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Hysteresis and process stability in reactive high power impulse magnetron sputtering of metal oxides
Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics.
Uppsala University, Sweden.
Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics.
Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.ORCID iD: 0000-0003-2864-9509
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2011 (English)In: Thin Solid Films, ISSN 0040-6090, E-ISSN 1879-2731, Vol. 519, no 22, 7779-7784 p.Article in journal (Refereed) Published
Abstract [en]

In the further development of reactive sputter deposition, strategies which allow for stabilization of the transition zone between the metallic and compound modes, elimination of the process hysteresis, and increase of the deposition rate, are of particular interest. In this study, the hysteresis behavior and the characteristics of the transition zone during reactive high power impulse magnetron sputtering (HiPIMS) of Al and Ce targets in an Ar-O(2) atmosphere as a function of the pulsing frequency and the pumping speed are investigated. Comparison with reactive direct current magnetron sputtering (DCMS) reveals that HiPIMS allows for elimination/suppression of the hysteresis and a smoother transition from the metallic to the compound sputtering mode. For the experimental conditions employed in the present study, optimum behavior with respect to the hysteresis width is obtained at frequency values between 2 and 4 kHz, while HiPIMS processes with values below or above this range resemble the DCMS behavior. Al-O films are deposited using both HiPIMS and DCMS. Analysis of the film properties shows that elimination/suppression of the hysteresis in HiPIMS facilitates the growth of stoichiometric and transparent Al(2)O(3) at relatively high deposition rates over a wider range of experimental conditions as compared to DCMS.

Place, publisher, year, edition, pages
Elsevier , 2011. Vol. 519, no 22, 7779-7784 p.
Keyword [en]
Reactive sputtering, High power impulse magnetron sputtering, Aluminum oxide, Cerium oxide, Hysteresis, Process stability
National Category
Engineering and Technology
URN: urn:nbn:se:liu:diva-71797DOI: 10.1016/j.tsf.2011.06.021ISI: 000295057000027OAI: diva2:453995

Funding Agencies|Swedish Research Council (VR)|621-2008-3222|Strategic Research Center in Materials Science for Nanoscale Surface Engineering (MS2E)||Ministry of Science and Technology, Thailand||VR|623-2009-7348|

Available from: 2011-11-04 Created: 2011-11-04 Last updated: 2014-10-29
In thesis
1. Reactive High Power Impulse Magnetron Sputtering of Metal Oxides
Open this publication in new window or tab >>Reactive High Power Impulse Magnetron Sputtering of Metal Oxides
2013 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

The work presented in this thesis deals with reactive magnetron sputtering processes of metal oxides with a prime focus on high power impulse magnetron sputtering (HiPIMS). The aim of the research is to contribute towards understanding of the fundamental mechanisms governing a reactive HiPIMS process and to investigate their implications on the film growth.

The stabilization of the HiPIMS process at the transition zone between the metal and compound modes of Al-O and Ce-O was investigated for realizing the film deposition with improved properties and higher depositionrate and the results are compared with direct current magnetron sputtering (DCMS) processes. The investigations were made for different sputtering conditions obtained by varying pulse frequency, peak power and pumping speed. For the experimental conditions employed, it was found that reactive HiPIMS can eliminate/suppress the hysteresis effect for a range of frequency, leading to a stable deposition process with a high deposition rate. The hysteresis was found to be eliminated for Al-O while for Ce-O, it was not eliminated but suppressed as compared to the DCMS. The behavior of elimination/suppression of the hysteresis may be influenced by high erosion rate during the pulse, limited target oxidation between the pulses and gas rarefaction effects in front of the target. Similar investigations were made for Ti-O employing a larger target and the hysteresis was found to be suppressed as compared to the respective DCMS, but not eliminated. It was shown that the effect of gas rarefaction is a powerful mechanism for preventing oxide formation upon the target surface. The impact of this effect depends on the off-time between the pulses. Longer off-times reduce the influence of gas rarefaction.

To gain a better understanding of the discharge current-voltage behavior in a reactive HiPIMS process of metal oxides, the ion compositions and ion energy distributions were measured for Al-O and Ti-O using time averaged and time-resolved mass spectrometry. It was shown that the different discharge current behavior between non-reactive and reactive modes couldn’t be explained solely by the change in the secondary electron emission yield from the sputtering target. The high fluxes of O1+ ions contribute substantially to the discharge current giving rise to an increase in the discharge current in the oxide mode as compared to the metal mode. The results also show that the source of oxygen in the discharge is both, the target surface (via sputtering) as well as the gas phase.

The investigations on the properties of HiPIMS grown films were made by synthesizing metal oxide thin films using Al-O, Ti-O and Ag-Cu-O. It was shown that Al2O3 films grown under optimum condition using reactive HiPIMS exhibit superior properties as compared to DCMS. The HiPIMS grown films exhibit higher refractive index as well as the deposition rate of the film growth was higher under the same operating conditions. The effect of HiPIMS peak power on TiO2 film properties was investigated and the results are compared with the DCMS. The properties of TiO2 films such as refractive index, film density and phase structure were experimentally determined. The ion composition during film growth was investigated and an explanation on the correlation of the film properties and ion energy was made. It was found that energetic and ionized sputtered flux in reactive HiPIMS can be used to tailor the phase formation of the TiO2 films with high peak powers facilitating the rutile phase while the anatase phase can be obtained using low peak powers. These phases can be obtained at room temperature without external substrate heating or post-deposition annealing which is in contrast to the reactive DCMS where both, anatase and rutile phases of TiO2 are obtained at either elevated growth temperatures or by employing post deposition annealing. The effect of HiPIMS peak power on the crystal structure of the grown films was also investigated for ternary compound, Ag-Cu-O, for which films were synthesized using reactive HiPIMS as well as reactive DCMS. It was found that the stoichiometric Ag2Cu2O3 can be synthesized by all examined pulsing peak powers. The oxygen gas flow rate required to form stoichiometric films is proportional to the pulsing peak power in HiPIMS. DCMS required low oxygen gas flow to synthesis the stoichiometric films. The HiPIMS grown films exhibit more pronounced crystalline structure as compared to the films grown using DCMS. This is likely an effect of highly ionized depositing flux which facilitates an intense ion bombardment during the film growth using HiPIMS. Our results indicate that Ag2Cu2O3film formation is very sensitive to the ion bombardment on the substrate as well as to the backattraction of metal and oxygen ions to the target.

Place, publisher, year, edition, pages
Linköping: Linköping University Electronic Press, 2013. 51 p.
Linköping Studies in Science and Technology. Dissertations, ISSN 0345-7524 ; 1519
National Category
Natural Sciences
urn:nbn:se:liu:diva-91259 (URN)978-91-7519-622-0 (print) (ISBN)
Public defence
2013-05-17, Planck, Fysikhuset, Campus Valla, Linköpings universitet, Linköping, 10:15 (English)
Available from: 2013-04-18 Created: 2013-04-18 Last updated: 2013-10-30Bibliographically approved

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