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  • 51.
    Böhlmark, Johan
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics . Linköping University, The Institute of Technology.
    Gudmundsson, J. T.
    Alami, Jones
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics . Linköping University, The Institute of Technology.
    Lattemann, Martina
    Linköping University, Department of Physics, Chemistry and Biology. 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.
    Spatial electron density distribution in a high-power pulsed magnetron discharge2005In: IEEE Transactions on Plasma Science, ISSN 0093-3813, E-ISSN 1939-9375, Vol. 33, no 2, p. 346-347Article in journal (Refereed)
    Abstract [en]

    The spatial electron density distribution was measured as function of time in a high-power pulsed magnetron discharge. A Langmuir probe was positioned in various positions below the target and the electron density was mapped out. We recorded peak electron densities exceeding 1019 m-3 in a close vicinity of the target. The dynamics of the discharge showed a dense plasma expanding from the "race-track" axially into the vacuum chamber. We also record electrons trapped in a magnetic bottle where the magnetron magnetic field is zero, formed due to the unbalanced magnetron.

  • 52.
    Böhlmark, Johan
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating 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.
    VanZeeland, Michael
    Large Plasma Device (LAPD), University of California Los Angeles, USA.
    Axnäs, I.
    Division of Plasma Physics, Alfvén Laboratory, Royal Institute of Technology, Stockholm, Sweden.
    Alami, Jones
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics . Linköping University, The Institute of Technology.
    Brenning, Nils
    Division of Plasma Physics, Alfvén Laboratory, Royal Institute of Technology, Stockholm, Sweden.
    Measurement of the magnetic field change in a pulsed high current magnetron discharge2004In: Plasma Sources Science and Technology, ISSN 0963-0252, Vol. 13, no 4, p. 654-661Article in journal (Refereed)
    Abstract [en]

    In this paper we present a study of how the magnetic field of a circular planar magnetron is affected when it is exposed to a pulsed high current discharge. Spatially resolved magnetic field measurements are presented and the magnetic disturbance is quantified for different process parameters. The magnetic field is severely deformed by the discharge and we record changes of several millitesla, depending on the spatial location of the measurement. The shape of the deformation reveals the presence of azimuthally drifting electrons close to the target surface. Time resolved measurements show a transition between two types of magnetic perturbations. There is an early stage that is in phase with the axial discharge current and a late stage that is not in phase with the discharge current. The later part of the magnetic field deformation is seen as a travelling magnetic wave. We explain the magnetic perturbations by a combination of E × B drifting electrons and currents driven by plasma pressure gradients and the shape of the magnetic field. A plasma pressure wave is also recorded by a single tip Langmuir probe and the velocity (~103 m s−1) of the expanding plasma agrees well with the observed velocity of the magnetic wave. We note that the axial (discharge) current density is much too high compared to the azimuthal current density to be explained by classical collision terms, and an anomalous charge transport mechanism is required.

  • 53.
    Böhlmark, Johan
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
    Lattemann, Martina
    Linköping University, Department of Physics, Chemistry and Biology. Linköping University, The Institute of Technology.
    Gudmundsson, J.T.
    Department of Electrical and Computer Engineering, University of Iceland, Reykjavik, Iceland; and Science Institute, University of Iceland, Reykjavik, Iceland.
    Ehiasarian, A.P.
    Materials and Engineering Research Institute, Sheffield Hallam University, Sheffield, UK.
    Aranda Gonzalvo, Y.
    Hiden Analytical Ltd., Warrington, UK.
    Brenning, N.
    Division of Plasma Physics, Alfvén Laboratory, Royal Institute of Technology, Stockholm, Sweden.
    Helmersson, Ulf
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
    The ion energy distributions and ion flux composition from a high power impulse magnetron sputtering discharge2006In: Thin Solid Films, ISSN 0040-6090, E-ISSN 1879-2731, Vol. 515, no 4, p. 1522-1526Article in journal (Refereed)
    Abstract [en]

    The energy distribution of sputtered and ionized metal atoms as well as ions from the sputtering gas is reported for a high power impulse magnetron sputtering (HIPIMS) discharge. High power pulses were applied to a conventional planar circular magnetron Ti target. The peak power on the target surface was 1-2 kW/cm2 with a duty factor of about 0.5 %. Time resolved, and time averaged ion energy distributions were recorded with an energy resolving quadrupole mass spectrometer. The ion energy distributions recorded for the HIPIMS discharge are broader with maximum detected energy of 100 eV and contain a larger fraction of highly energetic ions (about 50 % with Ei > 20 eV) as compared to a conventional direct current magnetron sputtering discharge. The composition of the ion flux was also determined, and reveals a high metal fraction. During the most intense moment of the discharge, the ionic flux consisted of approximately 50 % Ti1+, 24 % Ti2+, 23 % Ar1+, and 3 % Ar2+ ions.

  • 54.
    Böhlmark, Johan
    et al.
    Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics .
    Lattemann, Martina
    Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics .
    Stranning, H.
    Selinder, T.
    AB Sandvik Tooling.
    Carlsson, J.
    Chemfilt Ionsputtering AB.
    Helmersson, Ulf
    Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics .
    Reactive Film Growth of TiN by Using High Power Impulse Magnetron Sputtering (HIPIMS)2006In: Society of Vacuum Coaters, 49th Annual Technical Conference Proceedings,2006, 2006, p. 334-337Conference paper (Other academic)
  • 55.
    Böhlmark, Johan
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
    Östbye, M.
    Linköping University, Department of Physics, Chemistry and Biology. Linköping University, The Institute of Technology.
    Lattemann, Martina
    Linköping University, Department of Physics, Chemistry and Biology. Linköping University, The Institute of Technology.
    Ljungcrantz, H.
    Impact Coatings AB, Sweden.
    Rosell, T.
    Impact Coatings AB, Sweden.
    Helmersson, Ulf
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
    Guiding the deposition flux in an ionized magnetron discharge2006In: Thin Solid Films, ISSN 0040-6090, E-ISSN 1879-2731, Vol. 515, no 4, p. 1928-1931Article in journal (Refereed)
    Abstract [en]

    A study of the ability to control the deposition flux in a high power impulse magnetron sputtering discharge using an external magnetic field is presented in this article. Pulses with peak power of 1.4 kWcm-2 were applied to a conventional planar magnetron equipped with an Al target. The high power creates a high degree of ionization of the sputtered material, which opens for an opportunity to control of the energy and direction of the deposition species. An external magnetic field was created with a current carrying coil placed in front of the target. To measure the distribution of deposition material samples were placed in an array surrounding the target and the depositions were made with and without the external magnetic field. The distribution is significantly changed when the magnetic field is present. An increase of 80 % in deposition rate is observed for the sample placed in the central position (right in front of the target center) and the deposition rate is strongly decreased on samples placed to the side of the target. The measurements were also performed on a conventional direct current magnetron discharge, but no major effect of the magnetic field was observed in that case.

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  • 56.
    Calamba, Katherine
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Nanostructured Materials. Linköping University, Faculty of Science & Engineering. Univ Lorraine, France.
    Barrirero, Jenifer
    Linköping University, Department of Physics, Chemistry and Biology, Nanostructured Materials. Linköping University, Faculty of Science & Engineering. Saarland Univ, Germany.
    Joesaar, M. P. Johansson
    SECO Tools AB, Sweden.
    Bruyere, S.
    Univ Lorraine, France.
    Boyd, Robert
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Pierson, J. F.
    Univ Lorraine, France.
    Le Febvrier, Arnaud
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
    Muecklich, F.
    Saarland Univ, Germany.
    Odén, Magnus
    Linköping University, Department of Physics, Chemistry and Biology, Nanostructured Materials. Linköping University, Faculty of Science & Engineering.
    Growth and high temperature decomposition of epitaxial metastable wurtzite (Ti1-x,Al-x)N(0001) thin films2019In: Thin Solid Films, ISSN 0040-6090, E-ISSN 1879-2731, Vol. 688, article id 137414Article in journal (Refereed)
    Abstract [en]

    The structure, growth, and phase stability of (Ti1-x,Al-x)N films with high Al content were investigated. (Ti1-x,Al-x)N (x= 0.63 and 0.77) thin films were grown on MgO (111) substrates at 700 degrees C using a UHV DC magnetron sputtering system. The (Ti-0.37,Al-0.63)N film is a single crystal with a cubic NaCl (B1) structure while the (T-i0.23,Al-0.77)N film only shows epitaxial growth of the same cubic phase in the first few atomic layers. With increasing film thickness, epitaxial wurtzite (B4) forms. The thin cubic layer and the wurtzite film has an orientation relationship of c-(Ti-0.23,Al-0.77)N(111)[110]parallel to w-(Ti-0.23,Al-0.77)N(0001)[11 (2) over bar0]. Continued deposition results in a gradual break-down of the epitaxial growth. It is replaced by polycrystalline growth of wurtzite columns with a high degree of 0001 texture, separated by a Tienriched cubic phase. In the as-deposited state, c-(Ti-0.27,Al-0.63)N displays a homogeneous chemical distribution while the w-(Ti-0.23,Al-0.77)N has segregated to Al- and Ti-rich domains. Annealing at 900 degrees C resulted in the spinodal decomposition of the metastable c-(Ti-0.27,Al-0.63)N film and formation of coherent elongated c-AlN and cTi-N-rich domains with an average width of 4.5 +/- 0.2 nm while the width of the domains in the w-(Ti-0.23,Al-0.77)N film only marginally increases to 2.8 +/- 0.1 nm. The slower coarsening rate of the wurtzite structure compared to cubic is indicative of a higher thermal stability.

  • 57.
    Calamba, Katherine
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Nanostructured Materials. Linköping University, Faculty of Science & Engineering. Univ Lorraine, France.
    Jöesaar Johansson, Mats
    Linköping University, Department of Physics, Chemistry and Biology, Nanostructured Materials. Linköping University, Faculty of Science & Engineering. SECO Tools AB, Sweden.
    Bruyere, S.
    Univ Lorraine, France.
    Pierson, J. F.
    Univ Lorraine, France.
    Boyd, Robert
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Andersson, J. M.
    SECO Tools AB, Sweden.
    Odén, Magnus
    Linköping University, Department of Physics, Chemistry and Biology, Nanostructured Materials. Linköping University, Faculty of Science & Engineering.
    The effect of nitrogen vacancies on initial wear in arc deposited (Ti-0.52,Ti- Al-0.48)N-y, (y < 1) coatings during machining2019In: Surface & Coatings Technology, ISSN 0257-8972, E-ISSN 1879-3347, Vol. 358, p. 452-460Article in journal (Refereed)
    Abstract [en]

    Nitrogen deficient c-(Ti0.52Al0.48)Ny, y = 0.92, y = 0.87, and y = 0.75 coatings were prepared in different N-2/Ar discharges on WC-Co inserts by reactive cathodic arc deposition. The microstructure of the y = 0.92 coating show that spinodal decomposition has occurred resulting in the formation of coherent c-TiN- and c-AIN rich domains during cutting. The y = 0.87 and y = 0.75 coatings have exhibited a delay in decomposition due to the presence of nitrogen vacancies that lowers the free energy of the system. In the decomposed structure, grain boundaries and misfit dislocations enhance the diffusion of elements from the workpiece and the substrate (e.g. Fe, Cr, and Co) into the coatings and it becomes more susceptible to crater wear. The y = 0.87 sample displays the highest crater wear resistance because of its dense grain boundaries that prevent chemical wear. The y = 0.92 sample has the best flank wear resistance because the decomposition results in age hardening. The y = 0.75 sample contains the MAX-phase Ti(2)AIN after cutting. The chemical alteration within the y = 0.75 sample and its high amount of macroparticles cause its low wear resistance. The different microstructure evolution caused by different amount of N-vacancies result in distinctive interactions between chip and coating, which also causes difference in the initial wear mechanism of the (Ti,Al)/N-y coatings.

  • 58.
    Calamba, Katherine
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Nanostructured Materials. Linköping University, Faculty of Science & Engineering. Univ Lorraine, France.
    Pierson, J. F.
    Univ Lorraine, France.
    Bruyere, S.
    Univ Lorraine, France.
    Le Febvrier, Arnaud
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. 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.
    Barrirero, Jenifer
    Linköping University, Department of Physics, Chemistry and Biology, Nanostructured Materials. Linköping University, Faculty of Science & Engineering. Saarland Univ, Germany.
    Muecklich, F.
    Saarland Univ, Germany.
    Boyd, Robert
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Jöesaar Johansson, Mats
    Linköping University, Department of Physics, Chemistry and Biology, Nanostructured Materials. Linköping University, Faculty of Science & Engineering. SECO Tools AB, Sweden.
    Odén, Magnus
    Linköping University, Department of Physics, Chemistry and Biology, Nanostructured Materials. Linköping University, Faculty of Science & Engineering.
    Dislocation structure and microstrain evolution during spinodal decomposition of reactive magnetron sputtered heteroepixatial c-(Ti-0.37,Al-0.63)N/c-TiN films grown on MgO(001) and (111) substrates2019In: Journal of Applied Physics, ISSN 0021-8979, E-ISSN 1089-7550, Vol. 125, no 10, article id 105301Article in journal (Refereed)
    Abstract [en]

    Heteroepitaxial c-(Ti-0.37,Al-0.63)N thin films were grown on MgO(001) and MgO(111) substrates using reactive magnetron sputtering. High resolution high-angle annular dark-field scanning transmission electron micrographs show coherency between the film and the substrate. In the as-deposited state, x-ray diffraction reciprocal space maps show a strained epitaxial film. Corresponding geometric phase analysis (GPA) deformation maps show a high stress in the film. At elevated temperature (900 degrees C), the films decompose to form iso-structural coherent c-Al- and c-TiN-rich domains, elongated along the elastically soft amp;lt;100amp;gt; directions. GPA analysis reveals that the c-TiN domains accommodate more dislocations than the c-AlN domains. This is because of the stronger directionality of the covalent bonds in c-AlN compared with c-TiN, making it more favorable for the dislocations to accumulate in c-TiN. The defect structure and strain generation in c-(Ti,Al)N during spinodal decomposition is affected by the chemical bonding state and elastic properties of the segregated domains.

  • 59.
    Cemin, Felipe
    et al.
    Univ Paris Saclay, France.
    Tsukamoto, Makoto
    Tokyo Metropolitan Univ, Japan.
    Keraudy, Julien
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Antunes, Vinicius Gabriel
    Univ Estadual Campinas, Brazil.
    Helmersson, Ulf
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Alvarez, Fernando
    Univ Estadual Campinas, Brazil.
    Minea, Tiberiu
    Univ Paris Saclay, France.
    Lundin, Daniel
    Univ Paris Saclay, France.
    Low-energy ion irradiation in HiPIMS to enable anataseTiO(2) selective growth2018In: Journal of Physics D: Applied Physics, ISSN 0022-3727, E-ISSN 1361-6463, Vol. 51, no 23, article id 2353011Article in journal (Refereed)
    Abstract [en]

    High power impulse magnetron sputtering (HiPIMS) has already demonstrated great potential for synthesizing the high-energy crystalline phase of titanium dioxide (rutile Ti-O2) due to large quantities of highly energetic ions present in the discharge. In this work, it is shown that the metastable anatase phase can also be obtained by HiPIMS. The required deposition conditions have been identified by systematically studying the phase formation, microstructure and chemical composition as a function of mode of target operation as well as of substrate temperature, working pressure, and peak current density. It is found that films deposited in the metal and transition modes are predominantly amorphous and contain substoichiometric TiOx compounds, while in compound mode they are well-crystallized and present only O2- ions bound to Ti4+, i.e. pure TiO2. Anatase TiO2 films are obtained for working pressures between 1 and 2 Pa, a peak current density of similar to 1 A cm(-2) and deposition temperatures lower than 300 degrees C. Rutile is favored at lower pressures (amp;lt; 1 Pa) and higher peak current densities (amp;gt;2 A cm(-2)), while amorphous films are obtained at higher pressures (greater than or similar to 5 Pa). Microstructural characterization of selected films is also presented.

  • 60.
    Ehiasarian, A. P.
    et al.
    Sheffield Hallam University, Sheffield, UK.
    Hovsepian, P. Eh.
    Sheffield Hallam University, Sheffield, UK.
    Hultman, Lars
    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.
    Comparison of microstructure and mechanical properties of chromium nitride-based coatings deposited by high power impulse magnetron sputtering and by the combined steered cathodic arc/unbalanced magnetron technique2004In: Thin Solid Films, ISSN 0040-6090, E-ISSN 1879-2731, Vol. 457, no 2, p. 270-277Article in journal (Refereed)
    Abstract [en]

    Sliding, abrasive, and impact wear tests were performed on chromium nitride (CrN)-based coatings deposited on mirror-polished M2 high speed steel substrates by the novel high power impulse magnetron sputtering (HIPIMS) utilising high peak cathode powers densities of 3000 W cm−2. The coatings were compared to single layer CrN and multilayer superlattice CrN/NbN coatings deposited by the arc bond sputtering (ABS) technique designed to improve the coating substrate adhesion by a combined steered cathodic arc/unbalanced magnetron (UBM) sputtering process. The substrates were metal ion etched using non-reactive HIPIMS or steered cathodic arc at a substrate bias voltage of −1200 V. Subsequently a 2- to 3-μm thick CrN or CrN/NbN coating was deposited by reactive HIPIMS or UBM. No bias was used during the HIPIMS deposition, while the bias during UBM growth was in the range 75–100 V. The ion saturation current measured by a flat electrostatic probe reached values of 50 mA cm−2 peak for HIPIMS and 1 mA cm−2 continuous during UBM deposition. The microstructure of the HIPIMS coatings observed by transmission electron microscopy was fully dense in contrast to the voided columnar structure observed in conventional UBM sputtered CrN and CrN/NbN. The sliding wear coefficients of the HIPIMS CrN films of 2.3×10−16 m3 N−1 m−1 were lower by a factor of 4 and the roughness of the wear track was significantly reduced compared to the UBM-deposited CrN. The abrasive wear coefficient of the HIPIMS coating was 2.2×10−13 m3 N−1 m−1 representing an improvement by a factor of 3 over UBM deposited CrN and a wear resistance comparable to that of the superlattice CrN/NbN. The adhesion of the HIPIMS deposited CrN was comparable to state-of-the-art ABS technology.

  • 61.
    Ehiasarian, A.P.
    et al.
    Sheffield Hallam University.
    Hovsepian, P.Eh.
    Sheffield Hallam University.
    Lattemann, Martina
    Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics .
    Böhlmark, Johan
    Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics .
    Helmersson, Ulf
    Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics .
    High Power Impulse Magnetron Sputtering (HIPIMS) Pre-treatment for the Deposition of Hard Coatings2005In: 48th Annual Technical Conference Society of Vacuum Coaters,2005, 2005, p. 480-484Conference paper (Other academic)
  • 62.
    Ehiasarian, A.P.
    et al.
    Materials Res. Inst., Sheffield-Hallam Univ., Howard St., Sheffield S1 1WB, United Kingdom.
    Munz, W.-D.
    Münz, W.-D., Materials Res. Inst., Sheffield-Hallam Univ., Howard St., Sheffield S1 1WB, United Kingdom.
    Hultman, Lars
    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.
    Petrov, I.
    Frederick Seitz Mat. Res. Lab., University of Illinois, 104 S. Goodwin Avenue, Urbana, IL 61801, United States.
    High power pulsed magnetron sputtered CrNx films2003In: Surface & Coatings Technology, ISSN 0257-8972, E-ISSN 1879-3347, Vol. 163-164, p. 267-272Article in journal (Refereed)
    Abstract [en]

    Microstructure and macroscopic properties of droplet free CrN films deposited by the recently developed high power pulsed magnetron sputtering (HIPIMS) technique are presented. Magnetron glow discharges with peak power densities reaching 3000 W cm-2 were used to sputter Cr targets in both inert and reactive gas atmospheres. The flux arriving at the substrates consisted of neutrals and ions (approx. 70/30) of the sputtered metal and working gas atoms (Ar) with significantly elevated degree of ionization compared to conventional magnetron sputtering. The high-speed steel and stainless steel substrates were metal ion etched using a bias voltage of -1200 V prior to the deposition of CrN films. The film-to-substrate interfaces, observed by scanning transmission electron microscope cross-sections, were clean and contained no phases besides the film and substrate ones or recrystallized regions. CrN films were grown by reactive HIPIMS at floating potential reaching -160 V. Initial nucleation grains were large compared to conventional magnetron sputtered films, indicating a high adatom mobility in the present case. The films exhibited polycrystalline columnar growth morphology with evidence of renucleation. No intercolumnar voids were observed and the corrosion behavior of the film was superior to arc deposited CrNx. A high density of lattice defects was observed throughout the films due to the high floating potential. A residual compressive stress of 3 GPa and a hardness value of HK0.025=2600 were measured. A low friction coefficient of 0.4 and low wear rates against Al2O3 in these films are explained by the absence of droplets and voids known to contribute to extensive debris generation.

  • 63.
    Ehiasarian, A.P.
    et al.
    Materials Research Institute, Sheffield Hallam University, Howard Street, Sheffield S1 1WB, United Kingdom.
    New, R.
    Materials Research Institute, Sheffield Hallam University, Howard Street, Sheffield S1 1WB, United Kingdom.
    Munz, W.-D.
    Münz, W.-D., Materials Research Institute, Sheffield Hallam University, Howard Street, Sheffield S1 1WB, United Kingdom.
    Hultman, Lars
    Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics.
    Helmersson, Ulf
    Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics .
    Kouznetsov, V.
    Chemfilt R and D AB, Kumla Gårdsvägen 28, SE-145 63 Norsborg, Sweden.
    Influence of high power densities on the composition of pulsed magnetron plasmas2002In: Vacuum, ISSN 0042-207X, E-ISSN 1879-2715, Vol. 65, no 2, p. 147-154Article in journal (Refereed)
    Abstract [en]

    The application of high power pulses with peak voltage of -2 kV and peak power density of 3 kWcm-2 to magnetron plasma sources is a new development in sputtering technology. The high power is applied to ordinary magnetron cathodes in pulses with short duration of typically some tens of microseconds in order to avoid a glow-to-arc transition. High plasma densities are obtained which have been predicted to initiate self-sputtering. This study concerns Cr and Ti cathodes and presents evidence of multiply charged metal ions as well as of Ar ions in the dense plasma region of the high power pulsed magnetron discharge and a substantially increased metal ion production compared to continuous magnetron sputtering. The average degree of ionisation of the Cr metal deposition flux generated in the plasma source was 30% at a distance of 50 cm. Deposition rates were maintained comparable to conventional magnetron sputtering due to the low pressure of operation of the pulsed discharge - typically 0.4 Pa (3mTorr) of Ar pressure was used. Observations of the current-voltage characteristics of the discharge confirmed two modes of operation of the plasma source representing conventional pulsed sputtering at low powers (0.2 kWcm-2) and pulsed self-sputtering at higher powers (3 kWcm-2). The optical emission from the various species in the plasma showed an increase in metal ion-to-neutral ratio with increasing power. The time evolution within a pulse of the optical emission from Ar0, Cr0, Cr1+, and Cr2+ showed that at low powers Cr and Ar excitation develops simultaneously. However, at higher powers a distinct transition from Ar to Cr plasma within the duration of the pulse was observed. The time evolution of the discharge at higher powers is discussed. © 2002 Elsevier Science Ltd. All rights reserved.

  • 64. Order onlineBuy this publication >>
    Ekeroth, Sebastian
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Plasma Synthesis and Self-Assembly of Magnetic Nanoparticles2019Doctoral thesis, comprehensive summary (Other academic)
    Abstract [en]

    Nanomaterials are important tools for enabling technological progress as they can provide dramatically different properties as compared to the bulk counterparts. The field of nanoparticles is one of the most investigated within nanomaterials, thanks to the existing, relatively simple, means of manufacturing. In this thesis, high-power pulsed hollow cathode sputtering is used to nucleate and grow magnetic nanoparticles in a plasma. This sputtering technique provides a high degree of ionization of the sputtered material, which has previously been shown to aid in the growth of the nanoparticles. The magnetic properties of the particles are utilized and makes it possible for the grown particles to act as building blocks for self-assembly into more sophisticated nano structures, particularly when an external magnetic field is applied. These structures created are termed “nanowires” or “nanotrusses”, depending on the level of branching and inter-linking that occurs.

    Several different elements have been investigated in this thesis. In a novel approach, it is shown how nanoparticles with more advanced structures, and containing material from two hollow cathodes, can be fabricated using high-power pulses. The dual-element particles are achieved by using two distinct and individual elemental cathodes, and a pulse process that allows tuning of individual pulses separately to them. Nanoparticles grown and investigated are Fe, Ni, Pt, Fe-Ni and Ni-Pt. Alternatively, the addition of oxygen to the process allows the formation of oxide or hybrid metal oxide – metal particles. For all nanoparticles containing several elements, it is demonstrated that the stoichiometry can be easily varied, either by the amount of reactive gas let into the process or by tuning the amount of sputtered material through adjusting the electric power supplied to the different cathodes.

    One aim of the presented work is to find a suitable material for the use as a catalyst in the production of H2 gas through the process of water splitting. H2 is a good candidate to replace fossil fuels as an energy carrier. However, rare elements (such as Ir or Pt) needs to be used as the catalyst, otherwise a high overpotential is required for the splitting to occur, leading to a low efficiency. This work demonstrates a possible route to avoid this, by using nanomaterials to increase the surface-to-volume ratio, as well as optimizing the elemental ratio between different materials to lower the amount of noble elements required. 

    List of papers
    1. Catalytic Nanotruss Structures Realized by Magnetic Self-Assembly in Pulsed Plasma
    Open this publication in new window or tab >>Catalytic Nanotruss Structures Realized by Magnetic Self-Assembly in Pulsed Plasma
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    2018 (English)In: Nano letters (Print), ISSN 1530-6984, E-ISSN 1530-6992, Vol. 18, no 5, p. 3132-3137Article in journal (Refereed) Published
    Abstract [en]

    Tunable nanostructures that feature a high surface area are firmly attached to a conducting substrate and can be fabricated efficiently over significant areas, which are of interest for a wide variety of applications in, for instance, energy storage and catalysis. We present a novel approach to fabricate Fe nanoparticles using a pulsed-plasma process and their subsequent guidance and self-organization into well-defined nanostructures on a substrate of choice by the use of an external magnetic field. A systematic analysis and study of the growth procedure demonstrate that nondesired nanoparticle agglomeration in the plasma phase is hindered by electrostatic repulsion, that a polydisperse nanoparticle distribution is a consequence of the magnetic collection, and that the formation of highly networked nanotruss structures is a direct result of the polydisperse nanoparticle distribution. The nanoparticles in the nanotruss are strongly connected, and their outer surfaces are covered with a 2 nm layer of iron oxide. A 10 mu m thick nanotruss structure was grown on a lightweight, flexible and conducting carbon-paper substrate, which enabled the efficient production of H-2 gas from water splitting at a low overpotential of 210 mV and at a current density of 10 mA/cm(2).

    Place, publisher, year, edition, pages
    American Chemical Society (ACS), 2018
    Keywords
    Nanotrusses; nanowires; nanoparticles; iron; electrocatalysis; pulsed sputtering
    National Category
    Materials Chemistry
    Identifiers
    urn:nbn:se:liu:diva-148107 (URN)10.1021/acs.nanolett.8b00718 (DOI)000432093200055 ()29624405 (PubMedID)
    Funder
    Knut and Alice Wallenberg Foundation, KAW 14.0276
    Available from: 2018-05-30 Created: 2018-05-30 Last updated: 2019-11-11
    2. Growth of semi-coherent Ni and NiO dual-phase nanoparticles using hollow cathode sputtering
    Open this publication in new window or tab >>Growth of semi-coherent Ni and NiO dual-phase nanoparticles using hollow cathode sputtering
    Show others...
    2019 (English)In: Journal of nanoparticle research, ISSN 1388-0764, E-ISSN 1572-896X, Vol. 21, no 2, article id 37Article in journal (Refereed) Published
    Abstract [en]

    Anisotropic heterogenous Ni/NiO nanoparticles with controlled compositions are grown using a high-power pulsed hollow cathode process. These novel particles can be tuned to consist of single-phase Ni via two-phase Ni/NiO to fully oxidized NiO, with a size range of 5-25 nm for individual crystals. A novelty of this approach is the ability to assemble multiple particles of Ni and NiO into a single complex structure, increasing the Ni-NiO interface density. This type of particle growth is not seen before and is explained to be due to the fact that the process operates in a single-step approach, where both Ni and O can arrive at the formed nanoparticle nuclei and aid in the continuous particle growth. The finished particle will then be a consequence of the initially formed crystal, as well as the arrival rate ratio of the two species. These particles hold great potential for applications in fields, such as electro- and photocatalysis, where the ability to control the level of oxidation and/or interface density is of great importance.

    Place, publisher, year, edition, pages
    SPRINGER, 2019
    Keywords
    Ni; NiO; Anisotropic; Nanoparticles; Hollow cathode; Nanoparticle assembly
    National Category
    Materials Chemistry
    Identifiers
    urn:nbn:se:liu:diva-154838 (URN)10.1007/s11051-019-4479-4 (DOI)000458657800001 ()
    Note

    Funding Agencies|Knut and Alice Wallenberg Foundation [KAW 2014.0276]; Swedish Government Strategic Research Area in Materials Science on Functional Materials at Linkoping University [2009 00971]; Tokyo Metropolitan University; Linkoping University

    Available from: 2019-03-07 Created: 2019-03-07 Last updated: 2019-11-11
    3. Impact of nanoparticle magnetization on the 3D formation of dual-phase Ni/NiO nanoparticle-based nanotrusses
    Open this publication in new window or tab >>Impact of nanoparticle magnetization on the 3D formation of dual-phase Ni/NiO nanoparticle-based nanotrusses
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    2019 (English)In: Journal of nanoparticle research, ISSN 1388-0764, E-ISSN 1572-896X, Vol. 21, no 11, article id 21:228Article in journal (Refereed) Published
    Abstract [en]

    Magnetic nanoparticles with average size 30 nm were utilized to build three-dimensional framework structures—nanotrusses. In dual-phase Ni/NiO nanoparticles, there is a strong correlation between the amount of magnetic Ni and the final size and shape of the nanotruss. As it decreases, the length of the individual nanowires within the trusses also decreases, caused by a higher degree of branching of the wires. The position and orientation of the non-magnetic material within the truss structure was also investigated for the different phase compositions. For lower concentrations of NiO phase, the electrically conducting Ni-wire framework is maintained through the preferential bonding between the Ni crystals. For larger concentrations of NiO phase, the Ni-wire framework is interrupted by the NiO. The ability to use nanoparticles that are only partly oxidized in the growth of nanotruss structures is of great importance. It opens the possibility for using not only magnetic metals such as pure Ni, Fe, and Co, but also to use dual-phase nanoparticles that can strongly increase the efficiency of e.g. catalytic electrodes and fuel cells.

    Place, publisher, year, edition, pages
    Springer-Verlag New York, 2019
    Keywords
    Ni, NiO, Nanotruss, Nanoparticle, Magnetic assembly
    National Category
    Materials Chemistry
    Identifiers
    urn:nbn:se:liu:diva-161747 (URN)10.1007/s11051-019-4661-8 (DOI)000494039300001 ()
    Note

    Funding agencies

    Available from: 2019-11-08 Created: 2019-11-08 Last updated: 2019-11-19Bibliographically approved
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  • 65.
    Ekeroth, Sebastian
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Ikeda, Shuga
    Department of Intelligent Mechanical Systems, Tokyo Metropolitan University, Tokyo, Japan.
    Boyd, Robert
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Münger, Peter
    Linköping University, Department of Physics, Chemistry and Biology, Theoretical Physics. Linköping University, Faculty of Science & Engineering.
    Shimizu, Tetsuhide
    Department of Intelligent Mechanical Systems, Tokyo Metropolitan University, Tokyo, Japan.
    Helmersson, Ulf
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Impact of nanoparticle magnetization on the 3D formation of dual-phase Ni/NiO nanoparticle-based nanotrusses2019In: Journal of nanoparticle research, ISSN 1388-0764, E-ISSN 1572-896X, Vol. 21, no 11, article id 21:228Article in journal (Refereed)
    Abstract [en]

    Magnetic nanoparticles with average size 30 nm were utilized to build three-dimensional framework structures—nanotrusses. In dual-phase Ni/NiO nanoparticles, there is a strong correlation between the amount of magnetic Ni and the final size and shape of the nanotruss. As it decreases, the length of the individual nanowires within the trusses also decreases, caused by a higher degree of branching of the wires. The position and orientation of the non-magnetic material within the truss structure was also investigated for the different phase compositions. For lower concentrations of NiO phase, the electrically conducting Ni-wire framework is maintained through the preferential bonding between the Ni crystals. For larger concentrations of NiO phase, the Ni-wire framework is interrupted by the NiO. The ability to use nanoparticles that are only partly oxidized in the growth of nanotruss structures is of great importance. It opens the possibility for using not only magnetic metals such as pure Ni, Fe, and Co, but also to use dual-phase nanoparticles that can strongly increase the efficiency of e.g. catalytic electrodes and fuel cells.

    Download full text (pdf)
    fulltext
  • 66.
    Ekeroth, Sebastian
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Ikeda, Shuga
    Tokyo Metropolitan Univ, Japan.
    Boyd, Robert
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Shimizu, Tetsuhide
    Tokyo Metropolitan Univ, Japan.
    Helmersson, Ulf
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Growth of semi-coherent Ni and NiO dual-phase nanoparticles using hollow cathode sputtering2019In: Journal of nanoparticle research, ISSN 1388-0764, E-ISSN 1572-896X, Vol. 21, no 2, article id 37Article in journal (Refereed)
    Abstract [en]

    Anisotropic heterogenous Ni/NiO nanoparticles with controlled compositions are grown using a high-power pulsed hollow cathode process. These novel particles can be tuned to consist of single-phase Ni via two-phase Ni/NiO to fully oxidized NiO, with a size range of 5-25 nm for individual crystals. A novelty of this approach is the ability to assemble multiple particles of Ni and NiO into a single complex structure, increasing the Ni-NiO interface density. This type of particle growth is not seen before and is explained to be due to the fact that the process operates in a single-step approach, where both Ni and O can arrive at the formed nanoparticle nuclei and aid in the continuous particle growth. The finished particle will then be a consequence of the initially formed crystal, as well as the arrival rate ratio of the two species. These particles hold great potential for applications in fields, such as electro- and photocatalysis, where the ability to control the level of oxidation and/or interface density is of great importance.

    Download full text (pdf)
    fulltext
  • 67.
    Ekeroth, Sebastian
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Münger, Peter
    Linköping University, Department of Physics, Chemistry and Biology, Theoretical Physics. Linköping University, Faculty of Science & Engineering.
    Boyd, Robert
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Ekspong, Joakim
    Umeå Univ, Sweden.
    Wågberg, Thomas
    Umeå Univ, Sweden.
    Edman, Ludvig
    Umeå Univ, Sweden.
    Brenning, Nils
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering. KTH Royal Inst Technol, Sweden.
    Helmersson, Ulf
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Catalytic Nanotruss Structures Realized by Magnetic Self-Assembly in Pulsed Plasma2018In: Nano letters (Print), ISSN 1530-6984, E-ISSN 1530-6992, Vol. 18, no 5, p. 3132-3137Article in journal (Refereed)
    Abstract [en]

    Tunable nanostructures that feature a high surface area are firmly attached to a conducting substrate and can be fabricated efficiently over significant areas, which are of interest for a wide variety of applications in, for instance, energy storage and catalysis. We present a novel approach to fabricate Fe nanoparticles using a pulsed-plasma process and their subsequent guidance and self-organization into well-defined nanostructures on a substrate of choice by the use of an external magnetic field. A systematic analysis and study of the growth procedure demonstrate that nondesired nanoparticle agglomeration in the plasma phase is hindered by electrostatic repulsion, that a polydisperse nanoparticle distribution is a consequence of the magnetic collection, and that the formation of highly networked nanotruss structures is a direct result of the polydisperse nanoparticle distribution. The nanoparticles in the nanotruss are strongly connected, and their outer surfaces are covered with a 2 nm layer of iron oxide. A 10 mu m thick nanotruss structure was grown on a lightweight, flexible and conducting carbon-paper substrate, which enabled the efficient production of H-2 gas from water splitting at a low overpotential of 210 mV and at a current density of 10 mA/cm(2).

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    Download (mov)
    Movie of electrocatalysis
  • 68.
    Ekholm, Marcus
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Theoretical Physics. Linköping University, The Institute of Technology.
    Larsson, Petter
    Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics.
    Alling, Björn
    Linköping University, Department of Physics, Chemistry and Biology, Theoretical 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.
    Abrikosov, Igor
    Linköping University, Department of Physics, Chemistry and Biology, Theoretical Physics. Linköping University, The Institute of Technology.
    Ab initio calculations and synthesis of the off-stoichiometric half-Heusler phase Ni1-xMn1+xSb2010In: JOURNAL OF APPLIED PHYSICS, ISSN 0021-8979, Vol. 108, no 9Article in journal (Refereed)
    Abstract [en]

    We perform a combined theoretical and experimental study of the phase stability and magnetism of the off-stoichiometric Ni1-xMn1+xSb in the half-Heusler crystal phase. Our work is motivated by the need for strategies to engineer the magnetism of potentially half-metallic materials, such as NiMnSb, for improved performance at elevated temperatures. By means of ab initio calculations we investigate Ni1-xMn1+xSb over the whole composition range 0 andlt;= x andlt;= 1 of Ni replacing Mn and show that at relevant temperatures, the half-Heusler phase should be thermodynamically stable up to at least x=0.20 with respect to the competing C38 structure of Mn2Sb. Furthermore we find that half-Heusler Ni1-xMn1+xSb retains half-metallic band structure over the whole concentration range and that the magnetic moments of substitutional Mn-Ni atoms display magnetic exchange interactions an order of magnitude larger than the Ni-Mn interaction in NiMnSb. We also demonstrate experimentally that the alloys indeed can be created by synthesizing off-stoichiometric Ni1-xMn1+xSb films on MgO substrates by means of magnetron sputtering.

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    FULLTEXT01
  • 69.
    Eklund, Per
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Frodelius, Jenny
    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.
    Lu, Jun
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
    Magnfält, Daniel
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
    Epitaxial growth of gamma-Al2O3 on Ti2AlC(0001) by reactive high-power impulse magnetron sputtering2014In: AIP Advances, ISSN 2158-3226, E-ISSN 2158-3226, Vol. 4, no 1, p. 017138-Article in journal (Refereed)
    Abstract [en]

    Al2O3 was deposited by reactive high-power impulse magnetron sputtering at 600 degrees C onto pre-deposited Ti2AlC(0001) thin films on alpha-Al2O3(0001) substrates. The Al2O3 was deposited to a thickness of 65 nm and formed an adherent layer of epitaxial gamma-Al2O3(111) as shown by transmission electron microscopy. The demonstration of epitaxial growth of gamma-Al2O3 on Ti2AlC (0001) open prospects for growth of crystalline alumina as protective coatings on Ti2AlC and related nanolaminated materials. The crystallographic orientation relationships are gamma-Al2O3(111)//Ti2AlC(0001) (out-of-plane) and gamma-Al2O3(2 (2) over bar0)//Ti2AlC(11 (2) over bar0) (in-plane) as determined by electron diffraction. Annealing in vacuum at 900 degrees C resulted in partial decomposition of the Ti2AlC by depletion of Al and diffusion into and through the gamma-Al2O3 layer.

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    fulltext
  • 70.
    Elofsson, Viktor
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
    Thin Film Growth using Pulsed and Highly Ionized Vapor Fluxes2014Licentiate thesis, comprehensive summary (Other academic)
    Abstract [en]

    Microstructure and morphology of thin films are decisive for many of their resulting properties. To be able to tailor these properties, and thus the film functionality, a fundamental understanding of thin film growth needs to be acquired. Film growth is commonly performed using continuous vapor fluxes with low energy, but additional handles to control growth can be obtained by instead using pulsed and energetic ion fluxes. In this licentiate thesis the physical processes that determine microstructure and morphology of thin films grown using pulsed and highly ionized vapor fluxes are investigated.

    The underlying physics that determines the initial film growth stages (i.e., island nucleation, island growth and island coalescence) and how they can be manipulated individually when using pulsed vapor fluxes have previously been investigated. Their combined effect on film growth is, however, paramount to tailor film properties. In the thesis, a route to generate pulsed vapor fluxes using the vapor-based technique high power impulse magnetron sputtering (HiPIMS) is established. These fluxes are then used to grow Ag films on SiO2 substrates. For fluxes with constant energy and deposition rate per pulse it is demonstrated that the growth evolution is solely determined by the characteristics of the vapor flux, as set by the pulsing frequency, and the average time required for coalescence to be completed.

    Highly ionized vapor fluxes have previously been used to manipulate film growth when deposition is performed both normal and off-normal to the substrate. For the latter case, the physical mechanisms that determine film microstructure and morphology are, however, not fully understood. Here it is shown that the tilted columnar microstructure obtained during  off-normal film growth is positioned closer to the substrate normal as the ionization degree of the flux increases, but only if certain nucleation characteristics are present.

    List of papers
    1. Time-domain and energetic bombardment effects on the nucleation and coalescence of thin metal films on amorphous substrates
    Open this publication in new window or tab >>Time-domain and energetic bombardment effects on the nucleation and coalescence of thin metal films on amorphous substrates
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    2013 (English)In: Journal of Physics D: Applied Physics, ISSN 0022-3727, E-ISSN 1361-6463, Vol. 46, no 21, article id 215303Article in journal (Refereed) Published
    Abstract [en]

    Pulsed, ionized vapour fluxes, generated from high power impulse magnetron sputtering (HiPIMS) discharges, are employed to study the effects of time-domain and energetic bombardment on the nucleation and coalescence characteristics during Volmer–Weber growth of metal (Ag) films on amorphous (SiO2) substrates. In situ monitoring of the film growth, by means of wafer curvature measurements and spectroscopic ellipsometry, is used to determine the film thickness where a continuous film is formed. This thickness decreases from ~210 to ~140 Å when increasing the pulsing frequency for a constant amount of material deposited per pulse or when increasing the amount of material deposited per pulse and the energy of the film forming species for a constant pulsing frequency. Estimations of adatom lifetimes and the coalescence times show that there are conditions at which these times are within the range of the modulation of the vapour flux. Thus, nucleation and coalescence processes can be manipulated by changing the temporal profile of the vapour flux. We suggest that other than for elucidating the atomistic mechanisms that control pulsed growth processes, the interplay between the time scales for diffusion, coalescence and vapour flux pulsing can be used as a tool to determine characteristic surface diffusion and island coalescence parameters.

    Place, publisher, year, edition, pages
    Institute of Physics (IOP), 2013
    National Category
    Engineering and Technology
    Identifiers
    urn:nbn:se:liu:diva-95508 (URN)10.1088/0022-3727/46/21/215303 (DOI)000319116300009 ()
    Note

    Funding Agencies|Swedish Research Council|VR 621-2011-4280|COST Action Highly Ionized Pulsed Plasmas|MP0804|Linkoping University via the LiU Research Fellows program||.

    The previous status of the article was Manuscript and the working title was Time-domain and energetic bombardment effects on the nucleation and post-nucleation characteristics during none-quilibrium film synthesis.

    Available from: 2013-07-05 Created: 2013-07-05 Last updated: 2017-12-06Bibliographically approved
    2. Unravelling the Physical Mechanisms that Determine Microstructural Evolution of Ultrathin Volmer-Weber Films
    Open this publication in new window or tab >>Unravelling the Physical Mechanisms that Determine Microstructural Evolution of Ultrathin Volmer-Weber Films
    2014 (English)In: Journal of Applied Physics, ISSN 0021-8979, E-ISSN 1089-7550, Vol. 116, no 4, p. 044302-Article in journal (Refereed) Published
    Abstract [en]

    The initial formation stages (i.e., island nucleation, island growth, and island coalescence) set characteristic length scales during growth of thin films from the vapour phase. They are, thus, decisive for morphological and microstructural features of films and nanostructures. Each of the initial formation stages has previously been well-investigated separately for the case of Volmer-Weber growth, but knowledge on how and to what extent each stage individually and all together affect the microstructural evolution is still lacking. Here we address this question using growth of Ag on SiO2 from pulsed vapour fluxes as a case study. By combining in situ growth monitoring, ex situ imaging and growth simulations we systematically study the growth evolution all the way from nucleation to formation of a continuous film and establish the effect of the vapour flux time domain on the scaling behaviour of characteristic growth transitions (elongation transition, percolation and continuous film formation). Our data reveal a pulsing frequency dependence for the characteristic film growth transitions, where the nominal transition thickness decreases with increasing pulsing frequency up to a certain value after which a steady-state behaviour is observed. The scaling behaviour is shown to result from differences in island sizes and densities, as dictated by the initial film formation stages. These differences are determined solely by the interplay between the characteristics of the vapour flux and time required for island coalescence to be completed. In particular, our data provide evidence that the steady-state scaling regime of the characteristic growth transitions is caused by island growth that hinders coalescence from being completed, leading to a coalescence-free growth regime.

    National Category
    Physical Sciences
    Identifiers
    urn:nbn:se:liu:diva-103920 (URN)10.1063/1.4890522 (DOI)000340710700078 ()
    Available from: 2014-02-03 Created: 2014-02-03 Last updated: 2018-01-11
    3. Tilt of the columnar microstructure in off-normally deposited thin films using highly ionized vapor fluxes
    Open this publication in new window or tab >>Tilt of the columnar microstructure in off-normally deposited thin films using highly ionized vapor fluxes
    2013 (English)In: Journal of Applied Physics, ISSN 0021-8979, E-ISSN 1089-7550, Vol. 113, no 17, p. 7 pages-Article in journal (Refereed) Published
    Abstract [en]

    The tilt of the columnar microstructure has been studied for Cu and Cr thin films grown off-normally using highly ionized vapor fluxes, generated by the deposition technique high power impulse magnetron sputtering. It is found that the relatively large column tilt (with respect to the substrate normal) observed for Cu films decreases as the ionization degree of the deposition flux increases. On the contrary, Cr columns are found to grow relatively close to the substrate normal and the column tilt is independent from the ionization degree of the vapor flux when films are deposited at room temperature. The Cr column tilt is only found to be influenced by the ionized fluxes when films are grown at elevated temperatures, suggesting that film morphology during the film nucleation stage is also important in affecting column tilt. A phenomenological model that accounts for the effect of atomic shadowing at different nucleation conditions is suggested to explain the results.

    Place, publisher, year, edition, pages
    American Institute of Physics (AIP), 2013
    National Category
    Engineering and Technology
    Identifiers
    urn:nbn:se:liu:diva-94608 (URN)10.1063/1.4804066 (DOI)000319292800398 ()
    Available from: 2013-06-27 Created: 2013-06-27 Last updated: 2017-12-06Bibliographically approved
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    Thin Film Growth using Pulsed and Highly Ionized Vapor Fluxes
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  • 71.
    Elofsson, Viktor
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Nanoscale engineering. Linköping University, Faculty of Science & Engineering.
    Almyras, Georgios
    Linköping University, Department of Physics, Chemistry and Biology, Nanoscale engineering. Linköping University, Faculty of Science & Engineering.
    Lu, B.
    Linköping University, Department of Physics, Chemistry and Biology, Nanoscale engineering. Linköping University, Faculty of Science & Engineering.
    Boyd, Robert
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Sarakinos, Kostas
    Linköping University, Department of Physics, Chemistry and Biology, Nanoscale engineering. Linköping University, Faculty of Science & Engineering.
    Atomic arrangement in immiscible Ag-Cu alloys synthesized far-from-equilibrium2016In: Acta Materialia, ISSN 1359-6454, E-ISSN 1873-2453, Vol. 110, p. 114-121Article in journal (Refereed)
    Abstract [en]

    Physical attributes of multicomponent materials of a given chemical composition are determined by atomic arrangement at property-relevant length scales. A potential route to access a vast array of atomic configurations for material property tuning is by synthesis of multicomponent thin films using vapor fluxes with their deposition pattern modulated in the sub-monolayer regime. However, the applicability of this route for creating new functional materials is impeded by the fact that a fundamental understanding of the combined effect of sub-monolayer flux modulation, kinetics and thermodynamics on atomic arrangement is not available in the literature. Here we present a research strategy and verify its viability for addressing the aforementioned gap in knowledge. This strategy encompasses thin film synthesis using a route that generates multi-atomic fluxes with sub-monolayer resolution and precision over a wide range of experimental conditions, deterministic growth simulations and nanoscale micro structural probes. Investigations are focused on structure formation within the archetype immiscible Ag-Cu binary system, revealing that atomic arrangement at different length scales is governed by the arrival pattern of the film forming species, in conjunction with diffusion of near-surface Ag atoms to encapsulate 3D Cu islands growing on 2D Ag layers. The knowledge generated and the methodology presented herein provides the scientific foundation for tailoring atomic arrangement and physical properties in a wide range of miscible and immiscible multinary systems. (C) 2016 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

  • 72.
    Elofsson, Viktor
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Nanoscale engineering. Linköping University, Faculty of Science & Engineering.
    Almyras, Georgios
    Linköping University, Department of Physics, Chemistry and Biology, Nanoscale engineering. Linköping University, Faculty of Science & Engineering.
    Lü, Bo
    Linköping University, Department of Physics, Chemistry and Biology, Nanoscale engineering. Linköping University, Faculty of Science & Engineering.
    Garbrecht, Magnus
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
    Boyd, Robert
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Sarakinos, Kostas
    Linköping University, Department of Physics, Chemistry and Biology, Nanoscale engineering. Linköping University, Faculty of Science & Engineering.
    Structure formation in Ag-X (X = Au, Cu) alloys synthesized far-from-equilibrium2018In: Journal of Applied Physics, ISSN 0021-8979, E-ISSN 1089-7550, Vol. 123, no 16Article in journal (Refereed)
    Abstract [en]

    We employ sub-monolayer, pulsed Ag and Au vapor fluxes, along with deterministic growth simulations, and nanoscale probes to study structure formation in miscible Ag-Au films synthesized under far-from-equilibrium conditions. Our results show that nanoscale atomic arrangement is primarily determined by roughness build up at the film growth front, whereby larger roughness leads to increased intermixing between Ag and Au. These findings suggest a different structure formation pathway as compared to the immiscible Ag-Cu system for which the present study, in combination with previously published data, reveals that no significant roughness is developed, and the local atomic structure is predominantly determined by the tendency of Ag and Cu to phase-separate.

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  • 73.
    Elofsson, Viktor
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
    Magnfält, Daniel
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
    Münger, Peter
    Linköping University, Department of Physics, Chemistry and Biology, Theoretical 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.
    Unravelling the Physical Mechanisms that Determine Microstructural Evolution of Ultrathin Volmer-Weber Films2014In: Journal of Applied Physics, ISSN 0021-8979, E-ISSN 1089-7550, Vol. 116, no 4, p. 044302-Article in journal (Refereed)
    Abstract [en]

    The initial formation stages (i.e., island nucleation, island growth, and island coalescence) set characteristic length scales during growth of thin films from the vapour phase. They are, thus, decisive for morphological and microstructural features of films and nanostructures. Each of the initial formation stages has previously been well-investigated separately for the case of Volmer-Weber growth, but knowledge on how and to what extent each stage individually and all together affect the microstructural evolution is still lacking. Here we address this question using growth of Ag on SiO2 from pulsed vapour fluxes as a case study. By combining in situ growth monitoring, ex situ imaging and growth simulations we systematically study the growth evolution all the way from nucleation to formation of a continuous film and establish the effect of the vapour flux time domain on the scaling behaviour of characteristic growth transitions (elongation transition, percolation and continuous film formation). Our data reveal a pulsing frequency dependence for the characteristic film growth transitions, where the nominal transition thickness decreases with increasing pulsing frequency up to a certain value after which a steady-state behaviour is observed. The scaling behaviour is shown to result from differences in island sizes and densities, as dictated by the initial film formation stages. These differences are determined solely by the interplay between the characteristics of the vapour flux and time required for island coalescence to be completed. In particular, our data provide evidence that the steady-state scaling regime of the characteristic growth transitions is caused by island growth that hinders coalescence from being completed, leading to a coalescence-free growth regime.

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  • 74.
    Elofsson, Viktor
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
    Magnfält, Daniel
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
    Samuelsson, M
    Impact Coatings, Linköping, Sweden .
    Sarakinos, Kostas
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
    Tilt of the columnar microstructure in off-normally deposited thin films using highly ionized vapor fluxes2013In: Journal of Applied Physics, ISSN 0021-8979, E-ISSN 1089-7550, Vol. 113, no 17, p. 7 pages-Article in journal (Refereed)
    Abstract [en]

    The tilt of the columnar microstructure has been studied for Cu and Cr thin films grown off-normally using highly ionized vapor fluxes, generated by the deposition technique high power impulse magnetron sputtering. It is found that the relatively large column tilt (with respect to the substrate normal) observed for Cu films decreases as the ionization degree of the deposition flux increases. On the contrary, Cr columns are found to grow relatively close to the substrate normal and the column tilt is independent from the ionization degree of the vapor flux when films are deposited at room temperature. The Cr column tilt is only found to be influenced by the ionized fluxes when films are grown at elevated temperatures, suggesting that film morphology during the film nucleation stage is also important in affecting column tilt. A phenomenological model that accounts for the effect of atomic shadowing at different nucleation conditions is suggested to explain the results.

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  • 75.
    Elofsson, Viktor
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Nanoscale engineering. Linköping University, The Institute of Technology.
    Saraiva, M.
    Sandvik Coromant AB, Sweden.
    Boyd, Robert
    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, Nanoscale engineering. Linköping University, The Institute of Technology.
    Double in-plane alignment in biaxially textured thin films2014In: Applied Physics Letters, ISSN 0003-6951, E-ISSN 1077-3118, Vol. 105, no 23, p. 233113-Article in journal (Refereed)
    Abstract [en]

    The scientific interest and technological relevance of biaxially textured polycrystalline thin films stem from their microstructure that resembles that of single crystals. To explain the origin and predict the type of biaxial texture in off-normally deposited films, Mahieu et al. have developed an analytical model [S. Mahieu et al., Thin Solid Films 515, 1229 (2006)]. For certain materials, this model predicts the occurrence of a double in-plane alignment, however, experimentally only a single in-plane alignment has been observed and the reason for this discrepancy is still unknown. The model calculates the resulting in-plane alignment by considering the growth of faceted grains with an out-of-plane orientation that corresponds to the predominant film out-of-plane texture. This approach overlooks the fact that in vapor condensation experiments where growth kinetics is limited and only surface diffusion is active, out-of-plane orientation selection is random during grain nucleation and happens only upon grain impingement. Here, we compile and implement an experiment that is consistent with the key assumptions set forth by the in-plane orientation selection model by Mahieu et al.; a Cr film is grown off-normally on a fiber textured Ti epilayer to pre-determine the out-of-plane orientation and only allow for competitive growth with respect to the in-plane alignment. Our results show unambiguously a biaxially textured Cr (110) film that possesses a double in-plane alignment, in agreement with predictions of the in-plane selection model. Thus, a long standing discrepancy in the literature is resolved, paving the way towards more accurate theoretical descriptions and hence knowledge-based control of microstructure evolution in biaxially textured thin films.

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  • 76.
    Enqvist, Erik
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
    Synthesis and Characterisation of Non-Evaporable Getter Films Based on Ti, Zr and V2011Independent thesis Advanced level (degree of Master (Two Years)), 20 credits / 30 HE creditsStudent thesis
    Abstract [en]

    Non-evaporable getters (NEG) are widely used in ultra high vacuum (UHV) systems for particle accelerators to assure distributed pumping speed. By heating the NEG to an activation temperature, the oxide layer on the surface dissolves into the material, leaving a clean (activated) surface. The activated NEG surface is capable of chemisorbing most of the residual gases present in a UHV system and will act as a vacuum pump. NEG can be sputter deposited on the inner wall of vacuum chambers, turning the whole wall from a source of gas into a pump. At the largest particle accelerator in the world, the Large Hadron Collider, more than 6 km of beam pipe has been NEG coated.

    In this work, a DC magnetron sputtering system dedicated for coating cylindrical vacuum chambers with NEG has been assembled, installed and commissioned. The system has been used to do NEG depositions on inner walls of vacuum chambers. The vacuum performance of the coating has been measured in terms of pumping speed, electron stimulated desorption and activation temperature. In addition, the thin film composition and morphology has been investigated by scanning electron microscopy (SEM).

    The work has resulted in an operational DC magnetron sputtering system, which can be used for further studies of NEG materials and compositions.

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  • 77.
    Eriksson, Jens
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Applied Sensor Science. Linköping University, Faculty of Science & Engineering.
    Puglisi, Donatella
    Linköping University, Department of Physics, Chemistry and Biology, Applied Sensor Science. Linköping University, Faculty of Science & Engineering.
    Strandqvist, Carl
    Linköping University, Department of Physics, Chemistry and Biology, Applied Sensor Science. Linköping University, Faculty of Science & Engineering. Graphensic AB Linköping, Sweden.
    Gunnarsson, Rickard
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Ekeroth, Sebastian
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Ivanov, Ivan Gueorguiev
    Linköping University, Department of Physics, Chemistry and Biology, Semiconductor Materials. Linköping University, Faculty of Science & Engineering.
    Helmersson, Ulf
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Uvdal, Kajsa
    Linköping University, Department of Physics, Chemistry and Biology, Molecular Surface Physics and Nano Science. Linköping University, Faculty of Science & Engineering.
    Yakimova, Rositsa
    Linköping University, Department of Physics, Chemistry and Biology, Semiconductor Materials. Linköping University, Faculty of Science & Engineering. Graphensic AB Linköping, Sweden.
    Lloyd Spetz, Anita
    Linköping University, Department of Physics, Chemistry and Biology, Applied Sensor Science. Linköping University, Faculty of Science & Engineering.
    Modified Epitaxial Graphene on SiC for Extremely Sensitive andSelective Gas Sensors2016In: Materials Science Forum, ISSN 0255-5476, E-ISSN 1662-9752, Vol. 858, p. 1145-1148Article in journal (Refereed)
    Abstract [en]

    Two-dimensional materials offer a unique platform for sensing where extremely high sensitivity is a priority, since even minimal chemical interaction causes noticeable changes inelectrical conductivity, which can be used for the sensor readout. However, the sensitivity has to becomplemented with selectivity, and, for many applications, improved response- and recovery times are needed. This has been addressed, for example, by combining graphene (for sensitivity) with metal/oxides (for selectivity) nanoparticles (NP). On the other hand, functionalization or modification of the graphene often results in poor reproducibility. In this study, we investigate thegas sensing performance of epitaxial graphene on SiC (EG/SiC) decorated with nanostructured metallic layers as well as metal-oxide nanoparticles deposited using scalable thin-film depositiontechniques, like hollow-cathode pulsed plasma sputtering. Under the right modification conditions the electronic properties of the surface remain those of graphene, while the surface chemistry can betuned to improve sensitivity, selectivity and speed of response to several gases relevant for airquality monitoring and control, such as nitrogen dioxide, benzene, and formaldehyde.

  • 78.
    Eriksson, Mats
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Chemical and Optical Sensor Systems. Linköping University, Faculty of Science & Engineering.
    Olsson, Lars
    Linköping University, Department of Medical and Health Sciences.
    Erlandsson, Ragnar
    Linköping University, Department of Physics, Chemistry and Biology, Chemical and Optical Sensor Systems. Linköping University, Faculty of Science & Engineering.
    Helmersson, Ulf
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Ekedahl, Lars-Gunnar
    Linköping University, Department of Physics, Chemistry and Biology.
    Morphology changes of thin Pd films grown on SiO2: influence of adsorbates and temperature1999In: Thin Solid Films, ISSN 0040-6090, E-ISSN 1879-2731, Vol. 342, no 1-2, p. 297-306Article in journal (Refereed)
    Abstract [en]

    Under certain conditions morphology changes occur when thin Pd films, grown on SiO2 at room temperature, are subject to elevated temperatures. First holes in the metal are observed, followed by network formation and finally isolation of metal islands. This process is known as agglomeration. The influence of gas exposures on this restructuring process has been studied by following variations in the capacitance of the structure and by atomic force microscopy, transmission electron microscopy and ultraviolet photoelectron spectroscopy. The capacitance measurements show that carbonaceous species have an impeding influence on the rate of agglomeration and may lock the film structure in a thermodynamic non-equilibrium state. By removing these species with oxygen exposure, i.e. by forming volatile CO and CO2, a clean surface is obtained and the agglomeration process can proceed. High oxygen or hydrogen coverages also lower the rate of restructuring, compared to the case of a clean surface. For the clean Pd surface, an apparent activation energy of 0.64 eV is found for the restructuring process.

  • 79.
    Eriksson, Peter
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Molecular Surface Physics and Nano Science. Linköping University, Faculty of Science & Engineering.
    Tal, Alexey
    Linköping University, Department of Physics, Chemistry and Biology, Theoretical Physics. Linköping University, Faculty of Science & Engineering.
    Skallberg, Andreas
    Linköping University, Department of Physics, Chemistry and Biology, Molecular Surface Physics and Nano Science. Linköping University, Faculty of Science & Engineering.
    Brommesson, Caroline
    Linköping University, Department of Physics, Chemistry and Biology, Molecular Surface Physics and Nano Science. Linköping University, Faculty of Science & Engineering.
    Hu, Zhang-Jun
    Linköping University, Department of Physics, Chemistry and Biology, Molecular Surface Physics and Nano Science. Linköping University, Faculty of Science & Engineering.
    Boyd, Robert
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Olovsson, Weine
    Linköping University, Department of Physics, Chemistry and Biology, Theoretical Physics. Linköping University, Faculty of Science & Engineering.
    Fairley, Neal
    Casa Software Ltd, Bay House, Teignmouth, United Kingdom.
    Abrikosov, Igor
    Linköping University, Department of Physics, Chemistry and Biology, Theoretical Physics. Linköping University, Faculty of Science & Engineering. Materials Modeling and Development Laboratory, National University of Science and Technology “MISIS”, Moscow, Russia.
    Zhang, Xuanjun
    Faculty of Health Sciences, University of Macau, Macau, SAR, China.
    Uvdal, Kajsa
    Linköping University, Department of Physics, Chemistry and Biology, Molecular Surface Physics and Nano Science. Linköping University, Faculty of Science & Engineering.
    Cerium oxide nanoparticles with antioxidant capabilities and gadolinium integration for MRI contrast enhancement2018In: Scientific Reports, ISSN 2045-2322, E-ISSN 2045-2322, Vol. 8, article id 6999Article in journal (Refereed)
    Abstract [en]

    The chelating gadolinium-complex is routinely used as magnetic resonance imaging (MRI) -contrast enhancer. However, several safety issues have recently been reported by FDA and PRAC. There is an urgent need for the next generation of safer MRI-contrast enhancers, with improved local contrast and targeting capabilities. Cerium oxide nanoparticles (CeNPs) are designed with fractions of up to 50% gadolinium to utilize the superior MRI-contrast properties of gadolinium. CeNPs are well-tolerated in vivo and have redox properties making them suitable for biomedical applications, for example scavenging purposes on the tissue-and cellular level and during tumor treatment to reduce in vivo inflammatory processes. Our near edge X-ray absorption fine structure (NEXAFS) studies show that implementation of gadolinium changes the initial co-existence of oxidation states Ce3+ and Ce4+ of cerium, thereby affecting the scavenging properties of the nanoparticles. Based on ab initio electronic structure calculations, we describe the most prominent spectral features for the respective oxidation states. The as-prepared gadolinium-implemented CeNPs are 3-5 nm in size, have r(1)-relaxivities between 7-13 mM(-1) s(-1) and show clear antioxidative properties, all of which means they are promising theranostic agents for use in future biomedical applications.

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  • 80.
    Erlandsson, Ragnar
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Chemical and Optical Sensor Systems. Linköping University, Faculty of Science & Engineering.
    Eriksson, Mats
    Linköping University, Department of Physics, Chemistry and Biology, Chemical and Optical Sensor Systems. Linköping University, Faculty of Science & Engineering.
    Olsson, Lars
    Linköping University, Department of Medical and Health Sciences.
    Helmersson, Ulf
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Lundström, Ingemar
    Linköping University, Department of Physics, Chemistry and Biology, Biosensors and Bioelectronics. Linköping University, Faculty of Science & Engineering.
    Petersson, Lars-Gunnar
    Gas-induced restructuring of palladium model catalysts studied with atomic force microscopy1991In: Journal of Vacuum Science & Technology B, ISSN 1071-1023, E-ISSN 1520-8567, Vol. 9, no 2, p. 825-828Article in journal (Refereed)
    Abstract [en]

    The structure of thin Pd films evaporated onto planar SiO2 substrates changes dramatically during oxygen/hydrogen exposures in ultrahigh vacuum. In this work we have used an atomic force microscope(AFM), operated in the attractive mode, to obtain the three‐dimensional morphology of the Pd surface for different film thicknesses and treatments, and compared the data with transmission electron microscopy(TEM) micrographs. During restructuring, a 100‐Å film changes from being a smooth continuous film with cracks into metal clusters dispersed on the SiO2 support. In the 5‐Å case the metal films are already well dispersed as fabricated. Here the gas exposure instead results in a clustering effect resulting in larger particles. The AFM gives results which are consistent with TEM micrographs but also gives additional information on metal particle shape which can lead to a further understanding of the restructuring process.

  • 81.
    Etula, Jarkko
    et al.
    Aalto Univ, Finland.
    Lahtinen, Katja
    Aalto Univ, Finland.
    Wester, Niklas
    Aalto Univ, Finland.
    Iyer, Ajoi
    Aalto Univ, Finland.
    Arstila, Kai
    Univ Jyvaskyla, Finland.
    Sajavaara, Timo
    Univ Jyvaskyla, Finland.
    Kallio, Tanja
    Aalto Univ, Finland.
    Helmersson, Ulf
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Koskinen, Jari
    Aalto Univ, Finland.
    Room-Temperature Micropillar Growth of Lithium-Titanate-Carbon Composite Structures by Self-Biased Direct Current Magnetron Sputtering for Lithium Ion Microbatteries2019In: Advanced Functional Materials, ISSN 1616-301X, E-ISSN 1616-3028, article id 1904306Article in journal (Refereed)
    Abstract [en]

    Here, an unidentified type of micropillar growth is described at room temperature during conventional direct-current magnetron sputtering (DC-MS) deposition from a Li4Ti5O12+graphite sputter target under negative substrate bias and high operating pressure. These fabricated carbon-Li2O-TiO2 microstructures consisting of various Li4Ti5O12/Li2TiO3/LixTiO2 crystalline phases are demonstrated as an anode material in Li-ion microbatteries. The described micropillar fabrication method is a low-cost, substrate independent, single-step, room-temperature vacuum process utilizing a mature industrial complementary metal-oxide-semiconductor (CMOS)-compatible technology. Furthermore, tentative consideration is given to the effects of selected deposition parameters and the growth process, as based on extensive physical and chemical characterization. Additional studies are, however, required to understand the exact processes and interactions that form the micropillars. If this facile method is further extended to other similar metal oxide-carbon systems, it could offer alternative low-cost fabrication routes for microporous high-surface area materials in electrochemistry and microelectronics.

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  • 82.
    Greiner, Franko
    et al.
    University of Kiel, Germany .
    Carstensen, Jan
    University of Kiel, Germany .
    Koehler, Nils
    University of Kiel, Germany .
    Pilch, Iris
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
    Ketelsen, Helge
    SENTECH Instruments GmbH, Germany .
    Knist, Sascha
    Graforce Hydro GmbH, Germany .
    Piel, Alexander
    University of Kiel, Germany .
    Imaging Mie ellipsometry: dynamics of nanodust clouds in an argon-acetylene plasma2012In: Plasma sources science & technology (Print), ISSN 0963-0252, E-ISSN 1361-6595, Vol. 21, no 6, p. 065005-Article in journal (Refereed)
    Abstract [en]

    For the in situ analysis of nano-sized particles in a laboratory plasma, Mie ellipsometry is a well established technique. We present a simple setup with two CCD cameras to gain online spatiotemporal resolved information of the growth dynamics of particles which are produced by plasma chemical processes in an argon-acetylene plasma. Imaging Mie ellipsometry proves to be a powerful technique to study the growth processes of nanodust in all its details.

  • 83.
    Gudmundsson, J. T.
    et al.
    Science Institute, University of Iceland, Reykjavík, Iceland.
    Alami, Jones
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating 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.
    Evolution of the electron energy distribution and plasma parameters in a pulsed magnetron discharge2001In: Applied Physics Letters, ISSN 0003-6951, Vol. 78, no 22, p. 3427-Article in journal (Refereed)
    Abstract [en]

    We demonstrate the creation of high-density plasma in a pulsed magnetron discharge. A 2.4 MW pulse, 100 µs wide, with a repetition frequency of 50 Hz is applied to a planar magnetron discharge to study the temporal behavior of the plasma parameters: the electron energy distribution function, the electron density, and the average electron energy. The electron density in the vicinity of the substrate, 20 cm below the cathode target, peaks at 8×1017 m–3, 127 µs after initiating the pulse. Towards the end of the pulse two energy groups of electrons are present with a corresponding peak in average electron energy. With the disapperance of the high-energy electron group, the electron density peaks, and the electron energy distribution appears to be Maxwellian like. Following the electron density peak, the plasma becomes more Druyvesteyn like with a higher average electron energy.

  • 84.
    Gudmundsson, J. T.
    et al.
    Department of Electrical Engineering and Science Institute, University of Iceland, Reykjavík, Iceland.
    Alami, Jones
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating 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.
    Spatial and temporal behavior of the plasma parameters in a pulsed magnetron discharge2002In: Surface and Coatings Technology, Vol. 161, no 2-3, p. 249-256Article in journal (Refereed)
    Abstract [en]

    We demonstrate the evolution of the electron, energy distribution and the plasma parameters in a high-density plasma in a pulsed magnetron discharge. The high-density plasma is created by applying a high power pulse (1–2.4 MW) with pulse length 100 μs and repetition frequency of 50 Hz to a planar magnetron discharge. The spatial and temporal behavior of the plasma parameters are investigated using a Langmuir probe; the electron energy distribution function, the electron density and the average electron energy. The electron energy distribution function during and shortly after the pulse can be represented by a bi-Maxwellian distribution indicating two energy groups of electrons. Furthermore, we report on the variation of the plasma parameters and electron energy distribution function with gas pressure in the pressure range 0.5–20 mtorr. We report electron density as high as 4×1018 m−3 at 10 mtorr and 9 cm below the target in a pulsed discharge with average power 300 W. We estimate the traveling speed of the electron density peak along the axis of the discharge. The traveling speed decreases with increased gas pressure from 4×105 cm/s at 0.5 mtorr to 0.87×105 cm s−1 at 10 mtorr. The effective electron temperature peaks at the same time independent of position in the discharge, which indicates a burst of high energy electrons at the end of the pulse.

  • 85.
    Gudmundsson, J. T.
    et al.
    University of Michigan.
    Brenning, N.
    KTH.
    Lundin, Daniel
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating 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.
    High power impulse magnetron sputtering discharge2012In: Journal of Vacuum Science & Technology. A. Vacuum, Surfaces, and Films, ISSN 0734-2101, E-ISSN 1520-8559, Vol. 30, no 030801Article, review/survey (Refereed)
    Abstract [en]

    The high power impulse magnetron sputtering (HiPIMS) discharge is a recent addition to plasma based sputtering technology. In HiPIMS, high power is applied to the magnetron target in unipolar pulses at low duty cycle and low repetition frequency while keeping the average power about 2 orders of magnitude lower than the peak power. This results in a high plasma density, and high ionization fraction of the sputtered vapor, which allows better control of the film growth by controlling the energy and direction of the deposition species. This is a significant advantage over conventional dc magnetron sputtering where the sputtered vapor consists mainly of neutral species. The HiPIMS discharge is now an established ionized physical vapor deposition technique, which is easily scalable and has been successfully introduced into various industrial applications. The authors give an overview of the development of the HiPIMS discharge, and the underlying mechanisms that dictate the discharge properties. First, an introduction to the magnetron sputtering discharge and its various configurations and modifications is given. Then the development and properties of the high power pulsed power supply are discussed, followed by an overview of the measured plasma parameters in the HiPIMS discharge, the electron energy and density, the ion energy, ion flux and plasma composition, and a discussion on the deposition rate. Finally, some of the models that have been developed to gain understanding of the discharge processes are reviewed, including the phenomenological material pathway model, and the ionization region model.

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  • 86.
    Gudmundsson, J. T.
    et al.
    KTH Royal Institute Technology, Sweden; University of Iceland, Iceland; University of Paris Saclay, France.
    Lundin, D.
    University of Paris Saclay, France.
    Brenning, Nils
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering. KTH Royal Institute Technology, Sweden.
    Raadu, M. A.
    KTH Royal Institute Technology, Sweden.
    Huo, Chunqing
    KTH Royal Institute Technology, Sweden.
    Minea, T. M.
    University of Paris Saclay, France.
    An ionization region model of the reactive Ar/O-2 high power impulse magnetron sputtering discharge2016In: Plasma sources science & technology (Print), ISSN 0963-0252, E-ISSN 1361-6595, Vol. 25, no 6, p. 065004-Article in journal (Refereed)
    Abstract [en]

    A new reactive ionization region model (R-IRM) is developed to describe the reactive Ar/O-2 high power impulse magnetron sputtering (HiPIMS) discharge with a titanium target. It is then applied to study the temporal behavior of the discharge plasma parameters such as electron density, the neutral and ion composition, the ionization fraction of the sputtered vapor, the oxygen dissociation fraction, and the composition of the discharge current. We study and compare the discharge properties when the discharge is operated in the two well established operating modes, the metal mode and the poisoned mode. Experimentally, it is found that in the metal mode the discharge current waveform displays a typical non-reactive evolution, while in the poisoned mode the discharge current waveform becomes distinctly triangular and the current increases significantly. Using the R-IRM we explore the current increase and find that when the discharge is operated in the metal mode Ar+ and Ti+ -ions contribute most significantly (roughly equal amounts) to the discharge current while in the poisoned mode the Ar+ -ions contribute most significantly to the discharge current and the contribution of O+ -ions, Ti+ -ions, and secondary electron emission is much smaller. Furthermore, we find that recycling of atoms coming from the target, that are subsequently ionized, is required for the current generation in both modes of operation. From the R-IRM results it is found that in the metal mode self-sputter recycling dominates and in the poisoned mode working gas recycling dominates. We also show that working gas recycling can lead to very high discharge currents but never to a runaway. It is concluded that the dominating type of recycling determines the discharge current waveform.

  • 87.
    Gudmundsson, J. T.
    et al.
    KTH Royal Institute Technology, Sweden; University of Iceland, Iceland.
    Lundin, D.
    University of Paris 11, France.
    Stancu, G. D.
    CentraleSupelec, France; CNRS, France.
    Brenning, Nils
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering. KTH Royal Institute Technology, Sweden.
    Minea, T. M.
    University of Paris 11, France.
    Are the argon metastables important in high power impulse magnetron sputtering discharges?2015In: Physics of Plasmas, ISSN 1070-664X, E-ISSN 1089-7674, Vol. 22, no 11, p. 113508-Article in journal (Refereed)
    Abstract [en]

    We use an ionization region model to explore the ionization processes in the high power impulse magnetron sputtering (HiPIMS) discharge in argon with a titanium target. In conventional dc magnetron sputtering (dcMS), stepwise ionization can be an important route for ionization of the argon gas. However, in the HiPIMS discharge stepwise ionization is found to be negligible during the breakdown phase of the HiPIMS pulse and becomes significant (but never dominating) only later in the pulse. For the sputtered species, Penning ionization can be a significant ionization mechanism in the dcMS discharges, while in the HiPIMS discharge Penning ionization is always negligible as compared to electron impact ionization. The main reasons for these differences are a higher plasma density in the HiPIMS discharge, and a higher electron temperature. Furthermore, we explore the ionization fraction and the ionized flux fraction of the sputtered vapor and compare with recent experimental work. (C) 2015 AIP Publishing LLC.

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  • 88.
    Gudmundsson, J T
    et al.
    University of Iceland.
    Sigurjonsson, P.
    University of Iceland.
    Larsson, Petter
    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.
    Helmersson, Ulf
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
    On the electron energy in the high power impulse magnetron sputtering discharge2009In: JOURNAL OF APPLIED PHYSICS, ISSN 0021-8979, Vol. 105, no 12Article in journal (Refereed)
    Abstract [en]

    The temporal variation of the electron energy distribution function (EEDF) was measured with a Langmuir probe in a high power impulse magnetron sputtering (HiPIMS) discharge at 3 and 20 mTorr pressures. In the HiPIMS discharge a high power pulse is applied to a planar magnetron giving a high electron density and highly ionized sputtered vapor. The measured EEDF is Maxwellian-like during the pulse; it is broader for lower discharge pressure and it becomes narrower as the pulse progresses. This indicates that the plasma cools as the pulse progresses, probably due to high metal content of the discharge.

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  • 89. Order onlineBuy this publication >>
    Gunnarsson, Rickard
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Controlling the growth of nanoparticles produced in a high power pulsed plasma2017Doctoral thesis, comprehensive summary (Other academic)
    Abstract [en]

    Nanotechnology can profoundly benefit our health, environment and everyday life. In order to make this a reality, both technological and theoretical advancements of the nanomaterial synthesis methods are needed. A nanoparticle is one of the fundamental building blocks in nanotechnology and this thesis describes the control of the nucleation, growth and oxidation of titanium particles produced in a pulsed plasma. It will be shown that by controlling the process conditions both the composition (oxidationstate) and size of the particles can be varied. The experimental results are supported by theoretical modeling.

    If processing conditions are chosen which give a high temperature in the nanoparticle growth environment, oxygen was found to be necessary in order to nucleate the nanoparticles. The two reasons for this are 1: the lower vapor pressure of a titanium oxide cluster compared to a titanium cluster, meaning a lower probability of evaporation, and 2: the ability of a cluster to cool down by ejecting an oxygen atom when an oxygen molecule condenses on its surface. When the oxygen gas flow was slightly increased, the nanoparticle yield and oxidation state increased. A further increase caused a decrease in particle yield which is attributed to a slight oxidation ofthe cathode. By varying the oxygen flow, it was possible to control the oxidation state of the nanoparticles without fully oxidizing the cathode. Pure titanium nanoparticles could not be produced in a high vacuum system because oxygen containing gases such as residual water vapour have a profound influence on nanoparticle yield and composition. In an ultrahigh vacuum system titanium nanoparticles without significantoxygen contamination were produced by reducing the temperature of the growth environment and increasing the pressure of an argon-helium gas mixture within whichthe nanoparticles grew. The dimer formation rate necessary for this is only achievable at higher pressures. After a dimer has formed, it needs to grow by colliding with a titanium atom followed by cooling by collisions with multiple buffer gas atoms. The condensation event heats up the cluster to a temperature much higher than the gas temperature, where it is during a short time susceptible to evaporation. When the clusters’ internal energy has decreased by collisions with the gas to less than the energy required to evaporate a titanium atom, it is temporarily stable until the next condensation event occurs. The temperature difference by which the cluster has to cool down before it is temporarily stable is exactly as many kelvins as the gas temperature.The addition of helium was found to decrease the temperature of the gas, making it possible for nanoparticles of pure titanium to grow. The process window where this is possible was determined and the results presented opens up new possibilities to synthesize particles with a controlled contamination level and deposition rate.The size of the nanoparticles has been controlled by three means. The first is to change the electrical potential around the growth zone, which allows for size (diameter) control in the order of 25 to 75 nm without influencing the oxygen content of the particles. The second means is by increasing the pressure which decreases the ambipolar diffusion rate of the ions resulting in a higher growth material density. By doing this, the particle size can be increased from 50 to 250 nm, however the oxygen content also increases with increasing pressure when this is done in a high vacuum system. The last means of size control was by adding a helium flow to the process where higher flows resulted in smaller nanoparticle sizes.

    When changing the pressure in high vacuum, the morphology of the nanoparticles could be controlled. At low pressures, highly faceted near spherical particles were produced. Increasing the pressure caused the formation of cubic particles which appear to ‘fracture’ at higher pressures. At the highest pressure investigated, the particles became poly-crystalline with a cauliflower shape and this morphology was attributed to a lowad atom mobility.

    The ability to control the size, morphology and composition of the nanoparticles determines the success of applying the process to manufacture devices. In related work presented in this thesis it is shown that 150-200 nm molybdenum particles with cauliflower morphology were found to scatter light in which made them useful in photovoltaic applications, and the size of titanium dioxide nanoparticles were found to influence the selectivity of graphene based gas sensors.

    List of papers
    1. Synthesis of titanium-oxide nanoparticles with size and stoichiometry control
    Open this publication in new window or tab >>Synthesis of titanium-oxide nanoparticles with size and stoichiometry control
    2015 (English)In: Journal of nanoparticle research, ISSN 1388-0764, E-ISSN 1572-896X, Vol. 17, no 9, p. 353-Article in journal (Refereed) Published
    Abstract [en]

    Ti-O nanoparticles have been synthesized via hollow cathode sputtering in an Ar-O-2 atmosphere using high power pulsing. It is shown that the stoichiometry and the size of the nanoparticles can be varied independently, the former through controlling the O-2 gas flow and the latter by the independent biasing of two separate anodes in the growth zone. Nanoparticles with diameters in the range of 25-75 nm, and with different Ti-O compositions and crystalline phases, have been synthesized.

    Place, publisher, year, edition, pages
    Springer Verlag (Germany), 2015
    Keywords
    Titanium dioxide; TiO2; Reactive sputtering; Size control; Composition control; Gas flow sputtering; Aerosols
    National Category
    Physical Sciences
    Identifiers
    urn:nbn:se:liu:diva-121300 (URN)10.1007/s11051-015-3158-3 (DOI)000360245300002 ()
    Note

    Funding Agencies|Knut and Alice Wallenberg foundation [KAW 2014.0276]; Swedish Research Council via the Linkoping Linneaus Environment LiLi-NFM [2008-6572]

    Available from: 2015-09-16 Created: 2015-09-14 Last updated: 2017-12-21
    2. The influence of pressure and gas flow on size and morphology of titanium oxide nanoparticles synthesized by hollow cathode sputtering
    Open this publication in new window or tab >>The influence of pressure and gas flow on size and morphology of titanium oxide nanoparticles synthesized by hollow cathode sputtering
    Show others...
    2016 (English)In: Journal of Applied Physics, ISSN 0021-8979, E-ISSN 1089-7550, Vol. 120, no 4, p. 044308-Article in journal (Refereed) Published
    Abstract [en]

    Titanium oxide nanoparticles have been synthesized via sputtering of a hollow cathode in an argon atmosphere. The influence of pressure and gas flow has been studied. Changing the pressure affects the nanoparticle size, increasing approximately proportional to the pressure squared. The influence of gas flow is dependent on the pressure. In the low pressure regime (107 amp;lt;= p amp;lt;= 143 Pa), the nanoparticle size decreases with increasing gas flow; however, at high pressure (p = 215 Pa), the trend is reversed. For low pressures and high gas flows, it was necessary to add oxygen for the particles to nucleate. There is also a morphological transition of the nanoparticle shape that is dependent on the pressure. Shapes such as faceted, cubic, and cauliflower can be obtained. Published by AIP Publishing.

    Place, publisher, year, edition, pages
    AMER INST PHYSICS, 2016
    National Category
    Fluid Mechanics and Acoustics
    Identifiers
    urn:nbn:se:liu:diva-131710 (URN)10.1063/1.4959993 (DOI)000382405400029 ()
    Note

    Funding Agencies|Knut and Alice Wallenberg foundation [KAW 2014.0276]; Swedish Research Council via the Linkoping Linneaus Environment LiLi-NFM [2008-6572]

    Available from: 2016-10-03 Created: 2016-09-30 Last updated: 2017-12-21
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  • 90. Order onlineBuy this publication >>
    Gunnarsson, Rickard
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Titanium oxide nanoparticle production using high power pulsed plasmas2016Licentiate thesis, comprehensive summary (Other academic)
    Abstract [en]

    This thesis covers fundamental aspects of process control when growing titanium oxide nanoparticles in a reactive sputtering process. It covers the influence of oxygen containing gas on the oxidation state of the cathode from which the growth material is ejected, as well as its influence on the particles oxidation state and their nucleation. It was found that a low degree of reactive gases was necessary for nanoparticles of titanium to nucleate. When the oxygen gas was slightly increased, the nanoparticle yield and particle oxygen content increased. A further increase caused a decrease in particle yield which was attributed to a slight oxidation of the cathode. By varying the oxygen flow to the process, it was possible to control the oxygen content of the nanoparticles without fully oxidizing the cathode. Because oxygen containing gases such as residual water vapour has a profound influence on nanoparticle yield and composition, the deposition source was re-engineered to allow for cleaner and thus more stable synthesis conditions.

    The size of the nanoparticles has been controlled by two means. The first is to change electrical potentials around the growth zone, which allows for nanoparticle size control in the order of 25-75 nm. This size control does not influence the oxygen content of the nanoparticles. The second means of size control investigated was by increasing the pressure. By doing this, the particle size can be increased from 50 – 250 nm, however the oxygen content also increases with pressure. Different particle morphologies were found by changing the pressure. At low pressures, mostly spherical particles with weak facets were produced. As the pressure increased, the particles got a cubic shape. At higher pressures the cubic particles started to get a fractured surface. At the highest pressure investigated, the fractured surface became poly-crystalline, giving a cauliflower shaped morphology.

    List of papers
    1. Synthesis of titanium-oxide nanoparticles with size and stoichiometry control
    Open this publication in new window or tab >>Synthesis of titanium-oxide nanoparticles with size and stoichiometry control
    2015 (English)In: Journal of nanoparticle research, ISSN 1388-0764, E-ISSN 1572-896X, Vol. 17, no 9, p. 353-Article in journal (Refereed) Published
    Abstract [en]

    Ti-O nanoparticles have been synthesized via hollow cathode sputtering in an Ar-O-2 atmosphere using high power pulsing. It is shown that the stoichiometry and the size of the nanoparticles can be varied independently, the former through controlling the O-2 gas flow and the latter by the independent biasing of two separate anodes in the growth zone. Nanoparticles with diameters in the range of 25-75 nm, and with different Ti-O compositions and crystalline phases, have been synthesized.

    Place, publisher, year, edition, pages
    Springer Verlag (Germany), 2015
    Keywords
    Titanium dioxide; TiO2; Reactive sputtering; Size control; Composition control; Gas flow sputtering; Aerosols
    National Category
    Physical Sciences
    Identifiers
    urn:nbn:se:liu:diva-121300 (URN)10.1007/s11051-015-3158-3 (DOI)000360245300002 ()
    Note

    Funding Agencies|Knut and Alice Wallenberg foundation [KAW 2014.0276]; Swedish Research Council via the Linkoping Linneaus Environment LiLi-NFM [2008-6572]

    Available from: 2015-09-16 Created: 2015-09-14 Last updated: 2017-12-21
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    fulltext
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    presentationsbild
  • 91.
    Gunnarsson, Rickard
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Brenning, Nils
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering. KTH Royal Inst Technol, Sweden.
    Boyd, Robert
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Helmersson, Ulf
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Nucleation of titanium nanoparticles in an oxygen-starved environment. I: experiments2018In: Journal of Physics D: Applied Physics, ISSN 0022-3727, E-ISSN 1361-6463, Vol. 51, no 45, article id 455201Article in journal (Refereed)
    Abstract [en]

    A constant supply of oxygen has been assumed to be necessary for the growth of titanium nanoparticles by sputtering. This oxygen supply can arise from a high background pressure in the vacuum system or from a purposely supplied gas. The supply of oxygen makes it difficult to grow metallic nanoparticles of titanium and can cause process problems by reacting with the target. We here report that growth of titanium nanoparticles in the metallic hexagonal titanium (alpha Ti) phase is possible using a pulsed hollow cathode sputter plasma and adding a high partial pressure of helium to the process instead of trace amounts of oxygen. The helium cools the process gas in which the nanoparticles nucleate. This is important both for the first dimer formation and the continued growth to a thermodynamically stable size. The parameter region, inside which the synthesis of nanoparticles is possible, is mapped out experimentally and the theory of the physical processes behind this process window is outlined. A pressure limit below which no nanoparticles were produced was found at 200 Pa, and could be attributed to a low dimer formation rate, mainly caused by a more rapid dilution of the growth material. Nanoparticle production also disappeared at argon gas flows above 25 sccm. In this case, the main reason was identified as a gas temperature increase within the nucleation zone, giving a too high evaporation rate from nanoparticles (clusters) in the stage of growth from dimers to stable nuclei. These two mechanisms are in depth explored in a companion paper. A process stability limit was also found at low argon gas partial pressures, and could be attributed to a transition from a hollow cathode discharge to a glow discharge.

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  • 92.
    Gunnarsson, Rickard
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Brenning, Nils
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering. KTH Royal Inst Technol, Sweden.
    Ojamäe, Lars
    Linköping University, Department of Physics, Chemistry and Biology, Chemistry. Linköping University, Faculty of Science & Engineering.
    Kalered, Emil
    Linköping University, Department of Physics, Chemistry and Biology, Chemistry. Linköping University, Faculty of Science & Engineering.
    Raadu, Michael Allan
    KTH Royal Inst Technol, Sweden.
    Helmersson, Ulf
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Nucleation of titanium nanoparticles in an oxygen-starved environment. II: theory2018In: Journal of Physics D: Applied Physics, ISSN 0022-3727, E-ISSN 1361-6463, Vol. 51, no 45, article id 455202Article in journal (Refereed)
    Abstract [en]

    The nucleation and growth of pure titanium nanoparticles in a low-pressure sputter plasma has been believed to be essentially impossible. The addition of impurities, such as oxygen or water, facilitates this and allows the growth of nanoparticles. However, it seems that this route requires such high oxygen densities that metallic nanoparticles in the hexagonal alpha Ti-phase cannot be synthesized. Here we present a model which explains results for the nucleation and growth of titanium nanoparticles in the absent of reactive impurities. In these experiments, a high partial pressure of helium gas was added which increased the cooling rate of the process gas in the region where nucleation occurred. This is important for two reasons. First, a reduced gas temperature enhances Ti-2 dimer formation mainly because a lower gas temperature gives a higher gas density, which reduces the dilution of the Ti vapor through diffusion. The same effect can be achieved by increasing the gas pressure. Second, a reduced gas temperature has a more than exponential effect in lowering the rate of atom evaporation from the nanoparticles during their growth from a dimer to size where they are thermodynamically stable, r*. We show that this early stage evaporation is not possible to model as a thermodynamical equilibrium. Instead, the single-event nature of the evaporation process has to be considered. This leads, counter intuitively, to an evaporation probability from nanoparticles that is exactly zero below a critical nanoparticle temperature that is size-dependent. Together, the mechanisms described above explain two experimentally found limits for nucleation in an oxygen-free environment. First, there is a lower limit to the pressure for dimer formation. Second, there is an upper limit to the gas temperature above which evaporation makes the further growth to stable nuclei impossible.

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  • 93.
    Gunnarsson, Rickard
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Helmersson, Ulf
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Pilch, Iris
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
    Synthesis of titanium-oxide nanoparticles with size and stoichiometry control2015In: Journal of nanoparticle research, ISSN 1388-0764, E-ISSN 1572-896X, Vol. 17, no 9, p. 353-Article in journal (Refereed)
    Abstract [en]

    Ti-O nanoparticles have been synthesized via hollow cathode sputtering in an Ar-O-2 atmosphere using high power pulsing. It is shown that the stoichiometry and the size of the nanoparticles can be varied independently, the former through controlling the O-2 gas flow and the latter by the independent biasing of two separate anodes in the growth zone. Nanoparticles with diameters in the range of 25-75 nm, and with different Ti-O compositions and crystalline phases, have been synthesized.

    Download full text (pdf)
    fulltext
  • 94.
    Gunnarsson, Rickard
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Pilch, Iris
    Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
    Boyd, Robert
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    Brenning, Nils
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering. KTH Royal Institute Technology, Sweden.
    Helmersson, Ulf
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Faculty of Science & Engineering.
    The influence of pressure and gas flow on size and morphology of titanium oxide nanoparticles synthesized by hollow cathode sputtering2016In: Journal of Applied Physics, ISSN 0021-8979, E-ISSN 1089-7550, Vol. 120, no 4, p. 044308-Article in journal (Refereed)
    Abstract [en]

    Titanium oxide nanoparticles have been synthesized via sputtering of a hollow cathode in an argon atmosphere. The influence of pressure and gas flow has been studied. Changing the pressure affects the nanoparticle size, increasing approximately proportional to the pressure squared. The influence of gas flow is dependent on the pressure. In the low pressure regime (107 amp;lt;= p amp;lt;= 143 Pa), the nanoparticle size decreases with increasing gas flow; however, at high pressure (p = 215 Pa), the trend is reversed. For low pressures and high gas flows, it was necessary to add oxygen for the particles to nucleate. There is also a morphological transition of the nanoparticle shape that is dependent on the pressure. Shapes such as faceted, cubic, and cauliflower can be obtained. Published by AIP Publishing.

    Download full text (pdf)
    fulltext
  • 95.
    Gylfason, K. B.
    et al.
    Science Institute, University of Iceland, Reykjavik, Iceland.
    Alami, Jones
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating 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.
    Gudmundsson, J. T.
    Science Institute, University of Iceland, Reykjavik, Iceland.
    Ion-accoustic solitary waves in a high power pulsed magnetron sputtering discharge2005In: Journal of Physics D: Applied Physics, ISSN 0022-3727, E-ISSN 1361-6463, Vol. 38, no 18, p. 3417-3421Article in journal (Refereed)
    Abstract [en]

    We report on the creation and propagation of ion-acoustic solitary waves in a high power pulsed magnetron sputtering discharge. A dense localized plasma is created by applying high energy pulses (4–12 J) of length 70 µs, at a repetition frequency of 50 pulses per second, to a planar magnetron sputtering source. The temporal behaviour of the electron density, measured by a Langmuir probe, shows solitary waves travelling away from the magnetron target. The velocity of the waves depends on the gas pressure but is roughly independent of the pulse energy.

  • 96.
    Hasan, Mohammad
    et al.
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology. Östergötlands Läns Landsting, Center for Diagnostics, Department of Clinical Pharmacology.
    Pilch, Iris
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology. Östergötlands Läns Landsting, Center for Diagnostics, Department of Clinical Pharmacology.
    Söderström, Daniel
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology. Östergötlands Läns Landsting, Center for Diagnostics, Department of Clinical Pharmacology.
    Lundin, D.
    Royal Institute Technology KTH, Sweden.
    Helmersson, Ulf
    Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology. Östergötlands Läns Landsting, Center for Diagnostics, Department of Clinical Pharmacology.
    Brenning, N.
    Royal Institute Technology KTH, Sweden.
    Modeling the extraction of sputtered metal from high power impulse hollow cathode discharges2013In: Plasma sources science & technology (Print), ISSN 0963-0252, E-ISSN 1361-6595, Vol. 22, no 3, p. 035006-Article in journal (Refereed)
    Abstract [en]

    High power impulse hollow cathode sputtering is studied as a means to produce high fluxes of neutral and ionized sputtered metal species. A model is constructed for the understanding and optimization of such discharges. It relates input parameters such as the geometry of the cathode, the electric pulse form and frequency, and the feed gas flow rate and pressure, to the production, ionization, temperature and extraction of the sputtered species. Examples of processes that can be quantified by the use of the model are the internal production of sputtered metal and the degree of its ionization, the speed and efficiency of out-puffing from the hollow cathode associated with the pulses, and the gas back-flow into the hollow cathode between pulses. The use of the model is exemplified with a special case where the aim is the synthesis of nanoparticles in an expansion volume that lies outside the hollow cathode itself. The goals are here a maximum extraction efficiency, and a high degree of ionization of the sputtered metal. It is demonstrated that it is possible to reach a degree of ionization above 85%, and extraction efficiencies of 3% and 17% for the neutral and ionized sputtered components, respectively.

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  • 97.
    Helmersson, Ulf
    Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics .
    High Power Impulse Magnetron Sputtering - HiPIMS2008In: The 11:th International Conference on Plasma Surface Engineering,2008, 2008Conference paper (Other academic)
  • 98.
    Helmersson, Ulf
    Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics .
    High Power Impulse Magnetron Sputtering for Improved Thin Films and Thin Film Processes2008In: The 5th Symposium on Functional Coatings and Surface Engineering,2008, 2008Conference paper (Other academic)
    Abstract [en]

      

  • 99.
    Helmersson, Ulf
    Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics .
    Ionized deposition using high power impulse magnetron sputtering2007In: The annual one day meeting on Plasmas, Surfaces and Thin Films,2007, 2007Conference paper (Other academic)
  • 100.
    Helmersson, Ulf
    Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics .
    Ionized physical vapor deposition (IPVD) and especially high power impulse magnetron sputtering (HIPIMS)2006In: 4e Journees detude sur les nouvelles tendances en procedes magnetron et arc pour le depot de couches minces,2006, Paris: Société Française du Vide , 2006Conference paper (Other academic)
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