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• 1.
Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Applied Optics . Linköping University, Faculty of Science & Engineering. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Uppsala University.
Effect of peak power in reactive high power impulse magnetron sputtering of titanium dioxide2011In: Surface & Coatings Technology, ISSN 0257-8972, E-ISSN 1879-3347, Vol. 205, no 20, p. 4828-4831Article in journal (Refereed)

The effect of peak power in a high power impulse magnetron sputtering (HiPIMS) reactive deposition of TiO(2) films has been studied with respect to the deposition rate and coating properties. With increasing peak power not only the ionization of the sputtered material increases but also their energy. In order to correlate the variation in the ion energy distributions with the film properties, the phase composition, density and optical properties of the films grown with different HiPIMS-parameters have been investigated and compared to a film grown using direct current magnetron sputtering (DCMS). All experiments were performed for constant average power and pulse on time (100W and 35 mu s, respectively), different peak powers were achieved by varying the frequency of pulsing. Ion energy distributions for Ti and O and its dependence on the process conditions have been studied. It was found that films with the highest density and highest refractive index were grown under moderate HiPIMS conditions (moderate peak powers) resulting in only a small loss in mass-deposition rate compared to DCMS. It was further found that TiO2 films with anatase and rutile phases can be grown at room temperature without substrate heating and without post-deposition annealing.

• 2.
Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics.
Uppsala University, Sweden. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
Hysteresis and process stability in reactive high power impulse magnetron sputtering of metal oxides2011In: Thin Solid Films, ISSN 0040-6090, E-ISSN 1879-2731, Vol. 519, no 22, p. 7779-7784Article in journal (Refereed)

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

• 3.
Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
Interdisciplinary Nanoscience Center (iNANO), Aarhus University, Denmark. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
Synthesis of amorphous carbon thin films using acetylene-based high power impulse magnetron sputtering discharges2013Manuscript (preprint) (Other academic)

Amorphous carbon (a-C) thin films are synthesized using high power impulse magnetron sputtering (HiPIMS) based Ne-Ar/C2H2 discharges. Plasma properties and film growth are investigated under different gas phase composition and operating pressures. Film mass densities, H content, hardness and compressive stresses are measured. Mass densities in the order of 2.2 g/cm3, hardness close to 25 GPa and H content as low as 11% are obtained. The film properties manifest a dependence on energy and flux of the depositing species and energetic ion bombardment driven structural changes in the films are found to govern the resulting film properties.

• 4.
Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology. Chimie des Interactions Plasma-Surface (ChIPS), University of Mons, Belgium. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Plasma and Coating Physics. Linköping University, The Institute of Technology.
Principles for designing sputtering-based strategies for high-rate synthesis of dense and hard hydrogenated amorphous carbon thin films2014In: Diamond and related materials, ISSN 0925-9635, E-ISSN 1879-0062, Vol. 44, p. 117-122Article in journal (Refereed)

In the present study we contribute to the understanding that is required for designing sputtering-based routes for high rate synthesis of hard and dense amorphous carbon (a-C) films. We compile and implement a strategy for synthesis of a-C thin films that entails coupling a hydrocarbon gas (acetylene) with high density discharges generated by the superposition of high power impulse magnetron sputtering (HiPIMS) and direct current magnetron sputtering (DCMS). Appropriate control of discharge density (by tuning HiPIMS/DCMS power ratio), gas phase composition and energy of the ionized depositing species leads to a route capable of providing ten-fold increase in the deposition rate of a-C film growth compared to HiPIMS Ar discharge (Aijaz et al. Diamond and Related Materials 23 (2012) 1). This is achieved without significant incorporation of H (< 10 %) and with relatively high hardness (> 25 GPa) and mass density (~2.32 g/cm3). Using our experimental data together with Monte-Carlo computer simulations and data from the literature we suggest that: (i) dissociative reactions triggered by the interactions of energetic discharge electrons with hydrocarbon gas molecules is an important additional (to the sputtering cathode) source of film forming species and (ii) film microstructure and film hydrogen content are primarily controlled by interactions of energetic plasma species with surface and sub-surface layers of the growing film.

• 5.
Helsinki University of Technology (TKK), Micronova, Department of Micro and Nanosciences, P.O. Box 3500, FIN-02015 TKK, Finland.
Helsinki University of Technology (TKK), Micronova, Department of Micro and Nanosciences, P.O. Box 3500, FIN-02015 TKK, Finland. Helsinki University of Technology (TKK), Micronova, Department of Micro and Nanosciences, P.O. Box 3500, FIN-02015 TKK, Finland. Helsinki University of Technology (TKK), Micronova, Department of Micro and Nanosciences, P.O. Box 3500, FIN-02015 TKK, Finland. Helsinki University of Technology (TKK), Micronova, Department of Micro and Nanosciences, P.O. Box 3500, FIN-02015 TKK, Finland. Helsinki University of Technology (TKK), Micronova, Department of Micro and Nanosciences, P.O. Box 3500, FIN-02015 TKK, Finland. Helsinki University of Technology (TKK), Micronova, Department of Micro and Nanosciences, P.O. Box 3500, FIN-02015 TKK, Finland. Department of Engineering Sciences, Uppsala University, P.O. Box 534, SE-75121 Uppsala, Sweden. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Reduced photoluminescence from InGaN/GaN multiple quantum well structures following 40 MeV iodine ion irradiation2009In: Physica. B, Condensed matter, ISSN 0921-4526, E-ISSN 1873-2135, ISSN 0921-4526, Vol. 404, no 23-24, p. 4925-4928Article in journal (Refereed)

The effects following ion irradiation of GaN-based devices are still limited. Here we present data on the photoluminescence (PL) emitted from InGaN/GaN multiple quantum well (MQW) structures, which have been exposed to 40 MeV I ion irradiation. The PL is reduced as a function of applied ion fluence, with essentially no PL signal left above 1011 ions/cm2. It is observed that even the ion fluences in the 109 ions/cm2 range have a pronounced effect on the photoluminescence properties of the MQW structures. This may have consequences concerning application of InGaN/GaN MQW’s in radiation-rich environments, in addition to defect build-up during ion beam analysis.

• 6.
European Spallation Source ESS AB, Lund, Sweden.
Institut Laue Langevin, Grenoble, Cedex 9, France. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Institut Laue Langevin, Grenoble, Cedex 9, France. Institut Laue Langevin, Grenoble, Cedex 9, France. European Spallation Source ESS AB, Lund, Sweden. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Institut Laue Langevin, Grenoble, Cedex 9, France. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Institut Laue Langevin, Grenoble, Cedex 9, France. Linköping University. Institut Laue Langevin, Grenoble, Cedex 9, France. Institut Laue Langevin, Grenoble, Cedex 9, France. European Spallation Source, Lund, Sweden.
10B multi-grid proportional gas counters for large area thermal neutrondetectors2013In: Nuclear Instruments and Methods in Physics Research Section A: Accelerators, Spectrometers, Detectors and Associated Equipment, ISSN 0168-9002, E-ISSN 1872-9576, Vol. 720, p. 116-121Article in journal (Refereed)

3He was a popular material in neutrons detectors until its availability dropped drastically in 2008. The development of techniques based on alternative convertors is now of high priority for neutron research institutes. Thin films of 10B or 10B4C have been used in gas proportional counters to detect neutrons, but until now, only for small or medium sensitive area. We present here the multi-grid design, introduced at the ILL and developed in collaboration with ESS for LAN (large area neutron) detectors. Typically thirty 10B4C films of 1 μm thickness are used to convert neutrons into ionizing particles which are subsequently detected in a proportional gas counter. The principle and the fabrication of the multi-grid are described and some preliminary results obtained with a prototype of 200 cm×8 cm are reported; a detection efficiency of 48% has been measured at 2.5 Å with a monochromatic neutron beam line, showing the good potential of this new technique.

• 7.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
Low-temperature growth of low friction wear-resistant amorphous carbon nitride thin films by mid-frequency, high power impulse, and direct current magnetron sputtering2015In: Journal of Vacuum Science & Technology. A. Vacuum, Surfaces, and Films, ISSN 0734-2101, E-ISSN 1520-8559, Vol. 33, no 5, article id 05E112Article in journal (Refereed)

Amorphous carbon nitride (a-CNx) thin films were deposited on steel AISI52100 and Si(001) substrates using mid-frequency magnetron sputtering (MFMS) with an MF bias voltage, high power impulse magnetron sputtering (HiPIMS) with a synchronized HiPIMS bias voltage, and direct current magnetron sputtering (DCMS) with a DC bias voltage. The films were deposited at a low substrate temperature of 150 °C and a N2/Ar flow ratio of 0.16 at the total pressure of 400 mPa. The negative bias voltage (Vs) was varied from 20 V to 120 V in each of the three deposition modes. The microstructure of the films was characterized by high-resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED), while the film morphology was investigated by scanning electron microscopy (SEM). All films possessed amorphous microstructure with clearly developed columns extending throughout the entire film thickness. Layers grown with the lowest substrate bias of 20 V exhibited pronounced intercolumnar porosity, independent of the technique used. Voids closed and dense films formed at Vs ≥ 60 V, Vs ≥ 100 V and Vs = 120 V for MFMS, DCMS and HiPIMS, respectively. X-ray photoelectron spectroscopy (XPS) revealed that the nitrogen-to-carbon ratio, N/C, of the films ranged between 0.2 and 0.24. Elastic recoil detection analysis (ERDA) showed that Ar content varied between 0 and 0.8 at% and increases as a function of Vs for all deposition techniques. All films exhibited compressive residual stress, σ, which depends on the growth method; HiPIMS produces the least stressed films with stress between – 0.4 and – 1.2 GPa for all Vs values, while for CNx films deposited by MFMS σ = – 4.2 GPa. Nanoindentation showed a significant increase in film hardness and reduced elastic modulus with increasing Vs for all techniques. The harder films were produced by MFMS with hardness as high as 25 GPa. Low friction coefficients, between 0.05 and 0.06, were recorded for all films. Furthermore, CNx films produced by MFMS and DCMS at Vs = 100 V and 120 V presented a high wear resistance with wear coefficients of k ≤ 2.3 x 10-5 mm3/Nm.

• 8.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Forschungszentrum Dresden Rossendorf. Linköping University, Department of Physics, Chemistry and Biology. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Formation of basal plane fiber-textured Ti2AlN films on amorphous substrates2010In: PHYSICA STATUS SOLIDI-RAPID RESEARCH LETTERS, ISSN 1862-6254, Vol. 4, no 05-Jun, p. 121-123Article in journal (Refereed)

The synthesis of fiber-textured Ti2AlN(0001) films on SiO2 was characterized by in-situ and ex-situ X-ray scattering and Rutherford backscattering spectrometry. Ti2AlN was formed by solid-state reaction between sequentially deposited Ti and AlN layers. A deposition at 275 degrees C yields a Ti(0001) out-of-plane orientation which is maintained for the following AlN(0001)/Ti(0001) layers. Annealing to 600 degrees C yields AlN decomposition and diffusion of Al and N into Ti, with consecutive transformation into (TiAlN)-Al-3(111) and Ti2AlN(0001) plus AlN residuals. Despite preferred Ti2AlN(0001) out-of-plane orientation, the in-plane distribution is random, as expected from the self-organized pseudo-epitaxial growth.

• 9.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. University of Aveiro, Portugal; University of Aveiro, Portugal.
Infrared dielectric functions and optical phonons of wurtzite YxAl1-xN (0 less than= x less than= 0.22)2015In: Journal of Physics D: Applied Physics, ISSN 0022-3727, E-ISSN 1361-6463, Vol. 48, no 41, p. 415102-Article in journal (Refereed)

YAlN is a new member of the group-III nitride family with potential for applications in next generation piezoelectric and light emitting devices. We report the infrared dielectric functions and optical phonons of wurtzite (0001) YxAl1-xN epitaxial films with 0 less than= x less than= 0.22. The films are grown by magnetron sputtering epitaxy on c-plane Al2O3 and their phonon properties are investigated using infrared spectroscopic ellipsometry and Raman scattering spectroscopy. The infrared-active E-1(TO) and LO, and the Raman active E-2 phonons are found to exhibit one-mode behavior, which is discussed in the framework of the MREI model. The compositional dependencies of the E-1(TO), E-2 and LO phonon frequencies, the high-frequency limit of the dielectric constant, epsilon(infinity), the static dielectric constant, epsilon(0), and the Born effective charge Z(B) are established and discussed.

• 10.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
Institute Laue Langevin, France. Institute Laue Langevin, France. Institute Laue Langevin, France. Institute Laue Langevin, France. Institute Laue Langevin, France. European Spallat Source, Sweden; Mid Sweden University, Sweden. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering. Linköping University, Department of Physics, Chemistry and Biology. European Spallat Source, Sweden. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering. Institute Laue Langevin, France; European Spallat Source, Sweden. Institute Laue Langevin, France; European Spallat Source, Sweden.
Investigation of background in large-area neutron detectors due to alpha emission from impurities in aluminium2015In: Journal of Instrumentation, ISSN 1748-0221, E-ISSN 1748-0221, Vol. 10, p. 1-14Article in journal (Refereed)

Thermal neutron detector based on films of (B4C)-B-10 have been developed as an alternative to He-3 detectors. In particular, The Multi-Grid detector concept is considered for future large area detectors for ESS and ILL instruments. An excellent signal-to-background ratio is essential to attain expected scientific results. Aluminium is the most natural material for the mechanical structure of of the Multi-Grid detector and other similar concepts due to its mechanical and neutronic properties. Due to natural concentration of alpha emitters, however, the background from alpha particles misidentified as neutrons can be unacceptably high. We present our experience operating a detector prototype affected by this issue. Monte Carlo simulations have been used to confirm the background as alpha particles. The issues have been addressed in the more recent implementations of the Multi-Grid detector by the use of purified aluminium as well as Ni-plating of standard aluminium. The result is the reduction in background by two orders of magnitude. A new large-area prototype has been built incorporating these modifications.

• 11.
Norut No Research Institute Narvik.
Uppsala University. Linköping University, Department of Physics, Chemistry and Biology. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology. Linköping University, The Institute of Technology. Uppsala University. Uppsala University.
Structure and morphology of nickel-alumina/silica solar thermal selective absorbers2011In: JOURNAL OF NON-CRYSTALLINE SOLIDS, ISSN 0022-3093, Vol. 357, no 5, p. 1370-1375Article in journal (Refereed)

Nickel-alumina/silica thin film materials for the use in solar thermal absorbers have been investigated using Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM) and Elastic Recoil Detection Analysis (ERDA). The TEM images revealed that all layers have a very small thickness variation and that the layers are completely homogenous. High resolution images showed 5-10 nm (poly) crystalline nickel nano-particles. ERDA showed that both the silica and alumina compositions contain more oxygen than 2:1 and 3:2 respectively. SEM showed the surface morphology and characteristics of the top silica anti-reflection layer. Hybrid-silica has showed to generate a smoother surface with less cracking compared to pure silica. The final curing temperature revealed to be of importance for the formation of cracks and the surface morphology.

• 12.
Linköping University, Department of Physics, Chemistry and Biology, Applied Physics. Linköping University, The Institute of Technology.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Royal Institute Technology, KTH. Royal Institute Technology, KTH. Royal Institute Technology, KTH. Trinity College Dublin. Trinity College Dublin. Linköping University, Department of Physics, Chemistry and Biology, Applied Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Growth and characterization of epitaxial Ti3GeC2 thin films on 4H-SiC(0001)2012In: Journal of Crystal Growth, ISSN 0022-0248, E-ISSN 1873-5002, Vol. 343, no 1, p. 133-137Article in journal (Refereed)

Epitaxial Ti3GeC2 thin films were deposited on 4 degrees off-cut 4H-SiC(0001) using magnetron sputtering from high purity Ti, C, and Ge targets. Scanning electron microscopy and helium ion microscopy show that the Ti3GeC2 films grow by lateral step-flow with {11 (2) over bar0} faceting on the SiC surface. Using elastic recoil detection analysis, atomic force microscopy, and X-Ray diffraction the films were found to be substoichiometric in Ge with the presence of small Ge particles at the surface of the film.

• 13.
Linköping University, Department of Physics, Chemistry and Biology, Applied Physics . Linköping University, The Institute of Technology.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Applied Physics . Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Step-flow growth of nanolaminate Ti3SiC2 epitaxial layers on 4H-SiC(0 0 0 1)2011In: SCRIPTA MATERIALIA, ISSN 1359-6462, Vol. 64, no 12, p. 1141-1144Article in journal (Refereed)

Epitaxial Ti3SiC2(0 0 0 1) films were deposited on 4 degrees off-cut 4H-SiC(0 0 0 1) wafers using magnetron sputtering. A lateral step-flow growth mechanism of the Ti3SiC2 was discovered by X-ray diffraction, elastic recoil detection analysis, atomic force microscopy and electron microscopy. Helium ion microscopy revealed contrast variations on the Ti3SiC2 terraces, suggesting a mixed Si and Ti(C) termination. Si-rich growth conditions results in Ti3SiC2 layers with pronounced {1 1 (2) over bar 0) faceting and off-oriented TiSi2 crystallites, while stoichiometric growth yields truncated {1 (1) over bar 0 0) terrace edges.

• 14.
Linköping University, Department of Physics, Chemistry and Biology, Semiconductor Materials. Linköping University, The Institute of Technology.
Linköping University, Department of Physics, Chemistry and Biology, Semiconductor Materials. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Semiconductor Materials. Linköping University, The Institute of Technology.
Growth of High Quality Epitaxial Rhombohedral Boron Nitride2012In: Crystal Growth & Design, ISSN 1528-7483, E-ISSN 1528-7505, Vol. 12, no 6, p. 3215-3220Article in journal (Refereed)

Epitaxial growth of sp(2)-hybridized boron nitride (sp(2) BN) films on sapphire substrates is demonstrated in a hot wall chemical vapor deposition reactor at the temperature of 1500 degrees C, using triethyl boron and ammonia as precursors. The influence of the main important process parameters, temperature, N/B ratio, B/H-2 ratio, and carrier gas composition on the quality of the grown layers is investigated in detail. X-ray diffraction shows that epitaxial rhombohedral BN (r-BN) film can be deposited only in a narrow process parameter window; outside this window either turbostratic-BN or amorphous BN is favored if BN is formed. In addition, a thin strained AlN buffer layer is needed to support epitaxial growth of r-BN film on sapphire since only turbostratic BN is formed on sapphire substrate. The quality of the grown film is also affected by the B/H-2 ratio as seen from a change of the spacing between the basal planes as revealed by X-ray diffraction. Time-of-flight elastic recoil detection analysis shows an enhancement of the C and O impurities incorporation at lower growth temperatures. The gas phase chemistry for the deposition is discussed as well as the impact of the growth rate on the quality of the BN film.

• 15.
Linköping University, Department of Physics, Chemistry and Biology, Semiconductor Materials. Linköping University, The Institute of Technology.
Epitaxial CVD growthof sp2-hybridized boron nitrideusing aluminum nitride as buffer layer2011In: Physica Status Solidi. Rapid Research Letters, ISSN 1862-6254, E-ISSN 1862-6270, Vol. 5, no 10-11, p. 397-399Article in journal (Refereed)

Epitaxial growth of sp2-hybridized boron nitride (BN) using chemical vapour deposition, with ammonia and triethyl boron as precursors, is enabled on sapphire by introducing an aluminium nitride (AlN) buffer layer. This buffer layer is formed by initial nitridation of the substrate. Epitaxial growth is verified by X-ray diffraction measurements in Bragg–Brentano configuration, pole figure measurements and transmission electron microscopy. The in-plane stretching vibration of sp2-hybridized BN is observed at 1366 cm–1 from Raman spectroscopy. Time-of-flight elastic recoil detection analysis confirms almost perfect stoichiometric BN with low concentration of carbon, oxygen and hydrogen contaminations.

• 16.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
University of Poitiers. University of Poitiers. University of Poitiers. University of Poitiers. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Catholic University Louvain. Catholic University Louvain. University of Poitiers. University of Poitiers.
Epitaxial growth and electrical transport properties of Cr(2)GeC thin films2011In: Physical Review B. Condensed Matter and Materials Physics, ISSN 1098-0121, E-ISSN 1550-235X, Vol. 84, no 7, p. 075424-Article in journal (Refereed)

Cr(2)GeC thin films were grown by magnetron sputtering from elemental targets. Phase-pure Cr(2)GeC was grown directly onto Al(2)O(3)(0001) at temperatures of 700-800 degrees C. These films have an epitaxial component with the well-known epitaxial relationship Cr(2)GeC(0001)//Al(2)O(3)(0001) and Cr(2)GeC(11andlt;(2) overbarandgt;0)//Al(2)O(3)(1andlt;(1)over barandgt;00) or Cr(2)GeC(11andlt;(2) over barandgt;0)//Al(2)O(3)(andlt;(1) over barandgt;2andlt;(1) over barandgt;0). There is also a large secondary grain population with (10andlt;(1)overbarandgt;3) orientation. Deposition onto Al(2)O(3)(0001) with a TiN(111) seed layer and onto MgO(111) yielded growth of globally epitaxial Cr(2)GeC(0001) with a virtually negligible (10andlt;(1) over barandgt;3) contribution. In contrast to the films deposited at 700-800 degrees C, the ones grown at 500-600 degrees C are polycrystalline Cr(2)GeC with (10andlt;(1) over barandgt;0)-dominated orientation; they also exhibit surface segregations of Ge as a consequence of fast Ge diffusion rates along the basal planes. The room-temperature resistivity of our samples is 53-66 mu Omega cm. Temperature-dependent resistivity measurements from 15-295 K show that electron-phonon coupling is important and likely anisotropic, which emphasizes that the electrical transport properties cannot be understood in terms of ground state electronic structure calculations only.

• 17.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
Sandvik Coromant, Stockholm, Sweden. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering. Department of Applied Physics, Chalmers University of Technology, Göteborg, Sweden. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
Resolving Mass Spectral Overlaps in Atom Probe Tomography by Isotopic Substitutions: Case of TiSi15N2018In: Ultramicroscopy, ISSN 0304-3991, E-ISSN 1879-2723, Vol. 184, p. 51-60Article in journal (Refereed)

Mass spectral overlaps in atom probe tomography (APT) analyses of complex compounds typically limit the identification of elements and microstructural analysis of a material. This study concerns the TiSiN system, chosen because of severe mass-to-charge-state ratio overlaps of the 14N+ and 28Si2+ peaks as well as the 14N$\tiny\frac{+}{2}$ and 28Si2+ peaks. By substituting 14N with 15N, mass spectrum peaks generated by ions composed of one or more N atoms will be shifted toward higher mass-to-charge-state ratios, thereby enabling the separation of N from the predominant Si isotope. We thus resolve thermodynamically driven Si segregation on the nanometer scale in cubic phase Ti1-xSix15N thin films for Si contents 0.08 ≤ x ≤ 0.19 by APT, as corroborated by transmission electron microscopy. The APT analysis yields a composition determination that is in good agreement with energy dispersive X-ray spectroscopy and elastic recoil detection analyses. Additionally, a method for determining good voxel sizes for visualizing small-scale fluctuations is presented and demonstrated for the TiSiN system.

The full text will be freely available from 2019-08-12 11:24
• 18.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Arc deposition of Ti–Si–C–N thin films from binary and ternary cathodes — Comparing sources of C2012In: Surface & Coatings Technology, ISSN 0257-8972, E-ISSN 1879-3347, Vol. 213, p. 145-154Article in journal (Refereed)

Ti–Si–C–N thin films with composition of 1–11 at.% Si and 1–20 at.% C have been deposited onto cemented carbide substrates by arcing Ti–Si cathodes in a CH4 + N2 gas mixture and, alternatively, through arcing Ti–Si–C cathodes in N2. Films of comparable compositions from the two types of cathodes have similar structure and properties. Hence, C can be supplied as either plasma ions generated from the cathode or atoms from the gas phase with small influence on the structural evolution. Over the compositional range obtained, the films were dense and cubic-phase nanocrystalline, as characterized by X-ray diffraction, ion beam analysis, and scanning and transmission electron microscopy. The films have high hardness (30–40 GPa by nanoindentation) due to hardening from low-angle grain boundaries on the nanometer scale and lattice defects such as growth-induced vacancies and alloying element interstitials.

• 19.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Nanocolumnar Epitaxial Ti1-xSixN (0 ≤ x ≤ 0.18) Thin Films Grown by Dual Reactive Magnetron Sputtering on MgO (001), (011), and (111) Substrates2012Manuscript (preprint) (Other academic)

Ti1-xSixNy thin films and multilayers have been grown on single-crystal TiN-templated MgO (001), (011), and (111) substrates kept at 550 °C. Elemental Ti and Si targets were used in UVH reactive dual magnetron sputtering in a mixed Ar/N2 discharge. Composition analysis by time-of-flight energy elastic recoil detection analysis show that the films are close to stoichiometric (0.95 ≤ y ≤ 1.00) with respect to TiN over the wide range of Si concentrations 0 ≤ x ≤ 0.22. High-resolution transmission electron microscopy (TEM) combined with scanning TEM and energy dispersive Xray analysis show that all films grow epitaxially for x ≤ 0.18 and that as much as every fifth Ti atom can be replaced by Si (~10 at.%) in Ti1-xSixN(001). For the (011) and (111)-oriented films, however, only 1-2 at.% Si substitutes for Ti. Instead, Si segregates to form crystalline-to-amorphous SiNz (z ≈ 1) tissue phases, which promote the formation of epitaxial TiN nanocolumns. The nanocolumns have preferred {110} interfaces and {200} top facets and grow several hundreds  of nm in length.

• 20.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Materials Chemistry, RWTH Aachen University, Aachen, Germany. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Materials Chemistry, RWTH Aachen University, Aachen, Germany. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Influence of Ar and N2 Pressure on Plasma Chemistry, Ion Energy, and Thin Film Composition during Filtered Arc Deposition from Ti3SiC2 Cathodes2014In: IEEE Transactions on Plasma Science, ISSN 0093-3813, E-ISSN 1939-9375, Vol. 42, no 11, p. 3498-3507Article in journal (Refereed)

Arc plasma from Ti3SiC2 compound cathodes used in a filtered dc arc system has been characterized with respect to plasma chemistry and charge-state resolved ion energies. In vacuum, the plasma composition is dominated by Ti ions, with concentrations of 84.3, 9.3, and 6.4 at% for Ti, Si, and C ions, respectively. The reduced amount of Si and most notably C compared with the cathode composition is confirmed by analysis of film composition in corresponding growth experiments. The deposition of light-element deficient films is thus related to plasma generation or filter transport. The ion energy distributions in vacuum range up to 140, 90, and 70 eV for Ti, Si, and C, respectively. Corresponding average ion energies of 48, 36, and 27 eV are reduced upon introduction of gas, down to around 5 eV at 0.6 Pa Ar or 0.3 Pa N2 for all species. In vacuum, the charge state distributions of Si and C are shifted to higher values compared with corresponding elemental cathodes, likely caused by changed effective electron temperature of the plasma stemming from compound cathode material and/or by electron impact ionization in the filter. The average ion charge states are reduced upon addition of Ar, ranging between 1.97 and 1.48 for Ti, 1.91 and 1.46 for Si, and 1.25 and 1.02 for C. Similar effects are observed upon introduction of N2, though with more efficient charge state reduction with pressure. It is conceivable that the pressure-induced changes in ion energy and charge state are crucial for the film synthesis from a microstructure evolution point of view, as they affect the ion-surface interactions through supply of energy, especially when substrate biasing is employed during arc deposition from a compound cathode.

• 21.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Si incorporation in Ti1-xSixN films grown on TiN(001) and (001)-faceted TiN(111) columns2014In: Surface & Coatings Technology, ISSN 0257-8972, E-ISSN 1879-3347, Vol. 257, p. 121-128Article in journal (Refereed)

Thin films consisting of TiN nanocrystallites encapsulated in a fully percolated SiNy tissue phase are archetypes for hard and superhard nanocomposites. Here, we investigate metastable SiNy solid solubility in TiN and probe the effects of surface segregation during the growth of TiSiN films onto substrates that are either flat TiN(001)/MgO(001) epitaxial buffer layers or TiN(001) facets of length 1-5 nm terminating epitaxial TiN(111) nanocolumns, separated by voids, deposited on epitaxial TiN(111)/MgO(111) buffer layers. Using reactive magnetron sputter deposition, the TiSiN layers were grown at 550 degrees C and the TiN buffer layers at 900 degrees C On TiN(001), the films are NaCl-structure single-phase metastable Ti1-xSixN(001) with N/(Ti + Si) = 1 and 0 less than= x less than= 0.19. These alloys remain single-crystalline to critical thicknesses h(c) ranging from 100 +/- 30 nm with x = 0.13 to 40 +/- 10 nm with x = 0.19. At thicknesses h greater than h(c), the epitaxial growth front breaks down locally to form V-shaped polycrystalline columns with an underdense feather-like nanostructure. In contrast, the voided epitaxial TiN(111) columnar surfaces, as well as the TiN(001) facets, act as sinks for SiNy. For Ti1-xSixN layers with global average composition values less than x greater than = 0.16, the local x value in the middle of Ti1-xSixN columns increases from 0.08 for columns with radius r similar or equal to 2 nm to x = 0.14 with r similar or equal to 4 nm. The average out-of-plane lattice parameter of epitaxial nanocolumns encapsulated in SiNy decreases monotonically with increasing Si fraction less than x greater than, indicating the formation of metastable (Ti,Si)N solid solutions under growth conditions similar to those of superhard nanocomposites for which the faceted surfaces of nanograins also provide sinks for SiNy.

• 22.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Characterization of plasma chemistry and ion energy in cathodic arc plasma from Ti-Si cathodes of different compositions2013In: Journal of Applied Physics, ISSN 0021-8979, E-ISSN 1089-7550, Vol. 113, no 16Article in journal (Refereed)

Arc plasma from Ti-Si compound cathodes with up to 25 at. % Si was characterized in a DC arc system with respect to chemistry and charge-state-resolved ion energy. The plasma ion composition showed a lower Si content, diverging up to 12 at. % compared to the cathode composition, yet concurrently deposited films were in accordance with the cathode stoichiometry. Significant contribution to film growth from neutrals is inferred besides ions, since the contribution from macroparticles, estimated by scanning electron microscopy, cannot alone account for the compositional difference between cathode, plasma, and film. The average ion charge states for Ti and Si were higher than reference data for elemental cathodes. This result is likely related to TiSix phases of higher cohesive energies in the compound cathodes and higher effective electron temperature in plasma formation. The ion energy distributions extended up to ∼200 and ∼130 eV for Ti and Si, respectively, with corresponding average energies of ∼60 and ∼30 eV. These averages were, however, not dependent on Si content in the cathode, except for 25 at. % Si where the average energies were increased up to 72 eV for Ti and 47 eV for Si.

• 23.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Ti-Si-C-N Thin Films Grown by Reactive Arc Evaporation from Ti3SiC2 Cathodes2011In: Journal of Materials Research, ISSN 0884-2914, E-ISSN 2044-5326, Vol. 26, p. 874-881Article in journal (Refereed)

Ti-Si-C-N thin films were deposited onto WC-Co substrates by industrial scale arc evaporation from Ti3SiC2 compound cathodes in N2 gas. Microstructure and hardness were found to be highly dependent on the wide range of film compositions attained, comprising up to 12 at.% Si and 16 at.% C. Nonreactive deposition yielded films consisting of understoichiometric TiCx, Ti and silicide phases with high (27 GPa) hardness. At a nitrogen pressure of 0.25-0.5 Pa, below that required for N saturation, superhard, 45-50 GPa, (Ti,Si)(C,N) films with a nanocrystalline feathered structure were formed. Films grown above 2 Pa displayed crystalline phases of more pronounced nitride character, but with C and Si segregated to grain boundaries to form weak grain boundary phases. In abundance of N, the combined presence of Si and C disturb cubic phase growth severely and compromises the mechanical strength of the films.

• 24.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Layer Formation by Resputtering in Ti-Si-C Hard Coatings during Large Scale Cathodic Arc Deposition2011In: Surface & Coatings Technology, ISSN 0257-8972, E-ISSN 1879-3347, Vol. 205, no 15, p. 3923-3930Article in journal (Refereed)

This paper presents the physical mechanism behind the phenomenon of self-layering in thin films made by industrial scale cathodic arc deposition systems using compound cathodes and rotating substrate fixture. For Ti-Si-C films, electron microscopy and energy dispersive x-ray spectrometry reveals a trapezoid modulation in Si content in the substrate normal direction, with a period of 4 to 23 nm dependent on cathode configuration. This is caused by preferential resputtering of Si by the energetic deposition flux incident at high incidence angles when the substrates are facing away from the cathodes. The Ti-rich sub-layers exhibit TiC grains with size up to 5 nm, while layers with high Si-content are less crystalline. The nanoindentation hardness of the films increases with decreasing layer thickness.

• 25.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Seco Tools AB, SE-737 82 Fagersta, Sweden. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Thermal stability and mechanical properties of amorphous arc evaporated Ti-B-Si-N and Ti-B-Si-Al-N coatings grown by cathodic arc evaporation from TiB2, Ti33Al67, and Ti85Si15 cathodes2014In: Journal of Vacuum Science & Technology. A. Vacuum, Surfaces, and Films, ISSN 0734-2101, E-ISSN 1520-8559, Vol. 32, no 6, p. 061508-Article in journal (Refereed)

Ti-B-Al-N, Ti-B-Si-N, and Ti-B-Si-Al-N coatings were grown on cemented carbide substrates in an industrial scale cathodic arc evaporation system using Ti33Al67, Ti85Si15, and TiB2 cathodes in a reactiveN2 atmosphere. The microstructure of the as-deposited coatings changes from nanocrystalline to amorphous with addition of (B+Si+Al), or high amounts of (B+Si) to TiN. In the as-deposited state, the 4 μm-thick amorphous coatings are dense and homogenous, besides slight compositional modulation with Ti-rich layers induced by rotation of the substrate holder fixture during deposition, and have unusually few macroparticles. Annealing at temperatures ranging from 700 °C to 1100 °C results in that the coatings crystallize by clustering of TiN grains. The hardness of as-deposited amorphous coatings is 17-18 GPa, and increases to 21 GPa following annealing at 800 °C. At annealing temperatures of 1000 °C and above the hardness decreases due to inter-diffusion of Co from the substrate to the coating.

• 26.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Reactive DC magnetron sputtering of amorphous (Ti0.25B0.75)1−xSixNy thin films from TiB2 and Si targets2014Manuscript (preprint) (Other academic)

(Ti0.25B0.75)1−xSixNy, 0≤x≤0.89, 0.9≤y≤1.25, thin films were reactively grown on Si(001) substrates by dc magnetron sputtering from compound TiB2 and elemental Si targets. The films can be grown in a fully electron-diffraction amorphous state with x>0.46, as evidenced by XRD and HR-TEM investigations. With x=0, BN form onion-like sheets surrounding TiNnanograins. Substrate temperatures, Ts=100-600 ◦C, has a minor effect of the film structure and properties, due to limited surface diffusion.

Ion-assisted growth with substrate bias voltages, Vb, between -50 V and -200 V, favors densification of amorphous structures over nanocrystalline formation, and improves mechanical properties. A maximum hardness value of 26.8±0.7 GPa is found for an amorphous (Ti0.25B0.75)0.39Si0.61N1.15 film grown with substrate temperature Ts=400 °C and substrate bias voltage Vb=-100 V.

• 27.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Growth and properties of amorphous Ti-B-Si-N thin films deposited by hybrid HIPIMS/DC-magnetron co-sputtering from TiB2 and Si targets2014In: Surface & Coatings Technology, ISSN 0257-8972, E-ISSN 1879-3347, Vol. 259, p. 442-447Article in journal (Refereed)

Amorphous nitrides are explored for their homogenous structure and potential use as wear-resistant coatings, beyond their much studied nano-and microcrystalline counterparts. (TiB2)1−xSixNy thin films were deposited on Si(001) substrates by a hybrid technique of high power impulse magnetron sputtering (HIPIMS) combined with dc magnetron sputtering (DCMS) using TiB2 and Si targets in a N2/Ar atmosphere. By varying the sputtering dc power to the Si target from 200 to 2000 W while keeping the average power to the TiB2-target, operated in HIPIMS mode, constant at 4000 W, the Si content in the films increased gradually from x=0.01 to x=0.43. The influence of the Si content on the microstructure, phase constituents, and mechanical properties were systematically investigated. The results show that the microstructure of as-deposited (TiB2)1−xSixNy films changes from nanocrystalline with 2-4 nm TiN grains for x=0.01 to fully electron diffraction amorphous for x=0.22. With increasing Si content, the hardness of the films increases from 8.5 GPa with x=0.01 to 17.2 GPa with x=0.43.

• 28.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Hf-Al-Si-N multilayers deposited by reactive magnetron sputtering from a single Hf0.6Al0.2Si0.2 target using high-flux, low-energy modulated substrate bias: film growth and properties2014Manuscript (preprint) (Other academic)

Hf1−x−yAlxSiyN (0≤x≤0.14, 0≤y≤0.13) single layers and multilayer films are grown on Si(001) at a substrate temperature Ts=250 °C using ultrahigh vacuum magnetically-unbalanced reactive magnetron sputtering from a single Hf0.6Al0.2Si0.2 target in a 5%-N2/Ar atmosphere at a total pressure of 20 mTorr (2.67 Pa). The composition and nanostructure of Hf1−x−yAlxSiyN is controlled during growth by varying the ion energy (Ei) of the ions incident at the film surface, keeping the ion-to-metal flux ratio (Ji/JMe) constant at 8. By sequentially switching Ei between 10 and 40 eV, Hf0.77Al0.10Si0.13N/Hf0.78Al0.14Si0.08N multilayers with bilayer periods Λ = 2-20 nm are grown, in which the Si2p bonding state changes from predominantly Si-Si bonds for films grown at Ei = 10 eV, to mainly Si-N bonds at Ei = 40 eV. Multilayer hardness values increase monotonically from 20 GPa with Λ = 20 nm to 27 GPa with Λ = 2 nm, while multilayer fracture toughness increases with increasing Λ. Multilayers with Λ = 10 nm have the optimized property combination of being bothrelatively hard, H∼24 GPa, and fracture tough.

• 29.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
Novel hard, tough HfAlSiN multilayers, defined by alternating Si bond structure, deposited using modulated high-flux, low-energy ion irradiation of the growing film2015In: Journal of Vacuum Science & Technology. A. Vacuum, Surfaces, and Films, ISSN 0734-2101, E-ISSN 1520-8559, Vol. 33, no 5, p. 05E103-1-05E103-9Article in journal (Refereed)

Hf1-x-yAlxSiyN (0 less than= x less than= 0.14, 0 less than= y less than= 0.12) single layer and multilayer films are grown on Si(001) at 250 degrees C using ultrahigh vacuum magnetically unbalanced reactive magnetron sputtering from a single Hf0.6Al0.2Si0.2 target in mixed 5%-N-2/Ar atmospheres at a total pressure of 20 mTorr (2.67 Pa). The composition and nanostructure of Hf1-x-yAlxSiyN films are controlled by varying the energy Ei of the ions incident at the film growth surface while maintaining the ion-to-metal flux ratio constant at eight. Switching E-i between 10 and 40 eV allows the growth of Hf0.78Al0.10Si0.12N/Hf0.78Al0.14Si0.08N multilayers with similar layer compositions, but in which the Si bonding state changes from predominantly Si-Si/Si-Hf for films grown with E-i = 10 eV, to primarily Si-N with E-i = 40 eV. Multilayer hardness values, which vary inversely with bilayer period Lambda, range from 20 GPa with Lambda = 20 nm to 27 GPa with Lambda = 2 nm, while fracture toughness increases directly with Lambda. Multilayers with Lambda = 10nm combine relatively high hardness, H similar to 24GPa, with good fracture toughness. (C) 2015 American Vacuum Society.

• 30.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Phys Elect USA, USA . Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Phase stability and initial low-temperature oxidation mechanism of Ti2AlC thin films2013In: Journal of the European Ceramic Society, ISSN 0955-2219, E-ISSN 1873-619X, Vol. 33, no 2, p. 375-382Article in journal (Refereed)

Ti2AlC thin films deposited onto Al2O3 by magnetron sputtering were used as model for studying the early stages (andlt; 15 min) of relatively low-temperature (500 degrees C) oxidation of Ti2AlC. The well-defined microstructure of these films forms a surface of valleys, hillocks and plateaus comprised of basal-plane-oriented grains with a fraction of nonbasal-plane-oriented grains with out-of-plane orientation of (1 0 (1) over bar 3) and (1 0 (1) over bar 6) as shown by X-ray diffraction and s electron microscopy. During oxidation, Al2O3 clusters and areas of C-containing titania (TiOxCy) are formed on the surface. A mechanism is proposed in which the locations of the Al2O3 clusters are related to the migration of Al atoms diffusing out of Ti2AlC. The Al2O3 is initially formed in valleys or on plateaus where Al atoms have been trapped while TiOxCy forms by in-diffusion of oxygen into the Al-deficient Ti2AlC. At 500 degrees C, the migration of Al atoms is faster than the oxidation kinetics; explaining this microstructure-dependent oxidation mechanism.

• 31.
Linköping University, Department of Physics, Chemistry and Biology, Nanostructured Materials. Linköping University, The Institute of Technology.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. University of Illinois, IL 61801 USA; University of Illinois, IL 61801 USA. FEI Co, Netherlands. FEI Co, Netherlands. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. University of Illinois, IL 61801 USA; University of Illinois, IL 61801 USA. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Nanostructured Materials. Linköping University, The Institute of Technology.
Self-organized anisotropic (Zr1-xSix)N-y nanocomposites grown by reactive sputter deposition2015In: Acta Materialia, ISSN 1359-6454, E-ISSN 1873-2453, Vol. 82, p. 179-189Article in journal (Refereed)

The physical properties of hard and superhard nanocomposite thin films are strongly dependent on their nanostructure. Here, we present the results of an investigation of nanostructural evolution and the resulting mechanical properties of (Zr1-xSix)N-y films, with 0 less than= x less than= 1 and 1 less than= y less than= 1.27, grown on MgO(0 0 1) and Al2O3(0 0 0 1) substrates at temperatures T-s = 500-900 degrees C by reactive magnetron sputter deposition from Zr and Si targets. X-ray diffraction and transmission electron microscopy (TEM) results show that there is a T-s/composition window in which stoichiometric Zr-Si-N and amorphous a-Si3N4 phases mutually segregate and self-organize into encapsulated 3-5 um wide ZrN-rich (Zr1-xSix)N columns which extend along the growth direction with a strong (002) texture. Lattice-resolved scanning TEM and energy-dispersive X-ray spectroscopy reveal that the (Zr1-xSix)N-y nanocolumns are separated by a bilayer tissue phase consisting of a thin crystalline SiNy-rich (Zr1-xSix)N-y layer with an a-Si3N4 overlayer. Incorporation of metastable SiN into NaCl-structure ZrN leads to an enhanced nanoindentation hardness H which is a function of T-s and film composition. For nanocomposites with composition (Zr(0.8)Sio(0.2))N-1.14 (10 at.% Si) H, increases from 26 GPa at 500 degrees C to 37 GPa at 900 degrees C. For comparison, the hardness of epitaxial ZrN/MgO(0 0 1) layers grown at T-s = 800 degrees C is 24 GPa. (C) 2014 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

• 32.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Sandvik Tooling RTC. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Microstructure control of CrNx films during high power impulse magnetron sputtering2010In: SURFACE and COATINGS TECHNOLOGY, ISSN 0257-8972, Vol. 205, no 1, p. 118-130Article in journal (Refereed)

The microstructure and composition of CrNx (0 andlt;= x andlt;= 1) films grown by reactive high power pulsed magnetron sputtering (HIPIMS or HPPMS) have been studied as a function of the process parameters: N-2-to-Ar discharge gas ratio, (f(N2/Ar)), negative substrate bias (V-s), pulsing frequency, and energy per pulse. The film stoichiometry is found to be determined by the composition of the material flux incident upon the substrate during the active phase of the discharge with no nitrogen uptake between the high power pulses. Scanning electron microscopy investigations reveal that for 0andlt;f(N2/Ar)andlt;0.15 and 150 V bias, a columnar film growth is suppressed in favor of nano-sized grain structure. The phenomenon is ascribed to the high flux of doubly charged Cr ions and appears to be a unique feature of HIPIMS. The microstructure of column-less films for 100 V andlt;= V-s andlt;= 150 V is dominated by the CrN and hexagonal beta-Cr2N phases and shows a high sensitivity to V-s. As the amplitude of V, decreases to 40 V and self-biased condition, the film morphology evolves to a dense columnar structure. This is accompanied by an increase in the average surface roughness from 0.25 nm to 2.4 nm. CrNx samples grown at f(N2/Ar)andgt;= 0.3 are columnar and show high compressive stress levels ranging from -7.1 GPa at f(N2/Ar)=0.3 to -9.6 GPa at f(N2/Ar)=1. The power-normalized deposition rate decreases with increasing pulse energy, independent of f(N2/Ar). This effect is found to be closely related to the increased ion content in the plasma as determined by optical emission spectroscopy. The HIPIMS deposition rate normalized to DC rate decreases linearly with increasing relative ion content in the plasma, independent of f(N2/Ar) and pulsing frequency, in agreement with the so-called target-pathways model. Increasing frequency leads to a finer grain structure and a partial suppression of the columnar growth, which is attributed to the corresponding increase of the time-averaged mean energy of film-forming ions arriving at the substrate.

• 33.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
X-ray photoelectron spectroscopy analyses of the electronic structure of polycrystalline Ti1-xAlxN thin films with 0 < x < 0.962014In: Surface Science Spectra, ISSN 1055-5269, E-ISSN 1520-8575, Vol. 21, p. 35-49Article in journal (Refereed)

Metastable Ti1-xAlxN (0 <  x <  0.96) alloy thin films are grown by reactive magnetron sputter deposition using a combination of high-power pulsed magnetron (HIPIMS) and dc magnetron sputtering (DCMS). Layers are deposited from elemental Ti and Al targets onto Si(001) substrates at 500 °C. All Ti1 xAlxN film surfaces are analyzed by x-ray photoelectron spectroscopy (XPS) employing monochromatic Al Ka radiation (hn = 1486.6 eV). Prior to spectra acquisition, TiAlN surfaces are sputter-cleaned in-situ with 4 keV Ar+ ions incident at an angle of 70° with respect to the surface normal. XPS results reveal satellite structures on the high binding energy side of the Ti2p, Ti3s, and Ti3p core-level signals. The intensities of the primary Ti features (Ti2p, Ti3s, and Ti3p) decrease with increasing AlN concentration such that the satellite peaks dominate spectra from films with x < 0.67. The density-of-states at the Fermi level also decrease with increasing x indicating that the satellite peaks are due to screening of core holes created by the photoionization event. Film compositions, obtained using XPS sensitivity factors, agree to within ±3% with values determined by time-of-flight elastic recoil detection analyses.

• 34.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
CrNx Films Prepared by DC Magnetron Sputtering and High-Power Pulsed Magnetron Sputtering: A Comparative Study2010In: IEEE TRANSACTIONS ON PLASMA SCIENCE, ISSN 0093-3813, Vol. 38, no 11, p. 3046-3056Article in journal (Refereed)

CrNx (0 andlt;= x andlt;= 0.91) films synthesized using high-power pulsed magnetron sputtering, also known as high-power impulse magnetron sputtering (HiPIMS), have been compared with those made by conventional direct-current (dc) magnetron sputtering (DCMS) operated at the same average power. The HiPIMS deposition rate relative to the DCMS rate was found to decrease linearly with increasing emission strength from the Cr ions relative to Cr neutrals, in agreement with the predictions of the target-pathway model. The low deposition rate in HiPIMS is thus a direct consequence of the high ionization level (similar to 56%) of the target material and effective capturing of Cr ions by the cathode potential. Although the HiPIMS deposition rate did not exceed 40% of the DCMS rate, the drop in the relative deposition rate upon increasing the N-2-to-Ar flow ratio, f(N2/Ar), was found to be similar for both sputtering techniques. Films prepared by HiPIMS contained similar amounts of atomic nitrogen as the dc-sputtered samples grown at the same f(N2/Ar), indicating that the nitride formation at the substrate takes place mostly during the time period of the high-power pulses, and the N-2 uptake between the pulses is negligible. The microstructure evolution in the two types of CrNx films, however, differed clearly from each other. A combination of a high substrate bias and a high flux of doubly charged Cr ions present during the HiPIMS discharge led to a disruption of the grain growth and renucleation, which resulted in column-free films with nanosized grains not observed in the conventional DCMS-based process. The comparison of nanoindentation hardness as a function of f(N2/Ar) revealed superior properties of HiPIMS-sputtered films in the entire range of gas compositions.

• 35.
Linköping University, Department of Physics, Chemistry and Biology. Linköping University, The Institute of Technology.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Mitigating the geometrical limitations of conventional sputtering by controlling the ion-to-neutral ratio during high power pulsed magnetron sputtering2011In: Thin Solid Films, ISSN 0040-6090, E-ISSN 1879-2731, Vol. 519, no 19, p. 6354-6361Article in journal (Refereed)

High power pulsed magnetron sputtering has been used to grow thin chromium layers on substrates facing and orthogonal to the target. It is demonstrated that at low peak target current density, j(T)less than0.6 A/cm(2) corresponding to a low ion-to-neutral flux ratio, films grown on substrates facing the target exhibit in-plane alignment. This is due to the rectangular shape of the target that yields an asymmetry in the off-normal flux of sputtered species. With increasing j(T) the biaxial alignment degrades, as the major portion of the incoming flux (ions) can be effectively steered by the electric field of the substrate to remove asymmetry imposed by geometrical restrictions. Eventually, at j(T)=1.7 A/cm(2) a fiber texture is obtained. For films grown on substrates orthogonal to the target, the large column tilt characteristic for growth at low j(T), decreases with increasing ion content in the flux and almost disappears at the highest value of j(T). The latter indicates that material flux to the substrate is highly ionized so that deposition takes place along substrate normal despite the high nominal inclination angle. Thus, in the limit of high j(T) the artifacts of conventional physical vapor deposition, resulting from the line-of-sight deposition, are effectively eliminated and the film growth proceeds more or less unaffected by the substrate orientation. Samples mounted orthogonally thus possess a similar texture, morphology, and topography as those facing the target.

• 36.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. CemeCon AG, Germany. CemeCon AG, Germany. CemeCon AG, Germany. CemeCon AG, Germany. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. University of Illinois, IL 61801 USA; University of Illinois, IL 61801 USA. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
A review of metal-ion-flux-controlled growth of metastable TiAlN by HIPIMS/DCMS co-sputtering2014In: Surface & Coatings Technology, ISSN 0257-8972, E-ISSN 1879-3347, Vol. 257, p. 15-25Article in journal (Refereed)

We review results on the growth of metastable Ti1-xAlxN alloy films by hybrid high-power pulsed and dc magnetron co-sputtering (HIPIMS/DCMS) using the time domain to apply substrate bias either in synchronous with the entire HIPIMS pulse or just the metal-rich portion of the pulse in mixed Ar/N-2 discharges. Depending upon which elemental target, Ti or Al, is powered by HIPIMS, distinctly different film-growth kinetic pathways are observed due to charge and mass differences in the metal-ion fluxes incident at the growth surface. Al+ ion irradiation during Al-HIPIMS/Ti-DCMS at 500 degrees C, with a negative substrate bias V-s = 60 V synchronized to the HIPIMS pulse (thus suppressing Ar+ ion irradiation due to DCMS), leads to single-phase NaCl-structure Ti1-xAlxN films (x less than= 0.60) with high hardness (greater than30 GPa with x greater than 0.55) and low stress (0.2-0.8 GPa compressive). Ar+ ion bombardment can be further suppressed in favor of predominantly Al+ ion irradiation by synchronizing the substrate bias to only the metal-ion-rich portion of the Al-HIPIMS pulse. In distinct contrast Ti-HIPIMS/Al-DCMSTi1-xAlxN layers grown with Ti+/Ti2+ metal ion irradiation and the same HIPIMS-synchronized V-s value, are two-phase mixtures, NaCl-structure Ti1-xAlxN plus wurtzite AlN, exhibiting low hardness (similar or equal to 18 GPa) with high compressive stresses, up to -3.5 GPa. In both cases, film properties are controlled by the average metal-ion momentum per deposited atom less thanp(d)greater than transferred to the film surface. During Ti-HIPIMS, the growing film is subjected to an intense flux of doubly-ionized Ti2+, while Al2+ irradiation is insignificant during Al-HIPIMS. This asymmetry is decisive since the critical less thanp(d)greater than limit for precipitation of w-AlN, 135 [eV-amu](1/2), is easily exceeded during Ti-HIPIMS, even with no intentional bias. The high Ti2+ ion flux is primarily due to the second ionization potential (IP2) of Ti being lower than the first IP (IP1) of Ar. New results involving the HIPIMS growth of metastable Ti1-xAlxN alloy films from segmented TiAl targets are consistent with the above conclusions.

• 37.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. CemeCon AG, Germany . CemeCon AG, Germany . CemeCon AG, Germany . CemeCon AG, Germany . Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Strain-free, single-phase metastable Ti0.38Al0.62N alloys with high hardness: metal-ion energy vs. momentum effects during film growth by hybrid high-power pulsed/dc magnetron cosputtering2014In: Thin Solid Films, ISSN 0040-6090, E-ISSN 1879-2731, Vol. 556, p. 87-98Article in journal (Refereed)

A hybrid deposition process consisting of reactive high-power pulsed and dc magnetron cosputtering (HIPIMS and DCMS) from Ti and Al targets is used to grow Ti1-xAlxN alloys, with x similar to 0.6, on Si(001) at 500 degrees C. Two series of films are deposited in which the energy and momentum of metal ions incident at the growing film are individually varied. In both sets of experiments, a negative bias V-s ranging from 20 to 280 V is applied to the substrate in synchronous, as determined by in-situ mass spectrometry, with the metal-ion-rich part of the HIPIMS pulse. Ion momentum is varied by switching the HIPIMS and dc power supplies to change the mass m and average charge of the primary metal ion. Al-HIPIMS/Ti-DCMS layers grown under Al+ (m(Al) = 26.98 amu) bombardment with 20 less than= V-s less than= 160 V are single-phase NaCl-structure alloys, while films deposited with V-s greater than 160 V are two-phase, cubic plus wurtzite. The corresponding critical average metal-ion momentum transfer per deposited atom for phase separation is less than p(d)*greater than greater than= 135 [eV-amu](1/2). In distinct contrast, layers deposited in the Ti-HIPIMS/Al-DCMS configuration with Ti+/Ti2+ (m(Ti) = 47.88 amu) ion irradiation are two-phase even with the lowest bias, V-s = 20 V, for which less than p(d)*greater than greater than 135 [eV-amu](1/2). Precipitation of wurtzite-structure AlN is primarily determined by the average metal-ion momentum transfer to the growing film, rather than by the deposited metal-ion energy. Ti-HIPIMS/Al-DCMS layers grown with V-s= 20 V are two-phase with compressive stress sigma= -2 GPa which increases to -6.2 GPa at V-s= 120 V; hardness H values range from 17.5 to 27 GPa and are directly correlated with sigma. However, for Al-HIPIMS/Ti-DCMS, the relatively low mass and single charge of the Al+ ion permits tuning properties of metastable cubic Ti0.38Al0.62 N by adjusting V-s to vary, for example, the hardness from 12 to 31 GPa while maintaining sigma similar to 0.

• 38.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. CemeCon AG, Germany . CemeCon AG, Germany . CemeCon AG, Germany . CemeCon AG, Germany . Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Metal versus rare-gas ion irradiation during Ti1-xAlxN film growth by hybrid high power pulsed magnetron/dc magnetron co-sputtering using synchronized pulsed substrate bias2012In: Journal of Vacuum Science & Technology. A. Vacuum, Surfaces, and Films, ISSN 0734-2101, E-ISSN 1520-8559, Vol. 30, no 6Article in journal (Refereed)

Metastable NaCl-structure Ti1-xAlxN is employed as a model system to probe the effects of metal versus rare-gas ion irradiation during film growth using reactive high-power pulsed magnetron sputtering (HIPIMS) of Al and dc magnetron sputtering of Ti. The alloy film composition is chosen to be x = 0.61, near the kinetic solubility limit at the growth temperature of 500 degrees C. Three sets of experiments are carried out: a -60V substrate bias is applied either continuously, in synchronous with the full HIPIMS pulse, or in synchronous only with the metal-rich-plasma portion of the HIPIMS pulse. Alloy films grown under continuous dc bias exhibit a thickness-invariant small-grain, two-phase nanostructure (wurtzite AlN and cubic Ti1-xAlxN) with random orientation, due primarily to intense Ar+ irradiation leading to Ar incorporation (0.2 at. %), high compressive stress (-4.6 GPa), and material loss by resputtering. Synchronizing the bias with the full HIPIMS pulse results in films that exhibit much lower stress levels (-1.8GPa) with no measureable Ar incorporation, larger grains elongated in the growth direction, a very small volume fraction of wurtzite AlN, and random orientation. By synchronizing the bias with the metal-plasma phase of the HIPIMS pulses, energetic Ar+ ion bombardment is greatly reduced in favor of irradiation predominantly by Al+ ions. The resulting films are single phase with a dense competitive columnar structure, strong 111 orientation, no measureable trapped Ar concentration, and even lower stress (-0.9 GPa). Thus, switching from Ar+ to Al+ bombardment, while maintaining the same integrated incident ion/metal ratio, eliminates phase separation, minimizes renucleation during growth, and reduces the high concentration of residual point defects, which give rise to compressive stress.

• 39.
Linköping University, Department of Physics, Chemistry and Biology. Linköping University, The Institute of Technology.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Seco Tools AB. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Selection of metal ion irradiation for controlling Ti1-xAlxN alloy growth via hybrid HIPIMS/magnetron co-sputtering2012In: Vacuum, ISSN 0042-207X, E-ISSN 1879-2715, Vol. 86, no 8, p. 1036-1040Article in journal (Refereed)

We demonstrate, for the first time, the growth of metastable single-phase NaCl-structure high-AlN-content Ti1-xAlxN alloys (x andlt;= 0.64) which simultaneously possess high hardness and low residual stress. The films are grown using a hybrid approach combining high-power pulsed magnetron (HPPMS/HIPIMS) and dc magnetron sputtering of opposing metal targets. With HIPIMS applied to the Al target, Aln+ ion irradiation (dominated by Aln+) of the growing film results in alloys 0.55 andlt;= x andlt;= 0.60 which exhibit hardness H similar to 30 GPa and low stress sigma = 0.2-0.7 GPa, tensile. In sharp contrast, films with corresponding AlN concentrations grown with HIPIMS applied to the Ti target, giving rise to Tin+ ion irradiation (with a significant Ti2+ component), are two-phase - cubic (Ti,Al)N and hexagonal AlN - with low hardness, H = 18-19 GPa, and high compressive stress ranging up to 2.7 GPa. Annealing alloys grown with HIPIMS applied to the Al target results in age hardening due to spinodal decomposition; the hardness of Ti0.41Al0.59N increases from 30 to 33 GPa following a 900 degrees C anneal.

• 40.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Sweden Seco Tools AB, Sweden . Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Role of Tin+ and Aln+ ion irradiation (n=1, 2) during Ti1-xAlxN alloy film growth in a hybrid HIPIMS/magnetron mode2012In: Surface & Coatings Technology, ISSN 0257-8972, E-ISSN 1879-3347, Vol. 206, no 19-20, p. 4202-4211Article in journal (Refereed)

Metastable Ti1-xAlxN (0.4 less than= x less than= 0.76) films are grown using a hybrid approach in which high-power pulsed magnetron sputtering (HIPIMS) is combined with dc magnetron sputtering (DCMS). Elemental Al and Ti metal targets are co-sputtered with one operated in HIPIMS mode and the other target in DCMS; the positions of the targets are then switched for the next set of experiments. In both cases, the AlN concentration in the co-sputtered films, deposited at T-s = 500 degrees C with R = 1.5-5.3 angstrom/s, is controlled by adjusting the average DCMS target power. Resulting films are analyzed by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, atomic force microscopy, elastic recoil detection analysis, and nanoindentation. Mass spectroscopy is used to determine ion energy distribution functions at the substrate. The distinctly different flux distributions obtained from targets driven in HIPIMS vs. DCMS modes allow the effects of Aln+ and Tin+ (n = 1, 2) ion irradiation on film growth kinetics, and resulting properties, to be investigated separately. Bombardment with Aln+ ions (primarily Al+ in the Al-HIPIMS/Ti-DCMS configuration) during film growth leads to NaCl-structure Ti1-xAlxN (0.53 less than= x less than= 0.60) films which exhibit high hardness (greater than30 GPa) with low stress (0.2-0.7 GPa tensile). In contrast, films with corresponding AlN concentrations grown under Tin+ metal ion irradiation (with a significant Ti2+ component) in the Ti-HIPIMS/Al-DCMS mode have much lower hardness, 18-19 GPa, and high compressive stress ranging up to 2.7 GPa. The surprisingly large variation in mechanical properties results from the fact that the kinetic AlN solubility limit x(max) in Ti1-xAlxN depends strongly on, in addition to T-s and R, the target power configuration during growth and hence the composition of the ion flux. AlN with x(max)similar to 64 mol% can be accommodated in the NaCl structure under Aln+ ion flux, compared with similar to 40 mol% for growth with Tin+ flux. The strong asymmetry in film growth reaction paths is due primarily to the fact that the doubly-ionized metal ion flux is approximately two orders of magnitude higher from the Ti target, than from Al, powered with HIPIMS. This asymmetry becomes decisive upon application of a moderate substrate bias voltage, -60 V, applied synchronously with HIPIMS pulses, during growth.

• 41.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
Control of Ti1-xSixN nanostructure via tunable metal-ion momentum transfer during HIPIMS/DCMS co-deposition2015In: Surface & Coatings Technology, ISSN 0257-8972, E-ISSN 1879-3347, Vol. 280, p. 174-184Article in journal (Refereed)

• 42.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Room-temperature heteroepitaxy of single-phase Al1-xInxN films with full composition range on isostructural wurtzite templates2012In: Thin Solid Films, ISSN 0040-6090, E-ISSN 1879-2731, Vol. 524, p. 113-120Article in journal (Refereed)

Al1-xInxN heteroepitaxial layers covering the full composition range have been realized by magnetron sputter epitaxy on basal-plane AlN, GaN, and ZnO templates at room temperature (RT). Both Al1-xInxN single layers and multilayers grown on these isostructural templates show single phase, single crystal wurtzite structure. Even at large lattice mismatch between the film and the template, for instance InN/AlN (similar to 13% mismatch), heteroepitaxy is achieved. However, RT-grown Al1-xInxN films directly deposited on non-isostructural c-plane sapphire substrate exhibit a polycrystalline structure for all compositions, suggesting that substrate surface structure is important for guiding the initial nucleation. Degradation of Al1-xInxN structural quality with increasing indium content is attributed to the formation of more point-and structural defects. The defects result in a prominent hydrostatic tensile stress component, in addition to the biaxial stress component introduced by lattice mismatch, in all RT-grown Al1-xInxN films. These effects are reflected in the measured in-plane and out-of-plane strains. The effect of hydrostatic stress is negligible compared to the effects of lattice mismatch in high-temperature grown AlN layers thanks to their low amount of defects. We found that Vegards rule is applicable to determine x in the RT-grown Al1-xInxN epilayers if the lattice constants of RT-sputtered AlN and InN films are used instead of those of the strain-free bulk materials.

• 43.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
IHI Ionbond AG, Industriestraße 211, Olten CH-4600, Switzerland. Linköping University, Department of Physics, Chemistry and Biology, Semiconductor Materials. Linköping University, Faculty of Science & Engineering. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
Silicon carbonitride thin films deposited by reactive high power impulse magnetron sputtering2018In: Surface & Coatings Technology, ISSN 0257-8972, E-ISSN 1879-3347, Vol. 335, p. 248-256Article in journal (Refereed)

Amorphous silicon carbonitride thin films for biomedical applications were deposited in an industrial coating unit from a silicon target in different argon/nitrogen/acetylene mixtures by reactive high power impulse magnetron sputtering (rHiPIMS). The effects of acetylene (C2H2) flow rate, substrate temperature, substrate bias voltage, and HiPIMS pulse frequency on the film properties were investigated. Low C2H2 flow rates (<10 sccm) resulted in silicon nitride-like film properties, seen from a dense morphology when viewed in cross-sectional scanning electron microscopy, a hardness up to ∼22 GPa as measured by nanoindentation, and Si-N bonds dominating over Si-C bonds in X-ray photoelectron spectroscopy core-level spectra. Higher C2H2 flows resulted in increasingly amorphous carbon-like film properties, with a granular appearance of the film morphology, mass densities below 2 g/cm3 as measured by X-ray reflectivity, and a hardness down to 4.5 GPa. Increasing substrate temperatures and bias voltages resulted in slightly higher film hardnesses and higher compressive residual stresses. The film H/E ratio showed a maximum at film carbon contents ranging between 15 and 30 at.% and at elevated substrate temperatures from 340 °C to 520 °C.

• 44.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
Silicon oxynitride films deposited by reactive high power impulse magnetron sputtering using nitrous oxide as a single-source precursor2015In: Journal of Vacuum Science & Technology. A. Vacuum, Surfaces, and Films, ISSN 0734-2101, E-ISSN 1520-8559, Vol. 33, no 5, p. 05E121-Article in journal (Refereed)

Silicon oxynitride thin films were synthesized by reactive high power impulse magnetron sputtering of silicon in argon/nitrous oxide plasmas. Nitrous oxide was employed as a single-source precursor supplying oxygen and nitrogen for the film growth. The films were characterized by elastic recoil detection analysis, x-ray photoelectron spectroscopy, x-ray diffraction, x-ray reflectivity, scanning electron microscopy, and spectroscopic ellipsometry. Results show that the films are silicon rich, amorphous, and exhibit a random chemical bonding structure. The optical properties with the refractive index and the extinction coefficient correlate with the film elemental composition, showing decreasing values with increasing film oxygen and nitrogen content. The total percentage of oxygen and nitrogen in the films is controlled by adjusting the gas flow ratio in the deposition processes. Furthermore, it is shown that the film oxygen-to-nitrogen ratio can be tailored by the high power impulse magnetron sputtering-specific parameters pulse frequency and energy per pulse. (C) 2015 Author(s). All article content, except where otherwise noted, is licensed under a Creative Commons Attribution 3.0 Unported License.

• 45.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
Stoichiometric silicon oxynitride thin films reactively sputtered in Ar/N2O plasmas by HiPIMS2016In: Journal of Physics D: Applied Physics, ISSN 0022-3727, E-ISSN 1361-6463, Vol. 49, no 13, article id 135309Article in journal (Refereed)

Silicon oxynitride (SiOxNy, x = 0.2 − 1.3, y = 0.2 − 0.7) thin films were synthesized by reactive high power impulse magnetron sputtering from a pure silicon target in Ar/N2O atmospheres. It is found that the composition of the material can be controlled by the reactive gas flow and the average target power. X-ray photoelectron spectroscopy (XPS) shows that high average powers result in more silicon-rich films, while lower target powers yield silicon-oxide-like material due to more pronounced target poisoning. The amount of nitrogen in the films can be controlled by the percentage of nitrous oxide in the working gas. The nitrogen content remains at a constant level while the target is operated in the transition region between metallic and poisoned target surface conditions. The extent of target poisoning is gauged by the changes in peak target current under the different deposition conditions. XPS also shows that varying concentrations and ratios of oxygen and nitrogen in the films result in film chemical bonding structures ranging from silicon-rich to stoichiometric silicon oxynitrides having no observable Si−Si bond contributions. Spectroscopic ellipsometry shows that the film optical properties depend on the amount and ratio of oxygen and nitrogen in the compound, with film refractive indices measured at 633 nm ranging between those of SiO2 and Si3N4.

• 46.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Reactive sputtering of delta-ZrH2 thin films by high power impulse magnetron sputtering and direct current magnetron sputtering2014In: Journal of Vacuum Science & Technology. A. Vacuum, Surfaces, and Films, ISSN 0734-2101, E-ISSN 1520-8559, Vol. 32, no 4, p. 041510-Article in journal (Refereed)

Reactive sputtering by high power impulse magnetron sputtering (HiPIMS) and direct current magnetron sputtering (DCMS) of a Zr target in Ar/H-2 plasmas was employed to deposit Zr-H films on Si(100) substrates, and with H content up to 61 at.% and O contents typically below 0.2 at.% as determined by elastic recoil detection analysis. X-ray photoelectron spectroscopy reveals a chemical shift of similar to 0.7 eV to higher binding energies for the Zr-H films compared to pure Zr films, consistent with a charge transfer from Zr to H in a zirconium hydride. X-ray diffraction shows that the films are single-phase delta-ZrH2 (CaF2 type structure) at H content greater thansimilar to 55 at.% and pole figure measurements give a 111 preferred orientation for these films. Scanning electron microscopy cross-section images show a glasslike microstructure for the HiPIMS films, while the DCMS films are columnar. Nanoindentation yield hardness values of 5.5-7 GPa for the delta-ZrH2 films that is slightly harder than the similar to 5 GPa determined for Zr films and with coefficients of friction in the range of 0.12-0.18 to compare with the range of 0.4-0.6 obtained for Zr films. Wear resistance testing show that phase-pure delta-ZrH2 films deposited by HiPIMS exhibit up to 50 times lower wear rate compared to those containing a secondary Zr phase. Four-point probe measurements give resistivity values in the range of similar to 100-120 mu Omega cm for the delta-ZrH2 films, which is slightly higher compared to Zr films with values in the range 70-80 mu Omega cm.

• 47.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Impact Coatings AB, Linkoping, Sweden . Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
beta-Ta and alpha-Cr thin films deposited by high power impulse magnetron sputtering and direct current magnetron sputtering in hydrogen containing plasmas2014In: Physica. B, Condensed matter, ISSN 0921-4526, E-ISSN 1873-2135, Vol. 439, p. 3-8Article in journal (Refereed)

Thin films of beta-Ta and alpha-Cr were deposited on Si(1 0 0) and 1000 angstrom SiO2/Si(1 0 0), by high power impulse magnetron sputtering (HiPIMS) and direct current magnetron sputtering (dcMS) in hydrogen-containing plasmas. The films were characterized by X-ray photoelectron spectroscopy (XPS), X-ray diffraction, scanning electron microscopy, elastic recoil detection analysis, and four-point probe measurements. The results showed that 001-oriented beta-Ta films containing up to similar to 8 at% hydrogen were obtained with HiPIMS, albeit with no chemical shift evident in XPS. The 110 oriented alpha-Cr films display a hydrogen content less than the detection limit of 1 at%, but H-2 favors the growth of high-purity films for both metals. The beta-Ta films deposited with dcMS are columnar, which seems independent of H-2 presence in the plasma, while the films grown by HIPIMS are more fine-grained. The latter type of microstructure was present for the alpha-Cr films and found to be independent on choice of technique or hydrogen in the plasma. The beta-Ta films show a resistivity of similar to 140-180 mu Omega cm, while alpha-Cr films exhibit values around 30 mu Omega cm; the lowest values obtained for films deposited by HiPIMS and with hydrogen in the plasma for both metals.

• 48.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Effects of volume mismatch and electronic structure on the decomposition of ScAlN and TiAlN solid solutions2010In: Physical Review B. Condensed Matter and Materials Physics, ISSN 1098-0121, E-ISSN 1550-235X, Vol. 81, no 22, p. 224101-Article in journal (Refereed)

Thin solid films of metastable rocksalt structure (c-) Sc1-xAlxN and Ti1-xAlxN were employed as model systems to investigate the relative influence of volume mismatch and electronic structure driving forces for phase separation. Reactive dual magnetron sputtering was used to deposit stoichiometric Sc0.57Al0.43N(111) and Ti0.51Al0.49N(111) thin films, at 675 °C and 600 °C, respectively, followed by stepwise annealing to a maximum temperature of 1100 °C. Phase transformations during growth and annealing were followed in situ using X-ray scattering. The results show that the as-deposited Sc0.57Al0.43N films phase separate at 1000 °C – 1100 °C into non-isostructural c-ScN and wurtzite-structure (w-) AlN, via nucleation and growth at domain boundaries. Ti0.51Al0.49N, however, exhibits spinodal decomposition into isostructural coherent c-TiN and c-AlN, in the temperature interval of 800 °C – 1000 °C. X-ray pole figures show the coherency between c-ScN and w-AlN, with AlN(0001) || ScN(001) and AlN<01ɸ10> || ScN<1ɸ10>. First principles calculations of mixing energy-lattice spacing curves explain the results on a fundamental physics level and open a route for design of novel metastable pseudobinary phases for hard coatings and electronic materials.

• 49.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. European Spallat Source ESS AB, Sweden.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering. Max Planck Institute Eisenforsch GmbH, Germany. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering. Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering. European Spallat Source ESS AB, Sweden; Mid Sweden University, Sweden.
Growth and oxidization stability of cubic Zr1-xGdxN solid solution thin films2015In: Journal of Applied Physics, ISSN 0021-8979, E-ISSN 1089-7550, Vol. 117, no 19, p. 195301-Article in journal (Refereed)

We report Zr1-xGdxN thin films deposited by magnetron sputter deposition. We show a solid solubility of the highly neutron absorbing GdN into ZrN along the whole compositional range, which is in excellent agreement with our recent predictions by first-principles calculations. An oxidization study in air shows that Zr1-xGdxN with x reaching from 1 to close to 0 fully oxidizes, but that the oxidization is slowed down by an increased amount of ZrN or stopped by applying a capping layer of ZrN. The crystalline quality of Zr0.5Gd0.5N films increases with substrate temperatures increasing from 100 degrees C to 900 degrees C.

• 50.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. European Spallat Source ESS AB, Sweden . Institute Max Von Laue Paul Langevin, France . Institute Max Von Laue Paul Langevin, France . Institute Max Von Laue Paul Langevin, France . Institute Max Von Laue Paul Langevin, France . Institute Max Von Laue Paul Langevin, France . European Spallat Source ESS AB, Sweden . Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. European Spallat Source ESS AB, Sweden Institute Max Von Laue Paul Langevin, France . Institute Max Von Laue Paul Langevin, France . European Spallat Source ESS AB, Sweden European Synchrotron Radiat Facil, France . CERN, Switzerland . Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
B4C thin films for neutron detection2012In: Journal of Applied Physics, ISSN 0021-8979, E-ISSN 1089-7550, Vol. 111, no 10, p. 104908-Article in journal (Refereed)

Due to the very limited availability of He-3, new kinds of neutron detectors, not based on 3He, are urgently needed. Here, we present a method to produce thin films of (B4C)-B-10, with maximized detection efficiency, intended to be part of a new generation of large area neutron detectors. B4C thin Films have been deposited onto Al-blade and Si wafer substrates by dc magnetron sputtering from (B4C)-B-nat and (B4C)-B-10 targets in an Ar discharge, using an industrial deposition system. The films were characterized with scanning electron microscopy, elastic recoil detection analysis, x-ray reflectivity, and neutron radiography. We show that the film-substrate adhesion and film purity are improved by increased substrate temperature and deposition rate. A deposition rate of 3.8 angstrom/s and substrate temperature of 400 degrees C result in films with a density close to bulk values and good adhesion to film thickness above 3 mu m. Boron-10 contents of almost 80 at. % are obtained in 6.3 m(2) of 1 mu m thick (B4C)-B-10 thin films coated on Al-blades. Initial neutron absorption measurements agree with Monte Carlo simulations and show that the layer thickness, number of layers, neutron wavelength, and amount of impurities are determining factors. The study also shows the importance of having uniform layer thicknesses over large areas, which for a full-scale detector could be in total similar to 1000 m(2) of two-side coated Al-blades with similar to 1 mu m thick (B4C)-B-10 films.

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