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Reactive Magnetron Sputter Deposition and Characterization of Thin Films from the Ti-Al-N and Sc-Al-N Systems
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
2009 (English)Licentiate thesis, comprehensive summary (Other academic)
Abstract [en]

This Thesis treats the growth and characterization of ternary transition metal nitride thin films. The aim is to probe deeper into the Ti-Al-N system and to explore the novel Sc-Al-N system. Thin films were epitaxially grown by reactive magnetron sputtering from elemental targets onto single-crystal substrates covered with a seed layer. Elastic recoil detection analysis and Rutherford backscattering spectroscopy were used for compositional analysis and depth profiling. Different x-ray diffraction techniques were employed, ex situ using Cu radiation and in situ during deposition using synchrotron radiation, to identify phases, to obtain information about texture, and to determine the thickness and roughness evolution of layers during and after growth. Transmission electron microscopy was used for overview and lattice imaging, and to obtain lattice structure information by electron diffraction. Film properties were determined using van der Pauw measurements of the electrical resistivity, and nanoindentation for the materials hardness and elastic modulus. The epitaxial Mn+1AXn phase Ti2AlN was synthesized by solid-state reaction during interdiffusion between sequentially deposited layers of (0001)-oriented AlN and Ti thin films. When annealing the sample, N and Al diffused into the Ti, forming Ti3AlN at 400 ºC and Ti2AlN at 500 ºC. The Ti2AlN formation temperature is 175 ºC lower than earlier reported results. Ti4AlN3 thin films were, however, not possible to synthesize when depositing films with a Ti:Al:N ratios of 4:1:3. Substrate temperatures at 600 ºC yielded an irregularly stacked Tin+1AlNn layered structure because of the low mobility of Al adatoms. An increased temperature led, however, to an Al deficiency due to an out diffusion of Al atoms, and formation of Ti2AlN phase and Ti1-xAlxN cubic solid solution. In the Sc-Al-N system the first ternary phase was discovered, namely the perovskite Sc3AlN, with a unit cell of 4.40 Å. Its existence was supported by ab initio calculations of the enthalpy showing that Sc3AlN is thermodynamically stable with respect to the binaries. Sc3AlN thin films were experimentally found to have a hardness of 14.2 GPa, an elastic modulus of 21 GPa, and a room temperature resistivity of 41.2 μΩcm.

Place, publisher, year, edition, pages
Linköping: Linköping University Electronic Press , 2009. , 42 p.
Series
Linköping Studies in Science and Technology. Thesis, ISSN 0280-7971 ; 1344
National Category
Natural Sciences
Identifiers
URN: urn:nbn:se:liu:diva-17683Local ID: LIU-TEK-LIC-2008:2ISBN: 978-91-7393-996-6 (print)OAI: oai:DiVA.org:liu-17683DiVA: diva2:211297
Presentation
2008-02-14, 00:00 (English)
Supervisors
Available from: 2009-04-14 Created: 2009-04-14 Last updated: 2016-08-31Bibliographically approved
List of papers
1. Topotaxial growth of Ti2AlN by solid state reaction in AlN/Ti(0001) multilayer thin films
Open this publication in new window or tab >>Topotaxial growth of Ti2AlN by solid state reaction in AlN/Ti(0001) multilayer thin films
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2007 (English)In: Applied Physics Letters, ISSN 0003-6951, E-ISSN 1077-3118, Vol. 90, no 174106Article in journal (Refereed) Published
Abstract [en]

The formation of Ti2AlN by solid state reaction between layers of wurtzite-AlN and α-Ti was characterized by in situ x-ray scattering. The sequential deposition of these layers by dual magnetron sputtering onto Al2O3(0001) at 200 °C yielded smooth, heteroepitaxial (0001) oriented films, with abrupt AlN/Ti interfaces as shown by x-ray reflectivity and Rutherford backscattering spectroscopy. Annealing at 400 °C led to AlN decomposition and diffusion of released Al and N into the Ti layers, with formation of Ti3AlN. Further annealing at 500 °C resulted in a phase transformation into Ti2AlN(0001) after only 5 min.

National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-17105 (URN)10.1063/1.2731520 (DOI)
Available from: 2009-04-14 Created: 2009-03-06 Last updated: 2017-12-13Bibliographically approved
2. The influence of substrate temperature and Al mobility on the microstructural evolution of magnetron sputtered ternary Ti-Al-N thin films
Open this publication in new window or tab >>The influence of substrate temperature and Al mobility on the microstructural evolution of magnetron sputtered ternary Ti-Al-N thin films
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2009 (English)In: Journal of Applied Physics, ISSN 0021-8979, E-ISSN 1089-7550, Vol. 106, no 6, 064915- p.Article in journal (Refereed) Published
Abstract [en]

Ternary Ti-Al-N films were deposited onto Al2O3 (0001) substrates by reactive co‑sputtering from elemental Ti and Al targets and analyzed by in situ and ex situ x-ray scattering, Rutherford backscattering spectroscopy, transmission electron microscopy and x-ray photoemission spectroscopy. The deposition parameters were set to values that yield Ti:Al:N ratios of 2:1:1 and 4:1:3 at room temperature. 2TiAlN depositions at 675 °C result in epitaxial Ti2AlN growth with basal planes parallel to the substrate surface. Nominal 4TiAl3N depositions at 675 °C and above, however, yield TiN and Ti2AlN domains due to Al loss to the vacuum. Depositions at a lower temperature of 600 °C yield films with correct 4:1:3 stoichiometry, but Ti4AlN3 formation is supposedly prevented by insufficient adatom mobility. Instead, an incoherent Tin+1AlNn structure with random twinned stacking sequences n is obtained, that exhibits both basal plane orientations parallel as well as nearly perpendicular to the substrate interface. X‑ray photoemission spectroscopy shows that in contrast to stoichiometric nitrides the Al is metallically bonded and hence acts as twinning plane within the Tin+1AlNn stackings. Domains with perpendicular basal plane orientation overgrowth those with parallel ones in a competitive growth mode. The resulting morphology is a combination of smooth‑surfaced parallel basal plane orientation domains interrupted by repeated facetted hillock-like features with perpendicular basal plane orientation.

National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-17107 (URN)10.1063/1.3208065 (DOI)
Available from: 2009-04-14 Created: 2009-03-06 Last updated: 2017-12-13Bibliographically approved
3. Sc3AlN: A New Perovskite
Open this publication in new window or tab >>Sc3AlN: A New Perovskite
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2008 (English)In: European Journal of Inorganic Chemistry, ISSN 1434-1948, E-ISSN 1099-1948, Vol. 2008, no 8, 1193-1195 p.Article in journal (Refereed) Published
Abstract [en]

Sc3AlN with perovskite structure has been synthesized as the first ternary phase in the Sc–Al–N system. Magnetron sputter epitaxy at 650 °C was used to grow single-crystal, stoichiometric Sc3AlN(111) thin films onto MgO(111) substrates with ScN(111) seed layers as shown by elastic recoil detection analysis, X-ray diffraction, and transmission electron microscopy. The Sc3AlN phase has a lattice parameter of 4.40 Å, which is in good agreement with the theoretically predicted 4.42 Å. Comparisons of total formation energies show that Sc3AlN is thermodynamically stable with respect to all known binary compounds. Sc3AlN(111) films of 1.75 μm thickness exhibit a nanoindentation hardness of 14.2 GPa, an elastic modulus of 249 GPa, and a roomtemperature electrical resistivity of 41.2 μΩ cm.

Keyword
Crystal growth, Density functional theory, Electron microscopy, Perovskite nitride phases, Thin films
National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-17106 (URN)10.1002/ejic.200701356 (DOI)
Available from: 2009-04-14 Created: 2009-03-06 Last updated: 2017-12-13Bibliographically approved

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Höglund, Carina

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