Chemical characterization of gallium droplets grown by LP-MOCVD.

International audience; This study is concerned with the chemical characterization of metallic gallium droplets, obtained on silicon (1 0 0) substrates with a single growth step, by the LP-MOCVD technique with TMGa like precursor. These structures are characterized by SIMS, XPS and TEM. The analyses results lead to a structure proposition for the droplets. The core is composed of metastable metallic gallium with a non-negligible carbon quantity probably coming from incomplete precursor decomposition. The outer part, composed of gallium oxide maintains the structure stability. Covering of the substrate by a thin gallium layer of gallium compounds is observed.

In-situ time resolved X-ray diffraction study of the formation of the nanocrystalline NbAl3 phase by mechanically activated self-propagating high-temperature synthesis reaction

The mechanically activated self-propagating high-temperature synthesis (MASHS) technique was used to produce a NbAl3 intermetallic compound. This process results from the combination of two steps: a mechanical activation of the Nb 3Al powder mixture which is followed by a self-propagating high-temperature synthesis (SHS) reaction, induced by the exothermal character of the reaction Nb3Al. An original experiment was designed to study in-situ the formation of the NbAl3 phase in the combustion front: time-resolved X-ray diffraction coupled with an infrared imaging technique and a thermocouple measurement were performed to monitor the structural and thermal evolution during the SHS reaction. Ow…

In-situ time-resolved X-ray diffraction experiments applied to self-sustained reactions from mechanically activated mixtures

Resume . Le procede MASHS (Mechanically activated self-propagating high-temperature synthesis) apparait etre un procede alternatif interessant pour elaborer des materiaux tels que des ceramiques, des composites ou des intermetalliques. La formation au cours d'une reaction de combustion autoentretenue d'intermetalliques, tels que NbAlj et M0S12, a ete suivie in-situ et en temps reel en couplant la diffraction des rayons X, produits par le rayonnement synchrotron (Ligne D43, LURE - Orsay) et, une thermographie infrarouge. A partir de temps d'acquisition tres courts (de 30 ms a 100ms par diffractogrammes), il a ete possible de determiner simultanement les evolutions structurales et thermiques.…

Synthesis of nanocrystalline NbAl3 by mechanical and field activation

Abstract The mechanically-activated, field-activated, and pressure-assisted synthesis (MAFAPAS) process, which combines the simultaneous synthesis and densification of nanophase materials, was utilized to produce nanocrystalline NbAl3 material from Nb+3Al mechanically activated powders. Nb+3Al elemental powders were co-milled for a short time in a specially designed planetary ball mill to obtain nanoscale distributed reactants but to avoid the formation of any product phases. These were then subjected to high AC currents (1500–1650 A) and uniaxial pressures (56–84 MPa). Under these conditions, a reaction is initiated by field activation and completed within a short period of time (3–6 min).…

Study of the mechanism of the NbAl3 formation by MASHS reaction using synchrotron time-resolved XRD analyses coupled with IR observations

Synthesis of niobium aluminides using mechanically activated self-propagating high-temperature synthesis and mechanically activated annealing process

The mechanically activated self-propagating high-temperature synthesis (MASHS) technique and the mechanically activated annealing process (M2AP) were used to produce NbAl3 intermetallic compound. The MASHS process results from the combination of two steps: first, a mechanical activation of the Nb 3Al powders mixture; second, a self-propagating high-temperature synthesis (SHS). The M2AP process also results from the combination of two steps: the first is the same; the second consists of the annealing of as-milled powders. Based on X-ray diffraction (XRD) analysis, scanning electron microscopy (SEM) and X-ray energy dispersive spectroscopy (EDXS), the as-milled powders, MASHS, and M2AP end-pr…

Growth and characterization of AP-MOCVD iron doped titanium dioxide thin films

Abstract Atmospheric pressure metal organic chemical vapor deposition (AP-MOCVD) was used to prepare iron doped titanium dioxide thin films. Thin films, between 40 and 150 nm thick, were deposited on Si, SiO 2 and Al 2 O 3 substrates using titanium tetra isopropoxide and ferrocene as metal organic precursors. TiO 2 iron doping was achieved in the range of 1–4 at.%. The film morphology and thickness, polycrystalline texture and doping content were studied using respectively scanning electron microscopy (SEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). The influence of growth temperature, deposition time, substrate type and dopant partial pressure were studied. Electr…

Oxidation behavior of γ-TiAl coated with zirconia thermal barriers

Abstract The applicability of the thermal barrier coating concept, which is an established concept for Ni-base alloys, was investigated for the first time for γ-TiAl. As potential bond coats, the following surface treatments were applied: Al-diffusion coating, Al-diffusion coating combined with short term pre-oxidation in air, short term pre-oxidation in oxygen of a rough surface finish γ-TiAl sample without aluminide coating. For the purpose of lowering the temperature of the γ-TiAl substrate surface, and thus, to prolong the life time, a zirconia thermal barrier coating (TBC) was applied on top of the above-mentioned modified TiAl surfaces. Oxidation resistance of the modified γ-TiAl allo…

"Study of Niobium Aluminide synthesis using MASHS and M2AP processes"

Role of the Microstructure on the High Temperature Oxidation Properties of the Intermetallic Compound NbAl<sub>3</sub>

The influence of the NbAl 3 microstructure on its oxidation mechanism was investigated in air under atmospheric pressure over the temperature range 500-1080°C. Different processing techniques as induction melting and mechanically-activated annealing processes (M2AP) were used to produce the intermetallic compound NbAl 3 . A protective external alumina scale grew only on Al-enriched NbAl 3 between 700 and 1080°C. Stoichiometric NbAl 3 exhibited the pesting phenomenon between 550-900°C, whereas a non protective lamellar oxide scale formed above 900°C. The proposed oxidation mechanism explains these observations which are in agreement with the oxidation study of powders with different crystall…

Investigations of the formation mechanism of nanostructured NbAl3 via MASHS reaction

Abstract The nanostructured NbAl3 intermetallic compound was synthesized using the mechanically-activated self-propagating high-temperature synthesis (MASHS) technique. This process results from the combination of two steps: a short duration ball-milling of a pure elemental Nb+3Al powder mixture followed by a self-propagating high-temperature synthesis (SHS) reaction induced by the Nb+3Al reaction exothermicity. Synchrotron time-resolved XRD coupled with a 2D infrared camera were used to investigate the structural and thermal evolutions during the SHS reaction, and to study in situ the mechanism of NbAl3 formation. The influence of the incoming heat flux and the mechanical activation effect…