We demonstrated size control of Au nanoparticles by heat treatment and their use as a catalyst for single-walled carbon nanotube (SWNTs) growth with narrow size distribution. We used uniformly sized Au nanoparticles from commercial Au colloid, and intentionally decreased their size through heat treatment at 800 oC under atmospheric Ar ambient. ST-cut quartz wafers were used as growth substrates to achieve parallel alignment of the SWNTs and to investigate the size relationship between Au nanoparticles and SWNTs. After the SWNTs were grown via chemical vapor deposition using methane gas, it was found that a high degree of horizontal alignment can be obtained when the particle density is low enough to produce individual SWNTs. The diameter of the Au nanoparticles gradually decreased from 3.8 to 2.9 nm, and the mean diameter of the SWNTs also changed from 1.6 to 1.2 nm for without and 60 min heat treatment, respectively. Raman results reconfirmed that the prolonged heat treatment of nanoparticles yields thinner tubes with narrower size distribution. This work demonstrated that heat treatment can be a straightforward and reliable method to control the size of catalytic nanoparticles and SWNT diameter.
We present a method of graphene synthesis with high thickness uniformity using the thermal chemical vapor deposition (TCVD) technique; we demonstrate its application to a grid supporting membrane using transmission electron microscope (TEM) observation, particularly for nanomaterials that have smaller dimensions than the pitch of commercial grid mesh. Graphene was synthesized on electron-beam-evaporated Ni catalytic thin films. Methane and hydrogen gases were used as carbon feedstock and dilution gas, respectively. The effects of synthesis temperature and flow rate of feedstock on graphene structures have been investigated. The most effective condition for large area growth synthesis and high thickness uniformity was found to be 1000˚C and 5 sccm of methane. Among the various applications of the synthesized graphenes, their use as a supporting membrane of a TEM grid has been demonstrated; such a grid is useful for high resolution TEM imaging of nanoscale materials because it preserves the same focal plane over the whole grid mesh. After the graphene synthesis, we were able successfully to transfer the graphenes from the Ni substrates to the TEM grid without a polymeric mediator, so that we were able to preserve the clean surface of the as-synthesized graphene. Then, a drop of carbon nanotube (CNT) suspension was deposited onto the graphene-covered TEM grid. Finally, we performed high resolution TEM observation and obtained clear image of the carbon nanotubes, which were deposited on the graphene supporting membrane.