The Journal of The Textile Institute

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Antimicrobial finishing of cotton fabrics based

on gamma irradiated carboxymethyl cellulose/
poly(vinyl alcohol)/TiO2 nanocomposites

Mervat R. Khafaga, Hussein E. Ali & Abdel Wahab M. El-Naggar

To cite this article: Mervat R. Khafaga, Hussein E. Ali & Abdel Wahab M. El-Naggar (2016)
Antimicrobial finishing of cotton fabrics based on gamma irradiated carboxymethyl cellulose/
poly(vinyl alcohol)/TiO2 nanocomposites, The Journal of The Textile Institute, 107:6, 766-773, DOI:
10.1080/00405000.2015.1061762

To link to this article: https://doi.org/10.1080/00405000.2015.1061762

Published online: 07 Jul 2015.

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The Journal of The Textile Institute, 2016
Vol. 107, No. 6, 766–773, http://dx.doi.org/10.1080/00405000.2015.1061762

Antimicrobial finishing of cotton fabrics based on gamma irradiated carboxymethyl cellulose/

poly(vinyl alcohol)/TiO2 nanocomposites
Mervat R. Khafaga, Hussein E. Ali and Abdel Wahab M. El-Naggar*
Radiation Chemistry Department, National Center for Radiation Research and Technology, Cairo, Egypt
(Received 16 November 2014; accepted 6 May 2015)

Synthesis of nanoparticles with antibacterial properties is of great interest for the development of textiles finishing, in
general, and cotton fabric, in particular. In this work, TiO2 nanoparticles at different concentrations were synthesized
using nitric acid as a reducing and stabilizing agent. Cotton fabrics were first impregnated, to a pick-up of 100%, in
colloidal solutions containing carboxymethyl cellulose (CMC)/polyvinyl alcohol(PVA)/TiO2 nanocomposites. After that,
the coated fabrics were exposed to gamma irradiation to produce TiO2 nanoparticles stabilized in cross-linked CMC/
PVA hydrogel. The formation of TiO2 nanoparticles was confirmed by ultra violet/visible (UV/vis) and transmission
electron microscopy, and the particle size distribution of the nanoparticles was determined using the dynamic light
scattering. The surface morphology of the finished fabrics was examined by scanning electron microscopy (SEM). The
SEM micrographs revealed that TiO2 nanoparticles were deposited on the surface of cotton fibers. The antibacterial
activity of the treated fabrics loaded with TiO2 nanoparticles was evaluated against Escherichia coli (Gram -ve) bacteria.
Keywords: cotton fabric; carboxymethyl cellulose; polyvinyl alcohol; TiO2 nanoparticles; gamma irradiation

Introduction work has been directed to apply TiO2 nanoparticles

Textile fabrics, especially those made of natural fibers
such as cotton and wool, can act as a media for the
growth of micro-organisms such as pathogenic or odor-
generating bacteria and fungi. The contact of such
materials with the human body offers an ideal
environment for microbial growth because of their large
surface area and ability to retain oxygen, moisture, and
warmth, as well as nutrients from spillages and body
exudates. Therefore, the antimicrobial finishing of
fabrics, used in different environments, has attracted
much attention in recent years (Kim, Kim, & Rhee,
2010).
Antimicrobial properties can be imparted to textile
materials by incorporating functional agents onto the
fabrics by chemical or physical methods. Recently,
attention has been focused on durable and
environmentally friendly agents. Previous studies have
shown that active agents in the form of nanoparticles
(NPs) can be considered as new antibacterial materials,
particularly silver nanoparticles (El-Rafie, Mohamed,
Shaheen, & Hebeish, 2010; Hebeish et al., 2011;
Hebeish, El-Shafei, Sharaf, & Zaghloul, 2011; Ilić et al.,
2009; Montazer, Alimohammadi, Shamei, & Rahimi,
2012; Xu, Shi, Ma Lv, Zhang & Mao, 2011).
TiO2 nanoparticles have many advantages such as
good stability, hydrophilic properties, UV blocking, and
excellent photocatalytic and antimicrobial activities
(Linsebigler, Lu, & Yates, 1995). Extensive research
stabilized by different composites as finishing agents for
cotton fabrics to impart microbial resistance. In this
regard, bleached untreated cotton fabrics and polyvinyl
pyrrolidone (PVP)-treated cotton fabrics were coated
with TiO2 nanowire and TiO2 nanowire-doped Ag-PVP
nanocomposites using the pad-dry-cure method (Hebeish,
Abdelhady, & Youssef, 2013). The antibacterial effect of
the synthesized sulfated β-cyclodextrin cross-linked
cotton fabric and its improved antibacterial activities
with ZnO, TiO2, and Ag nanoparticles’ coating were
investigated (Selvam et al., 2012). The antibacterial test
was done against Gram-positive Staphylococcus aureus
and Gram-negative Escherichia coli bacteria. Chitosan
was applied as an antibacterial agent to provide the
biocidal function for textiles (Cheng, Ma, Li, Ren, &
Huang, 2014). In this study, a new N-halamine chitosan
derivative was synthesized by introducing N-halamine
hydantoin precursor. The synthesized chitosan derivative,
1-Hydroxymethyl-5, 5-dimethylhydantoin chitosan
(chitosan-HDH), was coated onto the cotton fabric with
1,2,3,4-butanetetracarboxylic acid (BTCA) as a cross-
linking agent. The antibacterial activity of the cotton
fabric against S. aureus (Gram positive) and E. coli
(Gram negative) and its effect on the physical properties
of the cotton fabric were studied using the chitosan/
AgCl–TiO2 colloid (Arain, Khatri, Memon, & Kim,
2013). The results showed that the treated cotton fabrics
can render excellent antimicrobial activity upon exposure

*Corresponding author. Email: ab_nagga@yahoo.com

© 2015 The Textile Institute

 The Journal of The Textile Institute
to dilute household bleach. Morphology, photocleaning,
and water wetting properties of cotton fabrics, modified
with titanium dioxide coatings synthesized with plasma-
enhanced chemical vapor deposition technique, were
investigated (Guzenda et al., 2013). Sericin, as a
biological material extracted from raw silk by boiling in
hot water, and nano-TiO2 were dispersed in its solution
(Doakhan, Montazer, Rashidi, Moniri, & Moghadam,
2013). The prepared finishing agents with and without
polycarboxylic acid cross-linking agents were treated on
the cotton fabric using the pad-dry-cure method. The
antibacterial activity and the durability of modified
cotton fabrics were investigated against one Gram-
positive bacterium (S. aureus) and one Gram-negative
bacterium (E. coli). The finishing treatment on the cotton
fabric was found more effective against S. aureus than
E. coli. The antibacterial effect of the synthesized
sulfated β-cyclodextrin cross-linked cotton fabric and its
improved antibacterial activities with ZnO, TiO2, and Ag
nanoparticles’ coating were studied (Selvam et al.,
2012). Sulfated β-cyclodextrin was synthesized by the
sulfonation of β-cyclodextrin and the sulfated polymer
was cross-linked with the cotton fabric using
ethylenediaminetetraacetic acid as cross-linker. The
antibacterial test was done against the Gram-positive
Staphylococcus aureus and Gram-negative E. coli
bacterium. A novel N-halamine siloxane antibacterial
precursor, N-(3-triethoxysilylpropyl)-N′-(N″′-heptylcar-
bmido-N″-ethyl)-butanediamide (TSHCEB), was
synthesized and characterized (Wu, Xu, Cai, Zang, & Li,
2014). The compound was then tethered to the surface
of cotton fabrics through covalent ether linkages,
followed by the exposure to dilute sodium hypochlorite
solutions to confer the cotton fabric’s antibacterial
properties. The results showed that it provided excellent
antimicrobial properties against E. coli and S. aureus via
direct contacting for 2–15 min. The structure and
functional properties of hybrid nanomaterials based on
the TiO2-modified cellulose fibers of cotton were studied
(Galkina et al., 2014). The titania hydrosol was
successfully prepared using titanium tetraisopropoxide as
the precursor and nitric acid as the peptizing agent via
the low-temperature sol–gel synthesis in aqueous
medium and applied to the cotton fabric. The
antimicrobial activity of the treated TiO2 cotton fibers
was investigated against E. coli as model Gram-negative
bacteria after the exposure to UV-irradiation for 10 min.
Photocatalytic self-cleaning of the modified cotton
textiles by TiO2 clusters attached by chemical spacers
were reported (Meilert, Laub, & Kiwi, 2005). The
spacers were attached on the cotton by the formation of
an ester bond. The TiO2 binds to the cotton by chemical
means and the textiles present self-cleaning properties.
In previous studies, considerable attention has been
paid to the finishing of textiles using ionizing radiation
767
designed for protective clothing. These finishes include
protection against ultraviolet radiation (Zohdy, El
Hossamy, El-Naggar, Fathalla, & Ali, 2009), microbial
resistance (El-Naggar, Zohdy, Hassan, & Khalil, 2003;
Zohdy, Abdel Kareem, El-Naggar, & Hassan, 2003),
water resistance (El-Naggar, Zohdy, Mohammed, &
Alam, 2003), and crease recovery (Zohdy, Mohamed, &
El-Naggar, 2004). The present work is undertaken to
prepare TiO2 nanoparticles’ colloidal solutions of
different concentrations stabilized in carboxymethyl
cellulose (CMC)/polyvinyl alcohol hydrogel. Thus, the
cotton fabric was padded in the nanocomposite solutions
followed by gamma irradiation to form a cross-linked
structure with cotton cellulose. The antimicrobial activity
of the treated fabrics was evaluated against E. coli
(Gram -ve) bacteria.
Experimental
Materials
The cotton fabric used in this study was desized,
scoured, bleached, and was not subjected to any
finishing processes and was supplied by Misr for
Spinning, Weaving, El-Mehallah El-Kobra, Egypt. The
fabric samples were prepared in the shape of rectangular
stripes. CMC was a laboratory-grade chemical and
purchased from El-Gomhoria Co., Cairo, Egypt.
Polyvinyl alcohol (PVA) was a laboratory-grade
chemical and purchased from Backer Chemical Co.,
USA. It was in the form of powder, fully hydrolyzed
and has an average molecular weight of 125,000 g/mol.
Preparation of TiO2 nanoparticles
Ten milli liters of titanium isopropoxide (95%, Alfa,
Aesar, Germany) were added drop wise at room
temperature to 60-ml 0.1-M nitric acid solution under
continuous stirring (Essawy, Ali, & Abdel-Mottaleb,
2008). A white precipitate is formed instantaneously.
Immediately after the hydrolysis, the slurry is heated to
80 °C and stirred for 8 h in order to achieve peptization.
Preparation of CMC/PVA/TiO2 nanocomposites
An aqueous solution containing 20 wt.% from CMC and
PVA polymers was dissolved in distilled water at 80 °C
to obtain polymer blends of equal ratio. The solutions
were then mixed by continuous stirring for 4 h until
complete miscibility. The colloidal solution of TiO2
nanoparticles was diluted into two different
concentrations (0.002 and 0.005 M) with distilled water
at room temperature (25 °C) and added to CMC/PVA
solution. The mixture was made free of air by purging
nitrogen gas.
768 M.R. Khafaga et al.
Treatment of cotton fabrics with CMC/PVA/TiO2
nanocomposites
Padding is the most common finishing method for the
application of chemical formulation to textile materials
in continuous processes. Padding involves contacting the
textile material with the formulation, by immersion, and
squeezing the formulation out. Thus, the cotton fabric
samples were immersed in the colloidal solutions of
CMC/PVA/TiO2 nanocomposites for two minutes
followed by squeezing to 100% wet pick-up. The fabric
samples were then exposed to gamma irradiation.
Irradiation to the required doses was carried out in the
cobalt-60 gamma cell facility of National center for
radiation research and Technology (NCRRT), Cairo,
(made in Russia) at a dose rate of 4.8-kGy/h.
Characterizations and analysis
The formation of the TiO2 nanoparticles was determined
using Unicam 8625 UV/visible spectrophotometer,
Manshester, England. The morphology of the TiO2
nanoparticles was examined using transmission electron
microscopy (TEM), model JEM 100CS, Joel electron
microscopy, Tokyo, Japan. The TEM images were taken
at 80 kV. Scanning electron microscopy (SEM) was used
to examine the surface morphology of the cotton fabric
treated with TiO2-based nanocomposites before and after
gamma irradiation. The SEM micrographs were taken
with the Joel -JSM5400 (Tokyo, Japan). A sputter coater
was used to pre-coat conductive gold onto the fabric
surfaces before observing the microstructure at 30 kV.
The particle size distribution of the nanoparticles was
determined using the dynamic light scattering (DLS)
technique (Nicomp 380ZLS, PSSNICOMP, particle
sizing system, Santa Barbara, USA). The water
absorbance of the treated cotton fabrics with CMC/PVA/
TiO2 nanocomposites was evaluated according to the
AATCC test method 79-2007. This test method is
designed to measure the water absorbency of textiles by
measuring the time taken by a drop of water placed on
the fabric surface to be completely absorbed into the
fabric. In this test, the sample is placed over the top of a
beaker so that the center is unsupported. A measured
drop of water is placed on the fabric 1 cm from the
surface and the time is recorded until the water drop
absorbs completely. The recorded wetting time is the
average of five measurements in different positions along
the sample.
Antibacterial testing
The antibacterial activity of the cotton treated with TiO2-
based nanocomplexes was evaluated against the Gram-
negative bacterium E.coli as the model micro-organism.
The bacterial inoculum was prepared in Luria Bertani
(LB) nutrient broth (pH = 7) containing 10-g/L Tryptone
Peptone, 5-g/L Bacto Yeast extract, and 5-g/L NaCl at
37 °C for 12 h. All the test samples were cut into square
disks (10 mm in length). The zones of inhibition were
calculated to evaluate the antimicrobial activity. For the
zone of inhibition method, the control and the test
samples were placed on the E. coli growth agar plate
and incubated at 37 °C for 24 h. The inhibition zone was
calculated by measuring the diameter of the nearest
whole millimeter of the inhibited growth around the
sample disk and was performed in triplicates.
Results and discussion
Characterization of TiO2 nanoparticles
Figure 1 shows the UV/vis absorption spectroscopy for
TiO2 colloidal solutions prepared at 0.002 and 0.005 M.
It is clear that the band becomes stronger and more
symmetrical with a pronounced bell shape at λmax
350 nm. The band can be assigned to the plasmon
resonance of TiO2. These findings are in agreement with
previous literature which demonstrated that TiO2
nanoparticles, over 300–370 nm, have a very good UV
absorption property (Trung, Cho, & Ha, 2003).
Figures 2 and 3 show the TEM image and the
histogram of the size and size distribution of TiO2
(0.005 M), respectively. The images obtained indicated
that the resultant product contains a well-stabilized TiO2
solution with a diameter range of 30–120 nm. TiO2
solutions with such unique characteristics are
unequivocally feasible for industrial applications.
5
4
0.005M
0.002M
Absorbance (arbitrary units)
3
2
1
0
100 200 300 400 500
Wavelength (nm)
Figure 1. UV/vis absorbance of TiO2 nanoparticles’ colloidal
solutions prepared at 0.002 and 0.005-M concentrations.
 The Journal of The Textile Institute 769

(A) (B)

Figure 2. TEM images of TiO2 nanoparticles’ colloidal solutions prepared at (A) 0.005-M and (B) 0.002-M concentrations.

120
The mechanism of cross-linking of PVA in aqueous
solution can be briefly outlined as follows: (1) the
Intense-wt Gaussian Distribution polymer PVA-H and the solvent HOH absorb the gamma
100 120
radiation and go to the transient activated states PVAH
and HOH , which dissociate causing the formation of
100 the radicals PVA , HO , and H ; (2) the transfer of
80
80
the radical from water to polymer increases the
concentration of PVA radicals and increases the rate of
REL

60 cross-linking and gelation:

REL

60
40 PVA  H þ ðHO or HO Þ!PVA þ H2 O
20 (3) two polymer radicals PVA with m and n repeat units
40
0
combine to form a cross-linked point:
20 40 60 80 100 120 PVAm þ PVAn !PVAm  PVAn :
Diameter (nm)
20 The cross-linking of CMC by ionizing radiation was
reported in many research works (Wach, Mitomo,
Nagasawa, & Yoshii, 2003; Yoshii et al., 2003). The idea
0 is to apply high concentrated aqueous solutions of the
0 100 200 300 400 500
polymer of high degree of substitution. It was assumed
Diameter (nm) that the hydrogel formation by radiation is mainly due to
the mobility of side chains. Side chain radicals are formed
Figure 3. Histogram of TiO2 nanoparticles’ size distribution mostly via indirect effects by the abstraction of H atoms
measured by the DLS method. by the intermediate products of water radiolysis. The
radiation cross-linking of CMC of various degrees of
substitution at high concentration in aqueous solutions of
Radiation effects on the cotton fabrics finished with
natural pH was also studied (Wach, Mitomo, Yoshii, &
CMC/PVA/TiO2 nanocomposites
Kume, 2001). Thus, the formation of the network
Polyvinyl alcohol (PVA) is known to undergo radiation- structure of CMC/PVA/TiO2 with cotton could be formed.
induced polymerization and subsequent cross-linking to
form hydrogels. The cross-linking of vinyl monomers in
solutions by gamma radiation was early established by Scanning electron microscopy (SEM)
Chapiro (1962). Polymerization and cross-linking occur Figure 4 shows the SEM micrographs of the cotton
also by the products of the radiolysis of water, which is fabric before and after the treatment with CMC/PVA/
present in appropriate quantities, as follows: TiO2 followed by gamma irradiation at different doses.
Before gamma irradiation, it can be seen that because of
Gamma irradiation
ƒ! e
H2 O ƒƒƒƒƒ aq ; OH; H; H2 O2 ; H2
the treatment of the cotton fabric with the
nanocomposites, the outer layer of the cotton fibers was
770 M.R. Khafaga et al.

findings indicate that the nanocomplexes interacted with

the cotton fabric through cross-linking.

Water absorbance
The highly branched sites in PVA/CMC cross-linked
networks are separated by secondary hydroxyl and
carboxylic groups. As CMC polymer component has an
anionic nature, there is a strong ionic interaction between
(A) (B) PVA and CMC molecules; it is proposed that an
interpenetrating structure was formed. For this reason,
higher cross-linking density of PVA and CMC would
lead to the production of smaller pores, and thus
absorption of less water amount. The water absorbance
at room temperature of the cotton fabric before and after
treatment with CMC/PVA/TiO2 nanocomposites with
different concentrations of TiO2 nanoparticles was
determined according to the AATCC test method 79–
2007 as shown in Figure 5. As shown, the untreated
blank cotton fabric possessed higher water absorbance,
(C) (D)
in terms of wetting time, than the treated blank cotton
with 0.005-M TiO2 nanoparticles. The increase in water
absorbance associated with the increase in irradiation
dose may be attributed to the oxidative degradation of
cotton cellulose. It is clear that the treatment with CMC/
PVA/TiO2 nanocomposites decreased the water
absorbance of the blank cotton, regardless of TiO2
concentration. However, the treatment with higher
concentrations of CMC/PVA/TiO2 nanocomposites

(E) (F) 35

Figure 4. SEM micrographs of cotton fabrics: (A) Blank, (B)

30
unirradiated and treated with CMC/PVA/TiO2 (0.005-M TiO2),
(C) treated with CMC/PVA/TiO2 (0.002-M TiO2-10 kGy),
Wetting time (seconds)

(D) treated with CMC/PVA/TiO2 (0.002-M TiO2-30 kGy), (E)

treated with CMC/PVA/TiO2 (0.005-M TiO2-10 kGy), and (F) 25
treated with CMC/PVA/TiO2 (0.005-M TiO2-30 kGy).

20
covered with tiny particles of nanosize (Figure 4(B)). As
shown in Figure 4(C)–(F), the SEM micrographs showed
that the fiber thickness increased in diameter from 25 μm 15
for blank cotton to ~60 μm after finishing. This is due to
the branching of the cross-linked finishes induced by
Blank cotton
Blank cotton (0.005M TiO2)
gamma radiation and the interactions with cotton fibers. 10
(TiO2=0.002M)
Even though the treatment with CMC/PVA/TiO2 TiO2 (0.005M)

nanocomposites covered the fabric structure with the 5

networks, the density of covering increased with the 0 5 10 15 20 25 30 35
increase in irradiation dose and TiO2 concentration. The Irradiation dose (kGy)
notable thing about the finished/gamma-irradiated fabric
is that the voids between the fibers were partially filled
with CMC/PVA/TiO2 nanocomposites. This is due to the Figure 5. Effect of irradiation doses on the water absorbance,
at room temperature, of the blank cotton fabric before and after
weight increase after impregnation and drying. treatment with 0.005-M TiO2 nanoparticles and cotton fabrics
Moreover, the visual observation showed no difference treated with CMC/PVA/TiO2 nanocomposites containing
between the finished and unfinished fabrics. These different concentrations of TiO2 nanoparticles.
 The Journal of The Textile Institute 771

caused a further decrease in water absorbance.
Meanwhile, the water absorbance was shown to decrease
with the increase in irradiation dose. This is may be due
to the occurrence of high concentration of TiO2
nanoparticles in the network structure, interrupting the
hydrogen bonding interactions between the OH and
COOH groups of molecules, leading to the reduction of
pore sizes of PVA/CMC/TiO2 nanocomposites. The
decrease in water absorbance associated with the
increase in irradiation dose is attributed to the increase
of cross-linking density, in which the chains are compact
and thus block the voids for the diffusion of water
molecules (Nizam El-Din, Abd Alla, & El-Naggar,
2007).
Antimicrobial activity of cotton/CMC/PVA/TiO2
nanocomplexes
The growth of micro-organisms on textiles can cause
three main problems including changing the color of
samples, producing unpleasant odors, and increasing the
health risk of using such garments. These micro-
organisms can be found everywhere in our surroundings.
This process is expedited in places where necessary
breeding grounds such as nutrients, temperature, and
moisture exist. They can be multiplied quickly, thereby
affecting textiles negatively.
In this study, the antimicrobial properties of the
cotton treated with CMC/PVA/TiO2 nanocomposites and
gamma irradiated at the dose of 30 kGy were tested
against E. coli bacteria in terms of zone inhibition.
Figure 6 shows photographs of rectangular pieces of the
treated cotton fabrics placed on agar plates, in which the
E. coli bacteria grow. For the blank cotton samples,
either untreated or treated-unirradiated, no inhibition
zones were formed against the growth of E. coli bacteria
as shown in Figure 6(A) and (B). This finding indicates
that the untreated cotton fabrics have no microbial
resistance. On the other hand, cotton fabrics treated with
CMC/PVA/TiO2 showed clear antimicrobial properties,
in which inhibition zones were formed against the
growth of E. coli bacteria as shown in Figure 6(C) and

(A) (B)

(C) (D)

Figure 6. Photographs of the inhibition zones against E. coli bacteria of cotton fabrics treated with CMC/PVA/TiO2
nanocomposites: (A) Blank, (B) treated-unirradiated, (C) treated with 0.002-M TiO2-30 kGy, and (D) treated with 0.005-M TiO2-
30 kGy.
772 M.R. Khafaga et al.
(D). However, the inhibition zone was found to increase
relatively with the increase in TiO2 concentration. The
calculated inhibition zone of cotton fabrics treated with
CMC/PVA/TiO2 nanocomposites containing 0.002 and
0.005-M TiO2 nanoparticles was found to be ~10 and
12 mm, respectively.
The antimicrobial activity of TiO2 nanoparticles was
explained due its positive species produced by TiO2,
especially under UV rays whose energy level is higher
than that of its band gap (Montazer et al., 2012). This in
turn gives birth to the photocatalytic nature of TiO2
which reacts with negatively charged components at the
cell surface of bacteria, leading to the leakage of
intercellular substance. As a result, the normal
metabolism of micro-organisms is inhibited, leading to
the death of bacteria.
Conclusions
In this study, stabilized TiO2 nanoparticles’ colloidal
solutions with different concentrations of a diameter of
~30–120 nm were prepared using nitric acid as both a
reducing and stabilizing agent. The cotton fabric was
treated with TiO2 nanoparticles incorporated in PVA/
CMC composites to impart antimicrobial finishing. It
was found that using a concentration of 0.005-M TiO2
nanoparticles is enough to exhibit acceptable
antibacterial activity against E. coli bacteria. The SEM
micrographs indicated that the TiO2 nanoparticles are
well dispersed on the cotton fibers. Gamma radiation
was successfully used to form a cross-linked structure
with cotton cellulose, and thus enhanced the stabilization
of TiO2 nanoparticles. Therefore, this kind of treatment
may be considered as an environmentally friendly
process in the fabrication of antibacterial finishing of
textiles.
Disclosure statement
No potential conflict of interest was reported by the authors.
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