A new experimental setup for the time resolved x-ray diffraction study of self-propagating high-temperature synthesis

A new experimental setup for time resolved x-ray diffraction is described. Designed for the LURE H10 beamline and its 4 (+2) circles goniometer, it allows simultaneous recordings of x-ray patterns with a rate of 30 patterns per second, a maximum 2θ range of 120°, infrared thermography at the same rate, and thermocouples readings at a frequency of up to 3×104 Hz. Preliminary results obtained using this setup are presented, showing how it is possible to analyze a solid–solid or solid-liquid reaction. As an example, an in situ study of phase transformation and temperature evolution during the self-sustaining synthesis of an FeAl intermetallic compound starting from a mechanically activated mixture is investigated. The versatility of the setup was proved and could even be enhanced by the design of new sample holders, thus expanding its area of use at low cost.

[1]  D. Bétaille,et al.  H10:. A materials and high temperature beamline at LURE/DCI , 2001 .

[2]  E. Gaffet,et al.  Mechanical activation effect on the self-sustaining combustion reaction in the Mo-Si system , 2001 .

[3]  J. Gachon,et al.  Simultaneous IR and time-resolved X-ray diffraction measurements for studying self-sustained reactions. , 2000, Journal of synchrotron radiation.

[4]  E. Gaffet,et al.  Synthesis of niobium aluminides using mechanically activated self-propagating high-temperature synthesis and mechanically activated annealing process , 1999 .

[5]  E. Gaffet,et al.  Enhancement of self-sustaining reaction by mechanical activation: case of an FeSi system , 1999 .

[6]  F. Charlot,et al.  In situ synchrotron characterization of mechanically activated self-propagating high-temperature synthesis applied in Mo–Si system , 1999 .

[7]  F. Charlot,et al.  IN SITU TIME-RESOLVED DIFFRACTION COUPLED WITH A THERMAL I.R. CAMERA TO STUDY MECHANICALLY ACTIVATED SHS REACTION: CASE OF Fe-Al BINARY SYSTEM , 1999 .

[8]  J. Gachon,et al.  Real time X-ray diffraction study of the formation by SHS of the phases γ′ and H in the ternary system AlNiTi , 1997 .

[9]  E. Gaffet,et al.  Nanocrystalline MoSi2 phase formation induced by mechanically activated annealing , 1994 .

[10]  E. Gaffet,et al.  Solid state reaction induced by post-milling annealing in the FeSi system , 1993 .

[11]  J. Chevreul,et al.  Powder diffraction for solid state reaction studies , 1993 .

[12]  Rupp,et al.  Real-time probe of reaction centers in solid combustions on the subsecond time scale. , 1992, Physical review. B, Condensed matter.