Real-time acoustic sensing and control of metalorganic chemical vapor deposition precursor concentrations delivered from solid phase sources

We have investigated the performance and potential benefit of acoustic sensing for real-time monitoring and closed loop control of binary gas mixture compositions delivered from low vapor pressure metalorganic sources. Two solid phase sources were investigated in the presence of H 2 as a carrier gas: (1) trimethylindium (TMI) and (2) bis(cyclopentadienyl) magnesium ( Cp 2 Mg ) , which have room temperature ( 25 ° C ) vapor pressures of 2.5 and 0.04 Torr , respectively. An acoustic sensor was implemented on the gas feed line to measure the concentration-dependent speed of sound in the gas mixture. This enabled sensitivity and control at precursor levels as low as 0.6 ppm in H 2 . Closed loop process control was implemented to maintain TMI and Cp 2 Mg concentration target in the presence of intentionally introduced long term temperature drifts. Despite induced variations of the precursor vapor pressure up to 50 % , the delivered composition was controlled to within ± 0.15 % for TMI (at 0.5 mol % set point) and ± 0.3 % for Cp 2 Mg (at 0.01 mol % set point). Short term variability could also be substantially reduced by the control scheme. This work demonstrates the feasibility of sensor-driven control systems for stable delivery of low vapor pressure, normally problematic precursor materials. In turn, this opens the door to utilization of a broader range of species which can be synthesized as chemical precursors.