2 t he sealed ampoules were then shaken using an

Info iconThis preview shows page 1. Sign up to view the full content.

View Full Document Right Arrow Icon
This is the end of the preview. Sign up to access the rest of the document.

Unformatted text preview: m temperature and shaken vigorously in an attempt to break up any lumps of material and obtain a uniform mixture of any unreacted constituents then placed back into the oven for the remaining 4 - 8 d ay intercalation period. The final step in the preparation of the intercalated samples was to drop quench the ampoules (from 800 C - g roup A a nd 1 000 C - g roup B ) by dropping them into a beaker of cold tap water. The samples were then screened using a stainless steel sc'reen having 200 u m. holes to separate any remaining lumps of material before being tested. The resulting powders were in the form of hexagonal platelets having a typical size in the range. of 5 - 1 5 u m. x 1 - 3 u m . thick as determined from pictures taken using a scanning electron microscope. X-ray Fluorescence and X-ray data were then taken to verify the integrity and composition of the samples. P age - 23- C HAPTER 3 Sample Characterization 3-1 (a) XRF Sample Verification (GROUP A - q uenched from 800 C) X -ray fluorescence (XRF) spectra were obtained from of the A gxTiS2 p owder samples which were quench cooled f rom 8 0 0 C (group A ) a s a check of the ratio of Ag to T iS2. A S IEMENS KRISTALLOFLEX 2 X -ray generator was used to generate Z n K a ( 8.631 Kev.) and Z n K b ( 9 . 5 7 2 Kev.) X-rays. The energies of the emitted X-rays are characteristic of the element. The various (group A) powder samples ( 0 < x < 0 . 6 ) were placed on a polyester film ( < 4 u m. thick) over the incident Z n X-rays. A KEVEX-RAY 0800 S i(Li) d etector located 2 c m . from the sample perpendicular to the incident X-rays was used to detect the intensities of the fluorescent X-rays emitted from the sample. The data was collected using a NUCLEAR DATA ND-66 multi-channel analyzer with windows set up around the a nd silver L peaks. The intensities titanium K a' a' a o f the respective peaks are directly related to the weight sulfur K concentration of the element in the sample. Intensity ratios of S /Ti a nd A g/Ti w ere calculated from the intensity mea...
View Full Document

{[ snackBarMessage ]}

Ask a homework question - tutors are online