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sulfur ( 38, 4 1).
The ampoule containing titanium sponge at one end and
sulfur at the other end was then placed horizontally in a two
zone furnace. The ampoule was differentially heated from 255 C a nd 100 C ( titanium end and sulfur end respectively) to
5 1 5 C a nd 3 6 0 C at a rate of 1 . 7 5 C /hour i n order to allow s ome time for heat dissipation from the exothermic reaction of
the titanium and sulfur combining to form T iS 2 M ills (39)
' reports that temperatures of several thousand degrees may
result when elemental titanium and sulfur are reacted
directly. The ends of the ampoule were held at the high temperature limits ( 5 1 5 C a nd 3 6 0 C) for 48 h ours in order to
allow any remaining material to react. Finally the ampoule was removed from the furnace and shaken using an ultrasonic
vibrator to break up any lumps of material and thoroughly mix
the reacted product. The ampoule was again placed in an oven at 515 C f or 48 h ours to insure that all elements were
completely reacted. The total mass of the sample contained P age - 1 4 - w ithin the quartz ampoule was 7 0 grams.
The lattice parameters of the resulting powder were
determined using X-ray diffraction patterns of the powders.
The values of the lattice parameters (a
c = 5 . 6 9 1 2 0 .004 a) = 3 . 4 0 6 2 0.002 a s determined from the X-ray data agree with the lattice parameters of stoichiometric T iS
by Thompson e t . a l . (57).
determined to be 5 A, - 2 r eported T he grain size of the powder was 15 u m. i n the basal plane by 1 3 u m. - t hick using photographs of the powder taken with a scanning
2-2 ( c) Titanium Disulphide
TiS 2 - S toichiometry i s usually a metal rich compound with the excess titanium atoms residing in the Van der Waals gap between the
S-Ti-S layers. Winn e t . al. ( 53) d etermined the chemical diffusion coefficients of sodium and lithium in Na Ti S
a nd L ixTi S f rom electrochemical pulse experiments and
f ound that the degree of intercalation of T iS is highl...
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- Fall '09
- Diffraction, Sulfur, Intercalation, lattice parameters