Arab J Sci Eng
DOI 10.1007/s13369-015-1897-1
RESEARCH ARTICLE - CHEMISTRY
Removal of Oxidation Fragments from Multi-walled Carbon
Nanotubes Oxide Using High and Low Concentrations of Sodium
Hydroxide
Khalid I. Kabel
1
· Ahmed A. Farag
1
· Elsayed M. Elnaggar
2
·
Abdalrhman G. Al-Gamal
1
Received: 22 December 2014 / Accepted: 6 October 2015
© King Fahd University of Petroleum & Minerals 2015
Abstract Modification of multi-walled carbon nanotubes
surface (MWCNT) using the mixture of HNO
3
/H
2
SO
4
is
widely employed for MWCNT surface oxidation, but it also
leads to shortening and thinning of the CNT layers causing
fragmentation. The carbonaceous fragments had adsorbed
on the surface is not removed from the sample in conven-
tional treatments; however, the addition of NaOH success-
fully cleans the oxidized material. In this article, MWCNT
was functionalized using HNO
3
/H
2
SO
4
as oxidizing agent
and evaluate the impact of using high and low concentrations
of NaOH to purify CNT oxide. The presence of oxidized
groups as hydroxyl and carboxyl has been demonstrated by
FTIR. The thermal stability of MWCNT and MWCNT-O
after and before purification was studied by TGA, and the
degree of its crystallinity was examined by XRD. The defect
degree occurs during the oxidation process was confirmed
by Raman spectroscopy. TEM images showed the presence
and the absence of wrinkles and the adsorbed carbonaceous
fragments.
Keywords Oxidation of MWCNT · Effect of NaOH ·
Carbonaceous fragment removal · MCNT thermal stability ·
Degree of crystallinity
B Khalid I. Kabel
drkhalid1977@yahoo.com
1
Department of Petroleum Applications, Egyptian Petroleum
Research Institute (EPRI), Nasr City, P.B. 11727, Cairo, Egypt
2
Department of Applied Chemistry, Faculty of Science,
Al-Azher University, Cairo, Egypt
1 Introduction
The commonly noticed existence of carbon nanotubes (CNT)
in 1991 [1] opened new advancement paths because their
unique properties, chemical and thermal stability, electronic
properties, high-tensile strength, and ultralight weight [2–
6] which are matchless made researcher ot use it in several
scientific disciplines such as mechanical, electrical, thermo-
mechanical, optical, and sensor applications [7–9]. Multi-
walled carbon nanotubes (MWCNTs) can be considered as
a series of single-walled carbon nanotubes, i.e., graphene
sheets rolled into seamless cylinders, arranged coaxially with
regularly increasing the diameter [10]. Saleh and Gupta
reported that MWCNTs could enhance the photocatalytic
activity [11].
Functionalization of CNT could improve the dispersion
as well as promote interfacial bonding with polymers [12].
Oxygen-containing functional groups (hydroxyl, epoxy, car-
bonyl, and carboxyl) increase sp
3
carbon hybridization and
can be decorated at tube ends, as well as at along the side walls
of CNT through a liquid-phase oxidation process. These
functionalities promote CNT chemical reactivity and can
either directly used for composite [13–15]. Saleh proved
that, the extent of oxygen content into the MWCNT’s surface
is sensitive to oxidizing agent and the process temperature,
while the acidic site increases with increase in the treatment
temperature [16].
The most usual method for CNT oxidation is treatment
with acidic solutions or oxidizing agents, such as H
2
SO
4
[17], HNO
3
[18], H
2
SO
4
/HNO
3
[19], H
2
O
2
[20], H
2
O
2
/
HNO
3
[21], KMnO
4
[22], KMnO
4
/H
2
SO
4
[23] etc. It is
a very versatile, efficient and potential use [21, 24, 25]. The
most common reagent used for liquid-phase oxidation treat-
ment is HNO
3
/H
2
SO
4
[26].
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