Discovery of wall-selective carbon nanotube growth conditions via automated experimentation

Applications of carbon nanotubes continue to advance, with substantial progress in nanotube electronics, conductive wires, and transparent conductors to name a few. However, wider application remains impeded by a lack of control over production of nanotubes with the desired purity, perfection, chirality, and number of walls. This is partly due to the fact that growth experiments are time-consuming, taking about 1 day per run, thus making it challenging to adequately explore the many parameters involved in growth. We endeavored to speed up the research process by automating CVD growth experimentation. The adaptive rapid experimentation and in situ spectroscopy CVD system described in this contribution conducts over 100 experiments in a single day, with automated control and in situ Raman characterization. Linear regression modeling was used to map regions of selectivity toward single-wall and multiwall carbon nanotube growth in the complex parameter space of the water-assisted CVD synthesis. This development of the automated rapid serial experimentation is a significant progress toward an autonomous closed-loop learning system: a Robot Scientist.