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The fabrication of nanocomposite thin films with TiO2 nanoparticles by the layer-by-layer

deposition method for multifunctional cotton fabrics

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2010 Nanotechnology 21 325603

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IOP PUBLISHING NANOTECHNOLOGY
Nanotechnology 21 (2010) 325603 (8pp) doi:10.1088/0957-4484/21/32/325603

The fabrication of nanocomposite thin

films with TiO2 nanoparticles by the
layer-by-layer deposition method for
multifunctional cotton fabrics
Şule S Uǧur1,4 , Merih Sarıışık2 and A Hakan Aktaş3
1
Department of Textile Engineering, Süleyman Demirel University, Isparta 32260, Turkey
2
Department of Textile Engineering, Dokuz Eylül University, İzmir 35160, Turkey
3
Department of Chemistry, Süleyman Demirel University, Isparta 32260, Turkey

E-mail: sule@mmf.sdu.edu.tr

Received 7 December 2009, in final form 7 June 2010

Published 21 July 2010
Online at stacks.iop.org/Nano/21/325603

Abstract
A multilayer nanocomposite film composed of anatase TiO2 nanoparticles was fabricated on
cationically modified woven cotton fabrics by the layer-by-layer molecular self-assembly
technique. For cationic surface charge, cotton fabrics were pre-treated with
2,3-epoxypropyltrimethylammonium chloride (EP3MAC) by a pad-batch method. Attenuated
total reflectance Fourier transform infrared spectroscopy (FTIR), x-ray photoelectron
spectroscopy (XPS) and scanning electron microscopy (SEM) were used to verify the presence
of deposited nanolayers. Photocatalytic activities of the nanocomposite films were evaluated
through the degradation of red wine pollutant. Nano-TiO2 deposition enhanced the protection of
cotton fabrics against UV radiation in comparison with the untreated cotton fabrics. Air
permeability and whiteness value analysis was performed on the fabrics before and after the
treatment with TiO2 nanoparticles by the layer-by-layer deposition method. Tensile strength
tests of the warp and weft yarns were performed to evaluate the effect of solution pH value
changes during the alternate dipping procedures. For the first time the durability of the effect of
the self-assembled multilayer films on the cotton fabric functional properties was analyzed after
10 and 20 washing cycles at 40 ◦ C for 30 min.
(Some figures in this article are in colour only in the electronic version)

1. Introduction seemed to be suitable for deposition by the LbL method, but

The electrostatic attraction between oppositely charged
molecules provides an excellent basis for the creation of
nanolayer films. The sequential adsorption of oppositely
charged colloids was reported in a seminar paper in 1966 by
R Iler. Starting in the early 1990s, Decher’s group rediscovered
layer-by-layer (LbL) processing to fabricate multilayer thin
films from oppositely charged polyelectrolytes [1]. The LbL
process is based on the alternating adsorption of charged
cationic and anionic species. Most types of charged molecules,
nanoparticles, dyes, proteins and other supramolecular species
4 Author to whom any correspondence should be addressed.
generally polyelectrolytes have been employed [2–13]. That
any of these species in any order can be adsorbed layer by
layer is the greatest advantage of self-assembly. The oppositely
charged species are held together by strong ionic bonds and
form long-lasting, uniform and stable films, which are often
impervious to a solvent. Self-assembly is economical and
readily amenable to scaling up for the fabrication of large-
area defect-free devices on virtually any kind and shape of
surfaces [1–4].
The process begins by charging a substrate appropriately.
The charged substrate is then immersed in a dilute solution of
oppositely charged polyelectrolyte, for a time optimized for
the adsorption of a monolayer solution, then rinsed. Strong

0957-4484/10/325603+08$30.00 1 © 2010 IOP Publishing Ltd Printed in the UK & the USA
Nanotechnology 21 (2010) 325603
electrostatic attraction occurs between a charged surface and
an oppositely charged molecule in the solution. In principle,
the adsorption of molecules carrying more than one equal
charge allows for charge reversal on the surface. The next
step is the immersion of the one layer covered substrate into
a dilute dispersion of oppositely charged polyelectrolytes for
a time optimized for the adsorption of a monolayer, followed
by rinsing. In this way, an oppositely charged molecule is
adsorbed in a second step on the top of the first one. Both
adsorption steps can be repeated cyclically to form multilayer
structures on the surface of a substrate [1–5].
Multilayers containing nanoparticles have been studied
extensively for their potential use in various fields of science
(anti-static coatings for plastics, sensors, light emitting
diodes, fuel cells, polymer capsules etc), but only a few
studies have shown that the LbL process can be used
for textile materials. Hyde et al [12] examined the
possibility of creating polyelectrolyte thin film coatings
on textile materials by using the LbL deposition process.
Ding et al [14] fabricated self-assembled LbL ultrathin
hybrid TiO2 /PAA film coated CA nanofibrous mats by a
combination of electrospinning and electrostatic LbL self-
assembly techniques. Jantas and Polowinski [15] obtained very
thin polyelectrolyte nanolayers on PET fabric to change its
properties connected with the fiber surface. Dubas et al [16]
have demonstrated and characterized the possible deposition of
polyelectrolyte multilayer thin films assembled from cationic
poly(diallyldimethylammonium chloride) and scarlet dye onto
nylon fibers. Dubas et al [17] used the LbL process for coating
silk fibers with polyelectrolyte multilayer thin films to improve
their color fastness to washing. Polowinski [18] obtained
polymeric complex layers on polypropylene and polyester
non-woven fabrics via the LbL method. Chunder et al [19]
fabricated ultrathin fibers comprising poly(acrylic acid) and
poly(allylamine hydrochloride) by using the electrospinning
technique with the LbL process. Dubas et al [20] have
demonstrated coating of silk or nylon fibers with silver
nanoparticles for antimicrobial properties by following the LbL
method. According to the literature, nanoparticle multilayers
can be formed on textile fiber surfaces using the LbL process.
It is interesting to note that there is no report which investigates
the durability of multilayer films after washing procedures on
the textile materials.
The LbL process has opened the way for the easy
preparation of nanocomposite textile fibers, allowing the
preparation of functional textiles for protective clothing. The
LbL technique offers the possibility to tailor the surface
properties of textile fibers by depositing nanolayers of
polyelectrolytes, charged nanoparticles and non-reactive dyes
in a controlled manner.
The application of TiO2 nanoparticles to textile materials
has been the object of several studies aimed at producing
finished fabrics with different characteristics such as UV-
blocking, antibacterial and self-cleaning. The field of self-
cleaning coatings is divided into two categories: hydrophobic
and hydrophilic. Hydrophilic coatings chemically break
down dirt when exposed to light, a process known as
‘photocatalysis’. In recent years, interest in the photocatalytic
2
Ş S Uǧur et al
activity of anatase form TiO2 nanoparticles has been growing.
In the literature anatase titania thin films were prepared by
using relatively high temperature deposition methodologies,
such as chemical vapor deposition, sputtering, the sol–
gel process and dip-coating techniques. The formation of
photocatalytic titanium films at low temperature is important
for the fabrication of transparent films on textile substrates that
cannot withstand high temperature treatment [21–30].
In the present study, an attempt was made to improve
functional cotton fabrics by the deposition of anatase TiO2
nanoparticle multilayers. Cationic cotton was prepared by
a cationization process. Attenuated total reflectance Fourier
transform infrared spectroscopy (FTIR–ATR), scanning elec-
tron microscopy and x-ray photoelectron spectroscopy (XPS)
measurements were used to verify the presence of the deposited
nanolayers. The UV-protective and self-cleaning properties of
the fabrics connected with the character of the deposited TiO2
nanolayers were also tested. Air permeability, whiteness values
and tensile strength analyses were performed to examine the
LbL process effect on the cotton textile fabric properties. The
functional properties of multilayer films were analyzed after 10
and 20 washing cycles (40 ◦ C and 30 min).
2. Experimental details
2.1. Nanoparticle
Anatase titanium oxide nanoparticles (particle size < 25 nm,
specific surface area 200–220 m2 g−1 ) were purchased from
Aldrich and used for multilayer film composition as received.
The nanoparticle suspension was prepared at 40 W for 1 h by a
Sonics Vibra-Cell ultrasonic homogenizer. The concentration
of the suspension was adjusted to 0.1 wt%. The isoelectric
point of anatase TiO2 was at pH 4.7–6.2 [31]. To make cationic
and anionic TiO2 suspensions, the pH of the nanoparticle
suspension was adjusted to 9.0 and 2.5 by using HCl and
NaOH.
2.2. Substrate
Mercerized and bleached cotton woven fabric was used as the
substrate for the LbL process. The fabric properties were as
follows: plain woven; 138.84 g m−2 ; 56 thread cm−1 warp and
31 thread cm−1 weft; yarn count 50/1. The fabric was cut into
approximately 18 cm × 25 cm pieces before being chemically
pretreated to impart the cationic charges.
2.3. Substrate preparation
To impart cationic sites to the surface of the cotton
fibers, we used a chemical modification technique named
cationization [32]. Cationic cotton was prepared by us-
ing 2,3-epoxypropyltrimethylammonium chloride (EP3MAC).
EP3MAC was prepared in aqueous solution by react-
ing 3-chloro-2-hydroxypropyltrimethylammonium chloride
(CHP3MAC) with NaOH. EP3MAC reacts with the hydroxyl
groups of cellulose, creating cationic charges on the surface
of the sample. CHP3MAC, 65%, and NaOH crystals were
obtained from Aldrich. 100 g of CHP3MAC and 45.5 g of
Nanotechnology 21 (2010) 325603
NaOH were mixed into 200 ml of deionized water. This
solution was pad applied to the cotton specimens at 100% wet
pick-up and the fabric samples were kept for 24 h at ambient
conditions (20 ◦ C and 65% RH) in Ziploc bags. Cationized
cotton fabrics were dried in a commercial dryer at 60 ◦ C.
Random samples which were cut from the fabrics were dyed
with anionic dyes to ensure that the cationization process had
occurred.
2.4. Nanoparticle multilayer formation
For the multilayer deposition process, polypropylene transport
trays (20 cm × 30 cm) were used. In the deposition process,
the positively charged cotton fabrics were immersed into the
following solutions alternately for 5 min periods: (a) the
anionic TiO2 colloid solution; (b) the deionized water; (c) the
cationic TiO2 colloid solution; (d) the deionized water. This
deposition cycle was repeated until 10- and 16-layer TiO2 /TiO2
films were deposited on cotton fibers. Multilayer film coated
cotton fabrics were dried at 60 ◦ C and cured at 130 ◦ C for
3 min.
2.5. Characterization of nano-TiO2 deposited cotton fabrics
2.5.1. Fourier transform infrared attenuated total reflectance
(FTIR–ATR) measurements. A Bruker IFS 66/S FTIR
spectrometer was used to obtain the infrared spectra of surfaces
using an ATR sampler. The spectra were taken over a
wavenumber range of 4000–400 cm−1 with a resolution of
2 cm−1 at room conditions.
2.5.2. X-ray photoelectron spectroscopy (XPS) measurements.
XPS measurements were conducted using a SPECS spectrom-
eter with an Mg source and a spherical mirror analyzer working
in spectrum mode. The total pressure in the main vacuum
chamber during analysis was typically 4 × 10−7 Torr. The
chemical elements present on the samples were identified from
survey spectra. Survey scans were of the spectrum type with
an Mg Kα reference. The survey scans started at 1100 eV and
ended at 0.80 eV, taking 0.40 eV steps with a dwell time of
0.30 ms. High resolution scans were performed around peaks
of interest.
2.5.3. Scanning electron microscopy (SEM-EDS). A
QUANTA 400F field emission high resolution scanning
electron microscope (SEM) equipped with an energy
dispersive spectroscopic (EDS) microanalysis system was used
to examine the surfaces of woven cotton samples at an
acceleration voltage of 10 kV. The cotton fabric samples were
coated with 10 nm Au/Pd prior to SEM observation.
2.5.4. UV penetration and protection measurement. The
ability of a fabric to block UV light is given by the
ultraviolet protection factor (UPF) values. A UV Penetration
and Protection Measurement Systems Camspec M350 UV–
visible spectrophotometer (SDL/ATLAS) was used to obtain
the UPF value of the multilayered cotton fabrics according
to Australian–New Zealand Standard AS/NZS 4399:1996.
3
Ş S Uǧur et al
The Australian–New Zealand standard indicates a system of
classification of protective fabrics. UPF (ultraviolet protection
factor) ratings indicate how much the material reduces UV
exposure. For practical purposes UPF is used for rating
the protection given by clothing. A UPF value of 15–
24 is classified as good protection, 25–39 as very good
protection and above 40 as excellent protection against solar
UV radiation.
2.5.5. Air permeability measurement. A TexTest Instruments
FX 3300 Air Permeability Tester III instrument was used to
obtain the air permeability values of the untreated and nano-
TiO2 coated cotton fabrics at 100 Pa pressure according to the
EN ISO 9237 standard.
2.5.6. Whiteness value measurement. A Minolta 3600d
spectrophotometer was used to obtain the whiteness values of
the untreated, cationized and nano-TiO2 coated cotton fabrics
as the Stensby index using a D 65 light source to examine the
LbL process effect on the yellowing properties of the fabrics.
2.5.7. Tensile strength measurement. The mechanical tests
were performed on a Lloyd LR5K Plus electronic tensile
strength machine according to the EN ISO 2062 Standard. The
breaking strength and elongation of warp and weft yarns at
fracture were tested in this work. Twenty samples were used
for each test and the test results were evaluated with the SPSS
16.0 statistical analysis program.
2.5.8. Self-cleaning properties. The photocatalytic activity
of the nano-TiO2 coated cotton fabrics was determined by a
UV box with dimensions 45 cm × 45 cm × 60 cm. Cotton
fabrics were cut into 5 cm × 5 cm samples and labeled. The
red wine stains were introduced onto the cotton fabric using
a micro-syringe with 50 μl of neat red wine (grape wine
containing 10% alcohol). Fabric samples were placed in the
box and kept for 72 h under specific UV irradiation (Philips
TUW series UV-C lamp, 18 W, 254 nm wavelength, voltage
60 V, UVC radiation  Wuv-c 5,0, lamp current 0.37 A) with
air ventilation. The distance between the fabric samples and
UV lamps in the box was 40 cm. The fabrics’ self-cleaning
properties were determined according to the discoloration
change of the treated and untreated fabrics [33].
2.5.9. Washing procedure. Functional properties of nano-
TiO2 coated cotton fabrics such as self-cleaning and UV-
protective functions were analyzed after the LbL process. To
determine the durability of these functional properties, cotton
fabric samples were washed 10 and 20 times at 40 ◦ C for
30 min with a Gyrowash laboratory type washing machine.
The Gyrowash washing speed was 40 rpm. The multilayered
fabric samples were subjected to laundering according to
the EN ISO 20105-C01 standard test method, and AATCC
standard ECE detergent without optical brighteners was used
throughout the laundering cycles. A solution of detergent was
prepared with a concentration of 5 g l−1 . Then, the sample
was introduced into the laundry solution bath with a volume
of 125 ml. When a cycle was finished, samples were washing
twice with deionized water for 1 min.
Nanotechnology 21 (2010) 325603
Figure 1. XPS spectra for cationically charged woven cotton fabric.
Figure 2. XPS spectra for cationically charged woven cotton fabrics supporting 10 and 16 self-assembled layers of nano-TiO2 .
3. Results and discussion
X-ray photoelectron spectroscopy was used to examine the
surfaces of the woven cotton samples. Figure 1 illustrates
a survey spectrum of a cationized woven cotton fabric. As
expected, distinctive peaks at 283.95 and 530.11 eV indicate
the presence of carbon and oxygen, respectively. A trace
amount of N, generated during the cationization process, was
also detected at 399.6 eV. Figure 2 shows a survey spectrum of
10- and 16-layer TiO2 nanoparticle film supported cationized
cotton fabric substrates. Distinctive peaks at 283.95, 461.7
and 530.11 eV indicate the presence of carbon, titanium and
oxygen, respectively. With the LbL deposition process the
titanium peak shows increase in intensity with increase in layer
number.
Scanning electron microscopy was used to verify the
presence of the deposited nanolayers on cationized cotton
fabrics. Figure 3 shows SEM images of 10-layer TiO2
4
Ş S Uǧur et al
nanoparticle film supported cationized cotton fabric. TiO2
nanoparticles can be clearly seen on the fiber surfaces.
Figure 4 shows SEM images of 16-layer TiO2 nanoparticle
film supported cationized cotton fabric. The surface of the
cotton fibers appears to be covered by TiO2 nanoparticles,
and with the increase in the number of layers the nanoparticle
density increases too. The crystalline phase of anatase TiO2
remained unchanged in the resultant TiO2 film coated cotton
fibers, and nano-TiO2 film coated fibers showed rough surfaces
with grains due to the deposition of aggregated TiO2 particles.
SEM–EDS analysis was also performed to verify the
elemental composition of the deposited TiO2 nanoparticles on
the fiber surfaces. Figure 5 shows EDS survey spectra of
10- and 16-layer TiO2 nanoparticle film supported cationized
cotton fabric substrates. The titanium amount is determined
as 16.05% for 10-layer TiO2 nanoparticle film supported
cationized cotton fabric and 18.68% for 16-layer TiO2
nanoparticle film supported cationized cotton fabric on the
Nanotechnology 21 (2010) 325603 Ş S Uǧur et al

Figure 3. SEM images of cotton fabric coated with 10-layer nano-TiO2 .

Figure 4. SEM images of cotton fabric coated with 16-layer nano-TiO2 .

1.00 2.00 3.00 4.00 5.00 6.00 1.00 2.00 3.00 4.00 5.00 6.00

Figure 5. EDS spectra of (a) 10-layer TiO2 deposited cotton fabrics and (b) 16-layer TiO2 deposited cotton fabrics.

surface of the cotton fabrics. With the LbL deposition process
the titanium peak shows an increase in intensity with an
increase in layer number, similar to the XPS spectra. A trace
amount of N and Cl generated during the cationization process
was also detected in the EDS spectra of both multilayer TiO2
nanoparticle deposited fabrics.
The FTIR–ATR spectra of untreated, 10-layer and 16-
layer nano-TiO2 deposited cotton fabrics are shown in figure 6.
The untreated cotton fabric exhibited a number of FTIR
spectra absorption features. It can be seen that nano-TiO2
deposited cotton fabrics maintained the FTIR features of
untreated cotton fabric. For all samples a broad band between
3100 and 3700 cm−1 centered around 3360 cm−1 illustrated
characteristics of OH functional groups in cellulose. With the
LbL deposition process this band shows an increase in intensity
as the number of layers deposited increases, suggesting that
the hydroxyl functional groups were occupied with TiO2
nanoparticles. A strong adsorption band with a maximum at
1030 cm−1 is a result of the overlapping bands attributed to
functional groups of cellulose, namely the C–C, C–O and C–
O–C stretching vibrations. The same intensity increase is seen
in this band, too. A strong absorption peak around 450 cm−1
on the 10- and 16-layer nano-TiO2 deposited cotton fabrics’
FTIR spectra can be attributed to TiO2 nanoparticles.
The presence of nano-TiO2 nanoparticles on the cotton
fabric after the LbL process is verified with SEM, FTIR–
ATR and XPS analysis. Table 1 shows the UPF factors of
nano-TiO2 deposited cotton fabrics which were obtained from
UV–visible spectroscopy. The durability of the treatment to
repeated home laundering was evaluated by performing 10
and 20 washing cycles at 40 ◦ C for 30 min. For fabrics
with 10- and 16-layer nano-TiO2 deposited cotton fabrics the

5
Nanotechnology 21 (2010) 325603 Ş S Uǧur et al

Figure 6. FTIR spectra for a untreated cotton woven fabric and cotton fabrics coated with 10- and 16-layer nano-TiO2 .

Table 1. Rated UPF values of cotton fabrics coated with 10- and Table 2. Air permeability and whiteness values of untreated cotton
16-layer nano-TiO2 . fabric and cotton fabrics coated with 10- and 16-layer nano-TiO2 .
Rated UPF Air permeability Whiteness value
After 10 After 20 (m−2 s) (Stensby, D 65)
After coating washing cycles washing cycles Untreated fabric 56.68 85.549
TiO2 /TiO2 50+ 50+ 40 TiO2 /TiO2 10 layers 34.96 73.951
10 layers TiO2 /TiO2 16 layers 31.75 70.781
TiO2 /TiO2 50+ 50+ 45
16 layers
Table 3. Tensile strength of yarn from the untreated cotton fabric,
cotton fabrics coated with 10- and 16-layer nano-TiO2 .
UPF value is obtained as 50+. According to the AS/NZS Standard
4399:1996 standard test method the value of UPF > 40 Tensile strength Mean deviation Sig.
shows excellent protection against UV. The UPF values were Weft yarn Untreated fabric 4.12 0.87 0.016a
maintained after 10 washing cycles, but after 20 washing cycles Cationized fabric 4.22 0.62
the UPF values decreased to 40 and 45 for 10- and 16-layer TiO2 /TiO2 10 layers 4.39 0.79
nano-TiO2 deposited cotton fabrics, respectively. By the end TiO2 /TiO2 16 layers 3.69 0.38
Warp yarn Untreated fabric 5.05 0.69 0.000a
of 20 washing cycles, the UPF values decreased, but still they Cationized fabric 4.58 0.66
showed excellent UV protection. These results showed that TiO2 /TiO2 10 layers 4.11 0.78
layers deposited by the LbL deposition process had a good TiO2 /TiO2 16 layers 4.97 0.48
durability after washing cycles. a
Mean values are statistically significantly different with
Table 2 shows air permeability values and whiteness significance < 0.05 in the tensile strength between the control
values according to the Stensby index of untreated and and treated yarns.
multilayered fabrics. Air permeability tests showed that with
the increase in the number of layers, the air permeability values
of the fabric decreased. These results verified the presence of decreased statistically with cationization and LbL deposition
the deposited layers on the cotton fiber. The whiteness value of process.
the fabrics is decreased as the number of layers increases, too. Figure 7 shows the aspect of a red wine stain on 10-
Since the fabric tensile properties can be greatly affected and 16-layer nano-TiO2 cotton fabrics before and after 72 h
by solution pH value changes during the LbL process alternate Suntest visible light irradiation. In both cases for all samples, a
dipping procedures, 20 weft and warp yarns from the fabrics partial discoloration induced by light can be observed. This
were selected for tensile test. Table 3 shows the tensile strength means that wine stains are partially degraded on the nano-
of the untreated, cationized and 10- and 16-layer nano-TiO2 TiO2 deposited surfaces and will be more inclined to react to
deposited fabrics’ weft and warp yarns. The tensile strengths detergents during household washing.

6
Nanotechnology 21 (2010) 325603
Figure 7. Discoloration of red wine stains on the samples before irradiation and after 72 h Suntest irradiation.
4. Conclusions
In conclusion, we have demonstrated and characterized the
possible deposition of an anatase TiO2 nanoparticle assembly
onto woven cotton fabrics. Pre-treatment of the cotton samples
with 2,3-epoxypropyltrimethylammonium chloride was proven
to be an effective procedure to create cationic charges on
the fibers to initiate the multilayer assembly of nanoparticles.
FTIR–ATR, XPS and SEM–EDS verified the presence of the
nanocomposite multilayer films on the cotton fibers. The
crystalline phase of anatase TiO2 was retained in the resultant
nanocomposite multilayer film coated fibers. The fabrics
coated with the TiO2 nanoparticles exhibit attractive UV-
protection and self-cleaning properties, which could render
7
Ş S Uǧur et al
them useful in applications such as multifunctional or technical
textiles. The durability of the nanocomposite films after
washing cycles validates the feasibility of using the LbL
deposition process to develop potentially multifunctional
textiles for protective clothing and technical textiles.
Acknowledgments
This research work has been supported by research grants
from Süleyman Demirel University Scientific Research Project
1814-D-09. We would like to acknowledge Department of
Textile Engineering and the Department of Metallurgy and
Material Engineering of Dokuz Eylül University for their
technical support.
Nanotechnology 21 (2010) 325603
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