A Review of Antimicrobial Fabric Containing Nanostructures

Metal-Based Compound

Lee-Yae Tan,1 Lee Tin Sin ,1 Soo-Tueen Bee ,1 Chantara T. Ratnam,2 Kwan-Kit Woo,1
Tiam-Ting Tee,1 Abdul Razak Rahmat3
1
Department of Chemical Engineering, Faculty of Engineering and Science, Universiti Tunku Abdul Rahman,
Jalan Sungai Long, Bandar Sungai Long Cheras, Kajang 43000, Selangor, Malaysia
2
Radiation Processing Technology Division, Malaysian Nuclear Agency, Bangi, Kajang 43000, Selangor,
Malaysia
3
Department of Polymer Engineering, Faculty of Chemical Engineering, Universiti Teknologi Malaysia, 81310
UTM Skudai, Johor, Malaysia

Textile can be a potential microorganism’s propagation
site because it contacts with human skin endows opti-
mal conditions combination of nutrient sources, tem-
perature, and moisture which provides conducive
environment for microorganism growth. Thus, the
development of antibacterial textile is crucial to inhibit
the growth of microorganisms for protection the health
and safety of wearer. This review article focuses on
several metal-based nanoparticles possess biocidal
feature namely, Ag, ZnO, Cu based, TiO2, and other
minor metals based such as iron based, CeO2, Au,
SiO2, Ni, and Pt. The phenomenology of metal nano-
particles associated to the antibacterial effects and
possible mechanisms of action against bacteria have
been highlighted. This review also discussed the syn-
thesis techniques and effects of incorporation additive
materials of those metal-based nanoparticles to inhibit
the growth
growthofofmicroorganisms.
microorganisms.J. VINYL ADDIT.
J. VINYL TECHNOL.,
ADDIT. TECH-
25:E3–E27,
NOL., 2019. ©2017.
00:000–000, 2017 V
Society
C of Plastics
2017 Society Engineers
of Plastics Engineers
INTRODUCTION
Textile has been widely used for clothing application
since thousand years ago. Among these are wool (WO),
silk, cotton, nylon, etc. However, the vulnerability of
microorganisms attacking on textile could be a serious
problem. The optimal moisture affinity and natural feature
of those textiles could be favorable for microorganism’s
hostility especially those used in hospitals, infant wear,
underwear, and sportswear which have high chances of
contacting bacteria [1]. The infection caused by
Correspondence to: L.T. Sin; e-mail: direct.tinsin@gmail.com and S.-T.
Bee; e-mail: direct.beest@gmail.com
Contract grant sponsor: Ministry of Science, Technology and Innovations
(MOSTI) of The Federal Government of Malaysia under ScienceFund;
contract grant number: 03-02-11-SF0206.
DOI 10.1002/vnl.21606
Published online in Wiley Online Library (wileyonlinelibrary.com).
C 2017 Society of Plastics Engineers
V cidal textile field. These metallic based materials have
pathogenic microorganisms, particularly Escherichia coli,
Staphylococcus aureus, and Klebstella pneumoniae should
be controlled as the proliferation of microorganisms on
textile could lead to dramatic effects such as deterioration
of textile strength, defacement, and odors which can con-
taminate the textile as well as endanger the wearer [2].
Generally, the impacts of microorganism on textile
material could be performed by two main approaches,
namely assimilation and degradation. In fact, their metab-
olites revealed in occurrence of spots on textile surface,
formation of bubbles on colored surface of textile materi-
als, induction of bond breaks in fibrous materials, pene-
tration into cavity of natural fiber, and adverse effect on
mechanical strength, mass loss, alteration of chemical
properties, and other properties [3].
Owing to the improvement of healthcare concern
related with the infection of diseases by various microor-
ganisms, multifunctional textile has been developed in
order to prohibit the growth of bacteria onto the textile
where it will lead to adverse hygiene effect on wearer.
Nowadays, scientists are concerned about incorporation of
nanotechnology to produce multifunctional fabrics. Gener-
ally, nanotechnology is gaining interest to be used on
coating nanoparticles (NPs) on textile to avoid degrada-
tion and discoloration by microorganisms while prevent-
ing propagation of bacteria. Over the past few contracts,
metal-based NPs whose structures endowed novel func-
tionality and ability to improve pristine textile in term of
physical, chemical, and biological have been studied as
one of the most promising route to produce antibacterial
textile. Up-to-date, the common metallic based NPs used
in development of antibacterial textile are Ag, ZnO, Cu
based, and TiO2. Also, there were researches on other
metal-based NPs namely, iron based, CeO2, Au, SiO2, Ni,
and Pt which have been investigated to be applied on bio-

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their own unique properties beside antibacterial feature
which further improve the textile finishing.
Based on tremendous increase in the number of inves-
tigations and developments on the properties of suitable
metal-based NPs and their efficiencies on antibacterial
property, this review mainly focus on comprehensive
compilation of published metal-based NPs used to synthe-
size antibacterial textile finishing and the proposed syn-
thesis techniques. Moreover, it also concerned with the
mechanisms of action against bacterial cell death as well
as the factors influence the efficiency of antibacterial
performance.
TYPE OF TEXTILE
Textile can be categorized into three main sources
namely, animal-based, plant-based, and synthetic-based
textile. Each of them has its own unique characteristics
which are applied on different textile fields such as medi-
cal textile, sportswear, children’s wear, furniture’s uphol-
stery, and etc.
Animal-Based Textile
Animal-based textiles to be discussed are originated
from WO and silk. WO widely used on textile applica-
tions are the one made from goat, sheep, camel, and rab-
bit which possessed high extent of warmth [3]. Whereas,
silk is an animal fiber produced from cocoon with its
softness in fame.
Wool. WO is a natural animal fiber which mainly con-
stitutes of fibrous protein substance, called keratin which
contains more sulfur content compared to other types of
protein. These filaments of keratin are aligned in continu-
ous fiber axis in cortical cell, bounded by a lipid mem-
brane called cell membrane complex (CMC). The keratin
fibers with disulfide crosslinks between individual poly-
peptide chains have improved fabric’s strength and ther-
mal stability. Although the advantages of excellent in
chemical resistance and other mechanical strength, the
presence of cysteine bonds are susceptible to sunlight,
caused the fabric weakened by prolonged exposure to
sunlight [3]. Moreover, the WO fabric is subjected to
microorganism’s damage. The keratin is a major compo-
nent of WO, acts as a nutrition and energy source for
microbes and bacteria growth. Hence, the microorgan-
ism’s propagation on WO fabric induced health problems
such as skin irritating [4]. There are several researches
that studied the antibacterial activity of WO fabric func-
tionalized with different potential NPs such as Ag [5–11],
Cu [12, 13], TiO2 [14, 15], and SiO2 [16]. The features
of WO facilitate the bonding formation with NPs which
are favorable to a long-term antibacterial performance.
Based on the literature [5], amino acids and sulfurs in the
WO fibers provide binding sites for silver to form stable
silver mercaptides. Moreover, the nonkeratinous cell
membrane cortex region which is light crosslinked
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exhibits high water absorbency which able to absorb up
to 30%–38% of its original weight. It is proposed that
these reasons result the high affinity of NP’s adsorption
on WO fabric. Hence, it generates excellent antimicrobial
efficiency of WO fabric in the long run. According to
Heliopoulos et al., the usage of alginate increases the cop-
per sorbing capacity due to its structure comprised of
abundant carboxylic groups (ACOOH) that forms bonds
with mercapto groups, carboxylic or sulfonic groups of
WO keratin, thus offering excellent antibacterial effect
[12]. The CMC lipid layer inside cortical cell of WO
fiber making the surface of WO hydrophobic, results the
difficulties in process of dyeing and finishing of fabric.
Nevertheless, the embedment of silica NPs not only pro-
motes the uptake of NPs on WO, it also alters the wetta-
bility of WO gives the WO to be super-hydrophilic [5, 8].
Silk. The raw silk consists of two main components
called fibroin and sericin. However, the raw silk is not
suitable to be used as textile application directly. This is
probably due to once the presence of sericin inside the
human body, it is detected as an antigenic factor by T
cells and triggers immulogic reaction. Thus, extraction of
sericin is necessary before further processing and the pro-
cess is known as degumming process. Upon degumming
silk or silk fibroin, it appears shiny and feels soft to touch
and is highly demand in textile industry [17]. Silk fibroin
produced from the cocoon Bombyx mori, in particular, is
widely used in medical wound dressing due to its inher-
ently biocompatibility, proper strength, morphologic flexi-
bility, biodegradability, and permeability [17, 18]. Despite
of the advantages, the natural protein fiber of silk serves
as a carbon and nitrogen sources for microorganism’s
growth [19]. Adherence of microorganism adversely dete-
riorates the strength by deformation the surface and also
alters the original color by means of microbial secretions
or spores [20]. Thus, the development of multifunctional
silk textile particularly on antibacterial aspect by using
nanostructure metal-based materials have been studied
such as CeO2 [19], Ag [21, 22], TiO2 [22], and Au [23].
Plant-Based Textile
Cotton and bamboo pulp are two main sources for
plant-derived textiles. They are widely used on clothing
due to its abundance, comfortability, soft, and breathable
natural fiber. Moreover, there are semisynthetic textile
which is derived from natural sources, known as viscose
or rayon [3].
Cotton. Cotton, composes of celluloses and hemicellu-
loses, is the most abundant natural polymer on the Earth.
It is linked with a range from as low as 15 or less to as
high as 7,000–10,000 of linear, straight chain of D-glucose
units which condense through b (1!4)-glycosidic bonds.
As cellulose is one of the renewable carbon source, cotton
is susceptible for microbial degradation. Different degra-
dation mechanisms could be resulted for different types
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of microorganisms involved. The attack of fungi can be
initiated from the cracks on the cotton fiber surface or at
the ends of fiber causing the degradation occurs from the
inner to outer layer of the fibers. Whereas, it is opposed
from the cotton degradation by bacteria where the process
starts from fiber surface extends throughout to the inner
layers of fibers. In general, the depolymerization of cellu-
lose is the main cause for deterioration of cotton in terms
of weight and strength [24]. Biodegradation of cotton
causes discoloration, foul smelling, appearance disfigura-
tion, and hygiene issue in the products [25]. In order to
suppress the negative impacts of microorganism’s adher-
ence on cotton fabric, there are numerous of studies on
metal-based NPs coated on cotton fabric for aiming anti-
bacterial purpose such as Ag [26, 27], ZnO [28], Cu [29],
and Fe3O4 [30].
Bamboo. Bamboo-based textile has been commonly
used due to its wicking property, excellent water absorp-
tion, and permeability. The natural hollowness in the hori-
zontal cross sections, making bamboo has numerous
micro-holes and micro-gaps to absorb and evaporate the
moisture of human skin readily. This special feature cre-
ates superb ventilation and thus inhibits the growth of
bacteria. As comparison with cotton, bamboo has been
discovered more eco-friendly in terms of land use, irriga-
tion, and pesticide adoption. The propagation rate of bam-
boo is considered as one of the fastest growing plants,
which at 3 to 4 years growth rate. Moreover, bamboo
fiber requires less amount of dye and thus less waste pro-
duced to the environment [31]. Bamboo is a natural bio-
polymer made up of lignocellulose, which is categorized
as the grass family Poacease [32]. It has been found that
bamboo fiber has excellent antibacterial and bacteriostatic
bio-agent due to the presence of bambocane substance in
the fiber [3, 33]. However, due to the process of hydroly-
sis alkalization and multiphase bleaching in the refining
process, the intrinsic antibacterial feature disappeared
[33]. Thus, imparted ZnO [34], Ag [35], and Au [35] on
bamboo pulp fabric have been studied and the results
have revealed that the modified fabrics possessed antibac-
terial activity.
Viscose/Rayon. Viscose or rayon is regenerated fiber
derived from natural resource such as WO pulp or bam-
boo pulp. It is classified as semisynthetic fiber which
comprises of cellulose macromolecules made up of gluco-
pyranose rings link with b-1,4-glycoside bond and each
of glucopyranose ring is composed of three hydroxyl
alcohols. This is conducive for hydrogen bonding forma-
tion between hydroxyl group of viscose and water, mak-
ing viscose hydrophilic, breathable, and cool [36]. The
versatility of bamboo viscose fiber is widely employed in
the production of sanitary, apparel, geotextile, hygiene,
composites, and filtration fabrics. Similar to cotton, the
cellulosic components serve as a nutrient for microbial
growth and cause the viscose fabric’s degradation [33].
Several studies have been reported on coating metal-
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based materials on viscose fabric namely, Ag [36–41],
TiO2 [41], Cu-based material [32, 36, 42], Zn [42], Ni
[42], and SiO2 [43].
Synthetic-Based Textile
Synthetic textiles are textiles made from man-made
such as polyester, nylon, and acrylic, which are made up
by joining monomers into long polymer chains. These
textiles endow different features that some might not
inherited by that produced from natural sources such as
waterproof, elasticity, wrinkle-free, flame resistant, etc.
[44].
Polyester. Polyester fabric is a man-made fabric consti-
tutes of poly(ethylene terephthalate) (PET) that made up
almost 50% of all fiber materials with considerable
strength and chemical resistance with dimensional stabil-
ity [45, 46]. The outstanding characteristics of PET such
as better elasticity, wrinkle and shrinkage resistance, pleat
retention, good easy care properties, not undermined by
sunlight and weather making polyester extensively used
as children’s wear, lingerie, raincoat, pants, shirts, sport-
wears, separates, jackets, blouses, and dress. Also, by
blending polyester with WO, the composite endowed fea-
tures to eliminate crushing and reduce fading, which it
has widely employed on furniture’s upholstery and fiber-
fill in pillows [44]. However, the hydrophobicity of PET
leads to poor adhesion of the coating and shorten the
durability of finishing treatment. This is due to the pres-
ence of benzene rings and ACH2CH2A groups in PET
that endow nonpolar characteristic causes it not capable
to form hydrogen bonds with other molecules [47]. More-
over, the lack of hydrophilic property brings the fabric
susceptible to generate and accumulate static electric
charge, hard to clean during laundering, and prone to
pick up dirt which might deteriorate the hygiene and
health of wearer [46]. According to recent studies, the
authors are focused on modification of polyester into
more hydrophilic at the same time endowed antibacterial
property. Among the modification agents are Ag [48] and
Pt [49]. Blending both natural and synthetic fibers is an
important treatment to produce wide variety of yarns with
desirable attributes and at the mean time covers up nega-
tive characteristics of both fibers. Blending polyester with
cotton synthesizes fabric inherits merits of polyester and
cotton such as wear and easy care property and high
moisture absorbency, respectively. Meanwhile, it reduces
the features such as poor moisture absorption and static
dissipation from polyester and poor crease retention and
wrinkle recovery from cotton [44]. Rastgoo et al. have
studied to produce blended polyester/cotton fabric with
antibacterial, magnetic, photoactive, and sonocatalytic
properties via sonosynthesis of magnetite iron oxide NPs
[30]. Hanh et al. have immobilized Ag NPs on peco bed
sheets (65% polyester, 35% cotton) for antibacterial per-
formance evaluation [50]. The results proved that the
modified peco bed sheet successfully inhibited the growth
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of the clinical breed such as S. aureus, K. pneumoniae,
Acinetobacter spp., E. coli, Enterobacter spp., Proteus,
Pseudomonas aeruginosa, Provindencia spp., Streptococ-
cus pneumoniaea, and Staphylococcus epidermidis.
Kleme n cıc et al. have compared the antibacterial perform-
ances of Ag based on three different types of coated fab-
ric namely, WO, polyester (PET), and polyester blended
WO (PET/WO) [5]. The results showed that all the modi-
fied fabrics facilitate the bacterial reduction to a lesser or
greater extent, which strongly depend not only on the
concentration of Ag adherence on fabric but also the fea-
ture of fabric itself. According to the results, PET has the
lowest concentration of adsorbed Ag, followed by PET/
WO and WO fabric. However, their antibacterial perfor-
mance exhibited in opposite trend. This could be due to
the bonding between Ag and WO. The high affinity of
Ag to sulfur in the cuticles of the WO fiber tends to form
stable silver mercaptide, thus making it harder to release
silver cations. Conversely, the high antibacterial activity
on PET fabric is attributed to the weak physical bonding
with Ag, whereby the silver cations are more readily to
be leached into surrounding. Moreover, PET possesses
structure with more aromatic, higher crystalline, and
hydrophobic than WO fabric, caused it is more resistant
to microbial adherence and it is inherited on blended
PET/WO as well where the wettability decreases which
impairs the microbial growth.
Polyamide/Nylon. Polyamide, also known as nylon is
made up of monomers with one molecules having acid
group (COOH) attached to its end with another molecules
containing amine group (NH2). Generally, there are two
main compounds that have found widespread use in tex-
tile industry which are polyamide 6,6 and polyamide 6.
Due to high stretchability and elasticity recovery proper-
ties, it is widely used in women’s lingerie and hosiery. Its
abrasion resistance and low absorbency favor the use in
produce sport-wear, raincoats, ski and snow apparel, and
so on [44]. There are several researches on synthesis of
multifunctional nylon fabric coated with metal NPs (Ag
[51–54] and Cu [55]) having electroconductivity, UV pro-
tection, antibacterial properties, etc. Blending nylon with
cotton has found to have high abrasion resistance and
comfortability and it is used in labor cloth, uniform, and
dressing [56]. Accordingly, Meftahi et al. [56] have
employed ZnO/TiO2 nanocomposite on nylon/cotton and
have found there is considerable improvement in light,
washing fastness, and antibacterial properties against E.
coli and S. Aureus.
Acrylic. Acrylic fabric as one of the synthetic fabrics is
typically used in textile field due to its WO-like feel,
resilient, and resistant to outdoor exposure and chemical
substances [57]. Mekewi et al. have introduced Cu, Zn,
and Ni chelated on acrylic and viscose fabrics with ali-
phatic and aromatic amines as binding agents and have
found that acrylic fabric has more favor to metal uptake
and copper chelated amine coated for both fabrics have
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higher microorganism’s hostility resistance compared
with that those Zn- and Ni-coated fabrics [42]. The ele-
vated metal ions uptake by acrylic fabric is due to the
presence of tactical isotactic structure, which has the abil-
ity for coordinate bond formation with the pendant acry-
lonitrile groups of acrylic polymer chain as well as via
ionic bonding with the carboxylic groups of acrylic
molecules.
TYPE OF METAL-BASED ANTIBACTERIAL
AGENTS ON TEXTILE
Metal-based NPs on textile on the basis of containing
excellent antibacterial property have been studied. Among
those are Ag, ZnO, Cu-based, TiO2, and other minor met-
als namely iron based, CeO2, Au, SiO2, Ni, and Pt. They
are functionalized on textile either in dispersed form or
incorporation with polymer matrix to enhance its antibac-
terial activity.
Silver NPs (Ag NPs)
Ag NPs is one of the most promising metal-based bac-
tericidal and therapeutic agents that have been widely
used in numerous industry fields. It is reported that silver
is very versatile to inhibit approximate 650 species of
bacteria. The manufacturing of Ag grafted textiles has
been developed for domestic, medical, and other func-
tions. In medical application, it is applied to bandages,
wounds dressings, and surgical thread. While for domestic
clothing, it is used for sportswear, underwear, and mili-
tary uniform [58]. Its antibacterial effectiveness is superb
compared to other metal-based materials such as Cu-
based, ZnO, and TiO2. Ren et al. have reported that the
minimum bactericidal concentration of a range of micro-
organism strains needed for CuO, Cu, Cu2O, and ZnO are
higher compared to Ag [59]. Silver endows high antibac-
terial action even with small dose usage and it is not
harmful to human being. According to Lee and Jeong,
colloidal silvers with nanosized (2–3 nm and 30 nm) par-
ticles on textile fabric have ability to kill 99% of S.
aureus and K. pneumoniae and are proven skin-innoxious
when come into contact with human skin [60]. To manu-
facture effective antimicrobial-functionalized fabric, the
mechanisms of action against bacteria must be well
understood. However, the published literatures are varied
with conditions where physical and chemical modification
can be resulted and altered the interaction with bacteria
of interest. The method of synthesis of the material, addi-
tive or capping agent involved, bacteria strain used,
nature of test to assess it, and so on could lead to differ-
ent outcomes. However, most researchers have intuitively
attributed the inhibition growth of bacterial cell by Ag is
due to presence of Ag1 ions and Ag NPs. According to
Quay and Stellacci [61], Ag NPs agglomerate around the
bacterial membrane and cause diminution bacterial mem-
brane integrity and as a result leading to cellular death.
This physical mode of antibacterial action relies on the
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size of Ag NPs to facilitate the penetration of these par-
ticles through the cell membrane to the intracellular
matrix and trigger cytotoxic mechanism. Moreover, sev-
eral studies revealed that Ag NPs induce generation of
reactive oxygen species (ROS) which accumulate to cre-
ate very high oxidative stress inside the cell and inacti-
vate the cell. The role of Ag1 ions on inhibition
microorganism growth relies on high affinities for organic
phosphates, amines, and specially thiols. Those chemical
compound can be found mainly on DNA, peptides (com-
ponent of membrane-bound or intracellular component),
and cofactor. Silver is categorized as oligo-dynamic metal
and acts as a bridging agent to form bonds with several
thiols cause the irreversible aggregation of thiol-bearing
molecules and subsequently inactivate the biological sys-
tem of bacterial cell. Compared to other antibiotic agent,
Ag1 ions can bind nonspecifically to broad range of tar-
gets, disturbing the cellular metabolism and leading to
cell death [61]. Incorporation of other constituents inside
the NPs system could also enhance to the antibacterial
property on modified fabric. Among these additives are
TiO2/SiO2/alginate [4], silica [5, 8], trisodium citrate [7],
sodium bisulfite, and sodium dithionite [10], tris(2-car-
boxyethyl) phosphine [6, 21], lecithin [11], glucose [26],
butyl arylate [27], chitosan/polyvinyl alcohol [38], ethylene
glycol (EG)/polyvinylpyrrolidone (PVP) [40, 62], tinosan/
dimethylol dihydroxyethylene urea/PVP [41], TiO2/Fe3O4
[48], ammonia complex [51], Tollens’ agent [52], Tollens’
agent/PVP [53], 1,2,3,4-butanetetracarboxylic acid (BTCA)/
sodium hypophosphite (SHP) [54], hexadecyltrimethoxysi-
lane [63], polypyrrole [64], carboxymethylcellulose [65],
chitosan [66], starch [67, 68], sodium alginate [69], alginate
[70], chitosan-O-methoxy polyhydroxy ethylene glycol [71],
monochlorotriazinyl-b-cyclodextrin, and b-cyclodextrin (b-
CD) [72], poly(ethylene glycol) (PEG) [73], xanthan gum
[74], poly(diallyldimethylammonium chloride) (PDADMAC)
[75], Tragacanth gum/CA/SHP [76], AgBr-TiO2/DMDMS/
TEOS [77], amino-terminated hyperbranched polymer
(HBP-NH2) [78] and sulfated b-cyclodextrin [79], mercapto-
propyltriethoxysilane [80], ciprofloxacin, and cefobid [81].
According to Tang et al. [8], Ag endows localized sur-
face plasmon resonance which leads to obtain different col-
ors with different morphologies through photo-induction
method. The mixture of nanoprisms and nanospheres tend
to synthesize green color of Ag NPs. Blue color of Ag NPs
are obtained from solution with almost all nanoprisms struc-
ture of Ag while red and yellow color are obtained with
nanodisks structure. This phenomenon could be explained
due to the anisotropic property of Ag. Different shapes pos-
sess different plasmon resonance modes. From Tang et al.
experimental result, the bands at long wavelength of silver
nanoplates (610–710 nm for nanoprism and 440–500 nm for
nanodisk) were attributed to the in-plane dipole plasmon res-
onance mode. The bands at 330–340 nm of the silver nano-
plates were ascribed to the out-of-plane quadrupole plasmon
resonance mode of silver NPs. The band centred at 401 nm
of the green silver NP solution was suggested to be assigned
to the in-plane dipole plasmon resonance mode of silver
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nanospheres [8]. However, when the particle size decreases
the electronic band structure starts showing quantum size
effects below the critical size of that material. Particle size
decreases to 1–2 nm, the discrete energy levels tend to
match to the molecular energy level. At this level, Ag will
not behave as metal and there is no more metallic band
structure available to show surface plasmon effects and it
loses its characteristic color. The existence of silica on Ag
NPs-coated fabric could enhance the color of modified fab-
ric as well as prevent the Ag NPs from agglomeration [82].
Synthesis Method. There are varieties of application
techniques have been developed on coating Ag NPs onto
textile materials. Among these included: pad-dry-cure
method [4, 5, 38, 41, 53, 54, 60, 65, 68, 70–74, 76, 79,
83, 84], dip and dry [62], ex situ immersion [8, 78], direct
sorption [7, 10, 11, 26, 39, 52, 63, 64, 85, 86], spray coat-
ing [77], thermal reduction [80], hydrothermal [67],
microwave [40, 69], g-irradiation [50, 66], sonochemical
[27, 48, 51], electroless plating [6, 21], plasma treatment
[36, 81, 87], and self-assembly [75]. Table 1 shows the
summary of Ag NPs-coated textile and its antibacterial
effects.
The ex situ synthesis of Ag grafted textile via pad-dry-
cure method has been widely used in many researches.
Figure 1 illustrates steps of coating Ag NPs onto fabric
via pad-dry-cure process. Ag NPs are first prepared either
via wet chemical [60, 65, 68, 70–74, 76, 79] or biomass
filtrate [83, 84] before padding the textile into Ag NPs
colloidal solution, drying, and finally curing. However,
due to weak interaction on fabric surface itself without
any penetration into yarn level causes it not permanent
against washing. Thus, impregnation of capping agent
either synthetic polymer [41, 53, 54, 60, 72, 73] or natu-
ral biological agent [70, 74, 76] facilitates the stability of
Ag NPs on textile.
The incorporation of Ag NPs onto textile through in
situ immersion is generally carried out in two steps
namely, preactivation and sorption. The purpose of pr-
activation is to swell the fiber matrix inside the textile to
facilitate the diffusion of Ag NPs into fibers. The alkali
based material or reducing agent used in preactivation
step is to fully dissociate COOH in cellulose and thus
increases the affinity of Ag NPs adherence on textile. The
advantages of this method are facile, cheap, and can be
carried out at mild reaction conditions [85]. The reducing
agents used in preactivation step that have been studied
are trisodium citrate [7] and sulfur-based materials [10],
potassium hydroxide [63], and sodium hydroxide [85].
The combination of preoxidation of textile before carry
out in situ synthesis Ag NPs onto fabric has been studied
as well. Montazer and Nia have reported to use potassium
permanganate to oxidize polyamide chains which lead to
increased functional groups that served as active sites for
loading more Ag NPs on fabric surface. Incorporation of
ultrasound bath shortens the processing time and energy
consumption in coating process [52]. Emam et al. have
made comparison with both solventless sorption and
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 TABLE 1. Summary of Ag NPs-coated textile and its antibacterial effects.

Innoculus Incubation time/ Antibacterial

Additive matrix Synthesis method Type of textile NP size (nm) Microorganism (CFU/mL) contact time assay Effects Refs.

TiO2/SiO2/alginate Pad-dry-cure Wool 20 E. coli 108 — Count colony The maximum bacterial reduction was [4]
forming units found on fabric with combination
of TiO2/SiO2/Ag nanocomposites
followed by Ag alone.
Silica Pad-dry-cure Wool (WO), 30–200 E. coli, S. 105 24 h Count of colony The antibacterial performance on PET [5]
polyester (PET), aureus, A. niger forming units has highest efficiency, followed by
polyester/wool PET/WO and WO.
(PET/WO)
Chitosan/PVA Pad-dry-cure Viscose, viscose/ 6–10 E. coli, S. aureus — — Disc diffusion All the treated sample revealed anti- [38]
polyester bacterial activity.
Tinosan/DMDHEU/PVP Pad-dry-cure Viscose 10 E. coli, S. aureus — — Disc diffusion Inhibition zone of S. aureus is larger [41]
than E. coli
Tollen’s agent/PVP Pad-dry-cure Polyamide 91.4 E. coli, S. aureus 2 3 103 for S. aureus. 24 h Count of colony 99% of both bacterial reduction. [53]
2 3 1023 for E. coli. forming units
BTCA/SHP Pad-dry-cure Nylon 34 E. coli, S. aureus 2 3 103 for S. aureus. 24 h Count of colony A bacterium growth decrease above [54]
2 3 1023 for E. coli forming units 96% achieved with 200 ppm nano-
silver/BTCA/SHP
— Pad-dry-cure Polyester 2–3 E. coli, S. aureus, 105, 106, 107, 108 5, 15, 30 min Count of colony 99% reduction of all bacteria. [60]
and cotton K. pneumoniae forming units
Carboxymethylcellulose Pad-dry-cure Cotton — S. aureus, K. 1–2 3 105 24 h Count colony 99.9% reduction for both S. aureus [65]
pneumoniae forming units and K. pneumoniae
Starch Pad-dry-cure Cotton 2–30 E. coli, S. aureus 108 24–48 h Disc diffusion and All the treated sample revealed splen- [68]
count colony did antibacterial activity.
forming units
Alginate Pad-dry-cure Cotton 1–4 E. coli, S. aureus, 108 24–48 h Disc diffusion and Inhibition zone of S. aureus is larger [70]
P. aeruginosa count colony compared to others and exhibit
forming units 95% reduction of S. aureus number
under presence of binder
CTS-O-MPEG Pad-dry-cure Cotton 18 6 2 E. coli, S. aureus — 24 h Disc diffusion Inhibition zone of E. coli is larger [71]
than S. aureus.
b-cyclodextrin Pad-dry-cure Cotton — E. coli, S. aureus — — Disc diffusion Inhibition zone of S. aureus is larger [72]
than E. coli.
PEG Pad-dry-cure Cotton 12–16 E. coli, S. aureus — — Disc diffusion Inhibition zone of E. coli is larger [73]
than S. aureus.
Xanthan gum Pad-dry-cure Cotton 9.1 6 4.8 S. aureus 1.5 3 108 24 h Count of colony Exhibit 98.0 6 1.0% reduction of S. [74]
forming units aureus number.
Tragacanth gum/CA/SHP Pad-dry-cure Cotton 77.55 E. coli, S. aureus — 18 h Count of colony 98.01% and 99.69% reduction of E. [76]
forming units coli and S. aureus numbers,
respectively.
Sulfated b-cyclodextrin Pad-dry-cure Cotton 20–500 E. coli, S. aureus 12 3 105 for S. aureus; — Count colony The bacterial reduction for S. aureus [79]
6 3 105 for E. coli forming units and E. coli were found maximum
at 30 min with 92% and 99%,
respectively.
— Pad-dry-cure Cotton 8–15 E. coli, S. aureus 1.6 3 103 24 h Count of colony 97% and 91% reduction of S. aureus [83]
forming units and E. coli, respectively.
— Pad-dry-cure Cotton 8–20 — 24 h Disc diffusion [84]
TABLE 1. Continued
Innoculus Incubation time/ Antibacterial
Additive matrix Synthesis method Type of textile NP size (nm) Microorganism (CFU/mL) contact time assay Effects Refs.

B. subtilis, S. aureus, The maximum inhibition zone was

E. coli, P. aeruginosa, found on B. subtilis strain followed
K. pneumoniae, MRSA by S. aureus, P. aeruginosa, K.
pneumoniae, E. coli, and MRSA.
EG/PVP Dip and dry Cotton 46.4 6 4.5 E. coli, S. aureus 1 3 1023 24 h Colony forming 100% reduction of E. coli and S. [62]
units aureus growth.
Silica Ex situ immersion Wool 34.6 6 2.8 E. coli 108 18 h Count colony The reduction of CFU was 66% and [8]
forming units 71% for wool/Ag and wool/SiO2/
Ag.
HBP-NH2 Ex situ immersion Cotton 10.8 E. coli, S. aureus 3–4 3105 24–48 h Shake flask and 99.43% and 99.45% bacterial reduc- [78]
count colony tion for S. aureus and E. coli,
forming units respectively were obtained.
Trisodium citrate Direct sorption Cotton 20–90 for E. coli 1.5 3 108 24 h Count colony Both type of treated fabrics exhibit [7]
and wool cotton. forming units antibacterial reduction with 95%.
70–150
for wool
Sodium bisulfite and Direct sorption Wool 34–58 E. coli, S. aureus — — Count colony Both type of treated fabrics exhibit [10]
sodium dithionite forming units antibacterial reduction.
Lecithin Direct sorption Wool — E. coli, S. aureus 107 0, 0.5, 1, 2, Disc diffusion and Significant inhibition zone and with [11]
4, 6 min count colony 95% bacterial reduction were
forming units observed for both bacterial strains.
Glucose Direct sorption Denim 45 and 55 in E. coli, S. aureus — — Colony forming Presence of glucose reduces the anti- [26]
presence units bacterial ability.
and absence
of glucose
— Direct sorption Viscose 0–50 E. coli 1.5 3 108 24 h Colony forming 98% of bacterial reduction was [39]
units observed after 24 contact time.
Tollen’s agent Direct immersion Nylon 78 S. aureus — 24 h Disc diffusion The treated fabric exhibited significant [52]
bacterial reduction.
Hexadecyltrimetho Direct sorption Cotton 53 E. coli, S. aureus — 18–24 h Disc diffusion Significant inhibition zone was [63]
xysilane observed for both bacterial strains
5
Polypyrrole Direct sorption Cotton 20 E. coli, S. aureus 10 24 h Disc diffusion and Diameter of zone inhibition obtained [64]
count colony for the higher concentration of
forming units composites is about 11.2 and
9.8 mm against E. coli and S.
aureus, respectively.
— Direct sorption Cotton <80 E. coli, S. aureus 108 24–48 h Disc diffusion The coated fabric showed significant [85]
antibacterial activity.
— Direct sorption Cotton 14.9 E. coli, S. aureus 106–107 24 h Disc diffusion The treated fabric exhibit significant [86]
and padding antibacterial performance.
AgBr-TiO2/DMDMS/ Spray coating Cotton 400–600 E. coli 106 18 h Count colony The treated fabric showed higher bac- [77]
TEOS forming units terial reduction under presence of
light with 99.87% compared with
81.43% under dark condition.
Mercaptopropyltrietho Thermal reduction Cotton 20–100 E. coli, S. aureus 6 3 108 24 h Count colony The bacterial reduction increased [80]
xysilane forming units when concentration of silver carba-
mate precursor increased
TABLE 1. Continued
Innoculus Incubation time/ Antibacterial
Additive matrix Synthesis method Type of textile NP size (nm) Microorganism (CFU/mL) contact time assay Effects Refs.

Starch Hydrothermal Cotton 20 E. coli, S. aureus — — Disc diffusion The treated fabric exhibit significant [67]
antibacterial performance.
PVP Microwave Viscose 10–35 E. coli — — Count colony The treated fabric exhibit significant [40]
forming units antibacterial performance.
Sodium alginate Microwave Cotton 30–60 E. coli, S. aureus, 1.5 3 108 24 h Disc diffusion and The MIC values against S. aureus [69]
P. aeruginosa minimum inhibi- were lower compared to those
tory concentra- against P. aeruginosa and E. coli.
tion (MIC)
— g-Irradiation Peco 11 S. aureus, K. — 48 h Count colony 99% reduction for both S. aureus [50]
pneumoniae forming units (Sa) and K. pneumoniae
Chitosan g-Irradiation Cotton 12 E. coli, S. aureus 1–2 3 107 48 h Count colony 99% reduction for both S. aureus [66]
forming units and E. coli.
Butyl acrylate Sonochemical Cotton 25–30 E. coli, S. aureus 108 24 h Disc diffusion and 99% reduction for both S. aureus [27]
count colony and E. coli.
forming units
TiO2/Fe3O4 Sonochemical Polyester 40 E. coli, S. aureus — 24 h Count colony 100% bacterial reduction was [48]
forming units observed.
Ammonia complex Sonochemical Polyamide 20–150 E. coli, S. aureus 1.5–2 3 103 24 h Count colony The treated fabric exhibited significant [51]
forming units bacterial reduction.
TCEP Electroless plating Wool — E. coli, A. niger — — Count colony The treated fabric exhibited significant [6]
forming units bacterial reduction.
TCEP Electroless plating Silk — E. coli, S. aureus — 24 h — The antibacterial efficacy was 99.98% [21]
against E. coli and 99.83% against
S. aureus, respectively.
— Plasma treatment Viscose — E. coli, S. aureus, — 24 h Disc diffusion The treated fabric exhibited significant [36]
C. albians bacterial reduction.
Ciprofloxacin Plasma treatment Cotton, linen, 10–17 E. coli, S. aureus — — Disc diffusion The improvement of antibacterial per- [81]
and Cefobid viscose and formance decreasing order as lyo-
lyocell cell > viscose > cotton > linen.
— Plasma treatment Polyester — E. coli, S. aureus 106 24 h Count colony The antibacterial activity is more [87]
forming units effective on E. coli than S. aureus.
PDADMAC Self-assembly Nylon and silk 100 S. aureus — 24 h Count colony Resulted in 80% bacteria reduction for [75]
forming units the silk and 50% for the nylon.
 FIG. 1. Steps of coating Ag NPs onto fabric via pad-dry-cure method [60]. [Color figure can be viewed at wileyonlinelibrary.com]
padding methods on deposition of Ag NPs on cotton fab-
ric. Based on the result, sorption method has higher effi-
ciency on loading Ag NPs on textile compared to padding
method by 10 times. This could be due to the reduction
reaction preceded in the solution offering high concentra-
tion of Ag1 ion to Ag compared to that performed in
oven in case of using padding technique [86].
Thermal reduction of silver carbamate complex in organic
solvent has been studied to synthesize Ag NPs. The advan-
tage of this method is able to produce stable Ag NPs without
creating inorganic ions except amine and carbon dioxide by
reducing silver carbamate at low temperature. In Kwak
et al.’s study, Ag NPs have assembled on cotton fabric by
using 3-mercaptopropyltriethoxysilane and transparent alco-
holic solution of organometallic silver 2-ethylhexylcarbamate
under thermal heating at low temperature 1308. Figure 2
illustrates the 3-mercaptopropyltriethoxysilane reacts with
hydroxyl groups of cotton to create a ASH groups mono-
layer followed by decomposition silver carbamate complex
to silver metal through thermolysis. The synthesized Ag NPs
conveyed a homogeneous and continuous layer of silver
metal on fabric with average size of 20 to 100 nm exhibited
FIG. 2. Preparation of Ag NPs coated by thermolysis using silver carbamate complex [80]. [Color figure can be viewed at wileyonlinelibrary.com]
DOI 10.1002/vnl
high conductivity, electric resistance, and antibacterial perfor-
mance against E. coli and S. aureus [80]. Hydrothermal tech-
nique is also extensively used in synthesis nanostructure of
Ag on textile application. Raza et al. have studied the
impregnation of Ag NPs on enzymatic starch pretreated cot-
ton fabric under autoclave conditions of 103.42 kPa, 1218C
for 15 min. Figure 3 shows the impregnation mechanism of
Ag Ns on cotton fabric under pressurized heating treatment.
At this condition, the aldehyde terminal of starch able to
reduce silver ions which bound to the anionic oxygen site of
cotton fabric to silver atom and stabilized the NPs on fabric
surface. The obtained surface of treated cotton fabric
revealed multifunctions of antibacterial activity, hydrophobic-
ity, tensile strength, and is rougher than pristine cotton fabric
[67]. The microwave heating synthesis is advantageous over
conventional heating due to its rapid nucleation sites genera-
tion and thus enhances the reaction rates. Energy is supplied
by an electromagnetic field directly to the material results
fast heating. Su et al. have synthesized sodium alginate-
grafted Ag NPs on cotton fabric through microwave
irradiation under various conditions by manipulated sodium
alginate concentration (0.5%–2%), volume of reducing agent
JOURNAL OF VINYL & ADDITIVE TECHNOLOGY—2019 E11
 FIG. 3. Impregnation of Ag NPs on cotton fabric by hydrothermal [67]. [Color figure can be viewed at wileyonlinelibrary.com]
aniline (50,100, 150 lL) and duration of heat treatment (30–
240 s) in order to investigate the effects on antibacterial per-
formance [69]. Moreover, Rehan et al. used combination of
microwave heating and polyol method to synthesize Ag NPs
on viscose fabric with incorporation of PEG as reducing
agent and PVP as stabilizing agent. The microwave power
has increased from 50 to 90 W increased the kinetics of
reaction and generation of localized heat at reaction sites,
thereby increased the reaction rate. Hence, the reduction rate
of silver ions accelerated thus enhanced the antibacterial per-
formance [40].
In addition, the usage of g-irradiation to produce
hydrated electrons and radicals of hydrogen to transform
the silver ions into silvers and immobilize it on the fabric
has been studied also [50]. The effects of absorbed dose
and concentration of AgNO3 solution on impregnation of
Ag NPs on fabric with chitosan as additive has been
investigated by Hanh et al. [50, 66]. The absorbed dose
plays an important role in formation and growth of Ag
NPs. Based on the results, NPs did not form in low dose
but appeared at high dose. Whereas, increased concentra-
tion of AgNO3 from 0.5 to 5 mM enhanced the Ag con-
tent on cotton fabric and thus improved the inhibition of
bacterial growth.
Sonosynthesis has been proven as effective approach to
synthesize NPs at mild operation condition due to its unique
capability of generation energy by acoustic cavitation mean.
Harifi and Montazer have used sonosynthetic method to
deposit TiO2/Fe3O4/Ag nanocomposites on polyester fabric
to impart magnetic, enhanced antibacterial, and self-cleaning
features with considerable hydrophilicity/hydrophobicity at
mild temperature. The formation, growth, and implosive col-
lapse of bubbles, microturbulence, shock waves, and pres-
ence of localized hot zones induced smaller size NPs and
intensified mass transfer onto the textile lead to strong phys-
ical adsorption [48]. Montazer et al. have applied ultrasound
to synthesize silver complex [Ag(NH3)2]1 before cross-
linked with polyamide chain found that the synthesized Ag
NPs homogenous deposited on polyamide fabric surface
with the particle sizes range of 20 to 150 nm, exhibited anti-
bacterial properties against E. coli and S. aureus [51]. Ibra-
him and Hassan have synthesized Ag NPs-coated cotton
fabric using fungus Alternaria alternate to synthesize Ag
NPs, after that applied ultrasound to ensure homogeneous
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dispersion before treated fabric subjected to g-irradiation
and thermal curing [27].
Chemical electroless plating is another method
employed for coating Ag NPs onto textile surface. Yu
et al. have metalized silk and WO fabrics by using tris(2-
carboxyethyl) phosphine as reducer to create thiol groups
and ASH groups on corresponding fabrics for serving cat-
alytic seeds to form complexes ions between fabrics and
silver ions [6, 21]. The whole coating process is illus-
trated in Fig. 4. The chemical interaction of catalytic
seeds with silk fibers can lead to better bonding and
adhesion between fiber and metal layer. However, this
method has limitations associated with the use of expen-
sive materials and difficulty to create reactive groups on
the fiber’s surface.
Plasma treatment coating involves interaction of high
energy with quasineutral gas such as electrons, ions, and
excited molecules atoms under the presence of electric or
both electric and magnetic fields. These particles can be
used to alter the textile surface chemically and physically.
Generally, there are two common plasma techniques that
are used to modify the textile namely, atmospheric pres-
sure plasma and dielectric-barrier discharge (DBD). For
atmospheric pressure plasma technique, its discharge
employs high flow rate of inert carrier gas [88]. Deng
et al. have impregnated Ag NPs on PET fabric through
double layer of plasma deposited organosilicon thin film
which served as a reservation layer for silver immobilization
and controlled the adherence of silver on fabric. The silver
concentration in double layer coatings has successfully
reduced the growth of E. coli and S. aureus at 100% reduc-
tion at Ag NPs content at 7% [87]. Ibrahim et al. have pre-
surface modified different types of fabric namely, cotton,
linen, viscose, and lyocell to create active sites (ANH2
groups) for loading Ag NPs onto fabric surface by using N2
plasma with the DBD as plasma source. The evaluation of
antibacterial performance of modified fabric arranged in
decreasing order: lyocell > viscose > cotton > linen [81]. On
the other hand, the coating principle of DBD is through
bombardment of fabric surface with high speed electrons by
applying a pulsed voltage over an electrode pair of which at
least one is covered by a dielectric material. The dielectric
limits the flow of current and distributes over the whole fab-
ric, improves the uniformity during the treatment [88].
DOI 10.1002/vnl
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 FIG. 4. The process of silver fiber electroless plating [21]. [Color figure can be viewed at wileyonlinelibrary.com]
Kramar et al. have studied the aging effect of using DBD
with different exposure times (1, 7, 14, 21 days) on wetta-
bility and sorption ability of bactericidal ions, Ag1 and
Cu21 ions on viscose fabric. Obtained results showed that
both types of ion possessed different sorption capabilities
and antibacterial performances at different postplasma treat-
ment durations [36].
Polyelectrolyte multilayers (PEM) formed by layer-by-
layer self-assembly on coating NPs onto textile applica-
tion has gained interest due to its simplicity for develop-
ment of nanoscale structure with high stability. This
process is carried out by successive dipping alternative
polycations and polyanions followed by rinsing in water.
The coating replies on the electrostatic and hydrophobic
interactions and results in a film which thickness and
properties can be finely tuned. Dubas et al. [75] have
implemented Ag NPs-coated nylon and silk fabrics by
using layer-by-layer deposition approach on investigation
their antibacterial activity. The use of anionic poly(metha-
crylic acid) capped Ag NPs on silk and nylon fibers with
cationic PDADMAC formed 20 layers between them
have obtained. Based on the results, the affinity for PEM
on the nylon was lower compared with silk fabric due to
their different fiber structures. The silk endows carboxylic
functional groups inside the natural protein fiber, facili-
tates the adhesion of PDADMAC and the growth of film
layers. Whereas, nylon has lower surface charge which
nonconducive for deposition of PEM, thus leading to
slower and lesser amount of immobilized NPs. Hence, the
deposition of 20 PDADMAC/PMA-coated Ag layers onto
the fibers resulted in 80% bacteria reduction for the silk
fiber and 50% for the nylon [75].
Zinc Oxide NPs (ZnO NPs)
ZnO is II-VI semiconductor group and owns three
forms namely, hexagonal wurtzite, cubic zincblende, and
rarely observed cubic rocksalt. As compared with zinc-
blende form, wurtzite structure is more thermodynami-
cally stable in room temperature. The metastable
zincblende can be stabilized through growth techniques
[47]. Due to its unique lattice structure, it exhibits piezo-
electric property and has widely used in piezoelectric
devices, sensors, and elctroacoustic transducers. ZnO is a
n-type semiconductor, endows relatively wide direct band
gap (3.3 eV) with high excitonic binding energy (60
meV) at ambient environment and results it potentially
applied on electronic field such as solar cells, gas sensors,
varistor, photodiodes, and UV-light emitting devices.
DOI 10.1002/vnl
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Furthermore, ZnO possesses high optical absorption and
catalytic activities which favor its use in UV absorbers,
antireflection coatings, photocatalysis, and catalyst. ZnO
also can be utilized in ointments, lotions, and sunscreens
to protect skin from UV illumination due to it serves as
the broadest spectrum UVA (315–400 nm) and UVB
(280–315 nm) reflector [47, 89]. Recently, there are
numerous studies investigating the use of ZnO NPs as anti-
bacterial agent on diverse fields such as food [90], textile
[79, 91–106], and biomedical applications [107]. Devanand
Venkatasubbu et al. have applied ZnO on food pathogens
namely, Salmonella typhi, Klebsiella pneumoniae, and Shi-
gella flexneri for investigating its antibacterial performance
[90]. Liedtke and Vahjen have shown the antibacterial effect
of ZnO NPs against 75 intestinal bacteria. According to the
literature, ZnO NP is an amphoteric molecule and has dis-
played higher solubility in acidic environment. The results
showed that the intestinal bacteria’s resistance against ZnO
NPs is species specific and cannot be assigned based on
their taxonomic origin [108]. Premanathan et al. have stud-
ied the toxicity of ZnO NPs against the inhibition growth of
prokaryotic and eukaryotic cells. The authors have used
human myeloblastic leukemia cells (HL60) and normal
peripheral blood mononuclear cells (PBMCs) to evaluate the
cytotoxicity of ZnO NPs and at the same time, antibacterial
activity of ZnO NPs against Gram-negative bacteria E. coli
and P. aeruginosa, as well as the Gram-positive bacteria S.
aureus have been tested. The results showed that ZnO pos-
sessed abilities to kill cancerous HL60 cells and those
Gram-negative and positive bacteria through two mecha-
nisms namely, generation of ROS and induction of apoptosis
[109]. However, up-to-date, the cytotoxicity of ZnO on
mammalian cells is scarce and need more significant and
clear published literature before translating into medical use.
The synthesis of ZnO NPs-coated materials is usually done
by addition of additive or supporting matrix to stabilize and
increase durability of ZnO. ZnO is susceptible to agglomer-
ate in water due to high polarity of water leading to deposi-
tion [108]. Thus, ZnO has been incorporated with many
capping agents on synthesis of ZnO nanocomposite coated
on textile such as multiamide compound [34], sulfated b-
cyclodextrin [79], hexamethyltriethyylene tetramine [91],
chitosan [92, 95], acacia [93], PVP [94], silica [97], Traga-
canth gum [98], cellulose [28], polymer diallyl dimethyl
ammonium chloride-allyl glycidyl ether-methacrylic [102],
polystyrene-block-poly(acrylic acid) [101], hydrogel [104],
and sodium alginate [110].
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FIG. 5. Different possible mechanisms of ZnO NPs antibacterial activity, including ROS formation, Zn21 release, internalization of ZnO-NPs into
bacteria, and electrostatic interaction [47]. [Color figure can be viewed at wileyonlinelibrary.com]
There are several proposed ZnO antibacterial mecha-
nisms namely, direct physical contact with cell walls and
destruction of cell membrane’s integrity, dissolution of
ZnO NPs, and ROS formation. Figure 5 illustrates the dif-
ferent possible mechanisms of ZnO NPs antibacterial
activity. The ROS such as superoxide anion (O2–), hydro-
gen peroxide (H2O2), and hydroxide (OH–) involve the
destruction of cellular components such as lipids, DNA,
and proteins, thus trigger cell death. The released Zn21
induces active transport inhibition and amino acid metab-
olism as well as enzyme system disruption. Those are the
effects responsible for the inhibition of growth of bacte-
rial cell. The mechanisms are dependent on the presence
of UV illumination and morphology of ZnO [47]. Based
on the Joe et al.’s report, the toxicity mechanisms of ZnO
against S. aureus and K. pneumoniae under absence of
light condition has revealed that the inhibition of bacteria
is due to the physical attachment of ZnO on cell wall and
increasing release of Zn21 ions in bacterial cytoplasm
[111]. However, Ma et al. [112] presented their studies
on comparison of phototoxicity and antibacterial perfor-
mance of ZnO under natural sunlight (NSL) and ambient
artificial laboratory light (AALL) illumination with differ-
ent ZnO particle sizes. As regarding the phototoxicity,
both nano-ZnO and bulk ZnO under NSL has higher
methylene blue degradation which occurred as fast as 2 h
than those samples under AALL exposure which was
observed only after 24 h. The extent of toxicity under 2 h
NSL was higher than under 24 h exposure of AALL.
Both conditions seemed to be mediated with different
antibacterial mechanisms against Caenorhabditis elegans
growth as no significant methylene blue degradation
under AALL indicated bare or none generation of ROS
such as O2– and OH–. It should be noted that no photo-
toxicity of ZnO under AALL but NSL. The spectrum of
sunlight used in the study is assumed to be treated as
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typical radiation spectrum though it is varied by geo-
graphical conditions, atmospheric variability, weather
conditions, and so on. However, it is estimated around
8%–9% of solar energy falls in the UV electromagnetic
region which is sufficient to activate ZnO to generate
ROS and can eventually causes lipid peroxidation and
leads to cell death. Whereas, the source of AALL is typi-
cal “white cool” fluorescent lamp which possesses negli-
gible amount of UV (less than 400 nm) illumination that
cause deficient to excite the ZnO to create hydroxyl radi-
als and superoxide ions. It is found that the UV exposure
under fluorescent lamps for 8 h is corresponding to 1 min
of sunlight exposure. Moreover, based on the data
obtained, the dissolution of ZnO is estimated to be
5.6 mg/L as Zn is seemed not to be the cause for mortal-
ity of bacteria. Thus, the possible mechanism for increas-
ing lipid peroxidation and mortality of C. elegans under
AALL for 24 h exposure could be due to the oxidative
stress occurred within the bacterial cell. The precise
mechanisms of ZnO antibacterial activity in the absence
of light are highly debate and need further understand.
On the other hand, the particle size plays a major role in
influencing the degree of toxicity for ZnO. The results
showed the nanosized ZnO (60 6 25 mm) has greater meth-
ylene blue degradation percentage compared with bulk ZnO
(550 6 256 nm) [112]. This is good agreement with Cepin 
et al. studies that have found the antibacterial activity of E.
coli is clearly particle-size dependent [113].
Synthesis Method. There are several ZnO NPs coating
techniques studied such as pad-dry-cure [79, 91, 94, 97,
101], spraying and dipping [103] hydrothermal [34, 92,
93], sonochemical [28, 98, 100, 110], plasma treatment
[95], and pulse laser ablation [96]. Table 2 shows the
summary of ZnO NPs-coated textile and its antibacterial
effects. Shaheen et al. have developed amine-based
DOI 10.1002/vnl
DOI 10.1002/vnl
 TABLE 2. Summary of ZnO NPs-coated textile and its antibacterial effects.

Incubation time/
Additive matrix Synthesis method Type of textile NP size (nm) Microorganism Innoculus (CFU/mL) contact time Antibacterial assay Effects Refs.

Sulfated b-cyclodextrin Pad-dry-cure Cotton 40–200 E. coli, S. aureus 12 3 105 for S. aureus; 10, 15, 20, Count colony Both bacterial reduction for S. aureus [79]
6 3 105 for E. coli 30 min forming units and E. coli were found maximum at
30 min with 100%.
HMTETA Pad-dry-cure Cotton 198.5–2,520 E. coli, S. aureus — 24 h Count colony The reduction of S. aureus is higher [91]
forming units than E. coli at all concentration of
ZnO NPs.
PVP Pad-dry-cure Cotton — E. coli, S. aureus — 30, 60, 90 min Count colony The PVP/ZnO NPs-coated fabric [94]
forming units exhibited better antibacterial activity
than PVP modified fabric.
Silica Pad-dry-cure Cotton — E. coli, S. aureus. — — Disc diffusion The inhibition zone for S. aureus is [97]
larger than E. coli.
Polystyrene-block-poly Pad-dry-cure Cotton 21–31 E. coli, S. aureus — 12 h Disc diffusion The coated textile samples exhibited [101]
(acrylic acid) antibacterial activity against both
copolymer bacteria.
(PS-b-PAA)
— Spraying and Cotton 100–500 S. aureus, K. — 24 h Count colony The treated fabric exhibited >98% [103]
dipping pneumoniae forming units bacterial reduction against both
bacteria.
Multiamide Hydrothermal Bamboo pulp — — — — — — [34]
compound (HSDA)
Chitosan Hydrothermal Cotton 20.5–23 E. coli, S. aureus, — 48 h Disc diffusion The treated fabric exhibited bacterial [92]
Streptococcus pyogenes, reduction against all bacteria.
Klebsiella aeroenes.
Chalcone Hydrothermal Cotton 80–150 in width E. coli, S. aureus, 1 3 107 24 h Count colony The reductions were 99.58%, 99.99%, [93]
and 500 in length P. aeruginosa forming units and 99.89% for S. aureus, E. coli,
and P. aeroginosa, respectively.
Tragacanth gum Sonochemical Cotton 55–70 E. coli, S. aureus, 1 6 0.3 3 105 for count 18 h Disc diffusion and The treated cotton fabric using colony [98]
C. albicans colony forming unit; count colony count method indicated 100% reduc-
1.5 3 108 for disc forming units tion for all bacteria.
diffusion
Cellulase Sonochemical Cotton 30–160 E. coli, S. aureus. 0.5 3 105 24 h Count colony The bacterial reduction of S. aureus [28]
forming units and E. coli, respectively, with 67%
and 100%.
— Sonochemical Cotton 30 E. coli 106 1h Count colony >97% of bacterial reduction for less [100]
forming units than an hour.
Sodium alginate Sonochemical Cotton 25 6 5 E. coli — 48 h Disc diffusion The antibacterial efficacy of E. coli [110]
inhibition zone for all the fibers was
found to be in between 2.1 and
3.6 mm.
— Plasma Cotton 30–200 S. aureus, K. — 18 h Count colony The treated fabric exhibited significant [95]
treatment pneumoniae forming units antibacterial properties.
Carboxymethyl Pulse laser Cotton 10–150 E. coli, S. aureus, 3.0 3 105 for 24 h Count colony The treated fabric exhibited significant [96]
chitosan ablation B. subtilis count colony forming forming units antibacterial properties.
units. 105 for disc
diffusion
material with hexamethyltriethylene tetramine as precur-
sor which provided alkaline condition for formation of
ZnO NPs on cotton fabric through pad-dry-cure method,
found imparted antibacterial characteristics and UV pro-
tection [91]. Selvam and Sundrarajan have functionalized
poly-N-vinyl-2-pyrrolidone on cotton fiber surface exhib-
ited improved reactive dying and antibacterial activity via
pad-dry-cure approach [94]. Barani [97] has applied Zn
NPs on cotton fabric by embedding them into silica
matrix via two different ways of procedure and compared
its effects on morphological, structural, thermal, and anti-
bacterial properties. First method, the fabric was
immersed into the sol solution, dried, and cured the
treated fabric before immersed into zinc nitrate solution,
finally treated with sodium hydroxide solution and dried
it. The second method was adding the zinc nitrate into
solution before immersed fabric into solution, after that
dried and cured the treated fabric. The treated fabric was
then mixed with sodium hydroxide and dried it. The
results showed that the agglomeration of NPs occurred on
first method compared to that second method which pro-
duced spherical NPs. Thus, the antibacterial properties
against S. aureus and E. coli showed higher for fabric
treated by second method compared with first method
due to its higher surface area exposure [97]. Cakır et al.
have used reverse micelle cores of PS-b-PAA to synthe-
size ZnO NPs by atom transfer radical polymerization
and dip-coated on cotton fabric for giving long-term self-
cleaning, UV-protective, and antibacterial properties
[101]. Besides that, Prasad et al. have made comparison
in effectiveness of adhesion of ZnO on cotton fabric
between spraying and dipping approaches. As a result, the
spraying process resulted three times more deposition of
ZnO NPs than spraying process while exhibited consider-
ably similar antibacterial reduction [103].
In situ synthesis of ZnO NPs on bamboo pulp fabric
with incorporation of multiamide compound which served
as a template to entrap ZnO NPs through hydrothermal
impregnation method for rendering UV protective and
antibacterial properties have been presented by Zhang
et al. [34]. Sivakumar et al. have synthesized ZnO
flower-like nanorods coated on cotton fabric with the
additives chaconne and acacia as antibacterial agent and
binder, respectively through hydrothermal synthesis fol-
lowed by direct immersion approach [93]. Dhandapani
et al. have synthesized ZnO NPs grafted cotton fabric
using ureolytic bacteria, Serratia ureilytica to produce
biogenic ammonia as the base materials for ZnO NPs
synthesis on cotton fabric at temperature 50 C for differ-
ent durations (30, 60, 90 min). The results showed that
the ZnO morphologies changed upon varied heat treat-
ment duration times. From treatment time 30 to 60 min,
the spherical ZnO with particle sizes changed from 170–
250 nm to 300–600 nm with evident agglomeration was
observed. Further heat treatment of fabric to 90 min
resulted in progressive growth of ZnO NPs with grain
sizes of 185–360 nm nanoflower-shaped NPs. The cotton
fabric with treatment for 90 min exhibited greater
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antibacterial activity against E. coli and S. aureus com-
pared to that 30 and 60 min. The reason behind the
increased antibacterial activity with prolonged treatment
may be due to greater crystal growth of ZnO NPs [106].
Combination of enzymatic preactivation of cotton fiber
and sonochemical coating of ZnO NPs on fabric has been
investigated by Petkova et al. The ultrasound is employed
to boost the rate of enzymatic hydrolysis and create the
cotton surface more reducing sugars which act as an
anchoring points with ZnO NPs to increase the durability
of antibacterial effect. The controlled ultrasound ampli-
tude accelerates the mass transfer from the processing
solution towards cotton fiber without damaging the fiber,
thus results in better uniformity of enzymatic treatment
over a shorter period of time [28]. Application of natural
polymer as stabilizing agent on synthesis ZnO nanocom-
posite onto the cotton fabric through sonochemical
approach has been studied. Ghayempour and Montazer
used Tragacanth gum, a natural polysaccharide as reduc-
ing, stabilizing and binding agent for in situ synthesis of
ZnO NPs on cotton fabric via ultrasound irradiation. Fig-
ure 6 proposed the mechanism of in situ synthesis of ZnO
NPs on the fabric itself. Sodium hydroxide reduces the
hydroxyl groups and carboxylic groups of Tragacanth
gum to AO– and ACOO– and ionizes cellulose to cellulo-
sate with negative charge. The Zn ions from zinc nitrate
solution bond with hydroxyl groups and carboxyl groups
from Tragacanth gum and cotton before sonicate to form
ZnO NPs. The analysis showed that the star-like ZnO
NPs with average particle size of 62 nm with antibacterial
properties against S. aureus, E. coli, and C. albicans were
observed [98]. Varaprasad et al. has successfully fabri-
cated sodium alginate-ZnO NPs grafted cotton fabric by
sonochemical mean. The synthesized ZnO NPs revealed a
rod-like shape alignment with average grain size of 25 6
5 nm with good inhibition microbial growth of E. coli
[110]. Perelshtein et al. have conducted scale-up sono-
chemical coating of medical textile with ZnO NPs as anti-
bacterial agent. The clinical comparisons have made with
two different conditions where 21 patients used ZnO
NPs-coated medical textile while another 16 patients used
normal medical textile. The results demonstrated that the
patients using modified textiles were less contaminated
with nosomonial pathagens and the textiles did not show
toxicity compared to that uncoated NPs textile [100].
Plasma pretreatment for coating ZnO NPs on textile to
impart antibacterial property has been investigated by
Wang et al. The cotton was pretreated by cold oxygen
plasma and the ZnO/chitosan nanocomposite was coated
on treated cotton via facile pad-dry-cure method. There
was a significant enhancement of UV resistance and anti-
bacterial activity of the modified cotton fabric [95]. Svet-
lichnyi et al. have proposed to apply pulsed laser ablation
for synthesis ZnO NPs in the stable dispersion form under
two different types of system namely, water and ethanol.
In the case of water system, there were mixture of crys-
talline forms with different grain sizes and tend to
agglomerate. They appeared in spherical, hexagons and
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FIG. 6. The suggested mechanism of in situ synthesis of ZnO nanoparticles on the cotton fabric [98]. [Color figure can be viewed at wileyonlineli-
brary.com]
rod-like shaped in corresponding particle sizes of 150 nm,
50 to 80 nm, and 10 to 30 nm in width and up to 70 nm
in length, respectively. Whereas, the ZnO NPs synthe-
sized from ethanol system is mostly consisted of flat
square plates from 10 to 60 nm. Thus, the composites
obtained from ethanol dispersions revealed larger inhibi-
tion zones than those obtained from water dispersion sys-
tem [96].
Copper (Cu)-Based NPs
Copper is an excellent electrical and thermal conduc-
tivity due to its electronic structure, thus it is widely used
in electrical equipment. It is found that copper and its
derivatives such as copper oxide have antibacterial fea-
tures and are applied on diverse fields. Basically, there
are two forms of copper oxide that found to have
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antibacterial property namely; copper oxide (CuO) and
copper (II) oxide or cupric oxide (Cu2O). They are cate-
gorized as semiconducting material with monoclinic in
structure [59]. However, CuO appears to be more attrac-
tive compared to Cu2O due to its simplicity and stability.
The valence state of CuO (12) is more stable than
valence state of Cu2O (11) making CuO able to with-
stand high temperature above 1,020 C [114]. Owing to its
excellent superconductivity and serves as a critical p-type
semiconductor, CuO has been favorably applied on
diverse fields such as catalysis, gas sensors, batteries,
solar energy conversion, field emission emitters, and high
temperature conductors. Moreover, CuO endows narrow
band gap making it having photovoltaic and photoconduc-
tive functionalities [59]. Recent studies have proven CuO
in nanosized possesses antibacterial activity either in sus-
pended or incorporated into matrices [32, 36, 59, 114]. In
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order to sustain its antibacterial performance efficiency
and durability, it is more preferable to be coated with
supporting polymer matrix. This could be explained by
two main principles: (1) polymer facilitates the release of
ions in a long term by capping NPs on the material; (2)
polymer enhances the exposure of NPs to the outside
environment by increased the surface area, thus creates
high probability of reaching and inhibiting the surround-
ing bacteria [115]. Currently, there are different polymers
have been studied as matrix for immobilization of CuO
NPs for antibacterial hostility resistance namely: bamboo-
rayon [32], nylon [55], agar [116], bovine-serum albumin
[117], carboxymethyl cellulose hydrogel [118], cellulose
[119], chitosan [120], cotton [121], epoxy resin [122],
high-density polyethylene [123], hydrogel based on acryl-
amide and acrylic acid [124]. According to Ananth et al.,
the antimicrobial performance is dependent on numerous
factors such as surface area and morphology of structure.
Selection of suitable synthesis methods and conditions
could directly result differences in size and shape and
thus, influence the antibacterial performance. As men-
tioned above, the literature has reported the synthesis of
CuO using wet chemical and hydrothermal methods with
copper(II) nitrate trihydrate as source of copper and PEG
as surfactant with different conditions. In wet chemical
approach, the temperature of the solution was varied at
75 C and 100 C and the samples were denoted as CuO
75 and CuO 100. Whereas, in hydrothermal method, the
sample was synthesized at 1508C and denoted as HYD
150. The effect of incorporation of PEG on particle struc-
ture was determined via FESEM and its impact on inhibi-
tion growth of four bacterial strains namely E. coli,
Streptococcus iniae, Streptococcus parauberis, and Vibrio
anguillarum through disc diffusion method have been car-
ried out. All the CuO samples without PEG tend to be
aggregated compared with the samples with PEG as adhe-
sion agent appeared in fine dispersion. This could be
explained by the fact that PEG facilitates the reduction of
Gibb’s free energy while samples without surfactant
prone to aggregation to reduce Gibb’s free energy. For
morphology aspect, HYD 150 has plate-like particle,
while CuO 75 and CuO 100 exhibited rice-grain-like and
needle-like particle, respectively. However, particle size,
morphology, and extend of aggregation changed when
PEG concentration varied. In comparison in terms of
shape-dependent antibacterial performance, nanoplate-like
CuO synthesized by hydrothermal method has discovered
to have larger zone of inhibitory zone compared to CuO
75 and CuO 100. This could be due to the morphology-
dependent interaction with bacterial cell wall, thus easily
damages the bacteria and inhibits the growth [114]. Gen-
erally, there are three mechanisms associated with anti-
bacterial activities by CuO nanocomposites namely,
release of copper ions, copper NPs, and biofilm inhibi-
tion. Inhibited growth of bacteria by copper ions mainly
resulted from generation of ROS, caused increase in cell
permeability for copper ions diffuse into bacterial intra-
cellular matrix. The copper ions bind to the DNA and
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crosslink to the nucleic acid strands, caused disorder heli-
cal structure and as a consequence lead to protein and
nucleic acid denaturation and cell unable to replicate and
died. Moreover, the overwhelmed of ROS could poten-
tially resulted outbreak of oxidative stress, and burst
within the bacterial cell [115, 125]. Release of copper
NPs mechanism depends on its particle size and surface
charge. For particle between the ranges of 10 to 100 nm,
the copper particle attaches to cell membrane by endocy-
tosis while particle less than 10 nm, its hydrophobicity or
hydrophilicity on surface plays an important factor for the
interaction with cell membrane (lipid bilayer). Penetration
of copper into membrane releases copper ions and trig-
gers copper ions mechanism. Biofilm formation is where
the active outer layer of copper particles reduces signifi-
cantly the cell surface hydrophobicity and extracellular
polymeric substances causes the attachment of copper
particles around the cell membrane, consequently it
results similar copper NP mechanism on inhibition of
bacteria growth [115].
Synthesis Method. There are various methods to syn-
thesize Cu-based NPs either Cu NPs or CuO NPs-coated
fabric have been developed such as chemical reduction
[12, 29, 32, 55], ultrasound irradiation [13, 99, 121, 126],
and metal chelation technique [42]. Table 3 shows the
summary of Cu-based NPs-coated textile and its antibac-
terial effects.
Komeily-Nia et al. have in situ synthesized Cu NPs on
nylon fabric with incorporation of ascorbic acid as
reducer and cetyltrimethylammoniumbromide (CTAB) as
capping agent through facile chemical reduction tech-
nique. The results showed that most of the synthesized
Cu NPs were spherical, with minor presence of nano-
wired shaped that owned grain size less than 100 nm.
The inherited property of surface plasmon absorbance
showed colorant effect on fabric. CTAB as cationic sur-
factant has affected the particle size which resulted
smaller particles with improved antibacterial properties
[55]. Heliopoulos et al. have prepared alginate-Cu NPs-
coated WO fabric via chemical reduction, exhibited good
bacterial reduction against E. coli. There is a difference
in copper loading between WO/copper fabric and WO/
alginate/copper as the presence of alginate has the ability
to hold up more than 170.0 mg/g of copper ions [12].
Moreover, Teli and Sheikh have studied the antibacterial
characteristic of acrylamide-Cu NPs grafted bamboo
rayon fabric by chemical reduction synthesis. Addition of
acrylamide on coating served as a binding site for attach-
ment of Cu NPs on the fabric surface and thus enhanced
the bacterial reduction [32]. Yang et al. have impregnated
Cu NPs on cotton fabric with the use of polydopamine as
reductant and binder found exhibited durable sticky super-
hydrophobicity and considerable antibacterial activity.
According to the analysis, it has been found that they
mainly consisted of metallic state of Cu with the minor
presence of CuO on the cotton surface. The strong adhe-
sive property between Cu NPs and polydopamine enable
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TABLE 3. Summary of Cu-based NPs-coated textile and its antibacterial effects.

Innoculus Incubation time/

Additive matrix Synthesis method Type of textile NP size (nm) Microorganism (CFU/mL) contact time Antibacterial assay Effects Refs.

Sodium alginate Chemical reduction Wool — E. coli 1–5 3 108 for 18–24 h Disc diffusion and 100% bacterial reduction of [12]
disc diffusion. count colony E. coli after 24 h contact
1–2 3 105 for forming units time.
count colony
forming unit
Dopamine Chemical reduction Cotton 400–500 E. coli 106 18 h Count colony 99.9% bacterial reduction was [29]
forming units. achieved.
Acrylamide Chemical reduction Bamboo rayon <100 E. coli, S. aureus — — Count colony 100% bacterial reduction was [32]
forming units. achieved at 0.5% of
CuSO4.
Ascorbic acid/CTAB Chemical reduction Nylon 85 S. aureus — 24 h Disc diffusion The treated fabric exhibited [55]
significant antibacterial
properties.
— Ultrasound irradiation Nylon and 17–20 B. subtilis — 24 h Disc diffusion The antibacterial effect is [13]
wool increased by increasing the
dye concentration from
0.1% to 0.5% in both wool
and nylon fibers.
— Ultrasound irradiation Cotton 10–20 E. coli — 0, 30, 60, 120 min Count colony The CuO–cotton bandage [99]
forming units containing 0.65 and 1.50
wt% CuO demonstrated

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activity for killing E. coli.

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— Ultrasound irradiation Cotton 10–15 E. coli, S. aureus 107 1 and 3 h Count colony 100% bacterial reduction was [121]
forming units observed for both bacterial

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strains.
— Ultrasound irradiation Cotton 200–400 E. coli, S. aureus, — — — The treated fabric exhibited [126]
Klebsiella and MRSA significant antibacterial
properties.

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Epichlorohydrin (EP) Metal chelation Viscose and — E. coli, S. aureus — — Count colony 100% bacterial reduction of [42]
and benzedine (Bz) acrylic forming units both bacterial strains was
found on acrylic fabric.

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TECHNOLOGY—2017 E19
17
modified fabric still able to inhibit growth of bacteria
even it has washed 30 and 50 cycles with 95.5% and
88.5% reduction of initial E. coli presented [29].
Perelshtein et al. have prepared CuO NPs-coated cot-
ton fabric via in situ one-step ultrasound method and
found that the process resulted in a homogeneous disper-
sion of CuO NPs with 15 nm in size, owned significant
bactericidal effect against E. coli and S. aureus [121].
The synthesis of CuO NPs is through the reaction with
Cu ions with ammonia to form deep blue solution of
ammonium complex ions accompanied by hydrolysis and
sonochemical mirojets. The chemical reaction pathways
to form CuO NPs are depicted as following:
 21
Cu21 ðaqÞ 1 4NH3 H2 OðaqÞ ! CuðNH3 Þ4 ðaqÞ 1 4H2 O
(1)
 21
CuðNH3 Þ4 ðaqÞ 1 2OH2 ðaqÞ 1 4H2 O
! CuðOHÞ2ðsÞ 1 4NH3 H2 OðaqÞ (2)
D
CuðOHÞ2ðsÞ ƒ!CuOðsÞ (3)
According to Abramova et al., antibacterial CuO NPs
coated into textile using ultrasonic cavitation has synthe-
sized ellipsoidal shape and particle sizes range from 200 to
400 nm with good antibacterial activity against E. coli, K.
pneumoniae, S. aureus, and methicillin-resistant S. aureus
(MRSA) [126]. Shariatinia et al. have used two nanosized
copper(II) complexes including phosphoric triamide ligands
with formula Cu(NO3)2L2 and Cu(CH3COO)2L2 where L
represents 4-NO2C6H4NHP(O)(NC4H8O)2 coated on nylon
and WO fabrics, endowed yellow and green color, respec-
tively, with spherical morphology in average grain sizes of
17–20 nm. The complexes were synthesized through sono-
chemical approach and the yielded fabrics possessed excel-
lent wash fastness and antibacterial activity against
Bacillus subtilis while poor in lightfastness [13]. The pilot
scale sonochemical coating of CuO NPs onto cotton fabric
produced biocidal property has been studied by Abramov
et al. According to the results, it revealed that the coating
is homogeneous with particle sizes range from 10 to
20 nm. It is found that the homogeneity of metal deposi-
tion on fabric depends on the concentration of precursor
and the velocity of bandage passing between the sonicated
plates [99].
Mekewi et al. have presented antibacterial synthetic
viscose and acrylic fabrics by using metal chelation Cu
NPs to enhance antibacterial activities against E. coli and
S. aureus. The fabric has undergone amination with dif-
ferent types of chemical namely, ethylenediamine and
benzedine and the effect on its affinity to metal chelation
of Cu which indirectly influence the antibacterial activity
has been studied. The results showed that benzedine
treated fabric are more favorable for Cu metal uptake
than those fabric treated with ethylenediamine due to ben-
zedine molecules binding affinity to translation metal ions
through the nitrogen lone pairs. As a consequence,
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benzedine treated fabric has more prominent microorgan-
ism’s hostility resistance [42].
Titanium Oxide NPs (TiO2 NPs)
TiO2 exists in three famous crystalline structures
known as anatase, rutile, and brookite. Compared to ana-
tase and brookite, rutile is the most thermally stable due
to its more compact structure. When anatase and rutile
heated under high temperature, crystal growth induced
and altered the phase stability and ultimately caused ana-
tase and brookite are irreversibly transformed to the
rutile. Rutile has excellent characteristics such as greater
chemical stability, higher refraction index, and higher
specific gravity compared to anatase and brookite, making
it mostly used in pigments industry. Anatase in nanosize-
structure is metastable at ambient room temperature while
rutile phase is stable at room temperature in particle size
beyond 14 nm. Thus, thermodynamic stability is particle
size dependent and it is important in determination perfor-
mance of TiO2 in different applications. Due to its stabil-
ity at nanostructure, anatase is favorably used in
photocatalysis due to its high surface area. Its high photo-
catalytic property able to generate electrons and electric
hole pairs by absorption of UV illumination. The created
electrons and holes react with oxygen and water to form
O–2 and hydroxyl radicals. This ROS generation is postu-
lated could be the agent to kill the bacteria cell under
presence of light [127]. Wu et al. have been successfully
deposited TiO2 in anatase with particle size 3–5 nm on
cotton fabrics, possessed distinct self-cleaning and bacte-
ricidal activity under the fluorescent light. It suggests that
the antibacterial activity is due to the photocatalytic effect
of TiO2 coated fabric, leading to destruction of cell wall
and membrane by ROS [128]. However, due to its wide
energy band gap between conduction and valence bands
which is approximately 3.2 eV, it requires high energy to
create electrons and electric hole pairs. Thus, researchers
have been added noble metal and additive material to
extend the light absorption range of TiO2 from UV to vis-
ible light, which resulted in high generation of ROS.
These include silver/polysiloxane (XPs) [129], chitosan
[130], chitosan/AgCl [131, 132], and sericin/polycarbox-
ylic acid [133]. Notably, Ag-TiO2 coated cotton fabrics
have been studied due to the shifting of UV-vis absorp-
tion spectrum to long wavelength (>400 nm), thus enable
the enhancement of antibacterial activity under fluores-
cent light. Ag serves as an electron traps aiding electron-
hole separation by creating a local electric field which
facilitates the excitation of electron from valence band to
conduction band [89]. According to Daoud et al. litera-
ture, it suggested that the cytotoxicity of TiO2 not only
occurred under the presence of light but the reduction of
bacteria cells under dark condition have been observed
due to the nonsustenance nature of TiO2 by serving as a
protecting shield against formation of biofilm [134].
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 TABLE 4. Summary of TiO2 NPs-coated NPs textile and its antibacterial effects.

DOI
Incubation time/
Additive matrix Synthesis method Type of textile NP size (nm) Microorganism Innoculus (CFU/mL) contact time Antibacterial assay Effects Refs.

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Ag Pad-dry-cure Silk 20 S. aureus, E. coli, — 24 h Disc diffusion The treated fabric exhibited [22]
P. aeruginosa significant antibacterial
properties.
ZnO Pad-dry-cure Nylon/cotton — E. coli, S. aureus — — ASTM 100 method The highest antibacterial [56]
property against E. Coli
and S. aureus which was
appeared at 60 ppm of
ZnO/TiO2.
Sulfated b-cyclodextrin Pad-dry-cure Cotton 20–200 E. coli, S. aureus. 12 3 105 for S. aureus. 10, 15, 20, Count colony The bacterial reduction for S. [79]
6 3 105 for E. coli 30 min forming units aureus and E. coli were
found maximum at 30 min
with 90% and 85%,
respectively.
— Pad-dry-cure Cotton 3–5 — — 30 min Turbidity assessment The treated fabric exhibited [128]
significant antibacterial
properties.
Ag/polysiloxane Pad-dry-cure Polyester 25–30 S. aureus, E. coli 2 3 104 18 h Count colony Exhibit antibacterial property [129]
forming units
BTCA, SHP, Pad-dry-cure Cotton <25 S. aureus, E. coli, — — Disc diffusion The treated fabric exhibited [130]
chitosan phosphate A. flavus, C. albicans significant antibacterial
properties.
Chitosan/AgCl Pad-dry-cure Cotton — S. aureus, E. coli — 24 h Count colony 100% bacterial reduction [131]
forming units against S. aureus and E.
coli obtained with chitosan/
AgCl–TiO2 colloid at con-
centrations of 4 and 10 g/L,
respectively.
Sericin/polycarboxylic Pad-dry-cure Cotton 20–30 S. aureus, E. coli 104 for E. coli. 105 3h Count of colony Higher NTO concentration, [133]

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acid for S. aureus forming units 50 g/L exhibited higher

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antibacterial properties.
— Pad-dry-cure Cotton 10 S. aureus 1.5–3 3 105 24 h Count of colony The antibacterial property of [134]

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forming units TiO2 was found less effi-
cient in dark condition than
in presence of UV
radiation.

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— Sonochemical Wool 24–27 S. aureus, E. coli, — — Count of colony The antibacterial and antifun- [15]
C. albicans forming units gal activities of the sono-
treated samples with
TTIB13 were higher than
TTIP13.
Chitosan/PVA/PEG Sonochemical Cotton 187–664 S. aureus — — Count colony The TiO2 fabric treated with [132]
forming units 0.1% HW CS solution
exhibited highest antibacte-

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rial property compared to

TECHNOLOGY—2017 E21
others.

19
FIG. 7. Proposed stability mechanism for TiO2 NPs dispersions in the presence of polymers [132]. [Color figure can be viewed at wileyonlinelibrary.
com]
Synthesis Method. There are several techniques in
preparation of TiO2-coated fabric namely, pad dry cure
method [22, 56, 79, 128–131, 133, 134] and sonosynthe-
sis [15, 132] in which all of these methods are carried out
at low temperature. Table 4 shows the summary of TiO2
NPs-coated textile and its antibacterial effects.
For pad dry cure method, Dastjerdi et al. have synthe-
sized polysiloxane/silver on the TiO2 polyester fabric to
test the effect on antibacterial activity against S. aureus
and E. coli [129]. Arain et al. have studied the effect of
different blend ratios of chitosan to AgCl/TiO2 coated
onto fabric on antibacterial activity against S. aureus and
E. coli via pad dry cure method. Increasing concentration
of chitosan not only showed better antibacterial activity
but has advantages on tensile strength, fabric stiffness,
and wrinkle recovery angle [131]. Doakhan et al. have
prepared sericin/TiO2 grafted cotton fabric with polycar-
boxylic acid as crosslinking agent via pad dry cure
method. The presence of sericin acted as a glue to bind
the TiO2 on cotton and at the same time facilitated anti-
bacterial activity against S. aureus and E. coli. Its polyca-
tionic feature which has ability to interact with negatively
charged bacterial cell membrane, reduce cell membrane
integrity and ultimately leading to cell death [133]. El-
Shafei et al. have applied TiO2 (0%–9%) on cotton fabric
with the presence of different amounts of BTCA (0%–
8%), SHP (0%–8%), and chitosan (0%–10%) through
pad-dry-cure approach, exhibited flame retardant and anti-
bacterial properties [130]. Li et al. have designed nano-
sized TiO2 and Ag/TiO2 functionalized silk textile with
the aid of 3-(3,4-dyhydroxyphenyl) propionic acid,
BTCA, dimethylol dihydroxyethylene urea, and SHP,
which served as enhancing antiviral property, bridge
crosslink, color property, and catalyst, respectively,
through pad-dry-cure method. It is observed that TiO2 has
a diameter around 20 nm with irregular structure and was
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surrounded by nanosized Ag with grain size approxi-
mately 5 nm which enhanced photocatalysis and thereby
increased the antibacterial activity against E. coli, S.
aureus, and P. aeruginosa [22]. Wu et al. have used tetra-
butyl titanate as precursor for TiO2 production via pad-
dry-cure technique. The synthesized TiO2 possessed dom-
inant anatase crystalline morphology with almost uniform
in size 3–5 nm dispersing on cotton fabric surface. The
coated fabric showed self-cleaning ability in photocata-
lytic decolor of dyes and antibacterial activity [128].
Daoud et al. have used titanium isopropoxide (TTIP) as
source for TiO2 via pad-dry-cure method. The TiO2 char-
acterized semispherical morphology with particle size
around 10 nm in diameter on cotton surface. The authors
have compared the antibacterial assessment under UV
radiation and dark conditions and found that both condi-
tions possessed reduction of bacteria but with coated fab-
ric under UV irradiation has higher cytotoxicity compared
with that under absence of light [134].
Immobilization TiO2 onto textile material can be
through in situ sonosynthesis approach. This method not
only able to reduce surface of textile, but also enhance
the washing fast ability by trapping the NPs inside the
textile matrix. The simplicity of this method also provides
the formation of TiO2 on textile in one single step and
without involving of annealing process. Goyal et al. have
studied the role of chitosan with different molecular
weights, low molecular weight, and high molecular
weight of chitosan (LMW-CS and HMW-CS) on coating
TiO2 onto cotton fabric via sonosynthesis method. Figure
7 depicts the stabilization mechanism of adding HMW-
CS, LMW-CS, and ionic polymers which are polyvinyl
alcohol and PEG on TiO2 NPs. Incorporation of CS
enhances the chemical bonding by formation of hydrogen
bonds between polar groups of CS and hydroxyl groups
of TiO2 NPs. The cationic behavior of CS due to the
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presence of ANH1 3 on molecules increase the n potential
and stabilize the TiO2 dispersions on cotton. Also, the
role of steric hindrance by using a nonionic polymer acts
as stabilizing agent on TiO2/CS dispersion on cotton.
Both LMW-CS and HMW-CS coated with TiO2 on cotton
has self-cleaning, UV-protection, and antibacterial activ-
ity. However, with HMW-CS samples, there was an
increase in TiO2 particle size and dispersion stability due
to its high molecular weight able to create a thicker layer
around the TiO2 before the repulsion suppressed the depo-
sition of further chains [132]. Behzadnia et al. have used
sonochemical method at 608C–65 C to produce TiO2-
coated WO fabric by using two different precursors
namely TTIP and titanium butoxide. The synthesized
TiO2 resulted the formation of both anatase and rutile
phases with self-cleaning, antibacterial, and hydrophilicity
properties. The samples with titanium butoxide have
found to have higher photocatalytic activity compared to
samples with TTIP. This could be due to the longer
hydrocarbon chain changes the band gap of TiO2 but per-
suades several localized occupied states in the gap [15].
Other Metal-Based NPs
There are also embedment of other metal-based anti-
bacterial agents such as iron based [30], CeO2 [19, 135],
Au [23, 35, 136, 137], Ni [42], SiO2 [16, 43], and Pt
[49]. Table 5 shows the summary of other metal-based
NPs-coated textile and its antibacterial effects. For iron
based NPs, Rastgoo et al. have prepared Fe3O4 on
blended cotton/polyester fabric via ultrasound mediation
exhibited magnetic, photocatalytic, sonocatalytic, and
antibacterial characteristics [30].
CeO2 is one of the most abundant rare earth metal
oxides, which categorized in lanthanide series with two
stable oxidation forms trivalent state (13) and tetravalent
state (14). The ability in reversible switching between
two oxidation states along with the oxygen vacancies by
surface defects making it possesses antioxidative ability
which is widely applied on biomedical field by regenerat-
ing free-radical scavengers. Moreover, its relatively
smaller band gap compared to ZnO and TiO2, leading it
as alternative UV absorbent for sunscreen, photocatalyst,
textile fiber coating, and so on [19]. The toxicity of CeO2
on microorganisms has been studied by Rajan et al.
[135], and Lu et al. [19]. Lu et al. have immobilized
CeO2 NPs on silk fabric via simple dip-coating approach,
found endowed UV-shielding ability and antibacterial
activity. The synthesized CeO2 NPs tend to agglomerate
and lead to larger particle sizes ranging from 20 to 30 nm
which might affect the efficiency of antibacterial perfor-
mance. In order to enhance microbicidal effect of CeO2
on treated fabric, Rajan et al. [135] have incorporated
allicin on coating via wet chemical method found to have
more effective on inhibition growth of E. coli and S.
aureus.
Most of the studies regarding the synthesis of Au NPs-
coated textile use chloroauric acid (HAuCl4) as source of
DOI 10.1002/vnl
DOI 10.1002/vnl
Au. Tang et al. [35] have functionalized Au NPs-coated
bamboo pulp fabric through facile chemical reduction
method without any stabilizing agent used. The results
indicated that the morphology of Au NPs depend on the
concentration HAuCl4 solution, which induced different
colorant effect due to their localized surface plasmon res-
onance property. The imparted fabric showed good fast-
ness to light, UV protection, and antibacterial activity
[35]. Tang et al. also have presented another literature
based on the in situ of Au NPs-coated silk fabric by using
same method. The Au NPs-coated silk fabric possessed
remarkable antibacterial activity, UV protective, and ther-
mal conductivity [23]. Moreover, there are researches on
synthesis of Au NPs-coated textile with additional reduc-
ing agent either synthetic or natural. Ganesan and Guru-
mallesh Prabu have synthesized antibacterial Au NPs-
coated cotton fabric with HAuCl4 as precursor and extract
of Acorus calamus rhizome as green reducer via pad-dry-
cure method. The results revealed that the size of Au NPs
depend on the concentration of precursor. At low concen-
tration, NPs showed homogenous in size with spherical
morphology at particle size in below 100 nm, whereas at
high concentration of precursor, the synthesized NPs
showed bigger size in spherical structure at grain sizes
between 100 and 500 nm. The treated fabric showed
improved antibacterial activity and UV blocking property
compared to that untreated fabric [136]. Velmurugan
et al. have compared three different modes of synthesis
Au NPs on cotton, silk, and leather namely, green, chemi-
cal, and a composite of green and chemical synthesis. For
green synthesis, natural leaf powder extract, Ginkgo
biloba Linn is used as reducer while for chemical synthe-
sis, KBH4 is used as reducing agent. For composite syn-
thesis, G. biloba extract and KBH4 are used to color and
embed AuNPs in the fabrics. Based on the observation, it
is found that composite synthesis has more dead bacterial
cells than in green and chemical synthesis. The treated
leather is less affinity to take up Au NPs than silk and
cotton due to its collagen bundles interconnected with
large elastic fibers. Moreover, the incorporation of G.
biloba leaf extract is responsible for enhancing high anti-
bacterial activity [137].
Application of monodisperse silicon on development
of multifunctional textile has been studied by El-Gabry
et al. [43] and Wang et al. [16]. El-Gabry et al. have
incorporated acrylate based copolymer as binder on coat-
ing nanosized silica on viscose and polyester fabrics
through conventional pad-dry-cure method. It is found
that percentage of reduction E. coli bacteria before and
after 10 laundering cycles is higher for acrylate/silica
treated fabric compared to pristine and solely silica
coated fabrics, indicated the conducive trapping effect on
the treated fabric. Wang et al. have prepared nano-silica
with additional loading of Ag via plasma irradiation treat-
ment found to have spherical particles with average grain
size of 60 nm, exhibited high effective in killing bacteria
and excellent water resisting property.
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21
 TABLE 5. Summary of other metal-based NPs-coated textile and its antibacterial effects.

E24
Metal-based Synthesis Innoculus Incubation time/
NPs Additive matrix method Type of textile NP size (nm) Microorganism (CFU/mL) contact time (h) Antibacterial assay Effects Refs.

22 JOURNAL
CTAB Sonochemical Cotton/polyester 46 S. aureus, C. 106 18 Count colony The treated fabric exhibited [30]

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Fe3O4
albicans forming unit 95% and 99% growth
reduction of S. aureus and

OFVINYL
C. albicans, respectively.
CeO2 — Dip coating Silk 20–30 E. coli, S. aureus, 2 3 103 — Count colony The results found that E. coli [19]
P. aeruginosa, forming unit is least resistance to CeO2
B. subtilis followed by S. aureus, B.

VINYL&&ADDITIVE
subtilis, and P. aeruginosa.
CeO2 Allicin Wet chemical — 5–10 E. coli, S. aureus — 24 Disc diffusion The treated fabric exhibited [135]
significant antibacterial
properties.
Au — Wet chemical Silk 213 6 3.4 E. coli 30–300 18 Disc diffusion The treated fabric exhibited [23]
significant antibacterial
properties.

ADDITIVETECHNOLOGY—2017
TECHNOLOGY—2019
Au — Wet chemical Bamboo pulp — E. coli 30–300 18 Disc diffusion The treated fabric exhibited [35]
significant antibacterial
properties.
Au Acorus calamus Pad-dry-cure Cotton 10 E. coli, S. — 24 and 48 Count colony The percentage inhibition was [136]
rhizome aureus forming unit found to increase signifi-
cantly after 48 h compared
to 24 h.
Au Ginkgo biloba Wet chemical Silk and cotton 10–75 B. linens — — Live/dead BacLight Green and composite synthe- [137]
Linn and KBH4 sis is more effective than
chemical synthesis in anti-
bacterial performance.
Ni Epichlorohydrin (EP) Metal chelation Viscose and — E. coli, S. — — Count colony Benzidine treated fabric is [42]
and benzedine (Bz) acrylic aureus forming unit more preferable on antimi-
crobial function than
enthylenediamine
SiO2 Ag Wet chemical Wool 60 E. coli, S. 1–2 3 104 22 Count colony Increase concentration of [16]
aureus forming unit SiO2 and contact time
increases antibacterial per-
formance of treated fabric.
SiO2 Acrylate based Sol gel Viscose and <21 E. coli, S. 22,800 CFU/mL — Count colony The treated fabric in the pres- [43]
copolymer polyester aureus (for E. coli forming unit ence of binder exhibited
bacteria) and 100% antimicrobial
17,440 CFU/mL reduction.
(for S. aureus
bacteria)
Pt — DC magnetron Polyester — S. aureus 1 3 108 24 Count colony The existence of platinum [49]
sputtering forming unit itself, without any deriva-

DOI
tives of antibacterial agents,
does not show any antibac-
terial activity on the treated

DOI 10.1002/vnl
10.1002/vnl
fabric.
 For Pt NPs, Shahidi and Ghoranneviss have investi-
gated the antibacterial feature of Pt on polyester fabric
with different natural and synthetic dyes via DC magne-
tron sputtering mean. It revealed that the platinum itself
did not show any antibacterial activity without presence
of any derivatives of antibacterial agent [49].
FUTURE OUTLOOKS
In general, the metal based nanostructured materials
have spurred interests of researchers to apply on antimi-
crobial textile due to their excellent multifunctional fea-
tures. Based on the experience of past researches, many
studies are focusing to enhance the adherence of nano-
structured materials onto fabric in order to prevent leach-
ing into environment and leading to pollution. Hence, it
is important to ensure there is chemical reaction between
the agent and textile fiber. The pretreatment on the textile
fiber before coating is needed to form higher concentra-
tion of functional groups which serve as binding sites for
absorption. Furthermore, there are many factors still
worth to be studied to determine the effectiveness and
durability of textiles which mainly depend on the type of
polymer used, antibacterial agents, and synthesis tech-
nique used in the production.
Besides that, the type of polymers used improve the
durability of the fabric also undeniable important. Indeed,
the incorporation of antimicrobial agent on polymer matrix
is known promote a slower release during usage and pro-
longed its antibacterial function period of textile wear.
Upon the environmental protection priority, the utilization
of green natural biopolymers extracted from either animals
or plants, such as chitosan, sericin, alginate, etc., which are
renewable and environment friendly are potential to be the
critical resources for future sustainable multifunctional tex-
tile. These types of antibacterial agents endow different
modes of action on biocidal mechanisms associated with
their chemical, structure, and affinity extent to particular
target sites within microbial cells. On the other hand, the
synthesis techniques should has high efficiency, economi-
cal, practical without creating ecological hazard. There are
novel technologies such as plasma treatment, ultrasound,
UV radiation, etc. worth to replace conventional processes.
For instance, the employment of dry plasma treatment
does not use harmful chemical solutions (solvent-free pro-
cess) and does not contaminated water or induces mechani-
cal hazards for modified textile. In addition, through
ultrasound and UV irradiation can enhance the dispersion
of antibacterial agent onto the textile with better antibacte-
rial performance. Also, the application of specific reaction
catalyzed by enzymes such as glycosidases, proteases, lac-
case, and lipases can further enhance the antibacterial tex-
tile performance. In overall, it is expected that more
researches will be focused on environmental-friendly syn-
thesis approaches while promoting the usage of green
agents which possess potential long term antibacterial ben-
efits for better health and environment.
DOI 10.1002/vnl
DOI 10.1002/vnl
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JOURNALOF
JOURNAL OFVINYL
VINYL&&ADDITIVE
ADDITIVETECHNOLOGY—2019
TECHNOLOGY—2017 E27
25