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Radio frequency dual magnetron sputtering deposition and characterization of nanocomposite Al2O3-ZrO2 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.
Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics . Linköping University, The Institute of Technology.
Sandvik Tooling, Stockholm, Sweden.
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2006 (English)In: Journal of Vacuum Science & Technology. A. Vacuum, Surfaces, and Films, ISSN 0734-2101, Vol. 24, no 2, 309-316 p.Article in journal (Refereed) Published
Abstract [en]

Radio frequency magnetron sputtering from oxide targets has been used to synthesize crystalline alumina–zirconia nanocomposites at a relatively low temperature of 450  °C. Films of different compositions have been deposited ranging from pure zirconia to pure alumina, the compositions being measured with Rutherford backscattering and elastic recoil detection analysis. X-ray diffraction studies show the presence of the monoclinic zirconia phase in pure zirconia films. Addition of alumina into the film results in the growth of the cubic zirconia phase and amorphous alumina. No crystalline alumina was detected in either the composite or the pure alumina film. The microstructure of the films as studied by high resolution electron microscopy and scanning transmission electron microscopy shows a columnar growth mode in both the pure zirconia and nanocomposite films, but reveals differences in the intracolumnar structure. For the nanocomposite small equiaxed grains, ~5  nm in size, are found at the base of the columns at the interface with the substrate. An amorphous tissue of alumina was present between the small crystallites in the case of the nanocomposite.

Place, publisher, year, edition, pages
2006. Vol. 24, no 2, 309-316 p.
National Category
Engineering and Technology
Identifiers
URN: urn:nbn:se:liu:diva-14051DOI: 10.1116/1.2171709OAI: oai:DiVA.org:liu-14051DiVA: diva2:22530
Available from: 2006-10-06 Created: 2006-10-06 Last updated: 2016-08-31Bibliographically approved
In thesis
1. Nanocrystalline Alumina-Zirconia Thin Films Grown by Magnetron Sputtering
Open this publication in new window or tab >>Nanocrystalline Alumina-Zirconia Thin Films Grown by Magnetron Sputtering
2008 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Alumina-zirconia thin films have been deposited using dual magnetron sputtering. Film growth was performed at relatively low-to-medium temperatures, ranging from ~300°C to 810 °C. Different substrates were applied, including silicon (100), and industrially relevant materials, such as WC-Co hardmetal. Both radio-frequency sputtering and direct-current magnetron sputtering were utilised to achieve a range of film compositions. The influence of sputtering target was investigated; both ceramics and metals were used as sputtering sources. Microstructural characterisation was performed with a range of electron microscopy and x-ray diffraction techniques which show that the pure zirconia was deposited in the monoclinic phase. Reduced mobility of depositing species, as in the case of direct-current sputtering, yielded preferred crystallographic orientation in the {100} directions. The initial nucleation layer consisted of the metastable tetragonal zirconia phase. This phase could be grown over film thicknesses ~1 μm through the addition of ~3 at.% Al under similar low mobility conditions. For cases of higher mobility, as obtained through radio-frequency sputtering, the metastable cubic zirconia phase formed in the film bulk for alumina-zirconia nanocomposites. A combination of two mechanisms is suggested for the stabilisation of metastable zirconia phases: oxygen-deficiency and aluminium segregations with resultant restraint on the zirconia lattice. The sputter deposition process was investigated through energy resolved mass spectrometry in the case of radio-frequency sputtering; the sputter deposition flux contained a mixture of metallic ions, metaloxygen clusters, and oxygen ions. The presence of metal-oxygen clusters was found to be important in oxygen-stoichiometry and thus the phase selection of the resultant film. The energy distributions were similar when comparing sputtering from ceramic and metallic targets. A mass-balance model has also been developed for the transport phenomena and reactions of particles in reactive sputtering of two targets in a two-gas scenario for the alumina-zirconia system. Addition of nitrogen to the working gas was found to eliminate the hysteresis in the target poisoning for oxygen reactive sputtering. The higher reactivity of oxygen contributed to a higher oxygen content in resultant films compared to the oxygen content in the oxy-nitride working gas. The model was thus shown to be successful for tuning depositions in the alumina-zirconia oxy-nitride system.

Place, publisher, year, edition, pages
Linköping : Linköping University Electronic Presws, 2008. 68 p.
Series
Linköping Studies in Science and Technology. Dissertations, ISSN 0345-7524 ; 1153
National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-17529 (URN)978-91-85895-18-2 (ISBN)
Public defence
2008-02-22, Planck, Fysikhuset, Campus Valla, Linköpings universitet, Linköping, 10:15 (English)
Opponent
Supervisors
Available from: 2009-04-03 Created: 2009-03-27 Last updated: 2016-08-31Bibliographically approved
2. Synthesis and Characterisation of Magnetron Sputtered Alumina-Zirconia Thin Films
Open this publication in new window or tab >>Synthesis and Characterisation of Magnetron Sputtered Alumina-Zirconia Thin Films
2006 (English)Licentiate thesis, comprehensive summary (Other academic)
Abstract [en]

Alumina-Zirconia thin films were grown on a range of substrates using dual magnetron sputtering. Film growth was achieved at a relatively low temperature of 450 °C and at higher temperatures up to 810 °C. The films were grown on well-defined surfaces such as silicon (100) but also on industrially relevant substrates such as hardmetal (WC-Co). Radio frequency power supplies were used in combination with magnetron sputtering to avoid problems with target arcing. A range of film compositions were possible by varying the power on each target. The influence of sputtering target were investigated, both ceramic oxide targets and metallic targets being used.

The phase composition of the as-deposited films was investigated by x-ray diffraction. The pure zirconia films contained the monoclinic zirconia phase, while the pure alumina films appeared either amorphous or contained the gamma-alumina phase. The composite films contained a mixture of amorphous alumina, gamma-alumina and the cubic zirconia phase. In-depth high-resolution electron microscopy studies revealed that the microstructures consisted of phase-separated alumina and zirconia nanocrystals in the case of the nanocomposites. In-situ spectroscopy was also performed to characterise the nature of the bonding within the as-deposited films.

The oxygen stoichiometry in the films was investigated as a possible reason for the stabilisation of the cubic zirconia phase in the nanocomposite. Ion beam techniques such as Rutherford backscattering scattering and electron recoil detection analysis were used in these studies. The growth of films with ceramic targets led to films that may be slightly understoichiometric in oxygen, causing the phase stabilisation. The growth of films from metallic targets necessitates oxygen rich plasmas and it is not expected that such films will be oxygen deficient.

Initial attempts were also made to characterise the mechanical properties of the new material with nanoindentation. The nanocomposite appeared to have greater resistance to wear than the pure zirconia film. In doing so, some surface interactions and some material interactions have been studied.

Place, publisher, year, edition, pages
Institutionen för fysik, kemi och biologi, 2006. 48 p.
Series
Linköping Studies in Science and Technology. Thesis, ISSN 0280-7971 ; 1260
Series
Keyword
Alumina, Zirconia, NaKeywords: Alumina, Zirconia, Nanocomposite, Sputtering, Thin-Film, PVD, TEM, EELS
National Category
Materials Engineering
Identifiers
urn:nbn:se:liu:diva-7513 (URN)91-85523-40-2 (ISBN)
Presentation
2006-09-01, Planck, Fysikhuset, Campus Valla, Linköpings universitet, Linköping, 10:00 (English)
Opponent
Supervisors
Note
Report code: LIU-TEK-LIC-2006:41Available from: 2006-10-06 Created: 2006-10-06 Last updated: 2009-06-05

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Trinh, David HuyHögberg, HansAndersson, Jon M.Helmersson, UlfHultman, Lars

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