| 471. |
- Högberg, Hans, et al.
(författare)
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Reactive sputtering of delta-ZrH2 thin films by high power impulse magnetron sputtering and direct current magnetron sputtering
- 2014
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Ingår i: Journal of Vacuum Science & Technology. A. Vacuum, Surfaces, and Films. - : American Institute of Physics (AIP). - 0734-2101 .- 1520-8559. ; 32:4, s. 041510-
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Tidskriftsartikel (refereegranskat)abstract
- 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.
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| 472. |
- Höglund, Carina, et al.
(författare)
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Cubic Sc1-xAlxN solid solution thin films deposited by reactive magnetron sputter epitaxy onto ScN(111)
- 2009
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Ingår i: JOURNAL OF APPLIED PHYSICS. - : AIP Publishing. - 0021-8979 .- 1089-7550. ; 105:11, s. 132862-
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Tidskriftsartikel (refereegranskat)abstract
- Reactive magnetron sputter epitaxy was used to deposit thin solid films of Sc1-xAlxN (0 andlt;= x andlt;= 1) onto MgO(111) substrates with ScN(111) seed layers. Stoichiometric films were deposited from elemental Sc and Al targets at substrate temperatures of 600 S C. The films were analyzed by Rutherford backscattering spectroscopy, elastic recoil detection analysis, x-ray diffraction, and transmission electron microscopy. Results show that rocksalt structure (c)-Sc1-xAlxN solid solutions with AlN molar fractions up to similar to 60% can be synthesized. For higher AlN contents, the system phase separates into c- and wurtzite structure (w)-Sc1-xAlxN domains. The w-domains are present in three different orientations relative to the seed layer, namely, Sc1-xAlxN(0001)parallel to ScN(111) with Sc1-xAlxN[(1) over bar2 (1) over bar0]parallel to ScN[1 (1) over bar0], Sc1-xAlxN(10 (1) over bar1)parallel to ScN(111) with Sc1-xAlxN[(1) over bar2 (1) over bar0]parallel to ScN[1 (1) over bar0], and Sc1-xAlxN(10 (1) over bar1)parallel to ScN(113). The results are compared to first-principles density functional theory calculations for the mixing enthalpies of c-, w-, and zinc blende Sc0.50Al0.50N solid solutions, yielding metastability with respect to phase separation for all temperatures below the melting points of AlN and ScN.
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| 473. |
- Höglund, Carina, et al.
(författare)
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Effects of volume mismatch and electronic structure on the decomposition of ScAlN and TiAlN solid solutions
- 2010
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Ingår i: Physical Review B. Condensed Matter and Materials Physics. - 1098-0121 .- 1550-235X. ; 81:22, s. 224101-
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Tidskriftsartikel (refereegranskat)abstract
- 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.
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| 474. |
- Höglund, Carina, 1981-
(författare)
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Growth and Phase Stability Studies of Epitaxial Sc-Al-N and Ti-Al-N Thin Films
- 2010
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Doktorsavhandling (övrigt vetenskapligt/konstnärligt)abstract
- ¨This Thesis treats the growth and characterization of ternary transition metal nitride thin films. The aim is to probe deep into the Ti-Al-N system and to explore novel Sc-Al-N compounds. Thin films were epitaxially grown by reactive dual magnetron sputtering from elemental targets onto single-crystal substrates. Ion beam analyses were used for compositional analysis and depth profiling. Different X-ray diffraction techniques were employed, ex situ using Cu radiation and in situ during deposition using synchrotron radiation, to achieve information about phases, texture, and thickness of films, and to follow roughness evolution of layers during and after growth. Transmission electron microscopy was used for overview and lattice imaging, and to obtain lattice structure information by electron diffraction.In the Sc-Al-N system, the perovskite Sc3AlN was for the first time synthesized as a thin film and in single phase, with a unit cell of 4.40 Å. The hardness was found to be 14.2 GPa, the elastic modulus 21 GPa, and the room temperature resistivity 41.2 μΩcm. Cubic solid solutions of Sc1-xAlxN can be synthesized with AlN molar fraction up to ~60%. Higher AlN contents yield three different epitaxial relations to ScN(111), namely, #1 Sc1-xAlxN(0001) || ScN(111) with Sc1-xAlxN[11210] || ScN[110], #2 Sc1-xAlxN(1011) || ScN(110) with Sc1-xAlxN[1210] || ScN[110], and #3 Sc1-xAlxN(1011) || ScN(113). An in situ deposition and annealing study of cubic Sc0.57Al0.43N films showed volume induced phase separation into ScN and wurtzite structure AlN, via nucleation and growth at the domain boundaries. The first indications for phase separation are visible at 1000 °C, and the topotaxial relationship between the binaries after phase separation is AlN(0001) || ScN(001) and AlN<01ɸ10> || ScN <1ɸ10>. This is compared with Ti1-xAlxN, for which an electronic structure driving force leads to spinodal decomposition into isostructural TiN and AlN already at 800 °C. First principles calculations explain the results on a fundamental physics level. Up to ~22% ScN can under the employed deposition conditions be dissolved into wurtzite Sc1-xAlxN films, while retaining a single-crystal structure and with lattice parameters matching calculated values.In the Ti-Al-N system, the Ti2AlN phase was synthesized epitaxially by solid state reaction during interdiffusion between sequentially deposited layers of AlN(0001) and Ti(0001). When annealing the sample, N and Al diffused into the Ti layer, forming Ti3AlN(111) at 400 ºC and Ti2AlN(0001) at 500 ºC. The Ti2AlN formation temperature is 175 ºC lower than earlier reported results. Another way of forming Ti2AlN phase is by depositing understoichiometric TiNx at 800 °C onto Al2O3(0001). An epitaxial Ti2Al(O,N) (0001) oxynitride forms close to the interface between film and substrate through a solid state reaction. Ti4AlN3 was, however, not possible to synthesize when depositing films with a Ti:Al:N ratio of 4:1:3 due to competing reactions. A substrate temperature of 600 ºC yielded an irregularly stacked Tin+1AlNn layered structure because of the low mobility of Al ad-atoms. An increased temperature led to Al deficiency due to outdiffusion of Al atoms, and formation of the Ti2AlN phase and a Ti1-xAlxN cubic solid solution.
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| 475. |
- Höglund, Carina, 1981-
(författare)
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Reactive Magnetron Sputter Deposition and Characterization of Thin Films from the Ti-Al-N and Sc-Al-N Systems
- 2009
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Licentiatavhandling (övrigt vetenskapligt/konstnärligt)abstract
- This Thesis treats the growth and characterization of ternary transition metal nitride thin films. The aim is to probe deeper into the Ti-Al-N system and to explore the novel Sc-Al-N system. Thin films were epitaxially grown by reactive magnetron sputtering from elemental targets onto single-crystal substrates covered with a seed layer. Elastic recoil detection analysis and Rutherford backscattering spectroscopy were used for compositional analysis and depth profiling. Different x-ray diffraction techniques were employed, ex situ using Cu radiation and in situ during deposition using synchrotron radiation, to identify phases, to obtain information about texture, and to determine the thickness and roughness evolution of layers during and after growth. Transmission electron microscopy was used for overview and lattice imaging, and to obtain lattice structure information by electron diffraction. Film properties were determined using van der Pauw measurements of the electrical resistivity, and nanoindentation for the materials hardness and elastic modulus. The epitaxial Mn+1AXn phase Ti2AlN was synthesized by solid-state reaction during interdiffusion between sequentially deposited layers of (0001)-oriented AlN and Ti thin films. When annealing the sample, N and Al diffused into the Ti, forming Ti3AlN at 400 ºC and Ti2AlN at 500 ºC. The Ti2AlN formation temperature is 175 ºC lower than earlier reported results. Ti4AlN3 thin films were, however, not possible to synthesize when depositing films with a Ti:Al:N ratios of 4:1:3. Substrate temperatures at 600 ºC yielded an irregularly stacked Tin+1AlNn layered structure because of the low mobility of Al adatoms. An increased temperature led, however, to an Al deficiency due to an out diffusion of Al atoms, and formation of Ti2AlN phase and Ti1-xAlxN cubic solid solution. In the Sc-Al-N system the first ternary phase was discovered, namely the perovskite Sc3AlN, with a unit cell of 4.40 Å. Its existence was supported by ab initio calculations of the enthalpy showing that Sc3AlN is thermodynamically stable with respect to the binaries. Sc3AlN thin films were experimentally found to have a hardness of 14.2 GPa, an elastic modulus of 21 GPa, and a room temperature resistivity of 41.2 μΩcm.
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| 476. |
- Höglund, Carina, 1981-, et al.
(författare)
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Sc3AlN : A New Perovskite
- 2008
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Ingår i: European Journal of Inorganic Chemistry. - : Wiley. - 1434-1948 .- 1099-1948 .- 1099-0682. ; 2008:8, s. 1193-1195
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Tidskriftsartikel (refereegranskat)abstract
- Sc3AlN with perovskite structure has been synthesized as the first ternary phase in the Sc–Al–N system. Magnetron sputter epitaxy at 650 °C was used to grow single-crystal, stoichiometric Sc3AlN(111) thin films onto MgO(111) substrates with ScN(111) seed layers as shown by elastic recoil detection analysis, X-ray diffraction, and transmission electron microscopy. The Sc3AlN phase has a lattice parameter of 4.40 Å, which is in good agreement with the theoretically predicted 4.42 Å. Comparisons of total formation energies show that Sc3AlN is thermodynamically stable with respect to all known binary compounds. Sc3AlN(111) films of 1.75 μm thickness exhibit a nanoindentation hardness of 14.2 GPa, an elastic modulus of 249 GPa, and a roomtemperature electrical resistivity of 41.2 μΩ cm.
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| 477. |
- Höglund, Carina, 1981-, et al.
(författare)
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Topotaxial growth of Ti2AlN by solid state reaction in AlN/Ti(0001) multilayer thin films
- 2007
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Ingår i: Applied Physics Letters. - : AIP Publishing. - 0003-6951 .- 1077-3118. ; 90:174106
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Tidskriftsartikel (refereegranskat)abstract
- The formation of Ti2AlN by solid state reaction between layers of wurtzite-AlN and α-Ti was characterized by in situ x-ray scattering. The sequential deposition of these layers by dual magnetron sputtering onto Al2O3(0001) at 200 °C yielded smooth, heteroepitaxial (0001) oriented films, with abrupt AlN/Ti interfaces as shown by x-ray reflectivity and Rutherford backscattering spectroscopy. Annealing at 400 °C led to AlN decomposition and diffusion of released Al and N into the Ti layers, with formation of Ti3AlN. Further annealing at 500 °C resulted in a phase transformation into Ti2AlN(0001) after only 5 min.
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| 478. |
- Höglund, Carina, et al.
(författare)
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Wurtzite-structure Sc1-xAlxN solid solution films grown by reactive magnetron sputter epitaxy : structural characterization and first-principles calculations
- 2010
-
Ingår i: Journal of Applied Physics. - : American Institute of Physics. - 0021-8979 .- 1089-7550. ; 107:12, s. 123515-
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Tidskriftsartikel (refereegranskat)abstract
- AlN(0001) was alloyed with ScN with molar fractions up to ~22%, while retaining a singlecrystal wurtzite (w-) structure and with lattice parameters matching calculated values. Material synthesis was realized by magnetron sputter epitaxy of thin films starting from optimal conditions for the formation of w-AlN onto lattice-matched w-AlN seed layers on Al2O3(0001) and MgO(111) substrates. Films with ScN contents between 23% and ~50% exhibit phase separation into nanocrystalline ScN and AlN, while ScN-rich growth conditions yield a transformation to rocksalt-structure Sc1-xAlxN(111) films. The experimental results are analyzed with ion beam analysis, X-ray diffraction, and transmission electron microscopy, together with ab-initio calculations of mixing enthalpies and lattice parameters of solid solutions in wurtzite, rocksalt, and layered hexagonal phases.
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| 479. |
- Hörling, Anders, et al.
(författare)
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Phase stability and structural properties of Ti1-zZrzN (0<z<1) thin films
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Annan publikation (övrigt vetenskapligt/konstnärligt)abstract
- Single-phase [NaCl]-structure Ti1-zZrzN thin films (0<z<1) have been deposited using cathodic arc plasma deposition. The films were investigated using X-ray diffraction, transmission electron microscopy, differential scanning calorimetry, and nanoindentation. Theoretical calculations on phase stabilities using density-functional theory revealed that the pseudo-binary TiN-ZrN system exhibits a miscibility gap, with respect to phase transformation from the as-deposited single-phase [NaCl] structure into [NaCl]-strueture TiN and ZrN components up to 980°C for z=0.35. The films were found to retain their as-deposited single-phase [NaCl] structure during post-deposition annealing for 120 min at 600, 700, 1100 and 1200°C, and for as long as 195 h at 600°C. This effective thermal stability is explained by a limited driving force for phase transformation and insufficient atom diffusivity. For two film compositions deepest within the miscibility gap, however, results from nanoindentation show an essentially retained hardness at ~30 GPa after annealing at 1100-1200°C. The principal hardening mechanism for the Ti1-zZrzN fihns is thus proposed to be solid-solution hardening through localized lattice strain fields originating from difference in atomic radius of Ti and Zr. This particular system offers interesting opportunities for fundamental studies of time-temperature-transformations of ternary nitride thin films.
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| 480. |
- Hörling, Anders, et al.
(författare)
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Phase transformations in Ti1xA1xN thin films
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Annan publikation (övrigt vetenskapligt/konstnärligt)abstract
- We report ageing phenomena in arc-deposited Ti1-xA1xN (0≤x≤0.66) thin films probed by X-ray diffraction, differential scanning calorimetry, four-point probe sheet resistance, and transmission electron microscopy measurements. Annealing Ti1-xA1xN films at 500-900°C results in residual stress recovery through annihilation of deposition-induced lattice defects, followed by spinodal decomposition at 900-1400°C into coherent nanometer-size domains of [NaCl]-TiN, and [NaCl]-AIN that eventually transform into the stable [wurtzite]-AIN phase. Kinetics measurements reveal activation energies of 2.0-2.9 eV for lattice recovery processes, and 2.9-3.5 eV for transformation processes, indicating grain boundary and defect-assisted segregation of Ti and Al. The composition was shown to have large influence on the thermal stability of Ti1-xA1xN films. The results show that the phase transformations are initiated at lower temperatures with increasing Al content.
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