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Topotaxial growth of Ti2AlN by solid state reaction in AlN/Ti(0001) multilayer thin films
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
GKSS Research Center Geesthacht.
Institute of Ion Beam Physics and Materials Research, Forschungszentrum Dresen-Rossendorf.
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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.

Place, publisher, year, edition, pages
2007. Vol. 90, no 174106
National Category
Natural Sciences
Identifiers
URN: urn:nbn:se:liu:diva-17105DOI: 10.1063/1.2731520OAI: oai:DiVA.org:liu-17105DiVA: diva2:201941
Available from: 2009-04-14 Created: 2009-03-06 Last updated: 2017-12-13Bibliographically approved
In thesis
1. Reactive Magnetron Sputter Deposition and Characterization of Thin Films from the Ti-Al-N and Sc-Al-N Systems
Open this publication in new window or tab >>Reactive Magnetron Sputter Deposition and Characterization of Thin Films from the Ti-Al-N and Sc-Al-N Systems
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:nbn:se:liu:diva-17683 (URN)LIU-TEK-LIC-2008:2 (Local ID)978-91-7393-996-6 (ISBN)LIU-TEK-LIC-2008:2 (Archive number)LIU-TEK-LIC-2008:2 (OAI)
Presentation
2008-02-14, 00:00 (English)
Supervisors
Available from: 2009-04-14 Created: 2009-04-14 Last updated: 2016-08-31Bibliographically approved
2. Growth and Phase Stability Studies of Epitaxial Sc-Al-N and Ti-Al-N Thin Films
Open this publication in new window or tab >>Growth and Phase Stability Studies of Epitaxial Sc-Al-N and Ti-Al-N Thin Films
2010 (English)Doctoral 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 deep into the Ti-Al-N system and to explore novel Sc-Al-N compounds. Thin films were epitaxially grown by reactive dual magnetron sputtering from elemental targets onto single-crystal substrates. Ion beam analyses 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 achieve information about phases, texture, and thickness of films, and to follow 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.

In the Sc-Al-N system, the perovskite Sc3AlN was for the first time synthesized as a thin film and in single phase, with a unit cell of 4.40 Å. The hardness was found to be 14.2 GPa, the elastic modulus 21 GPa, and the room temperature resistivity 41.2 μΩcm. Cubic solid solutions of Sc1-xAlxN can be synthesized with AlN molar fraction up to ~60%. Higher AlN contents yield three different epitaxial relations to ScN(111), namely, #1 Sc1-xAlxN(0001) || ScN(111) with Sc1-xAlxN[11210] || ScN[110], #2 Sc1-xAlxN(1011) || ScN(110) with Sc1-xAlxN[1210] || ScN[110], and #3 Sc1-xAlxN(1011) || ScN(113). An in situ deposition and annealing study of cubic Sc0.57Al0.43N films showed volume induced phase separation into ScN and wurtzite structure AlN, via nucleation and growth at the domain boundaries. The first indications for phase separation are visible at 1000 °C, and the topotaxial relationship between the binaries after phase separation is AlN(0001) || ScN(001) and AlN<01ɸ10> || ScN <1ɸ10>. This is compared with Ti1-xAlxN, for which an electronic structure driving force leads to spinodal decomposition into isostructural TiN and AlN already at 800 °C. First principles calculations explain the results on a fundamental physics level. Up to ~22% ScN can under the employed deposition conditions be dissolved into wurtzite Sc1-xAlxN films, while retaining a single-crystal structure and with lattice parameters matching calculated values.

In the Ti-Al-N system, the Ti2AlN phase was synthesized epitaxially by solid state reaction during interdiffusion between sequentially deposited layers of AlN(0001) and Ti(0001). When annealing the sample, N and Al diffused into the Ti layer, forming Ti3AlN(111) at 400 ºC and Ti2AlN(0001) at 500 ºC. The Ti2AlN formation temperature is 175 ºC lower than earlier reported results. Another way of forming Ti2AlN phase is by depositing understoichiometric TiNx at 800 °C onto Al2O3(0001). An epitaxial Ti2Al(O,N) (0001) oxynitride forms close to the interface between film and substrate through a solid state reaction. Ti4AlN3 was, however, not possible to synthesize when depositing films with a Ti:Al:N ratio of 4:1:3 due to competing reactions. A substrate temperature of 600 ºC yielded an irregularly stacked Tin+1AlNn layered structure because of the low mobility of Al ad-atoms. An increased temperature led to Al deficiency due to outdiffusion of Al atoms, and formation of the Ti2AlN phase and a Ti1-xAlxN cubic solid solution.

Place, publisher, year, edition, pages
Linköping: Linköping University Electronic Press, 2010. 98 p.
Series
Linköping Studies in Science and Technology. Dissertations, ISSN 0345-7524 ; 1314
National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-56274 (URN)978-91-7393-391-9 (ISBN)
Public defence
2010-05-28, Visionen, Hus B, ingång 27, Campus Valla, Linköpings universitet, Linköping, 09:15 (English)
Opponent
Supervisors
Available from: 2010-05-06 Created: 2010-05-06 Last updated: 2016-08-31Bibliographically approved

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Höglund, CarinaBeckers, ManfredBirch, JensHultman, Lars

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