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Nanocrystalline Alumina-Zirconia Thin Films Grown by Magnetron Sputtering
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
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: urn:nbn:se:liu:diva-17529ISBN: 978-91-85895-18-2 (print)OAI: oai:DiVA.org:liu-17529DiVA: diva2:209761
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
List of papers
1. Radio frequency dual magnetron sputtering deposition and characterization of nanocomposite Al2O3-ZrO2 thin films
Open this publication in new window or tab >>Radio frequency dual magnetron sputtering deposition and characterization of nanocomposite Al2O3-ZrO2 thin films
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2006 (English)In: Journal of Vacuum Science & Technology. A. Vacuum, Surfaces, and Films, ISSN 0734-2101, E-ISSN 1520-8559, 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.

National Category
Engineering and Technology
Identifiers
urn:nbn:se:liu:diva-14051 (URN)10.1116/1.2171709 (DOI)
Available from: 2006-10-06 Created: 2006-10-06 Last updated: 2017-12-13Bibliographically approved
2. Nanocomposite Al2O3-ZrO2 thin films grown by reactive dual radio-frequency magnetron sputtering
Open this publication in new window or tab >>Nanocomposite Al2O3-ZrO2 thin films grown by reactive dual radio-frequency magnetron sputtering
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2008 (English)In: Thin Solid Films, ISSN 0040-6090, E-ISSN 1879-2731, Vol. 516, no 15, 4977-4982 p.Article in journal (Refereed) Published
Abstract [en]

Crystalline alumina–zirconia nanocomposites have been synthesized at 450 °C and 750 °C with reactive magnetron sputtering using radio-frequency power supplies. The composition of the films ranged from pure alumina to pure zirconia as measured by ion beam techniques. Microstructural characterization showed the presence of monoclinic zirconia in the pure zirconia films and γ-alumina in the pure alumina films while the nanocomposites contained either an amorphous compound, γ-alumina, cubic zirconia or a mixture of these. The grain size was 5 nm for the nanocomposite compared to larger grains in the pure oxide films. Electron energy loss spectroscopy showed a clear progression from the pure alumina to the pure zirconia.

Place, publisher, year, edition, pages
Elsevier, 2008
Keyword
Alumina, Zirconia, Magnetron sputtering, Electron microscopy
National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-17525 (URN)
Note
On the day of the defence date the status of the article was: In Press.Available from: 2009-03-27 Created: 2009-03-27 Last updated: 2016-08-31Bibliographically approved
3. DC Magnetron Sputtering Deposition of Nanocomposite Alumina - Zirconia Thin Films
Open this publication in new window or tab >>DC Magnetron Sputtering Deposition of Nanocomposite Alumina - Zirconia Thin Films
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2008 (English)In: Thin Solid Films, ISSN 0040-6090, E-ISSN 1879-2731, Vol. 516, no 23, 8352-8358 p.Article in journal (Refereed) Published
Abstract [en]

Mixed aluminium oxide-zirconium oxide thin solid films have been synthesized at ~300 °C by reactive DC magnetron sputtering from two targets. Partial pressure control of the oxygen gas ensured stoichiometric films without compromising the deposition rate. The composition of the films ranged from pure alumina to pure zirconia as measured by XRay Photoelectron Spectroscopy. Microstructural characterisation showed that the pure zirconium oxide films nucleated initially as the tetragonal zirconia phase, while the 100/010/001 textured monoclinic zirconia phase grew under steady state conditions with a columnar structure. Addition of aluminium to ~3 at.% caused the formation of tetragonal zirconia in the films, while further additions led to an amorphous structure as governed by the alumina under the present kinetic limitations.

Keyword
Alumina, Zirconia, Dual Reactive DC Magnetron Sputtering, X-Ray Diffraction, Nanocomposite
National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-17526 (URN)10.1016/j.tsf.2008.04.040 (DOI)
Available from: 2009-03-27 Created: 2009-03-27 Last updated: 2016-08-31Bibliographically approved
4. Experiments and Modelling of Dual Reactive Magnetron Sputtering Using Two Reactive Gases
Open this publication in new window or tab >>Experiments and Modelling of Dual Reactive Magnetron Sputtering Using Two Reactive Gases
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2008 (English)In: Journal of Vacuum Science & Technology. A. Vacuum, Surfaces, and Films, ISSN 0734-2101, E-ISSN 1520-8559, Vol. 26, no 4, 565-570 p.Article in journal (Refereed) Published
Abstract [en]

Reactive sputtering from two elemental targets, aluminium and zirconium, with the addition of two reactive gases, oxygen and nitrogen, is studied experimentally as well as theoretically. The complex behaviour of this process is observed and explained. It is shown that the addition of oxygen to a constant supply of nitrogen, significantly changes the relative content of aluminium with respect to zirconium in the film. Moreover, it is concluded that there is substantially more oxygen than nitrogen in the films even when the oxygen supply is significantly lower than the nitrogen supply. It is further shown that the addition of a certain minimum constant flow of nitrogen reduces, and eventually eliminates, the hysteresis with respect to the oxygen supply. It is concluded that the presented theoretical model for the involved reactions and mass balance during reactive sputtering of two targets in two reactive gases is in qualitative agreement with the experimental results and can be used to find optimum processing conditions for deposition of films of a desired composition.

Keyword
Reactive Sputtering, Modelling, Oxynitrides, Aluminium, Zirconium
National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-17527 (URN)10.1116/1.2913582 (DOI)
Available from: 2009-03-27 Created: 2009-03-27 Last updated: 2016-08-31Bibliographically approved
5. Mass-spectrometry of the positive-ion flux during radio-frequency sputter deposition of alumina-zirconia nanocomposites
Open this publication in new window or tab >>Mass-spectrometry of the positive-ion flux during radio-frequency sputter deposition of alumina-zirconia nanocomposites
(English)Manuscript (Other academic)
Abstract [en]

The flux of positive ions during radio-frequency magnetron sputter deposition of zirconium oxide and aluminium oxide has been studied by mass-spectrometry. Deposition from single ceramic and metallic targets as well as the combined process containing two targets has been investigated. The ratio of metal-oxide clusters to purely metallic ions in the plasma was measured. For metallic targets, this ratio increased for increasing pressure, while for ceramic targets the ratio remained constant at a level lower than that for the metallic targets. The increase in the proportion of clusters when comparing between sputtering from metallic and ceramic targets is linked to the formation of stoichiometric films in the former case. The amount of oxygen ions in the plasma available for the formation of the film was also studied and found to be reduced when sputtering two targets instead of one, increasing the likelihood of the formation of oxygen deficient films. The positive ion energy distributions for metallic ions in the aluminium and zirconium oxide systems and the dependence of plasma potential on the total pressure are also reported.

National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-17528 (URN)
Available from: 2009-03-27 Created: 2009-03-27 Last updated: 2016-08-31Bibliographically approved

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Trinh, David Huy

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