxidation of Ti2AlC bulk and spray deposited coatings
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    2010 (English)In: Corrosion Science, ISSN 0010-938X, E-ISSN 1879-0496, Vol. 52, no 12, p. 3955-3961Article in journal (Refereed) Published
    Abstract [en]

    The oxidation behaviour of Ti2AlC bulk and high velocity oxy-fuel spray deposited coatings has been investigated for temperatures up to 1200 °C. X-ray diffraction and electron microscopy show that bulk Ti2AlC forms a continuous layer of a-Al2O3 below a layer of TiO2 at temperatures as low as 700 °C. Oxidation of the Ti2AlC coatings is more complex, and also involves the phases Ti3AlC2, TiC, and TixAly, formed during the spraying process. a-Al2O3 is observed, however, it is unevenly distributed deep into the material, and does not form a continuous layer essential for good oxidation resistance.

    Place, publisher, year, edition, pages
    Elsevier, 2010
    Keywords
    Aluminium, Ceramic, Titanium, SEM, XRD, Oxidation
    National Category
    Natural Sciences
    Identifiers
    urn:nbn:se:liu:diva-57520 (URN)10.1016/j.corsci.2010.08.004 (DOI)000283961400015 ()
    Available from: 2010-06-22 Created: 2010-06-22 Last updated: 2017-12-12
    5. Sputter deposition from a Ti2AlC target: Process characterization and conditions for growth of Ti2AlC
    Open this publication in new window or tab >>Sputter deposition from a Ti2AlC target: Process characterization and conditions for growth of Ti2AlC
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    2010 (English)In: Thin Solid Films, ISSN 0040-6090, E-ISSN 1879-2731, Vol. 518, no 6, p. 1621-1626Article in journal (Refereed) Published
    Abstract [en]

    Sputter deposition from a Ti2AlC target was found to yield Ti-Al-C films with a composition that deviates from the target composition of 2:1:1. For increasing substrate temperature from ambient to 1000 degrees C, the Al content decreased from 22 at.% to 5 at.%, due to re-evaporation. The C content in as-deposited films was equal to or higher than the Ti content. Mass spectrometry of the plasma revealed that the Ti and Al species were essentially thermalized, while a large fraction of C with energies andgt;4 eV was detected. Co-sputtering with Ti yielded a film stoichiometry of 2:0.8:0.9 for Ti:Al:C, which enabled growth of Ti2AlC. These results indicate that an additional Ti flux balances the excess C and therefore provides for more stoichiometric Ti2AlC synthesis conditions.

    Place, publisher, year, edition, pages
    Elsevier, 2010
    Keywords
    MAX phase, Titanium carbide, Compound target, Physical vapor deposition, X-ray diffraction
    National Category
    Engineering and Technology
    Identifiers
    urn:nbn:se:liu:diva-54250 (URN)10.1016/j.tsf.2009.11.059 (DOI)000274812200001 ()
    Note
    Original Publication: Jenny Frodelius, Per Eklund, Manfred Beckers, Per Persson, Hans Högberg and Lars Hultman, Sputter deposition from a Ti2AlC target: Process characterization and conditions for growth of Ti2AlC, 2010, THIN SOLID FILMS, (518), 6, 1621-1626. http://dx.doi.org/10.1016/j.tsf.2009.11.059 Copyright: Elsevier Science B.V., Amsterdam. http://www.elsevier.com/ Available from: 2010-03-05 Created: 2010-03-05 Last updated: 2019-01-28
    6. Phase Stability and Initial Oxidation of Ti2AlC Thin Films at 500 °C
    Open this publication in new window or tab >>Phase Stability and Initial Oxidation of Ti2AlC Thin Films at 500 °C
    (English)Manuscript (preprint) (Other academic)
    Abstract [en]

    Ti2AlC thin films deposited onto Al2O3 by magnetron sputtering have been annealed in vacuum and ambient air. The films consist of basal-plane-oriented grains with a fraction of nonbasal-plane-oriented grains with an out-of-plane orientation of [1013] and [1016] as shown by x-ray diffraction and scanning electron microscopy. The surface of the basalplane-oriented grains has (0001) terraces growth. In situ x-ray diffraction shows that the Ti2AlC phase decomposes during vacuum annealing at 700 °C, which is lower than what have been reported for bulk material. When oxidized in ambient air at 500 °C for 5 min oxide clusters of amorphous Al2O3 form in valleys between terraces. The oxides are formed by out-diffusion of Al along the basal planes and migration over the surface. X-ray photoelectron spectroscopy of a Ti2AlC film oxidized at 500 °C for 15 min shows oxides due to a parallel oxidation of Ti and Al.

    National Category
    Natural Sciences
    Identifiers
    urn:nbn:se:liu:diva-57521 (URN)
    Available from: 2010-06-22 Created: 2010-06-22 Last updated: 2016-08-31
  • 6.
    Frodelius, Jenny
    et al.
    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.
    Beckers, Manfred
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Persson, Per
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Högberg, Hans
    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.
    Sputter deposition from a Ti2AlC target: Process characterization and conditions for growth of Ti2AlC2010In: Thin Solid Films, ISSN 0040-6090, E-ISSN 1879-2731, Vol. 518, no 6, p. 1621-1626Article in journal (Refereed)
    Abstract [en]

    Sputter deposition from a Ti2AlC target was found to yield Ti-Al-C films with a composition that deviates from the target composition of 2:1:1. For increasing substrate temperature from ambient to 1000 degrees C, the Al content decreased from 22 at.% to 5 at.%, due to re-evaporation. The C content in as-deposited films was equal to or higher than the Ti content. Mass spectrometry of the plasma revealed that the Ti and Al species were essentially thermalized, while a large fraction of C with energies andgt;4 eV was detected. Co-sputtering with Ti yielded a film stoichiometry of 2:0.8:0.9 for Ti:Al:C, which enabled growth of Ti2AlC. These results indicate that an additional Ti flux balances the excess C and therefore provides for more stoichiometric Ti2AlC synthesis conditions.

  • 7.
    Frodelius, Jenny
    et al.
    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.
    Phase Stability and Initial Oxidation of Ti2AlC Thin Films at 500 °CManuscript (preprint) (Other academic)
    Abstract [en]

    Ti2AlC thin films deposited onto Al2O3 by magnetron sputtering have been annealed in vacuum and ambient air. The films consist of basal-plane-oriented grains with a fraction of nonbasal-plane-oriented grains with an out-of-plane orientation of [1013] and [1016] as shown by x-ray diffraction and scanning electron microscopy. The surface of the basalplane-oriented grains has (0001) terraces growth. In situ x-ray diffraction shows that the Ti2AlC phase decomposes during vacuum annealing at 700 °C, which is lower than what have been reported for bulk material. When oxidized in ambient air at 500 °C for 5 min oxide clusters of amorphous Al2O3 form in valleys between terraces. The oxides are formed by out-diffusion of Al along the basal planes and migration over the surface. X-ray photoelectron spectroscopy of a Ti2AlC film oxidized at 500 °C for 15 min shows oxides due to a parallel oxidation of Ti and Al.

  • 8.
    Frodelius, Jenny
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Johansson, Emma M.
    Linköping University, Department of Physics, Chemistry and Biology, Nanostructured Materials. Linköping University, The Institute of Technology.
    Córdoba, José M.
    Linköping University, Department of Physics, Chemistry and Biology, Nanostructured Materials. Linköping University, The Institute of Technology.
    Odén, Magnus
    Linköping University, Department of Physics, Chemistry and Biology, Nanostructured Materials. 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.
    Annealing of thermally sprayed Ti2AlC coatings2011In: INTERNATIONAL JOURNAL OF APPLIED CERAMIC TECHNOLOGY, ISSN 1546-542X, Vol. 8, no 1, p. 74-84Article in journal (Refereed)
    Abstract [en]

    Phase transformations during annealing of coatings sprayed with the High Velocity Oxy-Fuel technique using Ti2AlC powder have been investigated by in-situ x-ray diffraction. The asdeposited coatings, consisting of Ti2AlC, Ti3AlC2, TiC, Ti-Al, and oxides, are stable up to 500 °C. Ti3AlC2 forms above 550 °C and Ti2AlC forms above 700 °C by intercalation of Al into TiCx. For temperatures between 900 and 1100 °C, Ti3AlC2 and Ti2AlC decompose by losing Al to the surrounding matrix resulting in TiCx, and Al2O3. The thermal expansion coefficient between ambient and 700°C is 11.9·10-6 K-1. The thermal diffusivity at room temperature is 1.9·10-6 m2/s.

  • 9.
    Frodelius, Jenny
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Lu, Jun
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Jensen, Jens
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Paul, Dennis
    Phys Elect USA, USA .
    Hultman, Lars
    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.
    Phase stability and initial low-temperature oxidation mechanism of Ti2AlC thin films2013In: Journal of the European Ceramic Society, ISSN 0955-2219, E-ISSN 1873-619X, Vol. 33, no 2, p. 375-382Article in journal (Refereed)
    Abstract [en]

    Ti2AlC thin films deposited onto Al2O3 by magnetron sputtering were used as model for studying the early stages (andlt; 15 min) of relatively low-temperature (500 degrees C) oxidation of Ti2AlC. The well-defined microstructure of these films forms a surface of valleys, hillocks and plateaus comprised of basal-plane-oriented grains with a fraction of nonbasal-plane-oriented grains with out-of-plane orientation of (1 0 (1) over bar 3) and (1 0 (1) over bar 6) as shown by X-ray diffraction and s electron microscopy. During oxidation, Al2O3 clusters and areas of C-containing titania (TiOxCy) are formed on the surface. A mechanism is proposed in which the locations of the Al2O3 clusters are related to the migration of Al atoms diffusing out of Ti2AlC. The Al2O3 is initially formed in valleys or on plateaus where Al atoms have been trapped while TiOxCy forms by in-diffusion of oxygen into the Al-deficient Ti2AlC. At 500 degrees C, the migration of Al atoms is faster than the oxidation kinetics; explaining this microstructure-dependent oxidation mechanism.

  • 10.
    Frodelius, Jenny
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Sonestedt, Marie
    Chalmers University of Technology, Microscopy and Microanalysis, Department of Applied Physics, Göteborg, Sweden.
    Björklund, Stefan
    University West, Department of Technology, Mathematics and Computer Science, Trollhättan, Sweden.
    Palmquist, Jens-Petter
    Kanthal AB, Hallstahammar, Sweden.
    Stiller, Krystyna
    Chalmers University of Technology, Microscopy and Microanalysis, Department of Applied Physics, Göteborg, Sweden.
    Högberg, Hans
    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.
    Ti2AlC coatings deposited by High Velocity Oxy-Fuel spraying2008In: Surface and Coatings Technology, ISSN 0257-8972, Vol. 202, no 24, p. 5976-5981Article in journal (Refereed)
    Abstract [en]

    High Velocity Oxy-Fuel has been utilized to spray coatings from Ti2AlC (MAXTHAL 211®) powders. X-ray diffraction showed that the coatings consist predominantly of Ti2AlC with inclusions of the phases Ti3AlC2, TiC, and Al–Ti alloys. The fraction of Ti2AlC in coatings sprayed with a powder size of 38 μm was found to increase with decreasing power of the spraying flame as controlled by the total gas flow of H2 and O2. A more coarse powder (56 μm) is less sensitive to the total gas flow and retains higher volume fraction of MAX-phase in the coatings, however, at the expense of increasing porosity. X-ray pole figure measurements showed a preferred crystal orientation in the coatings with the Ti2AlC (000l) planes aligned to the substrate surface. Bending tests show a good adhesion to stainless steel substrates and indentation yields a hardness of 3–5 GPa for the coatings sprayed with a powder size of 38 μm.

  • 11.
    Rech, S
    et al.
    Veneto Nanotech ScpA, Italy.
    Surpi, A
    Veneto Nanotech ScpA, Italy.
    Vezzu, S
    Veneto Nanotech ScpA, Italy.
    Patelli, A
    Veneto Nanotech ScpA, Italy.
    Trentin, A
    Veneto Nanotech ScpA, Italy.
    Glor, J
    Sandvik Mat Technology, Sweden.
    Frodelius, Jenny
    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.
    Eklund, Per
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Cold-spray deposition of Ti2AlC coatings2013In: Vacuum, ISSN 0042-207X, E-ISSN 1879-2715, Vol. 94, p. 69-73Article in journal (Refereed)
    Abstract [en]

    Ti2AlC coatings have been fabricated by cold-spray deposition. The microstructure evolution as a function of basic spray parameters temperature and pressure onto AA6060 aluminium alloy and 1.0037 steel substrates has been studied. Adherent and dense 50–80 μm thick Ti2AlC coatings were deposited on soft AA6060 substrates under gas temperature and pressure of 600 °C and 3.4 MPa, respectively, whilst comparable results were obtained on harder 1.0037 steel by using higher temperature (800 °C) and pressure (3.9 MPa).

  • 12.
    Sonestedt, Marie
    et al.
    Chalmers.
    Frodelius, Jenny
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Palmquist, Jens-Petter
    Kanthal AB.
    Högberg, Hans
    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.
    Stiller, Krystyna
    Chalmers.
    Microstructure of high velocity oxy-fuel sprayed Ti2AlC coatings2010In: Journal of Materials Science, ISSN 0022-2461, E-ISSN 1573-4803, Vol. 45, no 10, p. 2760-2769Article in journal (Refereed)
    Abstract [en]

    The microstructure formation and phase transformations in Ti2AlC-rich coatings deposited by High Velocity Oxy-fuel spraying of Maxthal 211(A (R)) powders is presented. High resolution electron microscopy analysis, using both scanning and transmission electron microscopy with energy dispersive spectrometry and energy filtering, combined with X-ray diffraction reveals that the coatings consist of Ti2AlC grains surrounded by regions of very small TiC grains embedded in Ti (x) Al (y) . The composition of the Ti (x) Al (y) depends on its surrounding and varies with size and distribution of the adjacent TiC grains. Impact of spray parameters on coating microstructure is also discussed. Two spray parameters were varied; powder size distribution and flame power. They were found to greatly affect the coating microstructure. Increasing powder size and decreasing flame power increase the amount of Ti2AlC, but produces thinner coatings with lower cohesion. Larger powder size will also decrease oxygen incorporation.

  • 13.
    Sonestedt, Marie
    et al.
    Chalmers University of Technology, Microscopy and Microanalysis, Department of Applied Physics, 412 96 Göteborg, Sweden.
    Frodelius, Jenny
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Sundberg, Mats
    Kanthal AB, 734 27 Hallstahammar, Sweden.
    Hultman, Lars
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Stiller, Krystyna
    Chalmers University of Technology, Microscopy and Microanalysis, Department of Applied Physics, 412 96 Göteborg, Sweden.
    Oxidation of Ti2AlC bulk and spray deposited coatings2010In: Corrosion Science, ISSN 0010-938X, E-ISSN 1879-0496, Vol. 52, no 12, p. 3955-3961Article in journal (Refereed)
    Abstract [en]

    The oxidation behaviour of Ti2AlC bulk and high velocity oxy-fuel spray deposited coatings has been investigated for temperatures up to 1200 °C. X-ray diffraction and electron microscopy show that bulk Ti2AlC forms a continuous layer of a-Al2O3 below a layer of TiO2 at temperatures as low as 700 °C. Oxidation of the Ti2AlC coatings is more complex, and also involves the phases Ti3AlC2, TiC, and TixAly, formed during the spraying process. a-Al2O3 is observed, however, it is unevenly distributed deep into the material, and does not form a continuous layer essential for good oxidation resistance.

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