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Overcoming Catalyst Residue Inhibition of the Functionalization of Single-Walled Carbon Nanotubes via the Billups–Birch Reduction

Kevin S. Zhang, David Pham, Olawale Lawal, Saunab Ghosh, Varun Shenoy Gangoli, Preston Smalley, Katherine Kennedy, Bruce E. Brinson, W. Edward Billups, Robert H. Hauge, W. Wade Adams, Andrew Barron Orcid Logo

ACS Applied Materials & Interfaces, Volume: 9, Issue: 43, Pages: 37972 - 37980

Swansea University Author: Andrew Barron Orcid Logo

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DOI (Published version): 10.1021/acsami.7b12857

Abstract

The Billups–Birch Reduction chemistry has been shown to functionalize single-walled carbon nanotubes (SWCNTs) without damaging the sidewalls, but has challenges in scalability. Currently published work uses a large mole ratio of Li to carbon atoms in the SWCNT (Li:C) to account for lithium amide for...

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Published in: ACS Applied Materials & Interfaces
ISSN: 1944-8244 1944-8252
Published: 2017
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URI: https://cronfa.swan.ac.uk/Record/cronfa36209
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spelling 2017-12-11T13:36:52.9705659 v2 36209 2017-10-24 Overcoming Catalyst Residue Inhibition of the Functionalization of Single-Walled Carbon Nanotubes via the Billups–Birch Reduction 92e452f20936d688d36f91c78574241d 0000-0002-2018-8288 Andrew Barron Andrew Barron true false 2017-10-24 CHEG The Billups–Birch Reduction chemistry has been shown to functionalize single-walled carbon nanotubes (SWCNTs) without damaging the sidewalls, but has challenges in scalability. Currently published work uses a large mole ratio of Li to carbon atoms in the SWCNT (Li:C) to account for lithium amide formation, however this increases the cost and hazard of the reaction. We report here the systematic understanding of the effect of various parameters on the extent of functionalization using resonant Raman spectroscopy. Addition of 1-iodododecane yielded alkyl-functionalized SWCNTs, which were isolated by solvent extraction and evaporation, and purified by a hydrocarbon wash. The presence of SWCNT growth catalyst residue (Fe) was shown to have a strong adverse effect on SWCNT functionalization. Chlorination-based SWCNT purification reduced the amount of residual Fe, and achieve a maximum ID/IG ratio using a Li:C ratio of 6:1 in a reaction time of 30 min. This result is consistent with published literature requiring 20-fold mole equivalents of Li per mole SWCNT with a reaction time of over 12 h. This new understanding of the factors influencing the functionalization chemistry will help cut down material and process costs, and also increase the selectivity of the reaction toward the desired product. Journal Article ACS Applied Materials & Interfaces 9 43 37972 37980 1944-8244 1944-8252 ammonia; Billups−Birch reduction; carbon nanotube; iron oxide; lithium 31 12 2017 2017-12-31 10.1021/acsami.7b12857 COLLEGE NANME Chemical Engineering COLLEGE CODE CHEG Swansea University 2017-12-11T13:36:52.9705659 2017-10-24T09:16:53.6023967 Faculty of Science and Engineering School of Engineering and Applied Sciences - Chemical Engineering Kevin S. Zhang 1 David Pham 2 Olawale Lawal 3 Saunab Ghosh 4 Varun Shenoy Gangoli 5 Preston Smalley 6 Katherine Kennedy 7 Bruce E. Brinson 8 W. Edward Billups 9 Robert H. Hauge 10 W. Wade Adams 11 Andrew Barron 0000-0002-2018-8288 12 0036209-24102017092009.pdf zhang2017(7).pdf 2017-10-24T09:20:09.3530000 Output 1435084 application/pdf Accepted Manuscript true 2018-10-23T00:00:00.0000000 true eng
title Overcoming Catalyst Residue Inhibition of the Functionalization of Single-Walled Carbon Nanotubes via the Billups–Birch Reduction
spellingShingle Overcoming Catalyst Residue Inhibition of the Functionalization of Single-Walled Carbon Nanotubes via the Billups–Birch Reduction
Andrew Barron
title_short Overcoming Catalyst Residue Inhibition of the Functionalization of Single-Walled Carbon Nanotubes via the Billups–Birch Reduction
title_full Overcoming Catalyst Residue Inhibition of the Functionalization of Single-Walled Carbon Nanotubes via the Billups–Birch Reduction
title_fullStr Overcoming Catalyst Residue Inhibition of the Functionalization of Single-Walled Carbon Nanotubes via the Billups–Birch Reduction
title_full_unstemmed Overcoming Catalyst Residue Inhibition of the Functionalization of Single-Walled Carbon Nanotubes via the Billups–Birch Reduction
title_sort Overcoming Catalyst Residue Inhibition of the Functionalization of Single-Walled Carbon Nanotubes via the Billups–Birch Reduction
author_id_str_mv 92e452f20936d688d36f91c78574241d
author_id_fullname_str_mv 92e452f20936d688d36f91c78574241d_***_Andrew Barron
author Andrew Barron
author2 Kevin S. Zhang
David Pham
Olawale Lawal
Saunab Ghosh
Varun Shenoy Gangoli
Preston Smalley
Katherine Kennedy
Bruce E. Brinson
W. Edward Billups
Robert H. Hauge
W. Wade Adams
Andrew Barron
format Journal article
container_title ACS Applied Materials & Interfaces
container_volume 9
container_issue 43
container_start_page 37972
publishDate 2017
institution Swansea University
issn 1944-8244
1944-8252
doi_str_mv 10.1021/acsami.7b12857
college_str Faculty of Science and Engineering
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hierarchy_top_id facultyofscienceandengineering
hierarchy_top_title Faculty of Science and Engineering
hierarchy_parent_id facultyofscienceandengineering
hierarchy_parent_title Faculty of Science and Engineering
department_str School of Engineering and Applied Sciences - Chemical Engineering{{{_:::_}}}Faculty of Science and Engineering{{{_:::_}}}School of Engineering and Applied Sciences - Chemical Engineering
document_store_str 1
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description The Billups–Birch Reduction chemistry has been shown to functionalize single-walled carbon nanotubes (SWCNTs) without damaging the sidewalls, but has challenges in scalability. Currently published work uses a large mole ratio of Li to carbon atoms in the SWCNT (Li:C) to account for lithium amide formation, however this increases the cost and hazard of the reaction. We report here the systematic understanding of the effect of various parameters on the extent of functionalization using resonant Raman spectroscopy. Addition of 1-iodododecane yielded alkyl-functionalized SWCNTs, which were isolated by solvent extraction and evaporation, and purified by a hydrocarbon wash. The presence of SWCNT growth catalyst residue (Fe) was shown to have a strong adverse effect on SWCNT functionalization. Chlorination-based SWCNT purification reduced the amount of residual Fe, and achieve a maximum ID/IG ratio using a Li:C ratio of 6:1 in a reaction time of 30 min. This result is consistent with published literature requiring 20-fold mole equivalents of Li per mole SWCNT with a reaction time of over 12 h. This new understanding of the factors influencing the functionalization chemistry will help cut down material and process costs, and also increase the selectivity of the reaction toward the desired product.
published_date 2017-12-31T03:45:12Z
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score 11.017797

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