| 1. |
- Bahr, A., et al.
(författare)
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Non-reactive HiPIMS deposition of NbCx thin films : Effect of the target power density on structure-mechanical properties
- 2022
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Ingår i: Surface & Coatings Technology. - : Elsevier. - 0257-8972 .- 1879-3347. ; 444
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Tidskriftsartikel (refereegranskat)abstract
- The exceptional mechanical properties of transition metal carbide coatings are known to be governed by the carbon content and its morphological distribution. Here, we verify the influence of the target peak power density on the chemical composition, microstructure, and mechanical properties of NbCx coatings grown by non-reactive high-power impulse magnetron sputtering (HiPIMS). By tuning the pulse parameters, the power density can be increased from 0.11 to 1.48 kW/cm2 leading to a decrease in the C/Nb ratio from 1.52 to 0.99 within the films - proven by combined elastic backscattering and time-of-flight elastic recoil detection analysis. This decrease in the C/Nb ratio is accompanied by microstructural changes from nanocomposite morphologies with an average grain size of 6.6 +/- 2.5 nm at 0.13 kW/cm2 into more columnar structures with an average column width of 65.2 +/- 18.7 nm at 1.48 kW/cm2. Independent from the C/Nb ratio, all films exhibit a single face-centered cubic structure. The mechanical properties correlate with the enhanced growth behavior dominated by ions at higher peak power densities and the varied C/Nb ratios. A maximum in hardness and fracture toughness of H = 38.7 +/- 3.6 GPa and KIc = 2.78 +/- 0.13 MPa center dot m1/2 (at 3.2 GPa residual compressive stress), is obtained for the nearly stoichiometric NbC coating exhibiting C/Nb ratio of 1.06.
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| 2. |
- Bakhit, Babak, 1983-, et al.
(författare)
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Systematic compositional analysis of sputter-deposited boron-containing thin films
- 2021
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Ingår i: Journal of Vacuum Science & Technology. A. Vacuum, Surfaces, and Films. - : American Vacuum Society. - 0734-2101 .- 1520-8559. ; 39:6
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Tidskriftsartikel (refereegranskat)abstract
- Boron-containing materials exhibit a unique combination of ceramic and metallic properties that are sensitively dependent on their given chemical bonding and elemental compositions. However, determining the composition, let alone bonding, with sufficient accuracy is cumbersome with respect to boron, being a light element that bonds in various coordinations. Here, we report on the comprehensive compositional analysis of transition-metal diboride (TMBx) thin films (TM = Ti, Zr, and Hf) by energy-dispersive x-ray spectroscopy (EDX), x-ray photoelectron spectroscopy (XPS), time-of-flight elastic recoil detection analysis (ToF-ERDA), Rutherford backscattering spectrometry (RBS), and nuclear reaction analysis (NRA). The films are grown on Si and C substrates by dc magnetron sputtering from stoichiometric TMB2 targets and have hexagonal AlB2-type columnar structures. EDX considerably overestimates B/TM ratios, x, compared to the other techniques, particularly for ZrBx. The B concentrations obtained by XPS strongly depend on the energy of Ar+ ions used for removing surface oxides and contaminants prior to analyses and are more reliable for 0.5 keV Ar+. ToF-ERDA, RBS, and NRA yield consistent compositions in TiBx. They also prove TiBx and ZrBx films to be homogeneous with comparable B/TM ratios for each film. However, ToF-ERDA, employing a 36-MeV 127I8+ beam, exhibits challenges in depth resolution and quantification of HfBx due to plural and multiple scattering and associated energy loss straggling effects. Compared to ToF-ERDA, RBS (for the film grown on C substrates) and NRA provide more reliable B/Hf ratios. Overall, a combination of methods is recommended for accurately pinpointing the compositions of borides that contain heavy transition metals.
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| 3. |
- Correa, S. A., et al.
(författare)
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A multipurpose set-up using keV ions for nuclear reaction analysis, high -resolution backscattering spectrometry, low-energy PIXE and in-situ irradiation experiments
- 2020
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Ingår i: Nuclear Instruments and Methods in Physics Research Section B. - : ELSEVIER. - 0168-583X .- 1872-9584. ; 478, s. 104-110
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Tidskriftsartikel (refereegranskat)abstract
- A new chamber for material analysis and modification using energetic ions with primary particle energies in the keV regime was developed at the single stage 350 kV high-current Danfysik implanter at the Tandem Laboratory, Uppsala University. The experimental set-up allows for B-11 and O-18 depth profiling by Nuclear Reaction Analysis using the B-11(p,alpha(0))Be-8 and O-18(p,alpha)N-15 nuclear resonances at 163 keV and at 151 keV, respectively. Additionally, a surface barrier detector with a cryogenic assembly enables High-Resolution Backscattering Spectrometry with average resolution approximate to 4 keV FWHM for protons. A silicon drift detector enables Low-Energy Particle Induced X-ray Emission analysis for elements with low atomic number (Z >= 8). The available instrumentation of the chamber assembly with its specifications are described in details with a series of applied and fundamental benchmark studies, together with some suggestions for future applications.
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| 4. |
- Cupak, C., et al.
(författare)
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Retention of deuterium in beryllium : A combined investigation using TDS, ERDA and EBS
- 2022
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Ingår i: Nuclear Materials and Energy. - : Elsevier. - 2352-1791. ; 33
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Tidskriftsartikel (refereegranskat)abstract
- We have studied the retention of deuterium in beryllium, implanted with an energy of 500 eV/D, using a combination of thermal desorption spectroscopy, elastic recoil detection analysis and elastic backscattering spectroscopy. The parallel use of these techniques allowed us to directly quantify the absolute deuterium content reduction of the sample for specific desorption peaks observed during thermal annealing. In addition, the presence of a beryllium oxide surface layer was observed, despite sputter-cleaning of the sample was initially conducted in-situ. A main result was that similar to 85 % of the retained deuterium got released during the primary desorption peak at 400 K. A smaller, secondary desorption peak was identified at 540 K. All deuterium could be removed from the Be sample by heating it to a temperature of 800 K.
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| 5. |
- Dittrich, Laura, et al.
(författare)
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Impact of ion irradiation and film deposition on optical and fuel retention properties of Mo polycrystalline and single crystal mirrors
- 2023
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Ingår i: Nuclear Materials and Energy. - : Elsevier BV. - 2352-1791. ; 37
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Tidskriftsartikel (refereegranskat)abstract
- Polycrystalline (PC) and single crystal (SC) molybdenum mirrors were irradiated with 98Mo+, 1H+, 4He+, 11B+ and 184W+. Energies were chosen to impact the optically active region (up to 30 nm deep) of Mo mirrors. Some surfaces were coated by magnetron sputtering either with B or W films 4–65 nm thick. The overall objective was to simulate the neutron-induced damage and transmutation (H, He), and the impact of H, He, B, W on the optical performance of test mirrors, and on fuel retention. In parallel, a set of PC Mo mirrors irradiated with 1.6 MeV 98Mo3+ to a damage of 2 dpa and 20 dpa was installed in the JET tokamak for exposure during deuterium-tritium campaigns. Data from spectrophotometric, ion beam and microscopy techniques reveal: (i) the irradiation decreased specular reflectivity, whereby the differences between PC and SC in reflectivity are very small, (ii) He is retained in bubbles within 25–30 nm of the subsurface layer in all irradiated materials, (iii) W, either deposited or implanted, decreases reflectivity, but the strongest reflectivity degradation is caused by B deposition. Laboratory studies show the correlation of damage and H retention. Several cycles of W deposition and its removal from SC-Mo mirrors by plasma-assisted methods were also performed.
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| 6. |
- Glechner, T., et al.
(författare)
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Influence of the non-metal species on the oxidation kinetics of Hf, HfN, HfC, and HfB2 coatings
- 2021
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Ingår i: Materials & design. - : Elsevier. - 0264-1275 .- 1873-4197. ; 211
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Tidskriftsartikel (refereegranskat)abstract
- The influence of the non-metal species on the oxidation resistance of transition metal ceramic based thin films is still unclear. For this purpose, we thoroughly investigated the oxide scale formation of a metal (Hf), carbide (HFC0.96), nitride (HfB1.5), and boride (HfB2.3) coating grown by physical vapor deposition. The non-metal species decisively affect the onset temperature of oxidation, ranging between 550 degrees C for HfC0.96 to 840 degrees C for HfN1.5. HfB2.3 and HfN1.5 obtain the slowest oxide scale kinetic following a parabolic law with k(p) values of 4.97.10(-10) and 5.66.10(-11) kg(2) m(-4) s(-1) at 840 degrees C, respectively. A characteristic feature for the oxide scale on Hf coatings, is a columnar morphology and a substantial oxygen inward diffusion. HfC0.96 reveals an ineffective oxycarbide based scale, whereas HfN(1.5 )features a scale with globular HfO2 grains. HfB(2.3 )exhibits a layered scale with a porous boron rich region on top, followed by a highly dense and crystalline HfO2 beneath. Furthermore, HfB(2.3 )presents a hardness of 47.7 +/- 2.7 GPa next to an exceptional low inward diffusion of oxygen during oxidation. This study showcases the strong influence of the non-metallic bonding partner despite the same metallic basis, as well as the huge potential for HfB2 based coatings also for oxidative environments.
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| 7. |
- Kretschmer, Andreas, et al.
(författare)
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Analysis of (Al,Cr,Nb,Ta,Ti)-nitride and-oxynitride diffusion barriers in Cu-Si interconnects by 3D-Secondary Ion Mass Spectrometry
- 2023
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Ingår i: Materials Characterization. - : Elsevier. - 1044-5803 .- 1873-4189. ; 197
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Tidskriftsartikel (refereegranskat)abstract
- We report on the barrier performance of a nitride, and three oxynitrides of the system Al-Cr-Nb-Ta-Ti between Cu and Si. Different high-entropy sublattice nitrides have been tested before as diffusion barriers in this system, by depositing thin barriers on single crystalline Si substrates, followed by a thick Cu layer on top, and subsequent vacuum annealing. We investigated a reversed stacking sequence, by sputtering 15-30 nm of (Al,Cr,Nb,Ta,Ti)-O-N (between 0.5 and 63.7 at.% O) on polished polycrystalline Cu substrates, followed by 200 nm of Si. The samples were then vacuum annealed at 600, 700, 800 and 900 degrees C for 30 min. All four investigated coatings perform similar. Secondary Ion Mass Spectrometry depth profiling in high-current-bunched mode (lateral res-olution +/- 1 mu m) shows breakthrough of Si even at 600 degrees C. But 3D constructed images with Burst Alignment mode (lateral resolution of +/- 2 nm) reveal that this failure is a highly localized phenomenon, likely related to coarsening effects at the Cu grain boundaries, leading to punctuation of the diffusion barrier. Aside from this penetration, the majority of the area of each barrier coating retains its function. This in-depth analysis shows that the barrier function of the nitride and oxynitride coatings mostly stays intact up to 800 degrees C and fails completely at 900 degrees C.
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| 8. |
- Kretschmer, Andreas, et al.
(författare)
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High-entropy alloy inspired development of compositionally complex superhard (Hf,Ta,Ti,V,Zr)-B-N coatings
- 2022
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Ingår i: Materials & design. - : Elsevier. - 0264-1275 .- 1873-4197. ; 218
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Tidskriftsartikel (refereegranskat)abstract
- Phase stability and mechanical properties of multimetal-boronnitride (Hf,Ta,Ti,V,Zr)-B-N is investigated by ab initio computations and experimental methods. (Hf,Ta,Ti,V,Zr)-B-N shows a strong energetic preference for the fcc NaCl-type structure over other structures up to a B:N ratio of 3.5. Reactively deposited (Hf,Ta,Ti,V,Zr)-B-N coatings show formation of X-ray amorphous BN, accompanied by a drastic hardness decrease with increasing B content. But non-reactively sputtered (Hf,Ta,Ti,V,Zr)-B-N coatings exhibit a single-phase fcc solid solution, up to the maximum B:N ratio of 1.12 studied, in good agreement with calculations. All non-reactively sputtered multimetal-boronnitride coatings contain a high Zr metal-fraction and approximate to 8at% C, stemming from impurities in the target. The single-phase coatings reach superhardness up to 46.3 GPa. Even after vacuum annealing to 1200 degrees C, the hardness of the coating with a B:N ratio of 1.03 is still 43.7 GPa, while that of ZrN0.72C0.28 decreased from 36.3 to 30.2 GPa. Our results demonstrate the importance of the deposition technique to deposit single-phased coatings with exceptional hardness and thermal stability. (C) 2022 The Authors. Published by Elsevier Ltd.
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| 9. |
- Moldarev, Dmitrii, et al.
(författare)
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Oxygen mobility in yttrium hydride films studied by isotopic labelling
- 2022
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Ingår i: EPJ Web of Conferences. - : EDP Sciences. - 2100-014X. ; 261, s. 01001-01001
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Tidskriftsartikel (refereegranskat)abstract
- The photochromic properties of oxygen-containing yttrium hydride thin films are directly dependent on the oxygen concentration in the material. We use 16O/18O labelling to study oxidation of YH2 films. Oxygen penetrates the film through grain boundaries and intercolumnar voids oxidising the whole film thickness, without pronounced surface oxidation or self-passivation. Once oxidised, the mobility of oxygen in the films is low and no detectable changes in chemical composition of 18O-labeled YHO films is found under illumination.
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| 10. |
- Pitthan, Eduardo, et al.
(författare)
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Assessing boron quantification and depth profiling of different boride materials using ion beams
- 2021
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Ingår i: Surface & Coatings Technology. - : Elsevier. - 0257-8972 .- 1879-3347. ; 417
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Tidskriftsartikel (refereegranskat)abstract
- We assessed the capability to quantify and depth profile boron in different materials by a number of ion beam-based techniques. Specifically, the depth resolution, probing depth, film homogeneity, and detection limit for boron using particle-particle nuclear reaction analysis (resonant and non-resonant mode), elastic backscattering spectrometry, and time-of-flight elastic recoil detection analysis using heavy primary ions were evaluated. Samples consisted of high and low-Z materials implanted by B-11(+) at different energies and fluences, Au/BN structures as well as bulk boride targets. Advantages and limitations for the individual techniques for the different sample types are discussed. As an example, while ToF-ERDA allows to efficiently depth profile B-10 and B-11 individually, limitations in probing depth and depth resolution, as well as quantification are apparent in particular for target materials containing high-Z species. While EBS presents large probing depth (similar to 14 mu m), the best detection limit (similar to 0.1 x 10(15)/cm(2)) is obtained from resonant-NRA.
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