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Sonolysis induced decomposition of metal carbonyls: kinetics and product characterization |
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| Authors: | Mahajan Devinder Papish Elizabeth T Pandya Kaumudi |
| Institution: | a Department of Energy Sciences and Technology, Brookhaven National Laboratory, Building 815, Upton, NY 11973-5000, USA b Department of Materials Science and Engineering, Stony Brook University, Stony Brook, NY 11794-2275, USA c Department of Chemistry, Salisbury University, Salisbury, MD 21801, USA d SFA, Advanced Technology Division, Largo, MD 20774, USA |
| Abstract: | The decomposition kinetics of Fe(CO)5 and Mo(CO)6 induced by sonolysis in hexadecane solvent was studied as a function of temperature (303–343 K) under an inert atmosphere. The decomposition data, obtained over at least two half lives in most of the runs, yielded first-order rate constant (k) values with correlation co-efficient (R2)>0.95. The products were characterized by various spectroscopic techniques. The transmission electron microscopy (TEM) yielded images from which the mean particle diameter (MPD) of  10 nm for Fe and <3 nm for Mo were estimated. The generation of amorphous Fe and semi-crystalline Mo particles was determined from line broadening and corresponding d-spacing values in the X-ray diffraction (XRD) spectra. The XAFS/XANES data were consistent with the production of Fe(0) metal but carbided Mo (Mo2C). The one-step production of high-yield pyrophoric products demonstrated the applicability of sonolysis to effectively produce gram-quantity of zero-valent metals. |
| Keywords: | Nano synthesis Sonolysis Metal carbonyls Decomposition kinetics |
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