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  • 1.
    Magnuson, Martin
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
    Tengdelius, Lina
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
    Eriksson, Fredrik
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
    Samuelsson, Mattias
    Linköping University, Department of Physics, Chemistry and Biology, Nanoscale engineering. Linköping University, Faculty of Science & Engineering.
    Broitman, Esteban
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
    Greczynski, Grzegorz
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
    Hultman, Lars
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
    Högberg, Hans
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
    Reactive magnetron sputtering of tungsten target in krypton/trimethylboron atmosphere2019In: Thin Solid Films, ISSN 0040-6090, E-ISSN 1879-2731, Vol. 688, article id 137384Article in journal (Refereed)
    Abstract [en]

    W-B-C films were deposited on Si(100) substrates held at elevated temperature by reactive sputtering from a W target in Kr/trimethylboron (TMB) plasmas. Quantitative analysis by Xray photoelectron spectroscopy (XPS) shows that the films are W-rich between ~ 73 and ~ 93 at.% W. The highest metal content is detected in the film deposited with 1 sccm TMB. The C and B concentrations increase with increasing TMB flow to a maximum of ~18 and ~7 at.%, respectively, while the O content remains nearly constant at 2-3 at.%. Chemical bonding structure analysis performed after samples sputter-cleaning reveals C-W and B-W bonding and no detectable W-O bonds. During film growth with 5 sccm TMB and 500 o C or with 10 sccm TMB and 300-600 o C thin film X-ray diffraction shows the formation of cubic 100-oriented WC1-x with a possible solid solution of B. Lower flows and lower growth temperatures favor growth of W and W2C, respectively. Depositions at 700 and 800 o C result in the formation of WSi2 due to a reaction with the substrate. At 900 o C, XPS analysis shows ~96 at.% Si in the film due to Si interdiffusion. Scanning electron microscopy images reveal a fine-grained microstructure for the deposited WC1-x films. Nanoindentation gives hardness values in the range from ~23 to ~31 GPa and reduced elastic moduli between ~220 and 280 GPa in the films deposited at temperatures lower than 600 o C. At higher growth temperatures the hardness decreases by a factor of 3 to 4 following the formation of WSi2 at 700-800 o C and Si-rich surface at 900 o C.

    The full text will be freely available from 2021-06-22 08:00
  • 2.
    Magnuson, Martin
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
    Tengdelius, Lina
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
    Greczynski, Grzegorz
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
    Eriksson, Fredrik
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
    Jensen, Jens
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
    Lu, Jun
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
    Samuelsson, Mattias
    Linköping University, Department of Physics, Chemistry and Biology, Nanoscale engineering. Linköping University, Faculty of Science & Engineering.
    Eklund, Per
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
    Hultman, Lars
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
    Högberg, Hans
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
    Compositional dependence of epitaxial Tin+1SiCn MAX-phase thin films grown from a Ti3SiC2 compound target2019In: Journal of Vacuum Science & Technology. A. Vacuum, Surfaces, and Films, ISSN 0734-2101, E-ISSN 1520-8559, Vol. 37, no 2, article id 021506Article in journal (Refereed)
    Abstract [en]

    The authors investigate sputtering of a Ti3SiC2 compound target at temperatures ranging from RT (no applied external heating) to 970 °C as well as the influence of the sputtering power at 850 °C for the deposition of Ti3SiC2 films on Al2O3(0001) substrates. Elemental composition obtained from time-of-flight energy elastic recoil detection analysis shows an excess of carbon in all films, which is explained by differences in the angular distribution between C, Si, and Ti, where C scatters the least during sputtering. The oxygen content is 2.6 at. % in the film deposited at RT and decreases with increasing deposition temperature, showing that higher temperatures favor high purity films. Chemical bonding analysis by x-ray photoelectron spectroscopy shows C–Ti and Si–C bonding in the Ti3SiC2 films and Si–Si bonding in the Ti3SiC2 compound target. X-ray diffraction reveals that the phases Ti3SiC2, Ti4SiC3, and Ti7Si2C5 can be deposited from a Ti3SiC2 compound target at substrate temperatures above 850 °C and with the growth of TiC and the Nowotny phase Ti5Si3Cx at lower temperatures. High-resolution scanning transmission electron microscopy shows epitaxial growth of Ti3SiC2, Ti4SiC3, and Ti7Si2C5 on TiC at 970 °C. Four-point probe resistivity measurements give values in the range ∼120 to ∼450 μΩ cm and with the lowest values obtained for films containing Ti3SiC2, Ti4SiC3, and Ti7Si2C5.

  • 3.
    Samuelsson, Mattias
    Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics .
    A Close Confinement Magnetron Design for use with HiPIMS2008In: The 11:th International Conference on Plasma Surface Engineering,2008, 2008Conference paper (Other academic)
  • 4.
    Samuelsson, Mattias
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
    Fundamental aspects of HiPIMS under industrial conditions2012Doctoral thesis, comprehensive summary (Other academic)
    Abstract [en]

    Fundamental aspects of the high power impulse magnetron sputtering (HiPIMS) process and its implication for film growth under industrial conditions have been studied. The emerging HiPIMS technique exhibits a higher plasma density and an enhanced degree of ionisation of sputtered material as compared to conventional direct current magnetron sputtering (DCMS). The increased ionisation permits control of the deposition flux and facilitates an intense ion bombardment of the growing films. The latter allows for growth of well adherent, smooth, and dense thin films. Moreover, the technique offers increased stability of reactive processes, control of film phase constitution as well as tailoring of e.g. optical and mechanical properties.

    In the present work, it was shown, for eight different metals (Al, Ti, Cr, Cu, Zr, Ag, Ta, and Pt), that films grown using HiPIMS exhibit a 5-15% higher density than films grown using DCMS under otherwise identical conditions. Through simulations of the fundamental ionisation processes in the plasma discharge, a correlation between high ionisation degree and film densification was established. The densification was suggested to be a consequence of increased ion irradiation of the growing films in the HiPIMS case. This knowledge was used to investigate the degree of ionisation in the deposition flux required for film modifications. Using a hybrid process, where DCMS and HiPIMS were combined on a single Cr cathode, independent control of the degree of ionisation from other experimental parameters was achieved. The results showed that the majority of the ion irradiation induced modifications of surface related film properties occurred when ~40% of the total average power was supplied by the HiPIMS generator. Under such conditions, the power normalised deposition rate was found to be ~80% of that of DCMS. This was attributed to a reduction in back-attracted ionised sputtered material, which is considered to be the main reason for the low deposition rate of HiPIMS. Thus, enhanced film properties were attainable largely without sacrificing deposition rate.

    Compound carbide and boride films were synthesised using both reactive processes and compound sources. Reactive deposition of TiC/a-C:H thin films using C2H2 as reactive gas, i.e. carbon source, was demonstrated. It was found that the high plasma density processes (i.e. HiPIMS) facilitated growth conditions for the film structure formation closer to thermodynamic equilibrium than did processes exhibiting lower plasma densities (i.e. DCMS). This was manifested in a high stoichiometry of the carbide phase, whilst excess a-C was removed by physical sputtering. Moreover, the feasibility of using HiPIMS for thin film growth from a compound source, obtaining the same composition in the films as the sputtering source, was demonstrated through synthesis of ZrB2 films.

  • 5.
    Samuelsson, Mattias
    Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics .
    High Power Impulse Magnetron Sputtering; An Overwiev of History, Properties and Current Status2008In: Nouvelles Tendances en Procedes Magnetron et Arc pour le Depot de Couches Minces New Trends in Magnetron and Arc Processing for Thin Film Deposition,2008, 2008Conference paper (Other academic)
  • 6.
    Samuelsson, Mattias
    Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics .
    High Power Impulse Magnetron Sputtering of Ti-Si-C Multifunctional Thin Films2008In: AVS 55th International Symposium,2008, 2008Conference paper (Other academic)
  • 7.
    Samuelsson, Mattias
    Linköping University, Department of Physics, Chemistry and Biology. Linköping University, The Institute of Technology.
    High power impulse magnetron sputtering under industrial conditions2011Licentiate thesis, comprehensive summary (Other academic)
    Abstract [en]

    In this thesis, the recent development step of magnetron sputtering, termed high power impulse magnetron sputtering (HiPIMS) has been studied. Compared to conventional magnetron sputtering HiPIMS provides a higher plasma density which can ionise the sputtered material. The beneficial influence of the coating properties due to this ionisation has been extensively shown in academic publications. Here, industrial conditions, i.e. no substrate heating and high vacuum conditions have been used during the studies, of which one was performed in an industrial deposition system.

    For eight metallic targets, films were deposited with HiPIMS and conventional sputtering. The films were evaluated by Rutherford back scattering analysis, scanning electron microscopy, and profilometry. It was found that the density of the HiPIMS grown films exhibited a statistically significant higher density of approximately 5-15% in comparison to films deposited using DCMS under identical conditions. A global plasma model was employed to evaluate the degree of ionisation for some of the target materials, and process conditions used in the study. Conformity between density increase and degree of ionisation as assessed by the plasma model was confirmed.

    The influence of using HiPIMS during reactive sputtering of TiC was also studied. A metallic Ti target was sputtered in a gas mixture of Ar and C2H2. The coatings were evaluated by X-ray photoelectron spectroscopy, X-ray diffraction, scanning electron microscopy, 4 point probe resistivity measurements, and nanoindentation. The coatings were found to be nanocomposite TiC/a-C:H. For the HiPIMS process the transition zone between metallic and compound target states was found to be significantly expanded over a wide reactive gas flow range. The implications of choice of deposition method for coating composition, chemical structure, as well as electrical and mechanical properties were evaluated for DCMS and HiPIMS. The process behaviour was suggested to be due to the pulsed nature of the HiPIMS, the high plasma density, and ion content of the particles reaching the substrate.

  • 8.
    Samuelsson, Mattias
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
    Jensen, Jens
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Helmersson, Ulf
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
    Hultman, Lars
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Högberg, Hans
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    ZrB2 thin films grown by high power impulse magnetron sputtering (HiPIMS) from a compound target2012In: Thin Solid Films, ISSN 0040-6090, E-ISSN 1879-2731, Vol. 526, p. 163-167Article in journal (Refereed)
    Abstract [en]

    ZrB2 thin films were grown on Si by high power impulse magnetron sputtering (HiPIMS) from a compound target in an industrial deposition system. By keeping a constant average power while modifying the HiPIMS pulse repetition frequency, the pulse peak current and thereby the degree of ionisation was varied. The films were characterised using X-ray diffraction techniques, scanning electron microscopy, time-of-flight elastic recoil detection analysis, and four-point probe measurements. It was found that the composition of the films matched closely that of the target material, and the films were low in contamination. The films were crystalline with a strong (000n) preferred orientation, and that the residual stress could be adjusted, from tensile to compressive, by increasing the degree of ionisation. The film morphology appeared dense, with a smooth surface, and the resistivity was found to range from 180 to 250 μΩcm with no clear dependence on frequency in the investigated parameter range.

  • 9.
    Samuelsson, Mattias
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
    Lundin, Daniel
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
    Jensen, Jens
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Raadu, Michael A
    Royal Institute of Technology.
    Gudmundsson, Jon Tomas
    University of Iceland.
    Helmersson, Ulf
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
    On the film density using high power impulse magnetron sputtering2010In: Surface & Coatings Technology, ISSN 0257-8972, E-ISSN 1879-3347, Vol. 205, no 2, p. 591-596Article in journal (Refereed)
    Abstract [en]

    The influence on thin film density using high power impulse magnetron sputtering (HIPIMS) has been investigated for eight different target materials (Al, Ti, Cr. Cu, Zr, Ag, Ta, and Pt). The density values as well as deposition rates have been compared to results obtained from thin films grown by direct current magnetron sputtering (DCMS) under the same experimental conditions. Overall, it was found that the HIPIMS deposited coatings were approximately 5-15% denser compared to the DCMS deposited coatings This could be attributed to the increased metal ion bombardment commonly seen in HIPIMS discharges, which also was verified using a global plasma model to assess the degree of ionization of sputtered metal One key feature is that the momentum transfer between the growing film and the incoming metal ions is very efficient due to the equal mass of film and bombarding species, leading to a less pronounced columnar microstructure As expected the deposition rates were found to be lower for HiPIMS compared to DCMS For several materials this decrease is not as pronounced as previously reported in the literature, which is shown in the case of Ta. Pt, and Ag with rate(HIPIMS)/rate(DCMS)-70-85%. while still achieving denser coatings

  • 10.
    Samuelsson, Mattias
    et al.
    Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics.
    Lundin, Daniel
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
    Sarakinos, Kostas
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
    Bjorefors, Fredrik
    Uppsala University, Sweden.
    Walivaara, Bengt
    Impact Coatings, Linköping, Sweden.
    Ljungcrantz, Henrik
    Impact Coatings, Linköping, Sweden.
    Helmersson, Ulf
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
    Influence of ionization degree on film properties when using high power impulse magnetron sputtering2012In: Journal of Vacuum Science & Technology. A. Vacuum, Surfaces, and Films, ISSN 0734-2101, E-ISSN 1520-8559, Vol. 30, no 3, p. 031507-Article in journal (Refereed)
    Abstract [en]

    Chromium thin films are deposited by combining direct current magnetron sputtering and high power impulse magnetron sputtering (HiPIMS) on a single cathode in an industrial deposition system. While maintaining a constant deposition rate and unchanged metal ion energy distribution function, the fraction of the total power supplied by either deposition technique is altered, and thereby also the metal ion to metal neutral ratio of the deposition flux. It is observed that the required total average power needed to be proportionally increased as the HiPIMS fraction is increased to be able to keep a constant deposition rate. The influence on microstructure, electrical, and electrochemical properties of the films is investigated and shows improvements with the use of HiPIMS. However, considerable influence of the studied properties occurs already when only some 40% of the total power is supplied by the HiPIMS technique. Further increase of the HiPIMS power fraction results in comparatively minor influence of the studied properties yet significant deposition rate efficiency reduction. The results show that the degree of ionization can be controlled separately, and that the advantages associated with using HiPIMS can be obtained while much of the deposition rate reduction, often reported for HiPIMS, can be avoided.

  • 11.
    Samuelsson, Mattias
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
    Sarakinos, Kostas
    Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics.
    Högberg, Hans
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Lewin, Erik
    Department of Materials Chemistry, The Ångström Laboratory, Uppsala University, Sweden.
    Jansson, Ulf
    Department of Materials Chemistry, The Ångström Laboratory, Uppsala University, Sweden.
    Wälivaara, Bengt
    Impact Coatings AB, Westmansgatan 29, SE-582 16 Linköping, Sweden.
    Ljungcrantz, Henrik
    Impact Coatings AB, Westmansgatan 29, SE-582 16 Linköping, Sweden.
    Helmersson, Ulf
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
    Growth of TiC/a-C:H nanocomposite films by reactive high power impulse magnetron sputtering under industrial conditions2012In: Surface & Coatings Technology, ISSN 0257-8972, E-ISSN 1879-3347, Vol. 206, no 8-9, p. 2396-2402Article in journal (Refereed)
    Abstract [en]

    Titanium carbide (TiC) films were deposited employing high power impulse magnetron sputtering (HiPIMS) and direct current magnetron sputtering (DCMS) in an Ar-C2H2 atmosphere of various compositions. Analysis of the structural, bonding and compositional characteristics revealed that the deposited films are nanocomposites; either hydrogenated amorphous carbon and TiC (TiC/a-C:H), or Titanium and TiC (Ti/TiC) depending on the C/Ti ratio of the films. It was found that TiC/a-C:H films grown by HiPIMS were dense, and within a certain C2H2 flow range (4-15 sccm) showed little changes in C/Ti ratio, which also saturated towards 1. The HiPIMS grown films also exhibited the tendency to form smaller fractions of amorphous C matrix, and incorporate smaller amounts of oxygen contaminants, as compared to films grown by DCMS. The TiC/a-C:H films exhibited resistivity and hardness values of 4-8×102 μΩcm and 20-27 GPa, respectively when deposited by HiPIMS. The corresponding values for films grown by DCMS at the same deposition rate as HiPIMS were >10×102 μΩcm and ~6-10 GPa respectively, likely due to abundant formation of free C and porosity, allowing oxygen contaminations.

  • 12.
    Samuelsson, Mattias
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
    Sarakinos, Kostas
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
    Lewin, Erik
    Laboratory of Nanoscale Materials Science Empa, Swiss Federal Laboratories for Materials Science and Technology, Dübendorf, Switzerland.
    Greene, Joseph
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Helmersson, Ulf
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
    The effect of plasma-surface interactions on the structure formation of vapour deposited TiC/a-C:H nanocomposite filmsManuscript (preprint) (Other academic)
    Abstract [en]

    Fundamental mechanisms determining the structure formation of nanocomposite TiC-/a-C:H thin films synthesised by reactive magnetron sputtering techniques have been studied. The investigation entailed varying the plasma density, composition, and substrate bias, thus altering ion-film interaction conditions. Moreover, by changing the vacuum pumping speed the influence of process stability was studied. The results show that the structure formation is predominantly controlled by energetic ion irradiation of the films, which, depending on the ion energies, provide increased adatom surface mobility and/or causes physical sputtering. No influence on the film structure formation due to process stability was seen, while influence of chemical sputtering could not be inferred. The present study explains previous results (Samuelsson et al., Surf. Coat. Technol. 206, 2396 (2012)), where the use of a high plasma density reactive sputtering technique resulted in film growth conditions favouring low presence of a-C:H and high stoichiometry of the TiC phase.

  • 13.
    Tengdelius, Lina
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Samuelsson, Mattias
    Linköping University, Department of Physics, Chemistry and Biology. Linköping University, The Institute of Technology.
    Jensen, Jens
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Lu, Jun
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Hultman, Lars
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Forsberg, Urban
    Linköping University, Department of Physics, Chemistry and Biology, Semiconductor Materials. Linköping University, The Institute of Technology.
    Janzén, Erik
    Linköping University, Department of Physics, Chemistry and Biology, Semiconductor Materials. Linköping University, The Institute of Technology.
    Högberg, Hans
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Direct current magnetron sputtered ZrB2 thin films on 4H-SiC(0001) and Si(100)2014In: Thin Solid Films, ISSN 0040-6090, E-ISSN 1879-2731, Vol. 550, p. 285-290Article in journal (Other academic)
    Abstract [en]

    ZrB2 thin films have been synthesized using direct current magnetron sputtering from a ZrB2 compound target onto 4H-SiC(0001) and Si(100) substrates kept at different temperatures (no heating, 400 °C, and 550 °C), and substrate bias voltage (-20 V to -80 V). Time-of-flight energy elastic recoil detection analysis shows that all the films are near stoichiometric and have a low degree of contaminants, with O being the most abundant (< 1 at.%). The films are crystalline, and their crystallographic orientation changes from 0001 to a more random orientation with increased deposition temperature. X-ray diffraction pole figures and selected area electron diffraction patterns of the films deposited without heating reveal a fiber-texture growth. Four point probe measurements show typical resistivity values of the films ranging from ~95 to 200 μΩcm, decreasing with increased growth temperature and substrate bias.

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