Thierry Cabioc’h

Microstructural study of a C–Fe alloy synthesized by ion-beam sputtering co-deposition

A carbon–iron thin film, composition 46 at. % Fe and thickness 26 nm, was synthesized by ion-beam sputtering with a substrate temperature of 573 K. The microstructure of the film was characterized by transmission electron microscopy and small-angle x-ray scattering under grazing incidence. It consisted of iron-rich particles, with an average in-plane diameter of 3.2 nm, uniformly dispersed in a graphite-like carbon matrix. These particles were elongated along the in-depth direction, that of the thin-film growth. After annealing at 623 K for 1 h, no modification in the microstructure of the film was observed. The present study shows that the co-sputtering of graphite and iron performed at low temperature in comparison with the conventional arc discharge method, is a useful synthesis method to obtain thin films of encapsulated nanoparticles which have a good thermal stability.

Synthesis of MAX Phases in the Zr-Ti-Al-C System

This study reports on the synthesis and characterization of MAX phases in the (Zr,Ti)n+1AlCn system. The MAX phases were synthesized by reactive hot pressing and pressureless sintering in the 1350-1700 °C temperature range. The produced ceramics contained large fractions of 211 and 312 (n = 1, 2) MAX phases, while strong evidence of a 413 (n = 3) stacking was found. Moreover, (Zr,Ti)C, ZrAl2, ZrAl3, and Zr2Al3 were present as secondary phases. In general, the lattice parameters of the hexagonal 211 and 312 phases followed Vegards law over the complete Zr-Ti solid solution range, but the 312 phase showed a non-negligible deviation from Vegards law around the (Zr0.33,Ti0.67)3Al1.2C1.6 stoichiometry. High-resolution scanning transmission electron microscopy combined with X-ray diffraction demonstrated ordering of the Zr and Ti atoms in the 312 phase, whereby Zr atoms occupied preferentially the central position in the close-packed M6X octahedral layers. The same ordering was also observed in 413 stackings present within the 312 phase. The decomposition of the secondary (Zr,Ti)C phase was attributed to the miscibility gap in the ZrC-TiC system.

Thermal Stability and Mechanical Characteristics of Densified Ti3AlC2-Based Material

The mechanical properties and temperature stability in air and hydrogen of the highly dense (ρ=4.27 g/cm3, porosity 1 %) material based on nanolaminated MAX phase Ti3AlC2 (89 % Ti3AlC2, 6 % TiC, 5 % Al2O3) manufactured by hot pressing (at 30 MPa) have been investigated. At room temperature the samplesexhibited microhardness HV = 4.6 GPa (at 5 N), hardness HV50 = 630 MPa (at 50 N ) and HRA=70 (at 600 N), Young modulus was 140 ± 29 GPa, fracture toughness K1C=10.2 MPa·m0.5compression strength 700 MPa and bending strength 500 MPa. After 1000 hours of exposition at 600 °C the oxide film (containing mainly Al2O3 and TiO2) formed on the surface and material demonstrated a higher oxidation resistance than chromium ferrite steels. Due to the surface oxidation the defects self-healing took place and the bending strength of the porous Ti3AlC2 (22% porosity) after exposition for 3 h at 600 oC in air slightly (for 3%) increased as compared to that at 20 oC. Besides, the porous Ti3AlC2 material resisted to high-temperature creep and after being kept in H2 at 600 °C for 3h its bending strength reduced by 5 %.

Study of the Thermal Stability and Mechanical Characteristics of MAX Phases of Ti-Al-C(N) System and their Solid Solutions

The DTA and TG study in air of Ti2Al (C1-xNx) and Ti3AlC2 synthesized under Ar 0.1 MPa pressure and densified in thermobaric conditions at 2 GPa, 1400 °C, for 1 h showed that the increase of the amount of TiC layers in Ti-Al-C MAX phases structures leads to the increase of their stability against oxidation: 321 MAX phase Ti3AlC2 are more stable than Ti2AlC and Ti2Al (C1-xNx) solid solutions both before and after thermobaric treatment. The oxide film formed on the surface of the highly dense (ρ=4.27 g/cm3, porosity 1 %) material based on nanolaminated MAX phase Ti3AlC2 (89 % Ti3AlC2, 6 % TiC, 5 % Al2O3) manufactured by hot pressing (at 30 MPa) made the material highly resistant in air at high temperatures: after 1000 hours of exposition at 600 °C it demonstrated a higher resistance to oxidation than chromium ferrite steels (Crofer GPU and JDA types). Due to the surface oxidation self-healing of defects took place. Besides, the Ti3AlC2 material demonstrated resistance against high-temperature creep and after being kept in H2 at 600 °C for 3h its bending strength reduced by 5 % only. At room temperature the Ti3AlC2 bulk exhibited microhardness Hμ = 4.6 GPa (at 5 N), hardness HV50 = 630 (at 50 N ) and HRA = 70 (at 600 N), Young modulus was 140 ± 29 GPa, bending strength =500 MPa, compression strength 700 MPa, and fracture toughness K1C=10.2 MPa·m0.5.

Evidence for Symmetry Reduction in Ti3(Al1−δCuδ)C2 MAX Phase Solid Solutions

Ti3[Al1-δCuδ]C2 MAX phase solid solutions have been synthesized by sintering compacted Ti3AlC2-Cu composites produced by mechanical milling. Using X-ray and neutron diffraction techniques, it is demonstrated that the Cu mixing into the Al site is accompanied by lattice distortion, which leads to symmetry reduction from a hexagonal to a monoclinic structure. Such symmetry reduction likely results from this mixing through deviation of the A-site position from the special (0, 0, 1/4) position within the P63/mmc space group of the original Ti3AlC2 structure. Moreover, it is demonstrated that the Cu admixture into the A site can be adjusted from the composition of the reactant mixture. The lattice parameter variation of the solid solution compounds, with 10-50 atom % Cu in the A site, is found to be consistent with Vegards law.