Revisiting behaviour of monometallic catalysts in chemical vapour deposition synthesis of single-walled carbon nanotubes

A catalyst is essential for the controlled synthesis of single-walled carbon nanotubes (SWNTs) by chemical vapour deposition (CVD). However, it is difficult to observe these nanosized particles in their original forms and in a statistical manner, which has resulted in a vague understanding of the behaviours of these particles. We present a technique to solve this long-standing issue. The key is to have an MEMS fabricated suspended SiO 2 layer, which is thick enough to support catalyst deposition and nanotube growth but thin enough to allow electron beams to transit. On a 20 nm SiO 2 film, we confirm that catalyst can be observed at an atomic resolution, and the catalyst–SWNT junctions can also be routinely observed. As a demonstration of this technique, we revisited the behaviour of monometallic catalysts through a systematic investigation of the size, chemical state and crystal structure of particles before and after high-temperature CVD. The active catalyst is found to follow a tangential growth mode, while the inactive catalyst is divided into three mechanisms: size growth, metal loss and inappropriate precipitation. The latter two mechanisms were not possible to observe by previous techniques.