An orientationally disordered crystalline (ODIC) plastic phase (γ) was observed in Trimethylolpropane (TRMP) during heating by high resolution thermal and X-ray diffraction analyses. TRMP is a potential thermal energy storage material. The enthalpies of solid-solid (α → γ at 327.8 K) and fusion (γ → liquid at 332.7 K) transitions are 16.36 kJ/mol and 0.9 kJ/mol, respectively. Supercooling was observed during solidification of melts, and this supercooled γ phase began to transform to a metastable crystalline phase, designated as α , after 20 minutes at room temperature. The lattice parameters of the monoclinic α phase, obtained from this study, are: a = 0.8427(5), b = 0.9580(5), c = 0.9185(6) nm, β = 98.958(3) • @ 298 K with Z = 4. The ODIC high temperature FCC γ phase has a lattice parameter: a = 0.9274(3) nm @ 328 K with Z = 4. Differential scanning calorimetry, in-situ Bragg-Brentano X-ray diffractometry, and high temperature and resolution Guinier X-ray diffraction systems were used to determine these phase transitions.

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Metal carbonyls are important for chemical vapor deposition (CVD) of metals and alloys and formation of high surface area metallic particles which have potential applications as catalysts. Rhodium carbonyl [Rh6(CO)16] produces high surface area metallic particles whose structure has been reported as monoclinic (I2/a) with lattice dimensions, a=17.00(±0.03)Å, b=9.78(±0.02)Å, c=17.53(±0.03)Å and β=121°45' ± 30' at room temperature. Generally, metal carbonyl crystals dissociate under vacuum as carbonyl gas and decompose to metallic crystals and carbon monoxide at higher temperatures. However, the behavior of rhodium carbonyl crystals is different; they decompose directly to metallic rhodium without the formation of rhodium carbonyl gas in vacuum. Several residual fine grains of rhodium metal are found after the decomposition in vacuum at relatively low temperatures. The metallic samples of rhodium were obtained from vapor pressure experiments using torsion Knudsen-effusion apparatus. X-ray diffraction analyses performed on these grains showed severely broadened Bragg reflections indicative of small particle size and/or lattice microstrain. In this study, a comparison of lattice strains and domain sizes obtained by integral breadth and Fourier methods has been made. In addition a comparison of the lattice strains and domain sizes has been made between the Cauchy, Gaussian, Cauchy-Gaussian and Aqua integral breadth methods.