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Growth of Ti3SiC2 thin films by elemental target magnetron sputtering
Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska högskolan.
Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska högskolan.
Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska högskolan.
Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska högskolan.ORCID-id: 0000-0001-9140-6724
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2004 (Engelska)Ingår i: Journal of Applied Physics, ISSN 0021-8979, E-ISSN 1089-7550, Vol. 96, nr 9, s. 4817-4826Artikel i tidskrift (Refereegranskat) Published
Abstract [en]

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 μΩ 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.

Ort, förlag, år, upplaga, sidor
2004. Vol. 96, nr 9, s. 4817-4826
Nationell ämneskategori
Naturvetenskap
Identifikatorer
URN: urn:nbn:se:liu:diva-29682DOI: 10.1063/1.1790571Lokalt ID: 15069OAI: oai:DiVA.org:liu-29682DiVA, id: diva2:250499
Tillgänglig från: 2009-10-09 Skapad: 2009-10-09 Senast uppdaterad: 2017-12-13
Ingår i avhandling
1. MAX phase thin films: unique multifunctional ceramics with the elements Ti, Si, Ge, Sn, and C
Öppna denna publikation i ny flik eller fönster >>MAX phase thin films: unique multifunctional ceramics with the elements Ti, Si, Ge, Sn, and C
2006 (Engelska)Doktorsavhandling, sammanläggning (Övrigt vetenskapligt)
Abstract [en]

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.

Ort, förlag, år, upplaga, sidor
Institutionen för fysik, kemi och biologi, 2006. s. 48
Serie
Linköping Studies in Science and Technology. Dissertations, ISSN 0345-7524 ; 1024
Nyckelord
Thin solid films, Single-crystal
Nationell ämneskategori
Fysik
Identifikatorer
urn:nbn:se:liu:diva-7449 (URN)91-85523-64-X (ISBN)
Disputation
2006-06-16, Planck, Fysikhuset, Campus Valla, Linköpings universitet, Linköping, 10:15 (Engelska)
Opponent
Tillgänglig från: 2006-09-27 Skapad: 2006-09-27 Senast uppdaterad: 2012-11-19

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Emmerlich, JensHögberg, HansPersson, PerHultman, Lars

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