Closed-loop control of laser assisted chemical vapor deposition growth of carbon nanotubes

Laser-assisted chemical vapor deposition growth is an attractive mask-less process for growing locally aligned nanotubes in selected places on temperature sensitive substrates. An essential parameter for a successful and reproducible synthesis of nanotubes is the temperature during growth. Here, we demonstrate a temperature feedback control mechanism based on the dynamic, in situ monitoring of the infrared radiation coupled with reflectivity information. With the information provided by these sensors, an infrared laser, focused on a silicon substrate covered with aluminum-oxide and iron catalyst layers, can be controlled. The growth takes place in a gaseous mixture of argon (carrier gas), hydrogen (process gas), and ethylene (carbon-containing gas). Scanning electron microscopy and Raman spectroscopy analysis demonstrate the excellent reproducibility of the closed-loop control process over multiple experiments. Furthermore, we developed a unique method to identify the onset for catalyst formation and activation by monitoring the fluctuation of the reflected laser beam.