Apparatus for Scalable Functionalization of Single-Walled Carbon Nanotubes via the Billups-Birch Reduction
Zhang, Kevin S.
Gangoli, Varun Shenoy
Ainscough, Thomas J.
Hauge, Robert H.
Adams, W. Wade
Barron, Andrew R.
A prototype design of a reactor for scalable functionalization of SWCNTs by the reaction of alkyl halides with Billups-Birch reduced SWCNTs is described. The Hauge apparatus is designed to allow for the safe handling of all the reagents and products under an inert atmosphere at controlled temperatures. The extent of reaction of Li/NH3 solution with the SWCNTs is measured in-situ by solution conduction, while homogenous mixing is ensured by the use of a homogenizer, and thermocouple are placed at different heights within the reactor flask. Addition of an alkyl halide yield alkyl-functionalized SWCNTs, which may be isolated by solvent extraction leaving a solid sample that is readily purified by hydrocarbon extraction. As an example, reaction of SWCNT/Li/NH3 with 1-iododecane yields dodecane-functionalized SWCNTs (C12-SWCNTs), which have been characterized by TG/DTA, XPS, and Raman spectroscopy. Sample extraction during the reaction allows for probing of the rate of the reaction in order to determine the end point of the reaction, which for C12-SWCNTs (at −78 °C) is 30 min.
carbon nanotube; lithium; reduction; functionalization; ammonia