Formation of Thermally Stable, High-Areal-Density, and Small-Diameter Catalyst Nanoparticles via Intermittent Sputtering Deposition for the High-Density Growth of Carbon Nanotubes

Nanomaterials (Basel). 2022 Jan 24;12(3):365. doi: 10.3390/nano12030365.


We report the formation of thermally stable catalyst nanoparticles via intermittent sputtering deposition to prevent the agglomeration of the nanoparticles during thermal chemical vapor deposition (CVD) and for the high-density growth of carbon nanotubes (CNTs). The preparation of high-areal-density and small-diameter catalyst nanoparticles on substrates for the high-density growth of CNTs is still a challenging issue because surface diffusion and Ostwald ripening of the nanoparticles induce agglomeration, which results in the low-density growth of large-diameter CNTs during high-temperature thermal CVD. Enhancing the adhesion of nanoparticles or suppressing their diffusion on the substrate to retain a small particle diameter is desirable for the preparation of thermally stable, high-areal-density, and small-diameter catalyst nanoparticles. The intermittent sputtering method was employed to deposit Ni and Fe metal nanoparticles on a substrate for the synthesis of high-areal-density CNTs for Fe nanoparticle catalyst films. The metal particles deposited via intermittent sputtering with an interval time of over 30 s maintained their areal densities and diameters during the thermal CVD process in a vacuum for CNT synthesis. An interval of over 30 s was expected to oxidize the metal particles, which resulted in thermal stability during the CVD process. The intermittent sputtering method is thus a candidate process for the preparation of thermally stable catalyst films for the growth of a high density of long CNTs, which can be combined with the present CNT production process.

Keywords: XRR; agglomeration; annealing; carbon nanotube forest; carbon nanotubes; catalyst particles; electric conductance; intermittent sputtering; magnetron sputtering deposition; oxidation; thermal CVD.