Nucleation of carbon-sulfur phases by manipulation of vertically-aligned mm-long films of iron-filled few-wall/multiwall carbon nanotubes

We report a novel investigation of the effects of sulfur-precursor concentration on the morphological, structural and magnetic properties of vertically aligned mm-long films of carbon nanotubes (CNTs) filled with Fe3C nanowires. Fabrication was carried out by sublimation and pyrolysis of ferrocene/s...

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Main Authors: Omololu Odunmbaku, Jiaxin Song, Shanling Wang, Ayoub Taallah, Yixin Dai, Wenkang Li, Wenxue Li, Yi He, Jian Guo, Hong Zhang, Filippo S. Boi
Format: Article
Language:English
Published: Elsevier 2021-10-01
Series:Carbon Trends
Subjects:
Online Access:http://www.sciencedirect.com/science/article/pii/S2667056921000791
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author Omololu Odunmbaku
Jiaxin Song
Shanling Wang
Ayoub Taallah
Yixin Dai
Wenkang Li
Wenxue Li
Yi He
Jian Guo
Hong Zhang
Filippo S. Boi
author_facet Omololu Odunmbaku
Jiaxin Song
Shanling Wang
Ayoub Taallah
Yixin Dai
Wenkang Li
Wenxue Li
Yi He
Jian Guo
Hong Zhang
Filippo S. Boi
author_sort Omololu Odunmbaku
collection DOAJ
description We report a novel investigation of the effects of sulfur-precursor concentration on the morphological, structural and magnetic properties of vertically aligned mm-long films of carbon nanotubes (CNTs) filled with Fe3C nanowires. Fabrication was carried out by sublimation and pyrolysis of ferrocene/sulfur mixtures in the presence of 0.65 ml of dichlorobenzene within a custom designed chemical vapour deposition (CVD) reactor, under an Ar flow of 10-100 ml/min. The employed quantity of sulfur was found to have an important impact on the structural properties of the as grown CNTs, yielding either few wall CNTs (FWCNTs) or multiwall CNTs (MWCNTs) in presence of 0.4 mg or 1.2 mg of sulfur (category 1,2). Appearance of RBM (radial breathing modes) bands with variable intensities, was demonstrated in category-1 samples by both point and mapping Raman spectroscopy. Further, an additional broad band indicative of a chlorine/sulfur-induced amorphization of the CNT-walls was detected. Structural manipulation of category-1 and-2 samples was sought through annealing, in an attempt to create carbon-sulfur phases. The latter system has been indeed recently identified as a possible superconductor, under certain conditions of doping. Our findings highlight two different regimes of carbon-sulfur manipulation of the CNT-layers which involve 1) the nucleation of covalent carbon-sulfur phases at T∼150 °C -300 °C, with appearance of Raman bands at 1250 cm−1 and 1450 cm−1 and 2) an enhancement of the CNT-defectiveness (D and D’ bands) at T∼600 °C.
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spelling doaj.art-5c4e5d259dcf413bb1b50c6554f4ca782022-12-21T19:37:56ZengElsevierCarbon Trends2667-05692021-10-015100102Nucleation of carbon-sulfur phases by manipulation of vertically-aligned mm-long films of iron-filled few-wall/multiwall carbon nanotubesOmololu Odunmbaku0Jiaxin Song1Shanling Wang2Ayoub Taallah3Yixin Dai4Wenkang Li5Wenxue Li6Yi He7Jian Guo8Hong Zhang9Filippo S. Boi10College of Physics, Sichuan University, Chengdu, China; MOE Key Laboratory of Low-grade Energy Utilization Technologies and Systems, CQU-NUS Renewable Energy Materials & Devices Joint Laboratory, School of Energy and Power Engineering, Chongqing University, Chongqing 400044, ChinaCollege of Physics, Sichuan University, Chengdu, ChinaAnalytical and Testing Center, Sichuan University, Chengdu, ChinaCollege of Physics, Sichuan University, Chengdu, ChinaCollege of Physics, Sichuan University, Chengdu, ChinaCollege of Physics, Sichuan University, Chengdu, ChinaCollege of Physics, Sichuan University, Chengdu, ChinaAnalytical and Testing Center, Sichuan University, Chengdu, ChinaCollege of Physics, Sichuan University, Chengdu, ChinaCollege of Physics, Sichuan University, Chengdu, China; Corresponding authors.College of Physics, Sichuan University, Chengdu, China; Corresponding authors.We report a novel investigation of the effects of sulfur-precursor concentration on the morphological, structural and magnetic properties of vertically aligned mm-long films of carbon nanotubes (CNTs) filled with Fe3C nanowires. Fabrication was carried out by sublimation and pyrolysis of ferrocene/sulfur mixtures in the presence of 0.65 ml of dichlorobenzene within a custom designed chemical vapour deposition (CVD) reactor, under an Ar flow of 10-100 ml/min. The employed quantity of sulfur was found to have an important impact on the structural properties of the as grown CNTs, yielding either few wall CNTs (FWCNTs) or multiwall CNTs (MWCNTs) in presence of 0.4 mg or 1.2 mg of sulfur (category 1,2). Appearance of RBM (radial breathing modes) bands with variable intensities, was demonstrated in category-1 samples by both point and mapping Raman spectroscopy. Further, an additional broad band indicative of a chlorine/sulfur-induced amorphization of the CNT-walls was detected. Structural manipulation of category-1 and-2 samples was sought through annealing, in an attempt to create carbon-sulfur phases. The latter system has been indeed recently identified as a possible superconductor, under certain conditions of doping. Our findings highlight two different regimes of carbon-sulfur manipulation of the CNT-layers which involve 1) the nucleation of covalent carbon-sulfur phases at T∼150 °C -300 °C, with appearance of Raman bands at 1250 cm−1 and 1450 cm−1 and 2) an enhancement of the CNT-defectiveness (D and D’ bands) at T∼600 °C.http://www.sciencedirect.com/science/article/pii/S2667056921000791Carbon nanotubesSulfurDopingCarbon-sulfurCVDMagnetic-manipulation
spellingShingle Omololu Odunmbaku
Jiaxin Song
Shanling Wang
Ayoub Taallah
Yixin Dai
Wenkang Li
Wenxue Li
Yi He
Jian Guo
Hong Zhang
Filippo S. Boi
Nucleation of carbon-sulfur phases by manipulation of vertically-aligned mm-long films of iron-filled few-wall/multiwall carbon nanotubes
Carbon Trends
Carbon nanotubes
Sulfur
Doping
Carbon-sulfur
CVD
Magnetic-manipulation
title Nucleation of carbon-sulfur phases by manipulation of vertically-aligned mm-long films of iron-filled few-wall/multiwall carbon nanotubes
title_full Nucleation of carbon-sulfur phases by manipulation of vertically-aligned mm-long films of iron-filled few-wall/multiwall carbon nanotubes
title_fullStr Nucleation of carbon-sulfur phases by manipulation of vertically-aligned mm-long films of iron-filled few-wall/multiwall carbon nanotubes
title_full_unstemmed Nucleation of carbon-sulfur phases by manipulation of vertically-aligned mm-long films of iron-filled few-wall/multiwall carbon nanotubes
title_short Nucleation of carbon-sulfur phases by manipulation of vertically-aligned mm-long films of iron-filled few-wall/multiwall carbon nanotubes
title_sort nucleation of carbon sulfur phases by manipulation of vertically aligned mm long films of iron filled few wall multiwall carbon nanotubes
topic Carbon nanotubes
Sulfur
Doping
Carbon-sulfur
CVD
Magnetic-manipulation
url http://www.sciencedirect.com/science/article/pii/S2667056921000791
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