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A study of the antimicrobial property of encapsulated copper oxide nanoparticles on cotton fabric
S. Anita, T. Ramachandran, R. Rajendran, CV Koushik and M. Mahalakshmi
Textile Research Journal 2011 81: 1081 originally published online 8 April 2011
DOI: 10.1177/0040517510397577

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Original article
Textile Research Journal
81(10) 1081–1088

A study of the antimicrobial property ! The Author(s) 2011

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of encapsulated copper oxide DOI: 10.1177/0040517510397577
trj.sagepub.com
nanoparticles on cotton fabric

S Anita1, T Ramachandran2, R Rajendran3, CV Koushik1

and M Mahalakshmi4

Abstract
Among the diverse fields of application of technical textiles, which are poised for tremendous growth in fast-developing
economies such as India and China, non-implantable healthcare and hygiene products are assuming significant importance
because of the specificity of their end uses. Today, the healthcare industry is increasingly concerned with the exposure
and transference of various microorganisms that are commonly present in the atmosphere. Studies have been carried out
in the present work to fine-tune the properties of copper oxide nanoparticles for special applications. Using copper
sulfate and sodium hydroxide as precursors and soluble starch as stabilizing agent, the copper oxide nanoparticles were
prepared by a wet chemical method. The copper oxide nanoparticles were microencapsulated by an ionic gelation
method and applied to plain weave cotton fabric by exhaustion as the first step, and in the second step by the
pad–dry–cure method. The antibacterial property of the coated fabric was determined quantitatively and qualitatively
using AATCC 100 and 147 test methods, respectively. Techniques such as scanning electron microscopy, X-ray diffraction
spectroscopy and physical and chemical characterization were employed to study the phase and morphology of the
nanoparticles. The results indicate that the coated fabric has high antibacterial efficiency. The nanoparticles synthesized in
this work have an average size of 50 nm, and the physical and chemical properties of the treated fabric are markedly
different from those of the untreated fabric. Insights into copper oxide encapsulated coated fabric prove their efficacy
against microbes and hence can be used in the manufacture of medical apparel.

Keywords
chemistry, coatings, encapsulation, finishing, synthesis

Nanotechnology is increasingly attracting worldwide
attention because it is widely perceived as offering
huge potential in a wide range of end uses. The
unique and new properties of nanomaterials have
attracted not only scientists and researchers but also
businesses, due to their huge economical potential.1
The impact of nanotechnology in textile finishing has
given rise to innovative finishes as well as new applica-
tion techniques. Particular attention has been paid to
making chemical finishing more controllable and more
thorough. Ideally, discrete molecules or nanoparticles
of finishes can be brought individually to designated
sites on textiles materials in a specific orientation and
trajectory through thermodynamic, electrostatic or
other technical approaches.2 Nanometric materials
can be dispersed into the matrix of textile fibers or
deposited on the textile fabric surface to give new
nanocomposites with improved performances and char-
acteristics. The spectrum of nanoparticles used for
preparing nanocomposites is large. It ranges from
metals, such as silver, to metal oxides, such as titanium
dioxide, to carbon nanotubes (CNT) and to clays.
1
Department of Fashion Technology, Sona College of Technology, Salem,
Tamil Nadu, India.
2
Karpagam Institute Of Technology, Coimbatore, India.
3
Department of Microbiology, PSG College of Arts and Science,
Coimbatore, Tamil Nadu, India.
4
Rndbio, The Biosolutions Company, Coimbatore, Tamil Nadu, India.
Corresponding author:
S Anita, Senior Lecturer, Department of Fashion Technology, Sona
College of Technology, Salem, Tamil Nadu, India
Email: anita_aft@yahoo.co.in

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1082
Therefore, a considerable number of characteristics and
performances can be obtained with the incorporation
of nanoparticles in textiles.
Nanotechnology research in textiles is being prac-
ticed rather intensively with two major objectives in
mind. The first objective aims at upgrading both
present functions and performance of textile materials.
For example, fabric manufactured with fibers contain-
ing nanosize fillers, e.g. nanoparticles, nanopowders,
and CNT will enhance the performance of the fabrics
to a greater extent. The second objective focuses on the
development of unique products, in particular smart/
functional textiles with fundamentally new features and
functions.
Textile products have progressed to a point where
they can provide a complete barrier to microbiological
agents. Today, expectations go beyond the barrier and
the world now seeks antimicrobial-finished fabric that
goes a step further and prevents transmission or prop-
agation of microorganisms. Textile product
manufacturing was facilitated by the diversity of
fibrous substances available directly from nature.
Cotton, linen, wool, silk, etc, although resulting in
comfortable garments, lack the ability to effectively
resist biological degradation and possess practically
no resistance to microbial growth.
Special finishes providing microbial protection can
be distinguished by their two-fold protective character-
istics. The first relates to the protection of the textile
from pathogenic or odor-causing microorganisms. The
second attribute is the protection of textile itself from
damage caused by mould, mildew or rot-producing
microorganisms.
Nanotechnology offers a good range of efficient tools
and techniques to protect desirable fabric characteris-
tics, most of these focusing on modifications of the
fabric surface using nanoparticles.3 Nanoparticles can
help to enhance the physical properties of conventional
textiles in areas such as antimicrobial properties, water
repellence, soil resistance, antistatic, anti-infrared and
flame-retardant properties.4 Nanotechnology tech-
niques can alter textile fabric at the molecular level,
thus creating advanced materials that can be several
times more effective than the untreated fabric.5
Copper has been recognized as a hygienic material
since the beginnings of civilization and, during the
last two centuries, anecdotal evidence has been amply
supported by scientific research to show that copper has
antimicrobial properties, i.e. it is capable of preventing
the growth of dangerous pathogens – bacteria, moulds,
algae, fungi and viruses.
Today, copper is used as a water purifier, algaecide,
fungicide and nematocide, and as an antibacterial and
antifouling agent.6 Gabbay et al.7 have reported that
impregnation or coating of cotton and polyester fibers
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Textile Research Journal 81(10)
with cationic copper endows them with potent broad-
spectrum antibacterial, antiviral, antifungal, and anti-
mite properties. The biocidal properties of fabrics
containing 3–10% copper-impregnated fibers are
permanent, are not affected by extreme washing condi-
tions and do not interfere with the manipulation of the
final products (e.g., color, press).
Copper nanoparticles have unique optical, catalytic
and chemical properties specific to the nano level.
Enhanced functionality of copper nanoparticles can
be achieved by binding them to CNT, an effect that
can be ascribed to the high surface areas, good electri-
cal conductivity and high gas transport rates of the
CNT. Multi-walled CNT are being developed for a
host of applications including glucose biosensors, ther-
mally conductive nanofluids and the electrochemical
determination of ammonia in drinking water.8 Most
recently, Tao et al.9 have reported antibacterial prop-
erties of nanocopper/polyacrylonitrile composite fibers
against E. coli, B. subtilis, and S. aureus. The average
efficiency of antibacterial properties was more than
90% within 15 h. The mechanical properties of nano-
copper/polyacrylonitrile composite fibers were found to
be superior to copper/polyacrylonitrile fibers.
The purpose of this study was to synthesize the
copper oxide nanoparticles by a wet chemical method,
to microencapsulate the copper oxide nanoparticles by
an ionic gelation method, and to examine the antibac-
terial activity of copper oxide nanoparticles-coated
cotton fabric against Staphylococcus aureus and
Escherichia coli by standard methods (AATCC test
method 100 and 147). Finally, the physical and chem-
ical characterization of cotton fabric finished with
encapsulated copper oxide nanoparticles was compared
with that of the unfinished cotton fabric.
Materials and methods
Materials
The materials used for the present research were as
follows:
. Plain weave 100% cotton fabric
. Copper oxide nanoparticles prepared by a wet-type
chemical method
. Spray gun for microencapsulation
. Standard cultures for testing antibacterial activity
(Escherichia coli and Staphylococcus aureus)
Synthesis of copper oxide nanoparticles
A fine-medium weight 100% cotton plain weave fabric
was used for the application purpose. Using copper
Anita et al.
sulfate and sodium hydroxide as precursors and soluble
starch as stabilizing agent, the copper oxide nanoparti-
cles were prepared by a wet chemical method; 0.1%
starch solution was prepared using a microwave oven,
and 0.1 M copper sulfate was added into the above
solution. The solution was then kept under constant
stirring using a magnetic stirrer to completely dissolve
the copper sulfate. After complete dissolution of copper
sulfate, 0.2 M of sodium hydroxide solution was added
under constant stirring, drop by drop touching the
walls of the vessel. The reaction was allowed to proceed
for 2 h after complete addition of sodium hydroxide.
The solution was allowed to settle overnight and the
supernatant solution was then discarded carefully.
The remaining solution was centrifuged at 10,000 g
for 10 min and the supernatant was discarded. The
obtained nanoparticles were washed three times using
distilled water. Washing was carried out to remove the
by-products and the excessive starch that were bound
with the nanoparticles. After washing, the nanoparti-
cles were dried at 80 C overnight. During drying, loss
of water molecule takes place which results in the
complete conversion of CuSO4 into CuO.10
Microencapsulation of copper oxide nanoparticles
Microencapsulation is a process in which tiny particles,
or a coating giving small capsules, surrounds droplets.
A microcapsule is a small sphere with a uniform wall
around it. The material inside the microcapsule is
referred to as the core, internal phase or fill, whereas
the wall is sometimes called a shell, coating or
membrane.
There are numerous reasons for microencapsulation.
In some cases, the core must be isolated from its sur-
roundings, as in isolating vitamins from the harmful
effects of oxygen, retarding evaporation of a volatile
core, improving the handling properties of a sticky
material, or isolating a reactive core from chemical
attack. In other cases, the objective is not to isolate
Control Sample
Figure 1. Antimicrobial activity of cotton fabric finished with encapsulated copper oxide nanoparticles (AATCC 147).
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1083
the core but to release it in a controlled manner; the
rate at which it leaves the microcapsule is controlled, as
in the controlled release of drugs or pesticides.
Microencapsulation by an ionic gelation
process. Microcapsules containing nanoparticles were
prepared employing sodium alginate, the nanoparticles
being the core material and sodium alginate the wall
material; the microencapsulation was carried out by the
ionic gelation method. We prepared 3% sodium algi-
nate, which was added to 2% nanoparticles. This was
sprayed into the gelation medium of calcium chloride
solution, which is a cross-linking reagent, by means of a
sprayer. The droplets were retained in calcium chloride
for 15 min. The microcapsules were obtained by decan-
tation and repeated washing with iso-propyl alcohol
followed by drying at 45 C for 12 h. The microcapsules
were then used for finishing selected fabrics.11
Application of microencapsulated copper oxide
nanoparticle to textile fabric. The fabric was first
exhausted in a bath containing 10 ml of the microen-
capsulated nanoparticles solution at 50 C for 30 min.
Then in the second step the fabric was removed, padded
and squeezed and dried at 80–85 C in an oven for
5 min, and finally cured at 150 C for 2 min.
Antimicrobial evaluation
Antibacterial tests – agar diffusion method (AATCC
147). Standard strains of bacteria, Staphylococcus
aureus (ATCC 6538) and Escherichia coli (ATCC
11230), were used as standard Gram-positive and
Gram-negative organisms, respectively. A surface coat-
ing capable of releasing metal species to a broth of
living organisms in a controlled manner is an extremely
interesting material for a number of biotechnological
applications.12
AATCC bacteriostasis broth/agar medium were
used as a growth medium for evaluation. Using a
S. aureus E. coli
1084
4-mm inoculating loop, the culture was transferred
daily to the nutrient/bacteriostasis broth for not more
than 2 weeks.
Test specimens (enzyme and antimicrobial treated)
and the untreated fabric samples (control) were cut into
circular pieces of convenient size (15-mm radius).
Sterilized nutrient/bacteriostasis agar medium, previ-
ously sterilized and cooled to 47  2 C, was dispensed
by pouring 15  2 ml into each of standard
(15  100 ml) flat-bottomed petri dishes. The agar was
allowed to solidify and was inoculated with a day
culture (slant cultures) of the test organisms. These
were placed on the petri dishes and allowed to
harden. The textile test specimen was placed on solid
agar and attached to it. For conditioning, the test dish
was stored for 24 h at 5 C and then placed in an incu-
bator. If the fabric curled, preventing intimate contact
with the inoculated surface, small sterile glass plates
were placed on the ends of the fabric to hold it in
place. The plates were then incubated at 37 C for
18–24 h.
At the end of the incubation time, the test specimens
were observed. The agar under the sample was also
evaluated. This was important if no zones of inhibition
existed. This assessment was made by visual examina-
tion as well as under a microscope with 40  magnifi-
cation. The evaluation was made on the basis of
absence or presence of bacterial effects in the contact
zone under the specimen and the possible formation of
a zone of inhibition around the test specimen; the zones
of bacteriostasis were measured in mm. The fabric was
evaluated for its antimicrobial efficacy after five washes
and 10 washes.
Shake flask method (AATCC 100). The antibacterial
activity was quantitatively evaluated against
Staphylococcus aureus (ATCC 6538), a Gram-positive
organism and Escherichia coli (ATCC 8739), and a
Gram-negative organism, according to the AATCC
100 test method. The fabric samples with 4.8  0.1 cm
diameter were placed in a 50 ml conical flask and inoc-
ulated with 0.5 ml of bacterial culture. After incubation
over contact periods of 24 h, the solution was serially
diluted. The diluted solution was plated on nutrient
agar and incubated for 24 h at 37  2 C. Colonies of
bacteria recovered on the agar plate were counted and
the percent reduction of bacteria (R) was calculated by
the following equation: R (%) ¼ (B – A)  100/B, where
R is the % reduction, A is the number of bacteria recov-
ered from the inoculated treated test specimen swatches
in the jar incubated over the desired contact period, and
B is the number of bacteria recovered from the inocu-
lated treated test specimen swatches in the jar immedi-
ately after inoculation (at ‘0’ contact time).
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Textile Research Journal 81(10)
The percentage reduction of bacteria by the treated
specimen against each test organism was recorded.
Wash durability
To evaluate the durability of antibacterial effect after
washing, test specimens of the treated fabric of size of
7.5  13.5 cm were washed according to the AATCC
61(1A)-2001 test method using AATCC standards
specified detergent WOB. One cycle of laundering by
this method is equivalent to five typical careful hand
launderings at a temperature of 40  3 C. The treated
samples were subjected to two cycles of consecutive
laundering, the first for five cycles and the second for
10 cycles. The washed specimens were then tested for
their antimicrobial activity at the end of the two stages
of laundering. The result of the bacterial reduction
before and after washing is given in the Figures 3
and 4, respectively.
Surface characterization of copper oxide
nanoparticles
Finished fabric. The surface topography observation
of microencapsulated copper oxide nanoparticle-
finished fabric was carried out with a scanning electron
microscope (SEM). The physical properties of the
finished fabric was analyzed and compared with that
of the unfinished fabric, which served as the control
fabric using standard methods. The microencapsulated
nanoparticle-finished fabrics were characterized using
X-ray diffraction (XRD 38) with the following condi-
tions. The target X-ray tube used copper with voltage
of 40 kV and current of 30 mA. Divergence and scatter
slits of 1.0 and a receiving slit of 0.3 mm were used. The
drive axis used for the nanoparticle-coated fabric was
theta–2theta, with the scan range of 10.0–90.0 , scan
speed of 10.0 /min and with a sampling pitch of 0.1 .
Results and discussion
Copper oxide nanomaterials have some excellent prop-
erties, such as exceptional mechanical strength, anti-
static, antibacterial and UV absorption properties.
They are also well known for their antimicrobial prop-
erties. Copper is one of the metals for which there are
daily recommended allowances. Copper is commonly
used as an antimicrobial agent in swimming pools
and elsewhere.13 It is considered safe to humans, as
demonstrated by the widespread and prolonged use
of copper intrauterine devices by women.14 In contrast
to the low sensitivity of human tissue (skin or other) to
copper,15 microorganisms are extremely susceptible to
copper. For example, it has recently been shown
that copper surfaces reduce survival of epidemic
Anita et al. 1085

methicillin-resistant Staphylococcus aureus in the
healthcare environment.16
The treated fabric showed very high antimicrobial
efficiency against Staphylococcus aureus and
Escherichia coli, with zones of clearance of 2.8 mm
and 2.5 mm, respectively, before washing as per the
AATCC test method in Table 1. Figure 2 shows how
the zone of clearance reduces only by few millimetres
after 10 washes.
In the AATCC 100 test method, the fabric showed
very a high percentage of reduction in bacteria at
99.99% and 92.71%, respectively, for the two test
organisms used (Table 2). The rate of antimicrobial
activity showed a marginal fall of 3.47% and 7.99%
after five washes and 10 washes, respectively, against
Staphylococcus aureus, and 3.59% and 6.71% after
five washes and 10 washes, respectively, against
Escherichia coli as clearly shown in Figure 3.
The copper oxide nanoparticles used in this work
have been found to be about 50 nm in size, and cotton
fibers are known to be around 5 nm in width. Figure 4
shows an SEM micrograph of microencapsulated
copper oxide nanoparticles on the treated cotton
fabric surface. It was demonstrated that copper oxide
nanoparticles are well distributed on the cotton
fabric surface.
The XRD patterns for both the treated and control
fabrics are shown in Figure 5. The results indicated that
compared with the control fabric, the nanoparticle-
coated fabric showed modified peaks.
Traditionally, the broadening of the peaks in the
XRD patterns of solids is attributed to particle size
effects.17 The broadening of peaks was observed
mainly due to the nanosize effect. Considering that
the microencapsulated copper oxide nanoparticle-
coated fabric is intended for use mainly for its func-
tional property of antimicrobial resistance, its slightly
decreased resistance to mechanical forces may not
really be a disadvantage. Hospital wear, for example,
for which this coated fabric would be ideally suited, will
normally be passed through a much smaller life-cycle
Table 2. Antimicrobial activity of cotton fabric containing
copper oxide nanoparticles against microorganisms by AATCC
100 test method

Table 1. Antimicrobial activities of cotton fabric containing Bacterial colonies after

copper oxide nanoparticles by AATCC 147 test method 24 h (cfu/ml) Antibacterial
activity
Zone of Clearance Control Treated (% Bacterial
Sample No. Test Organism in mm Test organism sample sample reduction)
1. Staphylococcus aureus 2.8 Staphylococcus aureus 03  107 09  102 >99.99
2. Escherichia coli 2.5 Escherichia coli 07  107 51  105 92.71

Figure 2. Antimicrobial activity of cotton fabric finished with microencapsulated copper oxide nanoparticles (AATCC 147).

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1086 Textile Research Journal 81(10)

Figure 3. Antimicrobial activity of cotton fabric containing copper oxide nanoparticles against microorganisms (AATCC 100).

Control fabric Coated fabric

Figure 4. SEM micrograph of microencapsulated copper oxide nano particles on cotton fabric.

Figure 5. XRD analysis of the control and nanoparticle-treated fabric.

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Anita et al.
Table 3. Physical characteristics of the uncoated fabric and fabric coated with micro-encapsulated copper oxide nanoparticles
S. No Physical Properties Uncoated fabric
1. Tensile strength Warp: 197 N
Weft: 222 N
2 Tear strength Warp: 3584 g (35.1 N)
Weft: 6003 g (58.8 N)
3. Resistance to abrasion No breakdown of the
specimen up to 15,000 rubs
4. Pilling rating 125 cycles 4–5 (slight surface fuzzing to no change
500 cycles 4 (slight surface fuzzing)
1000 cycles 4 (slight surface fuzzing)
2000 cycles 4 (slight surface fuzzing)
compared with that for a regular garment meant for
everyday use. The big advantage of the coated fabric
is the fact that it displays excellent resistance to bacte-
ria, a factor of prime importance for hospital wear.
The physical properties of the micro-encapsulated
copper oxide nanoparticle-coated fabric (Table 3) indi-
cate that the coated fabric retains 95% and 100%,
respectively, of its original warp-way and weft-way
tensile strength. The fabric also suffers a drop in tear
strength, the corresponding fall being 7% and 6%,
respectively, for the two directions of test. It is likely
that the nanoparticles reduce the free movement of the
cotton fibers in the fabric during the mechanical action
resulting from the tensile or tearing tests. This would
cause a reduction in the load-bearing elements at any
given time during the tests. The overall effect is to
reduce mechanical performance.
The abrasion resistance is similar to the unfinished
fabric. There is only a minimal change in the pilling
resistance. Thus the general mechanical behavior of
the coated fabric appears to be only marginally
reduced.
From the Table 3, it is found that the control fabric
and copper oxide nanoparticle microcapsule-finished
fabrics showed significant difference in the physical
properties when tested by standard methods.
Conclusion
In conclusion, it may be stated that the application of
microencapsulated copper oxide nanoparticles to
cotton fabric imparts the functional property of excel-
lent antibacterial resistance. The mechanical properties
of the fabric appear to be reduced, but this will not
diminish the overall performance of the fabric for the
specific use of antimicrobial wear. Similarly, the anti-
bacterial activity of the fabrics was also highest for the
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1087
Fabric coated with micro-encapsulated
copper oxide nanoparticles
Warp: 189 N
Weft: 220 N
Warp: 2624 g (25.7 N)
Weft: 4464 g (43.7 N)
No breakdown of the specimen
up to 15000 rubs
4 (slight surface fuzzing)
4 (slight surface fuzzing)
3–4 (Moderate to slight surface fuzzing)
3–4 (Moderate to slight surface fuzzing)
microcapsule-finished fabric compared with the
control fabric.
The inherent properties of the textile fibers provide
room for the growth of microorganisms. In addition,
the structure of substrates and chemical processes may
induce the growth of microbes. Humid and warm envi-
ronment further aggravate the problem. Infestation by
microbes causes cross-infection by pathogens and odor
development when the fabric is worn next to skin. With
this regard, the above research work was carried out to
develop antimicrobial resistant fabric where copper
oxide nanoparticles were prepared by a wet chemical
method, microencapsulated by an ionic gelation
method, and antibacterial activity was tested after
application on to cotton fabric. A higher antimicro-
bial activity was observed against Staphylococcus
aureus and Escherichia coli by both AATCC 100 and
147 methods. When the wash durability of the micro-
capsule-finished fabric was tested, the results showed
better antibacterial activity than the copper oxide nano-
particles finished by the pad–dry–cure method on the
cotton fabrics. The SEM analysis and the XRD analy-
sis revealed that the size of the nanoparticles synthe-
sized was about 50 nm and additional chemical groups
substituted in the treated fabric, respectively. The phys-
ical characteristics of the copper oxide nanoparticle-
coated fabric were compared with the control samples
and the results indicated that the coating did not bring
about major changes in the fabric characteristics.
Funding
This research received no specific grant from any funding
agency in the public, commercial, or not-for-profit sectors.
Conflict of interest
The authors declare that they have no conflicts of interest.
1088
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