26 3 3a x ray lattice parameters of the tis stock

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Unformatted text preview: k Powder . . . . . . . . . . . . . . . . . . . . . . . . . . . 27 2 3-3(b) X-ray .Lattice Parameters Group A samples (quenched from 800 C ) . . . . . . . 28 3-3(c) X-ray Lattice Parameters Group B samples (quenched from 1000 C) . . . . . . 29 3-4 X-ray Results from Group C Annealed from 1000 C) . . . . . . . . . . . . . . . . . . . . . . . 31 CHAPTER 4 DIFFERENTIAL SCANNING CALORIMETRY . . . . . . . . . . . . . . . . . . 33 General Discussion . . . . . . . . . . . . . . Two Standard Methods of DSC Theory of Operation . . . . . . . . Typical DSC Curves . . . . . . . . . Modifications .............. v PAGE 4 -6 Temperature Calibration. . . . . . . . . . . . . . . . . . . . . . 4 1 4-7(a) Cell Calibration Coefficient ( E ) . . . . . . . . . . . . 4 4 4-7(b) Cell Coefficient Check . . . . . . . . . . . . . . . . . . . . . . 46 CHAPTER 5 DSC RESULTS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4 8 5- 1 DSC Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48 5-2 Specific Heat Measurements of Pure T iS 2 ..... 49 5-3(a) DSC Transition Peaks for Sample A (quenched from 800 C) . . . . . . . . . . . . . . . . . . . . . . . 5 0 5-3(b) Sample A (quenched from 800 C) Low Temperature DSC . . . . . . . . . . . . . . . . . . . . . . . . . 51 5-4(a) Sample B (quenched from 1000 C) .DSC . . . . . . . 5 2 5-4(b) Sample B (quenched from 1000 C) Low Temperature DSC . . . . . . . . . . . . . . . . . . . . . . . . . 5 3 5-4(c) Low Temperature X-ray Patern (quenched from 1 000 C ) . . . . . . . . . . . . . . . . . . . . . . 5 3 5-5(a) Specific Heat Measurement ................... 54 5-5(b) Specific Heat Procedure and Results . . . . . . . . . 55 5-5(c) specific Heat Procedure and Results . . . . . . . . . 55 vi P AGE 5 - 5 ( d ) S pecific H eat o f Pure T iS2 . . . . . . . . . . . . . . . . . . 56 5 -5(e) S pecific Heat Comparison w ith C alculations by S chick et. al. (52) . . . . . . . . . 57 C HAPTER 6 C ONCLUSIONS ........... A PPENDIX DSC PROG...
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