First part presented in the research is purification of MWCNTs. The MWCNTs of high yield and no damage are obtained by microwave heating system with acid treatment. In the microwave system, acid rapidly absorbs microwave heat and energy and completely dissolve metals for purification without damage and of high quality.
The processing time of the microwave-assisted and acid treated system to dissolve metals in MWCNTs is below one hour. After purification, the amounts of residual catalyst metals in samples reduced from 30wt% to 5.15wt% for ECR-synthesized MWCNTs. The results show that multi-walled carbon nanotubes of no damage and with metals about 5wt% are obtained.
Investigated of purification efficiency of MWCNTs synthesized by thermal chemical vapor deposition with different parameters by using TGA, SEM, TEM and Raman spectroscopy and MWCNTs of high purity are expected. The results show that the purification efficiency increases with increasing acid treatment time. The amount of residual catalysts in purified samples was reduced to 0.1% after digestion for 90 min at 210°C. Microwave heating method has excellent prospect to yield carbon nanotubes of high purity if carbon nanotubes are small and uniform in diameter. In conclusion, microwave heating method may have great potential in mass purification.
Large amount of purified CNTs with high quality would be applied to more intrinsic studies and industrial applications.
The contents of metallic catalysts in the as-prepared MWCNTs can be effectively eliminated from 10.39 wt% to 1.515 wt% within 15 minute purification time at 120°C of 250W power. A possible reaction model was apparently proposed to describe this reaction, that is, the nano-scale metallic catalysts embedded at the tip end of MWCNTs could absorb microwave radiation energy in electromagnetic field by
magnetic resonance and interfacial electric polarization, and then form a localized hot area to combine with hot-surface effects around the tip-liquid interface of CNTs and significantly accelerate the reaction rate in the wall of CNTs near the tip.
Although microwave technology has been extensively applied in our daily life, there might be a great potential in microwave chemistry to apply microwave radiation energy on traditional chemical reaction processes. However, further intensive studies are expected to acquire complete understandings of the microwave-assisted chemical reaction.
In the second part of this thesis, Pt nanoparticles on CNTs were prepared by rapid and uniform microwave heating, which provided a more homogeneous temperature gradient for the quick nucleation and growth of Pt particles. The effects of temperature and time on the synthesis of Pt in microwave-assisted methods were clarified by individual careful control of the two factors, and the results, first reported by this work, showed the domination of temperature over the reaction time. Pt/CNTs electrocatalysts with suitable narrow distribution size and highly dispersed Pt nanoparticles were synthesized by a one-step microwave-assisted polyol method by adding proper amount of SDS to the synthesis solution. It was found that SDS in the solution could be used as a good agent to wrap a lot of PVP-adsorbed Pt nanoparticles around MWCNTs side by side without particle agglomeration, and the loading of Pt on CNTs could exceed 50 wt%, higher than the 20 wt% or below of conventional or other microwave methods without SDS addition. The synthesis method proposed in this paper is simple and fast, and has great potential to be developed for the preparation of other high loading supported metal and alloy systems.
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