Next Article in Journal
Graphene Encapsulated Silicon Carbide Nanocomposites for High and Low Power Energy Storage Applications
Previous Article in Journal
Activated Carbon, Carbon Nanotubes and Graphene: Materials and Composites for Advanced Water Purification
Previous Article in Special Issue
Catalyst Residue and Oxygen Species Inhibition of the Formation of Hexahapto-Metal Complexes of Group 6 Metals on Single-Walled Carbon Nanotubes
Article Menu
Issue 2 (June) cover image

Export Article

Open AccessArticle

Apparatus for Scalable Functionalization of Single-Walled Carbon Nanotubes via the Billups-Birch Reduction

Smalley-Curl nanoCarbon Center, Rice University, Houston, TX 77005, USA
Department of Chemistry, Rice University, Houston, TX 77005, USA
Energy Safety Research Institute, Swansea University Bay Campus, Swansea SA1 8EN, UK
Department of Materials Science and Nanoengineering, Rice University, Houston, TX 77005, USA
Died 17 March 2016.
Author to whom correspondence should be addressed.
Received: 25 May 2017 / Revised: 13 June 2017 / Accepted: 14 June 2017 / Published: 17 June 2017
Full-Text   |   PDF [3872 KB, uploaded 17 June 2017]   |  


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. View Full-Text
Keywords: carbon nanotube; lithium; reduction; functionalization; ammonia carbon nanotube; lithium; reduction; functionalization; ammonia

Graphical abstract

This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited (CC BY 4.0).

Share & Cite This Article

MDPI and ACS Style

Pham, D.; Zhang, K.S.; Lawal, O.; Ghosh, S.; Gangoli, V.S.; Ainscough, T.J.; Kellogg, B.; Hauge, R.H.; Adams, W.W.; Barron, A.R. Apparatus for Scalable Functionalization of Single-Walled Carbon Nanotubes via the Billups-Birch Reduction. C 2017, 3, 19.

Show more citation formats Show less citations formats

Note that from the first issue of 2016, MDPI journals use article numbers instead of page numbers. See further details here.

Article Metrics

Article Access Statistics



[Return to top]
C EISSN 2311-5629 Published by MDPI AG, Basel, Switzerland RSS E-Mail Table of Contents Alert
Back to Top