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Carbon based Thin Films Prepared by HiPIMS and DCMS
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
2012 (English)Licentiate thesis, comprehensive summary (Other academic)
Abstract [en]

The present thesis focuses on carbon based thin films prepared by high power impulse magnetron sputtering (HiPIMS) and direct current magnetron sputtering (DCMS). The properties of such thin films can be tailored to an extensive variety; the film microstructure, for example, ranges in the presented work from fully amorphous, graphitic films to fullerene like (FL). Consequently, the applications of these films migh be as wide spread as their properties.

Carbon nitride (CNx, 0 < x < 0.20) as well as carbon fluoride (CFx 0.16 < x < 0.35)thin films were synthesized in an industrial deposition chamber by reactive sputtering  ofgraphite in an Ar/N2 and Ar/CF4 ambient. In order to gain a better understanding of thegrowth processes the C/Ar/N2 and the C/Ar/CF4 plasma was investigated by ion massspectroscopy at room temperature. Further understanding in this context gave thedetailed evaluation of target current and target voltage waveforms, acquired whengraphite was sputtered in HiPIMS mode. First principle calculations were carried out forthe growth of CFx and gave additional grasp about the most probable plasma precursorsas well as structure defining defects. Data gained from these characterisations of thedeposition processes were successfully related to the film properties. In order to linkdifferent process parameters to film properties, the synthesized films werecharacterized with regards to their thickness and deposition rate (secondary electronmicroscopy, SEM), chemical composition (elastic recoil detection analysis, ERDA and xrayphotoelectron spectroscopy, XPS), the chemical bonding (XPS), microstructure (transmission electron spectroscopy, TEM and selected area electron diffraction, SAED).Another part on thin film characterization comprised measurements for possibleapplications. For this, mainly nanoindentation and surface energy measurements wereperformed.

Application-related measurements revealed a hardness of up to 23 GPa at high elastic recoveries of ~ 90 % for CNx (x = 0.1) films that exhibited a weakly pronounced fullerene like structure. The hardness correlated with the microstructure and N incorporation rate of the thin film. Evidence by TEM for an increased amount of N intercalations in CNx HiPIMS thin films is supported by ion mass spectroscopic measurements. As expected, higher ion particle energies as well as amounts particularly for C+ and N+ were measured in the reactive HiPIMS plasma.

CFx thin films were found to show surface energies equivalent to superhydrophobic material for x > 0.26 while such films were polymeric in nature accounting for hardnesses below 1 GPa. Whereas, an amorphous structure for carbon-based films with fluorine contents ranging between 16 % and 23 % was observed. For such films, the hardness increased with decreasing fluorine content and ranged between 16 GPa and 4 GPa.

Place, publisher, year, edition, pages
Linköping: Linköping University Electronic Press, 2012. , 58 p.
Series
Linköping Studies in Science and Technology. Thesis, ISSN 0280-7971 ; 1521
National Category
Natural Sciences
Identifiers
URN: urn:nbn:se:liu:diva-74748Local ID: LIU-TEK-LIC-2012:6ISBN: 978-91-7519-949-8 (print)OAI: oai:DiVA.org:liu-74748DiVA: diva2:491771
Presentation
2012-03-02, Planck, Fysikhuset, Campus Valla, Linköpings universitet, Linköping, 10:15 (English)
Opponent
Supervisors
Available from: 2012-02-07 Created: 2012-02-07 Last updated: 2016-08-31Bibliographically approved
List of papers
1. CF(x) thin solid films deposited by high power impulse magnetron sputtering: Synthesis and characterization
Open this publication in new window or tab >>CF(x) thin solid films deposited by high power impulse magnetron sputtering: Synthesis and characterization
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2011 (English)In: Surface & Coatings Technology, ISSN 0257-8972, E-ISSN 1879-3347, Vol. 206, no 4, 646-653 p.Article in journal (Refereed) Published
Abstract [en]

Fluorine containing amorphous carbon films (CF(x), 0.16 andlt;= x andlt;= 0.35) have been synthesized by reactive high power impulse magnetron sputtering (HiPIMS) in an Ar/CF(4) atmosphere. The fluorine content of the films was controlled by varying the CF(4) partial pressure from 0 mPa to 110 mPa at a constant deposition pressure of 400 mPa and a substrate temperature of 110 degrees C. The films were characterized regarding their composition, chemical bonding and microstructure as well as mechanical properties by applying elastic recoil detection analysis, X-ray photoelectron spectroscopy, Raman spectroscopy, transmission electron microscopy, and nanoindentation. First-principles calculations were carried out to predict and explain F-containing carbon thin film synthesis and properties. By geometry optimizations and cohesive energy calculations the relative stability of precursor species including C(2), F(2) and radicals, resulting from dissociation of CF4, were established. Furthermore, structural defects, arising from the incorporation of F atoms in a graphene-like network, were evaluated. All as-deposited CF(x) films are amorphous. Results from X-ray photoelectron spectroscopy and Raman spectroscopy indicate a graphitic nature of CF(x) films with x andlt;= 0.23 and a polymeric structure for films with x andgt;= 0.26. Nanoindentation reveals hardnesses between similar to 1 GPa and similar to 16 GPa and an elastic recovery of up to 98%.

Place, publisher, year, edition, pages
Elsevier, 2011
Keyword
Fluorine containing carbon thin films, HiPIMS, CF(x), First principle calculations, XPS, TEM
National Category
Engineering and Technology
Identifiers
urn:nbn:se:liu:diva-72809 (URN)10.1016/j.surfcoat.2011.06.055 (DOI)000297086700011 ()
Note

Funding Agencies|Hungarian Academy of Sciences||

Available from: 2011-12-09 Created: 2011-12-08 Last updated: 2017-12-08
2. CF(x): A first-principles study of structural patterns arising during synthetic growth
Open this publication in new window or tab >>CF(x): A first-principles study of structural patterns arising during synthetic growth
2011 (English)In: Chemical Physics Letters, ISSN 0009-2614, E-ISSN 1873-4448, Vol. 516, no 1-3, 62-67 p.Article in journal (Refereed) Published
Abstract [en]

Structural and bonding patterns arising from the incorporation of fluorine atoms in a graphene-like network relevant to the deposition of carbon fluoride (CF(x)) films were addressed by first-principles calculations. We find that large N-member (N = 8-12) rings, defects by sheet branching, and defects associated with bond rotation pertain to CF(x). The cohesive energy gains associated with these patterns are similar to 0.2-0.4 eV/at., which is similar to those for a wide range of defects in other C-based nanostructured solids. Fullerene-like CF(x) is predicted for F concentrations below similar to 10 at.%, while CF(x) compounds with higher F content are predominantly amorphous or polymeric.

Place, publisher, year, edition, pages
Elsevier, 2011
National Category
Engineering and Technology
Identifiers
urn:nbn:se:liu:diva-72251 (URN)10.1016/j.cplett.2011.09.045 (DOI)000296582400011 ()
Note

Funding Agencies|Swedish Governmental Agency for Innovation Systems (VINNOVA)||European Research Council (ERC)||

Available from: 2011-11-24 Created: 2011-11-24 Last updated: 2017-12-08
3. Ion mass spectroscopy investigations during high power pulsed 1 magnetron sputtering and DCMS of Carbon in an Ar and Ar/N2 discharge
Open this publication in new window or tab >>Ion mass spectroscopy investigations during high power pulsed 1 magnetron sputtering and DCMS of Carbon in an Ar and Ar/N2 discharge
(English)Manuscript (preprint) (Other academic)
Abstract [en]

The composition of carbon discharges were investigated during reactive high power impulse magnetron sputtering (HiPIMS) and direct current magnetron sputtering (DCMS) using mass spectroscopy measurements in an industrial deposition system. During the sputter process 16 the ion flux was analyzed with regards to composition and energy. The ion energy distribution was measured in time-averaged and time-resolved mode for Ar+, C+, N2+, N+, and CxNy+ ions. While the N2-to-Ar flow ratio (ƒN2 / Ar) was varied, a constant deposition pressure and comparable energy per pulses were kept.

The results show that an increase of the N2-to-Ar flow ratio (keeping the pulse width, pulse frequency and pulse energies constant) an significant increase in C+, N+- and CN+-energy, while other ion flux energies did not considerably vary with the changes in working gas chemistry. A comparison with DCMS measurements showed the expected increase in ion energies as well as a significant increase of C+ ions in the HiPIMS plasma. The time evolution of the plasma species was analyzed in detail and showed the sequential arrival of working gas ions, ions ejected from the target and later during the pulse on time molecular ions such as CN+ as well as C2N+. Mass spectroscopic results in combination with the evaluation 1 of target current and target voltage waveforms as well as TEM (transmission electron microscopy) images and SAED (selected area electron diffraction patterns) for films deposited in DCMS and HiPIMS mode help to explain the formation of fullerene-like structured CNx thin films.

Keyword
HiPIMS, CNx, mass spectroscopy, carbon, sputtering, high power impulse magnetron 8 sputtering, HPPMS, high power pulse magnetron sputtering
National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-74746 (URN)
Available from: 2012-02-07 Created: 2012-02-07 Last updated: 2016-08-31Bibliographically approved

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