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The liquid sulfur m p 1 1 9 c f iowed t o the cooler

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Unformatted text preview: d 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 electron microscope. 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 x Y2 a nd L ixTi S f rom electrochemical pulse experiments and Y2 f ound that the degree of intercalation of T iS is highl...
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