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J Nanosci Nanotechnol. 2012 Mar;12(3):2424-36.

Optimized CVD production of CNT-based nanohybrids by Taguchi robust design.

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Dept. of Mechanics and Materials, Univ. "Mediterranea" of Reggio Calabria, I-89122 Reggio Calabria, Italy.


Taguchi's robust design method is for the first time employed to optimize many aspects of the production of nanohybrids based on C nanotubes by iron-catalyzed chemical vapor deposition in i-C4H10 + H2 atmosphere. By analyzing the outcomes of the catalytic process in terms of selectivity, carbon yield, purity and crystalline arrangement of the hybrid-forming nanotubes, the influence is ranked of the following parameters: synthesis temperature (500-700 degrees C), support material (alumina, magnesia or sodium-exchanged montmorillonite), calcination- (450-750 degrees C) and reduction-(500-700 degrees C) temperatures of the 15 wt% Fe-catalyst. In the experiments initially performed for this purpose, the growth process had, on average, scarce selectivity (2 in a scale 1-5) and poor yield (130 wt%); carbonaceous deposits exhibited unsatisfactory graphitization degree (Raman D/G intensity ratio > 1.5) and contained large amounts of metal impurities (14 wt%) and amorphous carbon (5 wt%). The indications emerging from Taguchi approach to the process optimization are critically examined. The experimental conditions chosen for carrying out test experiments allow achieving excellent selectivity (5) or large yield (760 wt%), hybrids with well-graphitized nanotubes (D/G intensity ratio < 0.6), nearly free of metallic (0.3 wt%) or amorphous (0.4 wt%) inclusions, with consequent possibility of satisfying the different requisites that the specific application to be addressed may require.

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