Materials Today Communications 23 (2020) 100845

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Materials Today Communications

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Cementitious material reinforced by carbon nanotube-Nylon 66 hybrid T

nanofibers: Mechanical strength and microstructure analysis
Tri N.M. Nguyena, Doo-Yeol Yoob, Jung J. Kima,*
a
Dept. of Civil Engineering, Kyungnam University, 7 Kyungnamdaehakro, Changwon-si, Gyeongsangnam-do 51767, South Korea
b
Dept. of Architectural Engineering, Hanyang University, 222 Wangsimni-ro, Seongdong-gu, Seoul, 04763, South Korea

ARTICLE INFO ABSTRACT

Keywords: In this study, carbon nanotube (CNT) reinforced Nylon 66 nanofibers were used to modify the mechanical
Nylon 66 nanofibers properties of cementitious materials. Single-walled carbon nanotubes (SWCNTs) and multi-walled carbon na-
Cement notubes (MWCNTs) were dispersed into the polymer solution of Nylon 66. CNT reinforced Nylon 66 nanofibers
Electrospinning were fabricated and mixed directly with ordinary Portland cement through an electrospinning process using an
Carbon nanotubes
improved collector. Scanning electron microscope (SEM) and field emission transmission electron microscope
Tensile strength
Toughness
(FE-TEM) were employed to investigate the morphological characteristics of nanofibers as well as the perfor-
mance of nanofibers in the microstructure of hardened cement pastes. Moreover, the existence of CNTs in the
hardened cement pastes was clarified by means of micro-computed tomography (CT) technique and thermal
gravimetric analysis (TGA) method. The observations from mechanical strength tests showed the increase in
toughness by 49 %, 30 % and 12 % as well as the increase in the tensile strength by 28 %, 43 % and 57 % in that
order when adding Nylon 66 nanofibers, SWCNT reinforced Nylon 66 nanofibers and MWCNT reinforced Nylon
66 nanofibers into cement pastes.

1. Introduction
Due to its low cost, using available raw materials as well as the
outstanding mechanical strength, concrete becomes the priority mate-
rial of almost constructors. However, the disadvantage of this compo-
site material is the cracks frequently occurring in the cementitious
matrix, leading to reduce the strength of the whole material [1–3].
Conventionally, the way to enhance the strength of cementitious ma-
terial is introducing reinforced agents such as chemical admixtures,
micro-sized particle or micro-size fibers into cementitious materials.
Wang et al. [4] found the increase in the flexural strength of the har-
dened cement paste due to polymer latex films covered around the
surface of the hydration product as well as filled in the cracks and pores
when adding latex polymer into the cement paste. In addition, the
strength of ordinary Portland cement (OPC) could be improved by using
small-sized particles to refine the porous structure of this material.
There are many studies that verified the usefulness of coral sand
powder, nano-metakaolin, nano-alumina, nano-silica and so on, in im-
proving the strength of the cementitious material [5–8]. Recently,
nano-sized fibers have been gained the interest of many researchers on
reinforcing cementitious material. Azevedo and Gleize [9] enhanced
the compressive strength and the flexural strength of cement paste by
adding silicon carbide nanowhiskers. Brown and Sanchez [10] and
Goncalves et al. [11] reported the performance of cement pastes ex-
posing in sulfate environment with the reinforcement by carbon na-
nofibers and cellulose nanofibers. Saleh et al. [12] added iron slag and
titanate nanofibers into cement paste to create an anti-radioactive
material and reported the increase in compression resistance and dur-
ability of the new composite cementitious material.
Carbon nanotubes (CNTs), a synthetic material was discovered in
1991 by Sumio Iijima [13], which included a numerous of unique
characteristics like high aspect ratio with the hollow structure, high
thermal, electrical, especially high mechanical properties [14–19], have
become the most interesting reinforcing material not only on cement
but also on other kinds of materials [20–27]. Li et al. [28,29] conducted
two studies on mechanical strength and microstructural phase of ce-
ment composites incorporated by surface-treated multi-walled carbon
nanotubes (MWCNTs) and observed the higher in compressive strength
and flexural strength compared to the plain paste. Rocha et al. [30]
reported the increase up to 90 % in fracture energy, 46 % in flexural
strength and 47 % in tensile strength when reinforcing cement paste by
0.1 % of CNTs. Besides, the optimum proportion of CNTs for increasing
the mechanical strength of cement paste also found by Mohsen et al.
[31] and they clarified that the proportion of 0.25 wt% CNTs was the

⁎
Corresponding author.
E-mail addresses: nnmtri@utc2.edu.vn (T.N.M. Nguyen), dyyoo@hanyang.ac.kr (D.-Y. Yoo), jungkim@kyungnam.ac.kr (J.J. Kim).

https://doi.org/10.1016/j.mtcomm.2019.100845
Received 25 November 2019; Accepted 12 December 2019
Available online 14 December 2019
2352-4928/ © 2019 Elsevier Ltd. All rights reserved.
T.N.M. Nguyen, et al. Materials Today Communications 23 (2020) 100845

most optimization for getting the highest strength with a suitable cost. Table 1
The problem when incorporating CNTs with cementitious material was Properties of Nylon 66.
the poor dispersion of CNTs due to the strong Van der Waals binding Linear formular [-CO(CH2)4CONH(CH2)6NH-]n
associated with the CNT aggregates. However, there were some studies
showed the effect of sonication as well as surfactants in dispersing CNTs Molecular weight (g/mol) 262.35
Abrasion resistance (mg) 7
in the aqueous solution [28–39]. Then using the aqueous solution to
Autoignition temp (oC) 400
prepare the cement pastes [31–34,37] or drying them to treat the sur- Hardness 121
face of CNTs and mix with cement [28,29] or to prepare the powder of mp (oC (lit.)) 250–260
cement particles coated with CNTs [30]. In this study, we have pre- Tm (oC) 270
sented another approach to incorporate the CNTs into cement paste, the Density at 25 °C (g/ml) 1.14

new hybrid nanofibers including Nylon 66 [40,41] and CNTs were

fabricated by electrospinning (e-spinning) technique [42–44]. These
Table 2
hybrid nanofibers are combined directly with OPC for forming a com-
Properties of formic acid and chloroform.
posite cementitious material. In this approach, CNTs (outer diameter
around 1–10 nm) are introduced into cement paste in an indirect Properties Formic acid Chloroform
manner through Nylon 66 nanofibers (diameter around 200–300 nm),
Linear formular HCOOH CHCl3
therefore, the agglomerate phenomenon or unwell dispersion will be Molecular weight (g/mol) 46.03 119.38
resolved. It should be noted that, despite the literature-review showed Purity (%) – 99
CNTs were grown directly on the cement matrix and reported the good mp (oC) 8.4 −63
results in enhancing the mechanical strength of hardened cement pastes bp (oC) 100 60–61
Density (g/ml) 1.22 1.492
[28–31,45–47]. The approaching in this study is another manner to
Fp (oC) 69 29.5
incorporate CNTs into cementitious material and has not been reported
before. In addition, the obtained results on the mechanical strength of
hardened cement pastes are also effective and comparative to the re- Table 3
sults from former studies of CNTs applications to cement. Properties of single-walled carbon nanotubes and multi-walled carbon nano-
MWCNTs and single-walled carbon nanotubes (SWCNTs) are two tubes.
principal existences of CNTs. MWCNTs are described as a concentric
SWCNTs MWCNTs
assembly of more than two seamless cylinders of graphite layers [13].
In addition, Tsang et al. [48] found the SWCNTs when stripping off the Purity (%) 90 93–97
multiple outer layers of graphitic by heating in carbon dioxide gas and Outer diameter (nm) 1–2 9–10
Length ( µm ) 5–30 10–30
finally obtained the tubes with only one graphitic layer. Both MWCNTs
and SWCNTs are utilized in this study to estimate the effect of CNTs
reinforced Nylon 66 nanofibers on the mechanical strength of ce-
mentitious material. Due to their high aspect ratios, CNTs tend to in- and formic acid (HCOOH; Daejung, Korea) were utilized as the solvent
teract with each other and to form the agglomeration by the strong Van for preparing the dope solutions. All chemicals were used as received,
der Waals forces [49–51]. Hence, for obtaining the homogeneous so- the properties of Nylon 66 pellets, two aqueous chemicals and two type
lution, the ultrasonication process needs to be conducted to break the of CNTs were shown in Tables 1–3 respectively.
link formed by the interactions between CNTs molecules [52–55]. There are three dope solutions in this study, Nylon 66 dope solution,
Therefore, in this study, the ultrasonication processes were conducted SWCNT-Nylon 66 dope solution and MWCNT-Nylon 66 dope solution.
to disperse MWCNTs and SWCNTs in the solvents that containing First, Nylon 66 dope solution was prepared by stirring Nylon 66 pellets
formic acid and chloroform. in the solvent to yield the 10 % dope solution. In detailed, the solvent
In order to study the influence of Nylon 66 nanofibers as well as was obtained by merging formic acid and chloroform with the volume
hybrid nanofibers containing CNTs and Nylon 66 nanofibers on the proportion of 4:1 (formic acid: chloroform, respectively), and can be
mechanical behaviors of cementitious materials, strength tests had been called as “solvent”. Nylon 66 pellets can be dissolved completely by
conducted. The compressive strength test and direct tensile strength test formic acid solvent [40,56,57]. However, in this study, with the desire
were conducted on the hardened cement paste samples with and of fabricating the rough nanofibers, chloroform, a volatile agent was
without nanofibers after 28 days of curing. To investigate the mor- added into the acid solvent [58]. The second and third dope solutions
phological characteristics of nanofibers as well as the performance of were obtained from similar processes, where replacing 3.0 % mass of
nanofibers in the microstructure of hardened cement paste, scanning Nylon 66 by CNTs. In that manner, the second dope solution contained
electron microscope (SEM) and field emission transmission electron SWCNTs and the third dope solution contained MWCNTs. With the
microscope (FE-TEM) were employed. Moreover, the existence of CNT same dispersing process, carbon nanotubes were mixed with the solvent
reinforced Nylon 66 nanofibers in the hardened cement pastes was mentioned above. The ultra-sonication process was conducted to dis-
clarified by means of micro-computed tomography (micro-CT) tech- perse carbon nanotubes in the solvent. The proportions of CNT, Nylon
nique and thermal gravimetric analysis (TGA) method. 66 pellets and solvent in dope solutions are 0.3 %, 9.7 % and 90 %
respectively by weight.
2. Materials and methods In this study, nano-sized fibers were fabricated by electrospinning/
spray system. The electrospinning processes in this study were con-
2.1. Dope solution for electrospinning process ducted under the high voltage of 12 kV, using the 12 ml syringes and
the stainless steel needles size 20. It is worth noting that depending on
MWCNT (grade: CM-95; Hanos, Korea), SWCNT (grade: MKN- the viscoelasticity of the dope solution, needles size can vary from 20 to
SWCNT-P1; Mknano, Canada) and Nylon 66 pellets (C12H26N2O4; 25. Moreover, the Taylor cone-to-collector distance and the pump speed
Sigma-Aldrich Co, USA) were three main precursors for fabricating were kept constant of 60 mm and 30 µL/ min , respectively, as denoted
nanofibers in this study. Besides, chloroform (CHCl3; Daejung, Korea) in Fig. 1. In order to analyze the morphological characteristics by SEM,

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T.N.M. Nguyen, et al.
Fig. 1. Schematic of electrospinning system with the improved collector.
these nanofibers were spun into the 5 mm × 5 mm carbon tape pieces.
For FE-TEM analyzing, SWCNT reinforced Nylon 66 nanofibers and
MWCNT reinforced Nylon 66 nanofibers were spun directly onto the
copper grids. Besides, for decomposition temperature analyzing by
TGA, these nanofibers were spun onto the metal plate collector, then
they were stripped off from the plate collector as membranes.
2.2. Cementitious material preparation
A type I OPC compliance with ASTM C 150-18 [59] from Ssangyong
Co, Korea was utilized for cementitious material in this study. The
chemical components and physical characteristics of OPC is presented
in Table 4. For obtaining the hardened cement pastes including nano-
fibers, the electrospinning processes were conducted using an improved
collector system [60]. As can be seen in Fig. 1, the collector system
contains a magnetic stirrer machine, a stir bar and a metal bath with an
insulated wall, this system was connected to ground. For each turn, the
weight 95 g of OPC was mixed with nanofibers that spun from the
weight 5 g of dope solution, which was quantitatively calculated 5 wt%
of the dope solution compared to the weight of binder.
In order to investigate the influence of these nanofibers on the
mechanical strength of hardened cement paste, tensile strength test and
the compressive strength test were conducted. In that manner, the
hardened cement paste samples were prepared with the constant water
to binder ratio of 0.5, using the cement blended nanofibers as prepared
above. The mixing jobs were done with the help of the power-driven
revolving pan mixer comply with ASTM C 305-14 [61]. The samples for
tensile strength test and compressive strength test were prepared in
accordance to ASTM C307 - 03(2012) [62] and ASTM C109/109M - 16a
[63] about tensile strength test and compressive strength test of ce-
mentitious materials, respectively. The non-nanofibers hardened
Table 4
Chemical composition and physical properties of cement.
CaO Al2O3 SiO2 SO3 MgO Fe2O3
61.33 6.40 21.01 2.30 3.02 3.12
Materials Today Communications 23 (2020) 100845
cement paste samples were also prepared as the hardened control ce-
ment paste in this study. All samples were tested after 28 days of curing
and the samples dimension can be specified in Fig. 2. In addition, the
mix designs of all hardened cement paste samples were shown in
Table 5.
The broken samples after tensile strength test were used to in-
vestigate the failure surface by SEM. Four 0.5 mm-thin samples for SEM
analysis were prepare with the dimension of 5 mm × 5 mm for the
hardened control cement paste, the hardened cement pastes including
Nylon 66 nanofibers, SWCNT reinforced Nylon 66 nanofibers and
MWCNT reinforced Nylon 66 nanofibers.
2.3. Apparatus and testing methods
Tensile strength tests were conducted by means of the 5kN-capacity
mortar tensile strength test apparatus under the ASTM C307 - 03(2012)
[62], besides, the compressive strength tests were carried out by means
of the hydraulic universal testing machine with a loading capacity of
1000 kN, according to the ASTM C109/109 M - 16a [63]. Moreover, a
set of three briquette samples and three cubic samples of each mixture
after 28 days of curing in water were prepared for the test. In order to
investigate the morphological properties of nanofibers as well as the
behavior of the pastes that contain nanofibers, SEM analysis were done
under the accelerating voltage of 3–5 kV and the working distance of
7.1–7.9 mm. In addition, for higher definition observation, a 5 Å-pla-
tinum layer was sputter-coated onto the samples. In order to demon-
strate the existence of CNTs in Nylon 66 nanofibers, the field emission
transmission electron microscope (FE-TEM) analysis was done with an
acceleration voltage of 300 kV. The micro-CT analysis was conducted
using the synchrotron device with the X-ray source supply up to 60 keV.
The decomposition temperatures of nanofibers, as well as the existence
Ig. loss Specific surface area (cm2/g) Compressive strength, 28-day (MPa)
1.40 2800 42.5
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T.N.M. Nguyen, et al. Materials Today Communications 23 (2020) 100845

Fig. 2. Samples for the mechanical strength tests.

Table 5
Mix proportions of samples (by % mass).
Samples Binder (B) Water/B

OPC N66 NFs SWCNTs MWCNTs

Control paste 100 0 0 0 0.5

N66 MCP 99.5 0.5 0 0 0.5
SWCNTs-N66 MCP 99.5 0.485 0.015 0 0.5
MWCNTs-N66 MCP 99.5 0.485 0 0.015 0.5

“MCP” stands for “modified cement paste”.

of the hybrid nanofibers in the hardened cement pastes, were verified

by TGA technique. The TGA processes were conducted with the heating
range from ambient temperature to 1000 °C, under the Nitrogen at-
mosphere, the flow rate of 100 ml/min, and the heating velocity of
10 °C/min.

3. Results and discussion

3.1. Mechanical characteristics Fig. 3. Compressive strength results.

The mechanical characteristics of the hardened cement pastes that hardened cement pastes containing nanofibers increased in both
modified by nanofibers compared to the hardened control cement paste strength tests after 28 days of curing. Figs. 3 and 4 showed the results
were shown in Figs. 3–5. The results were summarized in Table 6. From from the compressive strength tests, the compressive strength of the
an overall perspective, it is evident that the mechanical strengths of the

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T.N.M. Nguyen, et al. Materials Today Communications 23 (2020) 100845

the typical compressive stress-strain curves in Fig. 4, the influence of

three types of nanofibers on the toughness of cementitious materials
was clarified. From the area of these curves, the toughness was calcu-
lated as 62,000 J/m3, 92,000 J/m3, 81,000 J/m3 and 69,000 J/m3 of
the hardened control cement paste, the hardened cement pastes con-
taining Nylon 66 nanofibers, SWCNT reinforced Nylon 66 nanofibers
and MWCNT reinforced Nylon 66 nanofibers, respectively. Based on
these observations, there was a significant increase in the toughness
characteristic of cement, approximately 12 %, 30 % and 49 % in that
order when modifying the hardened cement pastes by MWCNT re-
inforced Nylon 66 nanofibers, SWCNT reinforced Nylon 66 nanofibers,
and Nylon 66 nanofibers. As shown in Fig. 5, a significant increase in
the tensile strength was observed when introducing nanofibers into the
hardened cement pastes. For instance, the tensile strength of the har-
dened cement paste containing MWCNT reinforced Nylon 66 nanofibers
increased 57 % while this parameter increased 43 % in the hardened
cement pastes containing SWCNT reinforced Nylon 66 nanofibers and
28 % in the hardened cement paste containing Nylon 66 nanofibers.
Comparing the obtained results with the results reported by Rocha et al.
[30] base on the directly tensile strength test. They reported that the
Fig. 4. Stress-strain curves.
tensile strength of hardened cement paste increased by 40 % and 45 %
when adding the content of MWCNTs of 0.05 % and 0.1 % respectively.
The present result showed the increase up to 57 % when reinforcing
hardened cement paste by hybrid nanofibers containing MWCNTs with
the content of 0.015 %. Above all, the observations showed that there
was a better performance in the tensile strength rather than the com-
pressive strength when introducing Nylon 66 nanofibers as well as the
hybrid nanofibers containing Nylon 66 and CNTs into the hardened
cement pastes. This observation signified the feasibility of the ap-
proaching in enhancing the tensile strength of hardened cement paste
using nanofibers containing CNTs in this study.

3.2. Nanofibers morphological characteristics

Figs. 6–8 show the morphological characteristics of Nylon 66 na-

nofibers, SWCNT reinforced Nylon 66 nanofibers and MWCNT re-
inforced Nylon 66 nanofibers respectively in lower and higher magni-
fications by SEM analysis. From an overall perspective (Figs. 6–8(a)), all
nanofibers appeared as meshwork, with messing and disorientation
shape. The smooth, glossy surface and almost uniform diameter along
the axis of nanofibers can be observed in the SEM images of hybrid-
nanofibers such as SWCNT reinforced and MWCNT reinforced Nylon 66
nanofibers. There are thin membranes and beads formed and connected
Fig. 5. Tensile strength results.
between nanofibers with sparsely level. In contrast, there are no
membranes and beads connecting among the nanofibers, as well as the
Table 6 rough surface nanofibers were observed in the SEM images of Nylon 66
Mechanical strength results after 28 days.
nanofibers. This phenomenon is attributed to the evaporation of
Compressive strength Toughness (J/ Tensile strength Chloroform in the solvent during the e-spinning process [58]. In gen-
(MPa) m3) (MPa) eral, the mean diameter of Nylon 66 nanofibers, SWCNT reinforced
Nylon 66 nanofibers and MWCNT reinforced Nylon 66 nanofibers were
Control paste 35.17 (0.725) 62031 (5049.7) 1.14 (0.172)
N66 MCP 37.90 (2.376) 92179 (8229.3) 1.46 (0.348) 267 nm, 264 nm and 284 nm, respectively. It is worth adding that the
SWCNTs-N66 38.54 (3.077) 80882 (7196.5) 1.63 (0.080) hybrid structure of the nanofibers containing Nylon 66 and CNTs can be
MCP shown in Fig. 9 by FE-TEM analysis. As shown in Fig. 9(a), there are
MWCNTs-N66 40.16 (4.241) 69462 (9701.1) 1.79 (0.191)
many SWCNTs with diameter around 1 nm–2 nm gathered as bundle
MCP
along the axis of the Nylon 66 nanofiber with diameter around 200 nm.
The values in parentheses are standard deviation. In Fig. 9(b), there are some separate nanofibers consider as MWCNTs,
with diameter around 10 nm and rugged length along the nylon 66 axis.
hardened cement pastes modified by nanofibers increased slightly ap- These results are in agreement with the TEM result found by Saeed et al.
proximate 8, 10 and 14 % in that order when introducing Nylon 66 [64] and Baji et al. [65,66]. The existence of the CNTs, which tensile
nanofibers, SWCNT reinforced Nylon 66 nanofibers, and MWCNT re- strength is up to 10 GPa [14–16], has enhanced the strength of the
inforced Nylon 66 nanofibers into the hardened cement pastes. From hybrid Nylon 66 nanofibers.

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T.N.M. Nguyen, et al. Materials Today Communications 23 (2020) 100845

Fig. 6. Morphological characteristics of N66 Nanofibers.

Fig. 7. Morphological characteristics of SWCNT reinforced N66 Nanofibers.

Fig. 8. Morphological characteristics of MWCNT reinforced N66 Nanofibers.

3.3. Microstructural characteristics of hardened cement paste
The SEM observations from the fractured surface of the briquette
samples were shown in Figs. 10–12. As expected, there were many
nanofibers with the diameter larger than 200 nm stayed interleave
among the cement hydration products. The hydration products of ce-
ment can be determined by their morphologies. The calcium hydroxide
(CH) appeared as large prismatic crystals and the fibrous morphology
were calcium silicate hydrates (CSH). The diameter of these CSH varied
around 50 nm [67]. Therefore, it is easy to distinguish which is CSH and
the added nanofibers in the microstructure of hardened cement paste.
From the SEM images as shown in Figs. 10–12(a), these nanofibers
acted as the linking among the hydration products and also bridging
agent at the pores that formed in the cement matrix. In the higher
magnification images as shown in Figs. 10–12(b), the detailed of na-
nofibers surface were clarified. The surfaces of nanofibers all deformed
by the clinging of cement hydration products. These phenomena made
the surface of nanofibers become lumpy and non-glossy compared to
the pristine morphology as shown in Figs. 6–8. From this result, the
interaction between nanofibers and cement hydration products were
verified. Hence, in the microstructure of cement pastes, the added na-
nofibers with the deformed surface have shown the well-effect in
linking among hydration products [28]. As a consequence, higher
tensile strengths were formed. It is worth noting that the strength of

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T.N.M. Nguyen, et al.
Fig. 9. FE-TEM images of the hybrid nanofibers.
hybrid nanofibers was enhanced by CNTs as mentioned above. There-
fore, it explains that the tensile strength of the hardened cement pastes
containing MWCNT reinforced Nylon 66 nanofibers and SWCNT re-
inforced Nylon 66 nanofibers are higher than that containing Nylon 66
nanofibers.
3.4. Micro-computed tomography result
Micro-computed tomography is a nondestructive method that can
be used to identify the existence of nanofibers containing CNTs inside
the hardened cement paste. Fig. 13 shows the results obtained by micro-
CT analysis. Fig. 13(a) shows the 8-bit cross-sectional of the hardened
cement paste containing MWCNTs-N66 nanofibers. The 8-bit image
includes of pixels presented by the value from 0 to 255 (total 256 va-
lues) depend on the relative density, where 0 is black and 255 is white
in grayscale [68,69]. The 8-bit image in Fig. 13(a) consists of
1405 × 922 pixels, which the size of each pixel is 3.8 µm . As can be
seen from Fig. 13(b), the blue regions can be considered as the existence
of nanofibers that recognized by the set of pixels stay in the range from
13 to 57. This threshold range was determined by the values that does
not exist in the 8-bit micro CT image of the cross-sectional of the control
hardened cement paste. However, it was difficult to recognize the na-
nofibers containing CNTs inside the sample. Therefore, the binary
Fig. 10. Microstructure of the hardened cement paste containing Nylon 66 nanofibers.
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Materials Today Communications 23 (2020) 100845
image was created by the imaging processing tool from Matlab as
shown in Fig. 13(c). Fig. 13(d) shows the 3D image of the hardened
cement paste containing nanofibers that obtained by stacking a series of
1690 binary images through the z axial, about 6.4 mm. From the re-
sults, the distribution of nanofibers containing CNTs was verified
[68,69].
3.5. Thermal analysis
Fig. 14 shows the thermal analysis of N66 nanofibers and two hy-
brid nanofibers. From these graphs, the start temperature of weight loss
of N66 nanofibers could be determined at 300 °C and end at 410 °C. This
result agrees with others [70–72]. Besides, from the thermal analyza-
tions of SWCNTs-N66 nanofibers and MWCNTs-N66 nanofibers, the
onset of losing weight of these hybrid nanofibers were determined at
350 °C and finish at 460 °C [64,65]. The shift range between the
thermal analysis results of the Nylon 66 nanofibers with and without
CNTs could be explained by the adding of CNTs with the decomposition
temperature above 500 °C [64,73]. Moreover, the increase in the de-
composition temperature range of the hybrid nanofibers has indicated
the combination between CNTs and Nylon 66 nanofibers. Therefore, the
hybrid nanofibers have higher thermal stability [74].
Fig. 15 shows the TGA-DTG results of the control hardened cement
T.N.M. Nguyen, et al. Materials Today Communications 23 (2020) 100845

Fig. 11. Microstructure of the hardened cement paste containing SWCNT reinforced N66 nanofibers.

Fig. 12. Microstructure of the hardened cement paste containing MWCNT reinforced N66 nanofibers.

Fig. 13. The micro-CT results of the hardened cement paste containing CNT reinforced N66 nanofibers.

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T.N.M. Nguyen, et al.
Fig. 14. TGA results of three types of nanofibers.
paste and the hardened cement pastes containing SWCNT reinforced
Nylon 66 nanofibers and MWCNT reinforced Nylon 66 nanofibers, re-
spectively. In which, all of the samples were prepared with a w/c ratio
of 0.5 and a curing period of 28 days. The TGA-DTG result of the control
hardened cement paste as shown in Fig. 15(a) has also confirmed the
result from previous literature works [75–77]. For instance, the
Fig. 15. TGA-DTG results of hardened cement pastes non-containing and containing nanofibers.
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Materials Today Communications 23 (2020) 100845
temperature range from 145 °C to 200 °C was considered as the dehy-
dration range of water in CSH, while the temperature range from 400 °C
to 500 °C was considered as the dehydration range of water in CH. The
temperature range from 550 °C to 900 °C was considered as the dec-
arbonation range of carbon dioxide in calcium carbonate (CaCO3). It is
noticeable that the temperature range before 145 °C belongs with the
arbitrary water inside each hardened cement paste under the nitrogen
(N2) and free carbon dioxide (CO2) environment [78]. As shown in
Fig. 15(b), the weight decrease from 300 °C to 410 °C can be considered
as the weight loss of Nylon 66 nanofibers in the hardened cement paste.
Therefore, in order to estimate the proportion of Nylon 66 nanofibers in
the hardened cement paste, a comparison between TGA result of the
hardened control cement paste and the TGA result of the hardened
cement paste containing Nylon 66 nanofibers was employed with the
initial weight at 300 °C. Fig. 16(a) and Table 7 present the different
weight loss of 0.62 % at 410 °C, as consider the proportion of Nylon 66
nanofibers in the hardened cement paste. In Fig. 15(c) and (d), the
peaks between 350 °C–500 °C could be recognized as the evaporation of
water inside CH and also the decomposition of CNT reinforced Nylon
66nanofibers. As similarly, the comparisons between the TGA results of
the hardened cement paste containing two types of CNT reinforced
Nylon 66 nanofibers and the TGA result of the hardened control cement
paste were conducted with the initial weight at 350 °C. The difference
of weight loss at 460 °C showed the proportions of SWCNT reinforced
Nylon 66 nanofibers and MWCNT reinforced Nylon 66 nanofibers in the
hardened cement pastes of 0.55 % and 0.45 %, respectively (Fig. 16(b),
(c) and Table 8). The proportion of three types of nanofibers in the
hardened cement pastes analyzing by TGA showed similarly to the
T.N.M. Nguyen, et al.
Fig. 16. TGA results comparison between the hardened control cement paste
and the hardened cement pastes containing nanofibers.
proportion conducted in the electrospinning process as 0.5 % of the
precursors. In addition, the existence of SWCNTs reinforced Nylon 66
nanofibers and MWCNT reinforced Nylon 66 nanofibers in the har-
dened cement pastes were verified by TGA analysis.
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Materials Today Communications 23 (2020) 100845
Table 7
The portion of Nylon 66 nanofibers in the hardened cement
paste.
Temperature (oC) Weight loss - Δ (%)
300 100
410 0.62
Table 8
The portion of SWCNT reinforced Nylon 66 nanofibers and MWCNT reinforced
Nylon 66 nanofibers in the hardened cement paste.
Temperature (oC) Weight loss - Δ (%)
SWCNT-N66 MCP MWCNT-N66 MCP
350 100 100
460 0.55 0.45
4. Conclusions
The influence of Nylon 66 nanofibers containing carbon nanotubes
on the mechanical strength and microstructure of hardened cement
pastes have been estimated through this study. An improved collector
system is proposed for blending the nanofibers with OPC through the
electrospinning process. MWCNTs and SWCNTs were dispersed in
Nylon 66 nanofibers and enhanced the strength of the hybrid nanofi-
bers. The SWCNT reinforced Nylon 66 nanofibers and MWCNT re-
inforced Nylon 66 nanofibers have become promising candidates to
reinforce cementitious material due to the increase of mechanical
strength results of hardened cement pastes up to 43 % and 57 % in
tensile strength and 30 % and 12 % in toughness, respectively. The
increase in mechanical strength can be explained by the bridging effect
and the well-linking of nanofibers with cement hydration products
(CSH, CH) in the microstructure of hardened cement pastes. As a con-
sequence, the stronger bonds were formed and the higher strengths of
hardened cement pastes were observed. Besides, the existence of CNT
reinforced Nylon 66 nanofibers has been clarified through the micro-CT
analysis as well as TGA analysis.
In future works, we intend to carry out a study on enhancing me-
chanical properties of hardened cement pastes by silica nanofibers with
the purpose that the existence of Silica component in this material will
take part in the pozzolanic reaction during the hydration process of
cement. Additional directions for future research include the linking
mechanisms between the nanofibers and the cement matrix, as well as
the workability and the realization of concrete when using this com-
posite cementitious material.
CRediT authorship contribution statement
Tri N.M. Nguyen: Data curation, Formal analysis, Investigation,
Visualization, Writing - original draft, Writing - review & editing. Doo-
Yeol Yoo: Formal analysis, Methodology, Supervision, Validation,
Writing - review & editing. Jung J. Kim: Conceptualization, Data
curation, Formal analysis, Funding acquisition, Investigation,
Methodology, Project administration, Supervision, Validation, Writing -
original draft, Writing - review & editing.
Declaration of Competing Interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influ-
ence the work reported in this paper.
T.N.M. Nguyen, et al. Materials Today Communications 23 (2020) 100845

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