| 1. |
- Salamania, Janella, 1992-
(författare)
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Defects in Titanium Aluminum Nitride-Based Thin Films
- 2023
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Doktorsavhandling (övrigt vetenskapligt/konstnärligt)abstract
- Coatings and thin films inherently contain several types of defects. This thesis aims to enhance the understanding of the relationship of defects on the growth, structure, stability, and properties of titanium aluminum nitride films synthesized by physical vapor deposition techniques.Heteroepitaxial cubic and wurtzite films in the Ti-Al-N system grown by reactive magnetron sputtering were studied in relation to their defect structures. The dislocation structures of heteroepitaxial TiN and Ti1-xAlxNy films were analyzed by high-angle annular dark field scanning transmission electron microscopy (HAADF-STEM). Together with atomistic simulations, it was revealed that the presence of different dislocation types in TiN enhances the metal-metal bonds which locally weakens the directionally covalent metal-N bonds. In epitaxial cubic Ti1-xAlxN films, microstrain analysis shows that increasing N-vacancies influences the strain and compositional fluctuations in as-deposited states. During spinodal decomposition induced by annealing to high temperatures, the delay in coarsening and strain correlates with the amount of N vacancies. Detailed characterization of the decomposing domains exposed the formation of stacking faults and partial dislocations as a strain-relieving mechanism which also facilitates the known cubic-to-wurtzite transformation in Ti-Al-N.Cathodic arc deposited Ti1-xAlxN films were grown by applying a low duty cycle pulsed-substrate bias and high nitrogen pressures. This resulted into films with coarse grains and low lattice defects within them, indicating a kinetically controlled route to modify the defect structures in arc-deposited films. Applying the same technique on single crystalline TiN seed layer films kinetically stabilizes a pseudomorphic growth, allowing to form a highly textured, pseudo epitaxial wurtzite Ti1-xAlxN films by arc deposition. In combination with theoretical calculations, it was revealed that w-Ti1-xAlxN films also exhibit a miscibility gap which enables spinodal decomposition and thus age hardening when annealed. Finally, magnetron sputtered nitrogen-deficient w-Ti1-xAlxNy heteroepitaxial films were shown to exhibit a decomposition route that involves the formation of coherent intermediate MAX-like phases before transforming to pure c-TiN and w-AlN phases, which results to continued age hardening up to 1200°C.The findings in this work increase the fundamental understanding of the role of defects in Ti-Al-N films and open new routes for defect-based engineering strategies.
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| 2. |
- Salamania, Janella, 1992-, et al.
(författare)
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Elucidating dislocation core structures in titanium nitride through high-resolution imaging and atomistic simulations
- 2022
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Ingår i: Materials & design. - : Elsevier. - 0264-1275 .- 1873-4197. ; 224
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Tidskriftsartikel (refereegranskat)abstract
- Although titanium nitride (TiN) is among the most extensively studied and thoroughly characterizedthin-film ceramic materials, detailed knowledge of relevant dislocation core structures is lacking. Byhigh-resolution scanning transmission electron microscopy (STEM) of epitaxial single crystal (001)-oriented TiN films, we identify different dislocation types and their core structures. These include, besidesthe expected primary a/2{110}h110i dislocation, Shockley partial dislocations a/6{111}h112i and sessileLomer edge dislocations a/2{100}h011i. Density-functional theory and classical interatomic potentialsimulations complement STEM observations by recovering the atomic structure of the different disloca-tion types, estimating Peierls stresses, and providing insights on the chemical bonding nature at the core.The generated models of the dislocation cores suggest locally enhanced metal–metal bonding, weakenedTi-N bonds, and N vacancy-pinning that effectively reduces the mobilities of {110}h110i and {111}h112idislocations. Our findings underscore that the presence of different dislocation types and their effects onchemical bonding should be considered in the design and interpretations of nanoscale and macroscopicproperties of TiN.
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| 3. |
- Chen, Yu-Hsiang, et al.
(författare)
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Enhanced thermal stability and fracture toughness of TiAlN coatings by Cr, Nb and V-alloying
- 2018
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Ingår i: Surface & Coatings Technology. - : Elsevier. - 0257-8972 .- 1879-3347. ; 342, s. 85-93
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Tidskriftsartikel (refereegranskat)abstract
- The effect of metal alloying on mechanical properties including hardness and fracture toughness were investigated in three alloys, Ti 0.33Al0.50(Me) 0.17N (Me = Cr, Nb and V), and compared to Ti0.50Al0.50N, in the as-deposited state and after annealing. All studied alloys display similar as-deposited hardness while the hardness evolution during annealing is found to be connected to phase transformations, related to the alloy’s thermal stability. The most pronounced hardening was observed in Ti0.50Al0.50N, while all the coatings with additional metal elements sustain their hardness better and they are harder than Ti0.50Al0.50N after annealing at 1100 °C. Fracture toughness properties were extracted from scratch tests. In all tested conditions, as-deposited and annealed at 900 and 1100 °C, Ti0.33Al0.50Nb0.17N show the least surface and sub-surface damage when scratched despite the differences in decomposition behavior and h-AlN formation. Theoretically estimated ductility of phases existing in the coatings correlates well with their crack resistance. In summary, Ti0.33Al0.50Nb0.17N is the toughest alloy in both as-deposited and post-annealed states.
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| 4. |
- Chen, Yu-Hsiang
(författare)
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Mechanical and thermal stability of hard nitride coatings
- 2018
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Doktorsavhandling (övrigt vetenskapligt/konstnärligt)abstract
- Hard coating’s thermal stability is essential due to the high temperature environment of high-speed cutting applications, while the phase and microstructure evolution induced by exposing the coating to high temperature affects the mechanical properties. In this thesis, the mechanical stability of arc-evaporated, hard, transition metal nitride coatings annealed at high temperature is analyzed and related to the phase and microstructure evolution. In addition to hardness, fracture toughness is evaluated by surface and cross-sectional investigations by scanning/transmission electron microscopy of damage events following mechanical tests.The crack resistance of Ti1−xAlxN with a range of Al content (x = 0.23-0.82) was studied by contact fatigue tests, where the differences in the microstructure were found to play a major role. Superior mechanical properties were found in Ti0.63Al0.37N; in the as-deposited state as a result of a favorable grain size, and after annealing at 900o C due to the microstructure formed during spinodal decomposition.The mechanical and high-temperature properties of hard coatings can be enhanced by alloying or multi-layering. Within this work, quaternary Ti-Al-X-N (X = Cr, Nb and V) alloys were studied and superior toughness was found for TiAl(Nb)N in both the as-deposited and annealed (1100◦ C) states. The hexagonal (h)-AlN formation in cubic (c)-TixAl0.37Cr1−0.37−xN (x = 0.03 and 0.16) was analyzed by in-situ x-ray scattering during annealing. The energy for h-AlN formation was found to be dependent on the microstructure evolution during annealing, which varies with the coating composition.High Al content h-ZrAlN/c-TiN and h-ZrAlN/c-ZrN multilayers were investigated through scratch tests followed by focused ion-beam analysis of the crack propagation. A c-Ti(Zr)N phase forms in h-ZrAlN/c-TiN multilayers at high temperatures and that contributes to enhanced hardness and fracture toughness by keeping the semi-coherent sub-interfaces.Finally, an in-situ analysis of coatings by x-ray scattering during a turning process was carried out. It demonstrates the possibility of observation of stress evolution and thermal expansion of the coatings or the work piece material during machining. This experiment provides real-time information on the coating behavior during cutting.
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| 5. |
- Johnson, Lars, 1983-, et al.
(författare)
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Microstructure evolution and age hardening in (Ti,Si)(C,N) thin films deposited by cathodic arc evaporation
- 2010
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Ingår i: Thin Solid Films. - : Elsevier BV. - 0040-6090 .- 1879-2731. ; 519:4, s. 1397-1403
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Tidskriftsartikel (refereegranskat)abstract
- Ti1 − xSixCyN1 − y films have been deposited by reactive cathodic arc evaporation onto cemented carbide substrates. The films were characterized by X-ray diffraction, elastic recoil detection analysis, transmission electron microscopy, energy-dispersive X-ray spectroscopy, electron-energy loss spectroscopy and nanoindentation. Reactive arc evaporation in a mixed CH4 and N2 gas gave films with 0 ≤ x ≤ 0.13 and 0≤y≤0.27. All films had the NaCl-structure with a dense columnar microstructure, containing a featherlike pattern of nanocrystalline grains for high Si and C contents. The film hardness was 32–40GPa. Films with x > 0 and y > 0 exhibited age-hardening up to 35–44 GPa when isothermally annealed up to 900 °C. The temperature threshold for over-ageing was decreased to 700 °C with increasing C and Si content, due to migration of Co, W and Cr from the substrate to the film, and loss of Si. The diffusion pathway was tied to grain boundaries provided by the featherlike substructure.
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| 6. |
- Landälv, Ludvig, 1982-, et al.
(författare)
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Phase evolution of radio frequency magnetron sputtered Cr-rich (Cr,Zr)(2)O-3 coatings studied by in situ synchrotron X-ray diffraction during annealing in air or vacuum
- 2019
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Ingår i: Journal of Materials Research. - : CAMBRIDGE UNIV PRESS. - 0884-2914 .- 2044-5326. ; 34:22, s. 3735-3746
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Tidskriftsartikel (refereegranskat)abstract
- The phase evolution of reactive radio frequency (RF) magnetron sputtered Cr0.28Zr0.10O0.61 coatings has been studied by in situ synchrotron X-ray diffraction during annealing under air atmosphere and vacuum. The annealing in vacuum shows t-ZrO2 formation starting at similar to 750-800 degrees C, followed by decomposition of the alpha-Cr2O3 structure in conjunction with bcc-Cr formation, starting at similar to 950 degrees C. The resulting coating after annealing to 1140 degrees C is a mixture of t-ZrO2, m-ZrO2, and bcc-Cr. The air-annealed sample shows t-ZrO2 formation starting at similar to 750 degrees C. The resulting coating after annealing to 975 degrees C is a mixture of t-ZrO2 and alpha-Cr2O3 (with dissolved Zr). The microstructure coarsened slightly during annealing, but the mechanical properties are maintained, with no detectable bcc-Cr formation. A larger t-ZrO2 fraction compared with alpha-Cr2O3 is observed in the vacuum-annealed coating compared with the air-annealed coating at 975 degrees C. The results indicate that the studied pseudo-binary oxide is more stable in air atmosphere than in vacuum.
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| 7. |
- Moreno, Maiara, 1993-, et al.
(författare)
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Strain and phase evolution in TiAlN coatings during high-speed metal cutting : An in operando high-energy x-ray diffraction study
- 2024
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Ingår i: Acta Materialia. - : Elsevier. - 1359-6454 .- 1873-2453. ; 263
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Tidskriftsartikel (refereegranskat)abstract
- We report on phase and strain changes in Ti1-xAlxN (0 ≤ x ≤ 0.61) coatings on cutting tools during turning recorded in operando by high-energy x-ray diffractometry. Orthogonal cutting of AISI 4140 steel was performed with cutting speeds of 360–370 m/min. Four positions along the tool rake face were investigated as a function of time in cut. Formation of γ-Fe in the chip reveals that the temperature exceeds 727 °C between the tool edge and the middle of the contact area when the feed rate is 0.06 mm/rev. Spinodal decomposition and formation of wurtzite AlN occurs at the positions of the tool with the highest temperature for the x ≥ 0.48 coatings. The strain evolution in the chip reveals that the mechanical stress is largest closest to the tool edge and that it decreases with time in cut for all analyzed positions on the rake face. The strain evolution in the coating varies between coatings and position on the rake face of the tool and is affected by thermal stress as well as the applied mechanical stress. Amongst others, the strain evolution is influenced by defect annihilation and, for the coatings with highest Al-content (x ≥ 0.48), phase changes.
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| 8. |
- Moreno, Maiara, 1993-
(författare)
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Wear behavior of Ti1-xAlxN-based coatings during turning
- 2022
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Doktorsavhandling (övrigt vetenskapligt/konstnärligt)abstract
- Ti1-xAlxN coatings are extensively used on cutting tools used for metal cutting. In this thesis, the wear behavior of TiN, TiAlN with different Al-content, and TiAlWN and TiAlMoN coatings is investigated after turning, using electron microscopy and X-ray absorption spectroscopy techniques. An in operando study using high-energy X-ray diffraction during turning is also carried out, to understand the strain and phase evolution of TiAlN coatings during machining. The main wear mechanisms when cutting stainless steel 316L with cutting speeds from 60 m/min up to 220 m/min are investigated. The results show a difference in wear behavior with cutting speed. At low cutting speeds, adhesive wear is the main mechanism that generates coating failure, causing fracture of the coating. The higher Al-content coatings (x ≥ 0.53) perform better compared to lower Al-content coatings, likely due to a better fracture resistance. At higher cutting speeds, 220 m/min, crater wear due to abrasive wear and chemical reactions between coating and workpiece material occurs. In this case, the high temperatures achieved during turning results in formation of hexagonal (h)-AlN in Ti0.38Al0.62N coatings, which lowers their wear resistance. For TiAlMoN and TiAlWN, an improved wear behavior is observed compared to pure TiAlN, because it retards spinodal decomposition and the subsequent formation of h-AlN. Investigations of the sliding area using TEM, EDS and XANES spectra from the Ti 1s-edge reveals that there are differences in level of spinodal decomposition, thus differences in temperature, in different regions of the tool. During in operando orthogonal turning of alloy steel, spinodal decomposition was observed to take place after only 10 s of turning for the highest Al-content coatings. Decomposition occurs where the temperature of the rake face is the highest. In summary, the results achieved lead to a better understanding of the interactions between tool and workpiece material and the different wear mechanisms which may expand the application envelope for these coatings.
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| 9. |
- Rogström, Lina, 1983-
(författare)
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High temperature behavior of arc evaporated ZrAlN and TiAlN thin films
- 2012
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Doktorsavhandling (övrigt vetenskapligt/konstnärligt)abstract
- Hard coatings can extend the life time of a tool substantially and enable higher cutting speeds which increase the productivity in the cutting application. The aim with this thesis is to extend the understanding on how the microstructure and mechanical properties are affected by high temperatures similar to what a cutting tool can reach during operation.Thin films of ZrAlN and TiAlN have been deposited using cathodic arc-evaporation. The microstructure of as-deposited and annealed films has been studied using electron microscopy and x-ray scattering. The thermal stability has been characterized by calorimetry and thermogravity and the mechanical properties have been investigated by nanoindentation.The microstructure of Zr1−xAlxN thin films was studied as a function of composition, deposition conditions, and annealing temperature. The structure was found to depend on the Al content where a low (x < 0.38) Al-content results in cubic-structured ZrAlN while for x > 0.70 the structure is hexagonal. For intermediate Al contents (0.38 < x < 0.70), a nanocomposite structure with a mixture of cubic, hexagonal and amorphous phases is obtained.The cubic ZrAlN phase transforms by nucleation and growth of hexagonal AlN when annealed above 900 ◦C. Annealing of hexagonal ZrAlN thin films (x > 0.70) above 900 ◦C causes formation of AlN and ZrN rich domains within the hexagonal lattice. Annealing of nanocomposite ZrAlN thin films results in formation of cubic ZrN and hexagonal AlN. The transformation is initiated by nucleation and growth of cubic ZrN at temperatures of 1100 ◦C while the AlN-rich domains are still amorphous or nanocrystalline. Growth of hexagonal AlN is suppressed by the high nitrogen content of the films and takes place at annealing temperatures of 1400 ◦C.In the more well known TiAlN system, the initial stage of decomposition is spinodal with formation of cubic structured domains enriched in TiN and AlN. By a combination of in-situ xray scattering techniques during annealing and phase field simulations, both the microstructure that evolves during decomposition and the decomposition rate are found to depend on the composition. The results further show that early formation of hexagonal AlN domains during decomposition can cause formation of strains in the cubic TiAlN phase.
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| 10. |
- Rogström, Lina, 1983-, et al.
(författare)
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Structural changes in Ti1-xAlxN coatings during turning : A XANES and EXAFS study of worn tools
- 2023
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Ingår i: Applied Surface Science. - : Elsevier. - 0169-4332 .- 1873-5584. ; 612
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Tidskriftsartikel (refereegranskat)abstract
- Structural changes in Ti1-xAlxN coated tool inserts used for turning in 316L stainless steel were investigated by XANES, EXAFS, EDS, and STEM. For coarse-grained fcc-structured Ti1-xAlxN coatings, with 0 ≤ x ≤ 0.62, the XANES spectrum changes with Al-content. XANES Ti 1s line-scans across the rake face of the worn samples reveals that TiN-enriched domains have formed during turning in Ti0.47Al0.53N and Ti0.38Al0.62N samples as a result of spinodal decomposition. The XANES spectra reveal the locations on the tool in which the most TiN-rich domains have formed, indicating which part of the tool-chip contact area that experienced the highest temperature during turning. Changes in the pre-edge features in the XANES spectra reveal that structural changes occur also in the w-TiAlN phase in fine-grained Ti0.38Al0.62N during turning. EDS shows that Cr and Fe from the steel adhere to the tool rake face during machining. Cr 1s and Fe 1s XANES show that Cr is oxidized in the end of the contact length while the adhered Fe retains in the same fcc-structure as that of the 316L stainless steel.
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