| 1. |
- Emmerlich, Jens, 1974-, et al.
(författare)
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Growth of Ti3SiC2 thin films by elemental target magnetron sputtering
- 2004
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Ingår i: Journal of Applied Physics. - : AIP Publishing. - 0021-8979 .- 1089-7550. ; 96:9, s. 4817-4826
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Tidskriftsartikel (refereegranskat)abstract
- Epitaxial Ti3SiC2(0001) thin films have been deposited by dc magnetron sputtering from three elemental targets of Ti, C, and Si onto MgO(111) and Al2O3(0001) substrates at temperatures of 800–900 °C. This process allows composition control to synthesize Mn + 1AXn (MAX) phases (M: early transition metal; A: A-group element; X: C and/or N; n = 1–3) including Ti4SiC3. Depositions on MgO(100) substrates yielding the Ti–Si–C MAX phases with (105), as the preferred orientation. Samples grown at different substrate temperatures, studied by means of transmission electron microscopy and x-ray diffraction investigations, revealed the constraints of Ti3SiC2 nucleation due to kinetic limitations at substrate temperatures below 700 °C. Instead, there is a competitive TiCx growth with Si segregation to form twin boundaries or Si substitutional incorporation in TiCx. Physical properties of the as-deposited single-crystal Ti3SiC2 films were determined. A low resistivity of 25 µ cm was measured. The Young's modulus, ascertained by nanoindentation, yielded a value of 343–370 GPa. For the mechanical deformation response of the material, probing with cube corner and Berkovich indenters showed an initial high hardness of almost 30 GPa. With increased maximum indentation loads, the hardness was observed to decrease toward bulk values as the characteristic kink formation sets in with dislocation ordering and delamination at basal planes.
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| 2. |
- Högberg, Hans, 1968-, et al.
(författare)
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Epitaxial Ti2GeC, Ti3GeC2, and Ti4GeC3 MAX-phase thin films grown by magnetron sputtering
- 2005
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Ingår i: Journal of Materials Research. - 0884-2914 .- 2044-5326. ; 20:4, s. 779-782
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Tidskriftsartikel (refereegranskat)abstract
- We have grown single-crystal thin films of Ti2GeC and Ti3GeC2 and a new phase Ti4GeC3, as well as two new intergrown MAX-structures, Ti5Ge2C3 and Ti7Ge2C5. Epitaxial films were grown on Al2O3(0001) substrates at 1000 °C using direct current magnetron sputtering. X-ray diffraction shows that Ti–Ge–C MAX-phases require higher deposition temperatures in a narrower window than their Ti–Si–C correspondences do, while there are similarities in phase distribution. Nanoindentation reveals a Young’s modulus of 300 GPa, lower than that of Ti3SiC2. Four-point probe measurements yield resistivity values of 50–200 μΩcm. The lowest value is obtained for phase-pure Ti3GeC2(0001) films.
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| 5. |
- Emmerlich, Jens, 1974-
(författare)
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MAX phase thin films : unique multifunctional ceramics with the elements Ti, Si, Ge, Sn, and C
- 2006
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Doktorsavhandling (övrigt vetenskapligt/konstnärligt)abstract
- Mn+1AXn phases are ternary carbides or nitrides (X) consisting of an early transition metal (M), and (A)- group element (group III-V). They combine ceramic and metallic properties with high oxidation and thermal shock resistance as well as low resistivity. Depending on stoichiometry, they can be classified as 211 (n=1), 312 (n=2), and 413 (n=3) phases. The main purpose of this Thesis is to present the synthesis by epitaxial growth of Tin+1ACn (A: Si, Ge, Sn; n=1-3) thin solid films and to report on the material’s intrinsic mechanical and electrical properties. DC magnetron sputtering of MAX-phase carbides from three individual elemental targets is presented as an original and successful deposition method. The emphasis is on the archetypical Ti3SiC2, but I also demonstrate growth of a wide range of other single-crystal Tin+1ACn thin films, including Ti2GeC, Ti3GeC2, Ti2SnC, previously available only in bulk form, as well as completely new phases of Ti4SiC3, Ti4GeC3, and Ti3SnC2, together with some intergrown 523 (211+312) and 725 (312+413) structures.A combination of x-ray diffraction (XRD), transmission electron micrcoscopy (TEM) analysis, x-ray photoelectron spectroscopy, elastic recoil detection analysis, and Rutherford backscattering spectrometry of the films reveal single-phase and epitaxial growth of Tin+1SiCn(0001) (n = 2, 3) and Ti2GeC MAX phases at substrate temperatures (TS) above 700 to 1000 °C. For TS = 500 – 700 °C, Si is accommodated at twin boundaries between TiC(111) planes. Depositions at TS = RT – 350 °C yield nc-TiC/SiC nanocomposite films or TiC growth with substitutionally incorporated Si due to kinetic constraints. Vacuum-annealing with in situ XRD measurements of the films between 800 – 1400 °C revealed a thermal stability of up to ~1000 °C. A MAX-phase decomposition model is presented within this Thesis. It starts by Si out-diffusion and evaporation from the surface between ~1000 – 1100 °C and is accompanied by any O uptake and SiO evaporation. Subsequently, the free Ti3C2 slabs relax and undergo detwinning. The decomposition process is ended by TiC0.67 formation by C redistribution and recrystallization with void formation.The mechanical response to deformation was tested on Ti3SiC2(0001) films using nanoindentation. Small applied normal forces yielding a minimum on plastic deformation reveal hardness values of up to 24 GPa, which decrease with larger indentation depths. Young’s moduli between 320 and 343 GPa were measured. Atomic force microscopy (AFM) surface imaging and Focused Ion Beam cross-sectional TEM studies confirm that mechanical deformation in this ductile ceramic takes place by kink formation and delamination along basal planes, due to edge dislocation pile-ups forming the kink boundaries resulting in local deformation-energy dissipation. Friction measurements yield a friction coefficient (μ) of 0.1 for normal loads of FN = 100-200 μN. μ increases to 0.8 with increased FN up to 0.24 N, as delamination and kinking are introduced accompanied by third-body abrasion as shown by scanning electron microscopy. By comparing electrical resistivity values obtained by four-point probe measurements, it is found that all studied MAX-phase thin film systems exhibit good conduction properties.
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| 6. |
- Emmerlich, Jens, 1974-, et al.
(författare)
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Micro and macroscale tribological behavior of epitaxial Ti3SiC2 thin films
- 2008
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Ingår i: Wear. - Amsterdam, Netherlands : Elsevier. - 0043-1648 .- 1873-2577. ; 264:11-12, s. 914-919
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Tidskriftsartikel (refereegranskat)abstract
- Ti3SiC2(0 0 0 1) thin films prepared by magnetron sputtering were investigated for their response to tribomechanical strain induced during ball-on-disk experiments with 6 mm alumina balls and scratch tests with a 1 μm cono-spherical diamond tip. Normal loads of 100 μN to 0.24 N were applied resulting in a friction coefficient of 0.1 for the low loads. With higher applied normal loads, the friction coefficient increased up to 0.8. Analysis of the wear tracks using atomic force microscopy, scanning electron microscopy, and Raman spectroscopy revealed excessive debris resulting in third-body abrasion and fast wear. The formation of the debris can be explained by the generation of subsurface delamination cracks on basal planes. Subsequent kink formation obstructs the ball movement which results in the removal of the kinked film parts.
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| 7. |
- Emmerlich, Jens, 1974-
(författare)
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Thin film growth and characterization of Ti-Si-C MAX-phases
- 2004
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Licentiatavhandling (övrigt vetenskapligt/konstnärligt)abstract
- This thesis describes the growth of Ti-Si-C MAX-phases on A12O3(0001) and MgO(111) substrates with the emphasis on epitaxial Ti3SiC2 thin films by means of DC magnetron sputtering. Ti3SiC2, Ti4SiC3 as well as the two intergrown structures Ti5Si2C3 and Ti7Si2C5 were grown using sputtering from three individual elemental targets of Ti, Si, and C, respectively. X-ray diffraction analysis of the films revealed single-phase and epitaxial growth of Tin+1SiCn(0001) (n = 2, 3) MAX-phases at substrate temperatures above 700 °C. MgO(100) substrates as growth templates provided growth of Ti3SiC2 in a preferred orientation of (1015). TEM and XRD investigations showed that at 700 °C and below Si is accommodated at twin boundaries between TiC(111) planes. Depositions at substrate temperatures of 350 °C and RT resulted in nanocrystalline TiC growth with substitutionally-incorporated Si due to kinetic constraints.Mechanical properties were investigated using nanoindentation with cube corner and Berkovich indenters. With small indentation depth, hardness values of up to 24 GPa were measured for Ti3SiC2 films. Increasing maximum loads yielded lower hardnesses approaching bulk values. Young's moduli of 320 and 343 GPa were observed applying cube comer and Berkovich indenter, respectively. Cross-sectional TEM through indentations made with a Berkovich indenter were used to study the deformation behavior of the MAX-phases. Deformation energy is dissipated in kink formation, with edge dislocation pile-ups at the kink boundary, and delamination along basal planes.Four-point probe measurements on Ti3SiC2 MAX-phase thin films deposited at 900 °C showed a low room temperature resistivity of ~ 25 µΩcm, which increased with lower deposition temperatures. Ti4SiC3 films demonstrated an increased resistivity up to ~ 50 µΩcm.
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| 8. |
- Högberg, Hans, 1968-, et al.
(författare)
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Growth and characterization of MAX-phase thin films
- 2005
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Ingår i: Surface and Coatings Technology. - : Elsevier BV. - 0257-8972 .- 1879-3347. ; 193, s. 6-10
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Tidskriftsartikel (refereegranskat)abstract
- We report that magnetron sputtering can be applied to synthesize MAX-phase films of several systems including Ti–Si–C, Ti–Ge–C, Ti–Al–C, and Ti–Al–N. In particular, epitaxial films of the known phases Ti3SiC2, Ti3GeC2, Ti2GeC, Ti3AlC2, Ti2AlC, and Ti2AlN as well as the newly discovered thin film phases Ti4SiC3, Ti4GeC3 and intergrown structures can be deposited at 900–1000 °C on Al2O3(0001) and MgO(111) pre-seeded with TiC or Ti(Al)N. From XTEM and AFM we suggest a growth and nucleation model where MAX-phase nucleation is initiated at surface steps or facets on the seed layer and followed by lateral growth. Differences between the growth behavior of the systems with respect to phase distribution and phase stabilities are discussed. Characterization of mechanical properties for Tin+1Si–Cn films with nanoindentation show decreased hardness from about 25 to 15 GPa upon penetration of the basal planes with characteristic large plastic deformation with pile up dependent on the choice of MAX material. This is explained by cohesive delamination of the basal planes and kink band formation, in agreement with the observations made for bulk material. Measurements of the electrical resistivity for Ti–Si–C and Ti–Al–N films with four-point probe technique show values of 30 and 39 μΩ cm, respectively, comparable to bulk materials.
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