Metal-organic (MO)CVD processes using three different precursors (Bi(tmhd) 3 , 3 , and Bi(o-tol) 3 ) have been investigated. Combined, thermal, and mass spectroscopic investigations have provided information on their thermal robustness during sublimation processes. In-situ Fourier-transform infrared (FTIR) measurements have allowed the monitoring of masstransported precursors during MOCVD experiments. Temperature windows of 190±277 C, 170±270 C, and 150±220 C have proved suitable for the efficient vaporization of Bi(tmhd) 3 , Bi(p-tol) 3 , and Bi(o-tol) 3 , respectively, even though aryl precursors have proved to be more stable than b-diketonate during the sublimation and transport processes.Above 350 C, decomposition during the MOCVD processes has been observed for all the precursors. In the case of Bi(tmhd) 3 and Bi(o-tol) 3 it involves the ligand fragmentation, while for Bi(p-tol) 3 , dissociation of the intact aryl ring seems to occur.