Controlling the size and the activity of Fe particles for synthesis of carbon nanotubes

Published: November 01, 2012


See-Wee Chee, Renu Sharma


The properties of carbon nanotubes (CNTs) are controlled by their structure and morphology. Therefore, their selective synthesis, using catalytic chemical vapor deposition, requires precise control on a number of parameters including the size and activity of the catalyst nanoparticles. Previously, an environmental scanning transmission electron microscope (ESTEM) has been used to demonstrate that electron beam induced decomposition (EBID) of Fe containing precursor molecules can be used to selectively deposit Fe catalyst nanoparticles that are active for CNT growth. We have extended these in situ ESTEM observations to further our understanding of the EBID parameters, such as electron beam current, deposition time, and substrate temperature, that control the size and placement of Fe catalyst particles for two precursors, namely diiron nonacarbonyl (Fe2(CO)9) and ferrocene (Fe(C5H5)2). We found that the diameter of deposited particles increased with increasing deposition time. Electron energy-loss spectra,collected during deposition, show the incorporation of C in the Fe particles. The C content decreased as the substrate temperature was increased and was negligible at 100 C for Fe2(CO)9. However, C and Fe were co-deposited at all temperatures (up to 450 C) when Fe(C5H5)2 was used as an iron source. After deposition, the substrate was heated to the CNT growth temperature in flowing hydrogen to remove the co-deposited C, which was an important step to activate the deposited Fe catalyst for the growth using acetylene. Our measurements revealed that the Fe nanoparticles fabricated from Fe2(CO)9 had higher activity for CNT growth compared to the ones fabricated using Fe(C5H5)2. The deposited particles from Fe(C5H5)2 formed a core-shell structure with Fe surrounded by graphitic carbon at 300 °C to 400 °C. We also found that the co-deposited carbon in this case could not be removed by heating in hydrogen. We speculate that the reduced activity is due to the C content in the
Citation: Micron
Volume: 43
Issue: 11
Pub Type: Journals

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Carbon nanotubes, catalyst activity, electron beam induced deposition, in situ electron microscopy, iron catalysts
Created November 01, 2012, Updated February 19, 2017