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Industrial Textiles

Influence of nano titanium dioxide finish, prepared by sol-gel technique, on

the ultraviolet protection, antimicrobial, and self-cleaning of cotton fabrics
K Sundaresan, A Sivakumar, C Vigneswaran and T Ramachandran
Journal of Industrial Textiles published online 12 September 2011
DOI: 10.1177/1528083711414962

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DOI: 10.1177/1528083711414962
dioxide finish, prepared jit.sagepub.com

by sol-gel technique, on
the ultraviolet protection,
antimicrobial, and self-
cleaning characteristics
of cotton fabrics

K Sundaresan1, A Sivakumar2, C Vigneswaran3

and T Ramachandran4

Abstract
The performance of ultraviolet (UV) protection, antimicrobial activity, and self-cleaning
characteristics of nano titanium dioxide (TiO2) with acrylic binder were assessed on the
cotton fabric using pad-dry-cure method. Titanium iso-propoxide was used as precur-
sor with two different mediums of water and ethanol to synthesize nano-sol by sol-gel
technique. The synthesized nano-sol-gel was then characterized by using Fourier trans-
form infrared (FTIR) spectroscopy, particle size analyzer (PSA), X-ray powder diffrac-
tometry (XRD), and scanning electron microscopy (SEM). The nano TiO2 finished
cotton fabrics were tested for ultraviolet protection factor (UPF), antimicrobial activity,
self-cleaning action, and physical properties. The wash fastness of TiO2 nano finished
cotton fabrics for 5th, 10th, 15th, and 20th washes was assessed and also their ultra
protection factor values and the percentage reduction in bacteria in each stage were
reported. The self-cleaning activity was assessed for 12 hours, 24 hours, and 48 hours
duration by exposing coffee stain on the specimen fabrics to sunlight. The TiO2 nano-
particles had 12 nm when ethanol medium was used and 7 nm for water. The smaller
nanoparticles had showed better results regards antimicrobial activity and self-cleaning.

1
Department of Textile and Apparel Technology, PSG Polytechnic College, Coimbatore, Tamil Nadu, India.
2
Department of Apparel Technology, PSG Polytechnic College, Coimbatore, Tamil Nadu, India.
3
Department of Fashion Technology, PSG College of Technology, Coimbatore, Tamil Nadu, India.
4
Karpagam Institute of Technology, Coimbatore, Tamilnadu, India.

Corresponding author:
C Vigneswaran, Department of Fashion Technology, PSG College of Technology, Coimbatore, Tamil Nadu,
India
Email: cvw@fas.psgtech.ac.in

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2 Journal of Industrial Textiles 0(00)

In case of UV-protection function it was found that the fabrics treated with 12 nm
nanoparticles exhibit higher UPF values than the fabric treated with 7 nm nanoparticles.
The durability of the imparted function was in the range of 32–36 washes for antimi-
crobial activity and UV-protection property.

Keywords
antimicrobial activity, pad-dry-cure, self-cleaning activity, titanium iso-propoxide, ultra-
violet protection factor

Introduction
Nanotechnology is one of the key technologies of the 21st century. It is used in all
fields including textile industries for medical, hygienic, and technical textiles. In the
recent years, consumers have become increasingly aware of the need for sunrays
protection. The ultraviolet (UV) radiation can lead to acute and chronic reactions
and damage, such as acceleration of skin aging and sunburn. Approximately 10%
of sun protection of the skin against the action of solar radiation is a relatively new
objective of textile finishing, since the textile does not always guarantee adequate
protection [1]. Thus, a special additional sun protection finish is applied in the form
of UV stabilizers. Atmosphere absorbs most of the noxious radiations emitted by
the sun, only 5% of the harmful radiations reach to the surface of the earth [2–4].
Sun emits three types of UV radiation UV-A, UV-B, and UV-C [5,6]. The visible
spectrum is approximately of the range from 400 to 700 nm in wavelength. UV-B
rays range from 280 to 320 nm and they are the primary concern for protection.
The UV-A rays range from 320 to 400 nm. The actual damage to human skin from
UV radiation is a function of the wavelength of the incident radiation and the
wavelengths of maximum danger to skin are 305–310 nm. Therefore to be useful in
protecting the wearers from solar UV radiation, textiles must demonstrate
effectiveness in the 300–320 nm range [5]. The ozone layer blocks the sun output
of UV-C and most UV-B radiations. The UV-B radiation that reaches the earth
surface poses the greatest danger for sunburn and skin damages [7]. Personal risks
can be largely averted by avoiding exposure to the sun during the middle of the day
by covering up with appropriate clothing, headgear, and sunglasses, and by using
sun protection factor (SPF) 30+ sunscreen. The UV absorbers are compatible with
dyes and these finishes can be applied by normal pad-dry-cure method between 30
and 40 g/L depending on the type of fiber and its construction [8,9].
The awareness of UV radiation of health and hygiene has increased the demand
for functional textiles or protective textiles. One of the approaches to improve the
UV-blocking property, antimicrobial activity, and self-cleaning activity of fabrics is
to coat the surface with nanoparticles [10,11]. Zinc oxide (ZnO) nanoparticles

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Sundaresan et al. 3

embedded in polymer matrices like soluble starch are a good example of functional
nanostructures with potential for applications such as UV protection [12,13]. Metal
oxides like titanium dioxide (TiO2) and ZnO UV blockers are more stable
compared to organic UV-blocking agents [14]. TiO2 and other ceramic materials
have an absorption capacity in the UV region of 280–400 nm and reflects visible
and infrared (IR) rays [15,16]. Hence, a common nanosize TiO2 and ZnO will
enhance the UV-blocking property due to their increased surface area and intense
absorption in the UV region [17,18]. Moreover, treating the fabric with nanosized
silver particles found to improve antibacterial properties [19,20]. To certain degree,
sterilizing effect are displayed by metallic ions and metallic compound. A part of
the oxygen in the air or water is turned into active oxygen by means of catalysis
with the metallic ion, thereby dissolving the organic substance to create a sterilizing
effect. The use of nanosized particles would help to maximize antibacterial activity
as the number of particles per unit area is higher. TiO2 is a photocatalyst, when it is
illuminated by light with energy higher than its band gaps, the electrons in titanium
dioxide will jump from the valence bond to the conduction bond [21, 22]. Several
articles have discussed the use of the photocatalytic property of TiO2 in the field of
textiles. A fabric treated with TiO2 could provide effective protection against
bacteria and the discoloration of stains due to the photocatalytic activity of
nano TiO2.
In the present work, Titanium iso-propoxide is synthesized into nano-sol by
sol-gel technique with water (T1) or ethanol (T2) as a medium. Two sets of nano-
particles were successfully synthesized. The synthesized nano-sol was then charac-
terized using the typical methods of FTIR, PSA, XRD, and SEM. These nano-sols
were then applied on to the sample fabrics using a pad-dry-cure method. Then, the
treated fabric samples were tested for the functions of antimicrobial activity, ultra-
violet protection factor (UPF), and self-cleaning activity as per American
Association of Textile Chemists and Colorists (AATCC) standard tests. The trea-
ted samples were also tested for the durability of the effect after repeated washes.

Materials and methods

Materials
The bleached cotton plain woven fabric was fabricated with 40 s Ne count in both
warp and weft, cloth set of 38 ends/cm and 38 picks/cm, fabric mass of 118 grams
per square meter and 122 cm fabric width. Titanium iso-propoxide (AR Grade,
molecular weight [mol. Wt]: 284.26) procured from M/s. Himedia Laboratories (P)
Ltd, Mumbai, was used as precursor. Lissapol-N nonionic was used as surfactant
for dispersion on nanoparticles in acrylic binder (Texacryl binder SLN). Deionized
water was used for the hydrolysis of titanium iso-propoxide and for preparation of
sol-gel solution.

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Table 1. Sol-gel nanosynthesis techniques

Conditions of syntheses Notation used

for the resultant
Precursor used Temperature Concentration nanoparticles

Procedure I Titanium iso- 30 C Deionized water T1
propoxide (TIP) as medium
Procedure II 75 C Ethanol as medium T2

Synthesis of TiO2 nano-sol using titanium iso-propoxide as precursor

The typical procedures carried out for the synthesis of TiO2 nano-sol-gel techniques
are given in Table 1 and synthesis methods are given below:
Procedure I: Nano-sol TiO2 with water was prepared at 30 C temperature by
mixing titanium iso-propoxide (1%) with 100 mL of water containing nitric acid
(1%) to prepare stock solution. The mixture was vigorously stirred at 500 rpm for
20 hours using magnetic stirrer prior to coating.
Procedure II: The TiO2 gel containing anatase particles was prepared as the
30 wt % hydrogen peroxide (H2O2) solution was added to the 10 mL of 1 mol/L
ethanol solution of titanium iso-propoxide. The ratio of H2O2: TIP was kept as
12:1. The ethanol was added to the obtained solution and the total volume of the
solution was adjusted to 100 mL, the solution was then heated at 75 C for 12 hours
in a closed vessel.

Characterization of nanoparticles
The nanoparticles were characterized for their size, shape, chemical, and physical
structures using the following techniques.
X-ray powder diffraction method (XRD). The crystallinity of the nanoparti-
cles was determined by XRD using a SHIMADZU–XRD 6000 advanced X-ray
diffractometer equipped with a Cu Ka radiation,  = 1.5406 Å source (applied
voltage 30 kV, current 30 mA). The dried particles were deposited as a randomly
oriented powder onto a plexiglass sample container, and the XRD patterns
were recorded at angles between 10 –80 , with a scan speed of 5 /minute,
sampling pitch of 0.02 , and preset time 0.24 second. The crystallite domain
diameters (D) were obtained from XRD peaks according to the Debye-Scherrer’s
equation [8,10].

0:89  
D¼ : ð2:1Þ
W  cos y

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Sundaresan et al. 5

Where;

 is the wavelength of the incident X-ray beam (1.54 Å for the Cu Ka),
y is the Bragg’s diffraction angle, and
W is the full width of the X-ray pattern line at half peak-height in radians.
Fourier transform infrared spectroscopy (FTIR). The make/model of the FTIR
spectrometer used was SHIMADZU–FTIR 8400 S, spectral range of
400—4,000 cm1. Spectra were collected with a resolution of 0.9–1.0 cm1 and
given as the ratio of 200 single beam scans to the same number of background
scans in pure KBr (IR grade supplied by Alrich). KBr was ground to a fine powder
and mixed with samples (2% weight by weight [w/w]).
Particle size analyzer (PSA). The size distribution of nanoparticles was deter-
mined using PSA (windox 5). The size of the nanoparticles was obtained through
PSA, using a Sympatec GmbH, NANOPHOX (0143 P). The nanoparticles measur-
ing duration was 150.10 second, temperature 27 C, laser power 75%, and measuring
range 1–1,000 nm.
Scanning electron microscopy (SEM). The fabric samples treated with the nano-
particles were mounted on a specimen stub with double-sided adhesive tape
and coated with gold in a sputter coater and examined with a SEM, Jeol Model
JSM-6360.

Coating of nano-sol/nanoparticles on textile substrate

The bleached 100% cotton woven fabric of plain weave, 38 ends/cm, 38 picks/cm,
and 118 g/m2 were used. Before coating, the fabric was dried at 100 C for 5 minutes
by using oven to remove the moisture content present in the fabric. The cotton
fabric was immersed for 1 minute in aqueous nano-sol with 1% acrylic binder in
padding mangle.
Fabrics were coated with the nanosolution in different concentration levels such
as 1.0%, 1.5%, and 2.0%. TiO2 nano-sol/nanoparticles were applied on the cotton
fabric using pad-dry-cure method. The nanoparticle solution was evenly coated by
using laboratory padding mangle machine, running at a speed of 15 m/min with a
pressure of 15 kg/cm2. After padding the cotton fabric was dried at 70 C for 5 min-
utes and cured at 130 C for 3 minutes using curing chamber.

Evaluation of antimicrobial activity

The antimicrobial properties of treated cotton fabrics were evaluated by quantitative
assessment method as per AATCC test method 100-2004. The test was carried out
with Staphylococcus aureus and Klebesiella pneumoniae. The percentage reduction of
bacteria by the 100% cotton fabric is reported as R, [8,10].

R ¼ 100ðB  AÞ=B ð2:2Þ

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Where;

R – percentage reduction,
A – the number of bacteria recovered from the inoculated, treated test specimen
swatches in the jar incubated for over 24 hours, and
B – the number of bacteria recovered from the inoculated, treated test specimen
swatches in the jar immediately after inoculation (at ‘0’ contact time).

Evaluation of UV protection
The in vitro method is used for assessing the UV protection of the cotton fabric as
per the AATCC-183 (2004) test method. It measures the transmittance or blocking
of UV radiation through fabrics by UV-vis spectrophotometer. The make/model of
the instrument used was Varian, Cary 5000, spectral range of 175–3,300 nm. The
UV profiles of the untreated samples were compared to the spectra collected from
the same fabrics treated with nanoparticles, and the effectiveness in shielding UV
radiation was evaluated by measuring the UV protection, transmission, and reflec-
tion. Each measurement is the average of four scans obtained by rotating the
sample by 90 . The transmission data was used to calculate the UPF, according
to the following equation [3,8]:
P400
280 E  S  
UPF ¼ 4P
00
ð2:3Þ
E  S  T  
280

Where;

E– relative erythemal spectral effectiveness,

S – solar spectral IR radiance in Wm–2 nm–1,
T – spectral transmission of specimen obtained from UV spectrophotometer
experiments, and
 – the band width in nm.

Washing fastness
The wash fastness of TiO2 nanocoating on fabric was tested by following AATCC
method 61 (1996) test no. 2 A using Atlas Launderometer LEF instrument. One wash in
the Atlas launderometer LEF is equivalent to five home machine launderings.

Evaluation of self-cleaning activity

The self-cleaning action/photoactivity of the TiO2-coated cotton fabric was inves-
tigated by a procedure of exposing the samples containing adsorbed coffee stain to

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Sundaresan et al. 7

visible irradiation. The measured quantity of 5% coffee solution was introduced on

the cotton fabric and was allowed to spread. One half of each stain on the fabric
was exposed to sun light for 12–48 hours, while the other half was covered with a
black paper to prevent its irradiation from sunlight. The exposed part of the stain
was compared with that of the covered part for self-cleaning action. Model/make
of the instrument Premier colour scan SS 5100 A spectrophotometer was used to
measure the photo degradation of coffee stain. The self-cleaning action was quan-
tified by comparing K/S values of the exposed and unexposed portions of the same
stain [10,14].

ðK=SÞunexposed ðK=SÞexposed
% decrease in K=S of exposed part ¼  100 ð2:4Þ
ðK=SÞunexposed

Where

K – absorption and
S – scattering.

Physical testing of fabrics

The physical properties of the 100% cotton woven fabric such as fabric weight
(American Society for Testing and Materials (ASTM) D3776:2009), tensile strength
and elongation (ASTM D 5035:2006), crease recovery (AATCC 66:2008), stiffness
(ASTM D1388:2008), air permeability (ASTM D737:2008), tearing strength (ASTM
D1424:2009), drape coefficient, thickness (ASTM D1777:2007), abrasion resistance
(ASTM D 3884:2009), and bursting strength (ASTM D3786:2009) of both untreated
and treated samples were evaluated after conditioning the specimens at 65% Relative
Humidity (RH) and 27  2 C for 24 hours by bringing them to approximate mois-
ture equilibrium in the standard atmosphere for preconditioning textiles as directed
in Practice D 1776 in an environmental chamber (ASTM 2008).

Results and discussion

Characterizations of TiO2 nano-sol/nanoparticles
The results and interpretations of the various characterization tests of the two types
of TiO2 nanoparticles synthesized using the procedures I and II were discussed.
These analytical tests include: FTIR, XRD, PSA, and SEM.

Fourier transform infrared spectroscopy (FTIR).

The Figure 1(a) shows the FTIR spectra of untreated cotton fabric sample. The
spectrum of interference pattern obtained for the (T1) TiO2 nanoparticles obtained

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Figure 1. Fourier transform infrared (FTIR) spectrogram of (a) untreated fabric sample, (b) T1
nano-sol synthesized by procedure I, and (c) T2 nano-sol synthesized by procedure II.

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Sundaresan et al. 9

Figure 2. X-ray powder diffractometry (XRD) pattern of T2 nanoparticles synthesized by

procedure II.

by the synthesis procedure I (using the hydrolysis of titanium iso-propoxide with

water at room temperature) is shown in Figure 1(b). The spectrum of interference
pattern obtained for the (T2) TiO2 nanoparticles obtained by the synthesis proce-
dure II (using the hydrolysis of titanium iso-propoxide with ethanol at 75 C for 12
hours) is shown in Figure 1(c). The Figure 1(b) and (c) clearly shows that the TiO2
absorption band is near to 432 cm1. The Figure 1(a), FTIR spectra from untreated
sample, did not show any peak at 432 cm1, which confirm the presence of TiO2 at
the treated samples. The peaks at 3,000 and 1,200 cm1 indicate the presence of –
OH and C = O residues, probably due to atmospheric moisture and CO2,
respectively.
X-ray diffraction (XRD). The spectra shows well-defined peaks typical of TiO2
in the crystal structure of titania, according to the Joint Committee on Powder
Diffraction Standard (JCPDS) card number 29-1360. The XRD spectra patterns of
TiO2 nanoparticles obtained using titanium iso-propoxide precursor sample with
ethanol (T2) as medium is shown in Figure 2. The XRD patterns of sample T1
showed six distinctive TiO2 peaks, the distinctive TiO2 peaks were at 29.91, 47.87,
56.94, and 74.79. The mean crystallite size of a powder sample was estimated from
the full width at half-maximum (FWHM) of the diffraction peak according to the
Scherrer’s equation. Both figures exhibit peaks similar to those reported for TiO2,
which suggests the formation of TiO2 nanoparticles in anatase form. The XRD
pattern for TiO2 nanoparticles obtained with water (T1) medium shows much
sharper peaks than the pattern (T2) with ethanol medium. This means that the
crystallanity is more for T1 than that of T2. The XRD nanoparticles sizes are given
in Table 2, the particles obtained for T1 had smaller size (7 nm) than T2 (12 nm).
Particle size analysis (PSA). The particle size distribution of nano TiO2 synthe-
sized were determined using PSA and are shown in the Figure 3(a) and (b), nano-
sol TiO2 water and nano-sol TiO2 ethanol, respectively. The nano particles
had 7 nm for T1 and 12 nm for T2 and the density distribution for the maximum
peak is 1.4.
Scanning electron microscopy (SEM). Figure 4(a) shows the SEM micrograph
of the untreated 100% cotton woven fabric. Figure 4(b) and (c) SEM micrograph
show the nanoscaled TiO2 particles on cotton samples. The nanoparticles are well
dispersed on the fibre surfaces in both cases and are finely dispersed and embedded.

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Table 2. Nanoparticles size analyzed by XRD

Sample code Particle size (nm) Full width half-maximum (b) 2y (deg)

TiO2 (water) 7 1.3292 53.60

TiO2 (ethanol) 12 0.3877 53.87
XRD: X-ray powder diffractometry, TiO2: titanium dioxide.

Figure 3. Particle size analysis of (a) T1 nanoparticles (water as medium) and (b) T2 nanopar-
ticles (ethanol as medium).

From Figure 4(b) it is possible to observe that T1 nanoparticles were more

uniformly distributed over the fabric surface than fabric coated with T2 nanopar-
ticles, Figure 4(c), where uneven and agglomerated patchy coating is seen due to
larger nanoparticles size. The particles size plays a primary role in determining their
adhesion to the fibres: it is reasonable to expect that the larger particle agglomer-
ation will be easily removed from the fibre surface, while the smaller particles will
penetrate deeper and adhere strongly into the fabric matrix.

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Sundaresan et al. 11

Figure 4. Scanning electron microscope (SEM) analysis of (a) untreated 100% cotton fabric,
(b) TiO2-treated 100% cotton fabric for T1 nanoparticle (procedure I), and (c) TiO2-treated 100%
cotton fabric for T2 nanoparticle (procedure II).

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Figure 5. Antimicrobial activity of cotton fabric.

Figure 6. Antimicrobial activity of fabrics after washing.

Functional testing of antibacterial activity

The Figure 5 shows the comparison of antimicrobial activity of the treated fabrics
as percentage reduction of bacteria (for the two representative types S. aureus and
K. pneumoniae) for the fabric samples treated with two sets of TiO2 nanoparticles,
such as T1, and T2, with different concentration levels with respect to fabric weight
such as 1.0%, 1.5%, and 2.0%. The TiO2 (T1) nanoparticles show marginally better
antibacterial activity when compared to TiO2 (T2) nanoparticles. A decrease in the
size of particles fundamentally results in increase in the surface area. This in turn
results is more antimicrobial activity for T1 (7 nm) than T2 (12 nm).
Functional testing of antimicrobial activity after a number of washes. The antimi-
crobial activity was tested for the first use and after the 5th, 10th, 15th, and the 20th
washes, which are shown in Figure 6. The results indicate that efficacy of the finish

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Sundaresan et al. 13

Table 3. Number of washes predicted using the forecast statistical analysis for antibacterial
activity

Particulars No. of washes 1% 1.5% 2%

Percentage reduction in bacteria Untreated 0 0 0

for fabrics treated with T1 0 74.2 75.8 77.6
nanoparticles 5 71.8 73.4 75.2
10 67.1 68.7 70.3
15 51.2 52.7 54.3
20 31.6 34.7 34.7
Predicted number of washes for T1 35 36 36
Percentage reduction in bacteria Untreated 0 0 0
for fabrics treated with T2 0 71.2 72.9 74.5
nanoparticles 5 68.8 70.5 72.1
10 63.7 65.4 67.0
15 46.2 48.4 49.9
20 28.2 29.9 30.5
Predicted number of washes for T2 32 34 34

is getting from 74.2% to 31.6% for the nano-treated TiO2 7 nm (T1) on the cotton
fabric, and from 71.2% to 28.2% for the nano-treated TiO2 12 nm (T2) on the
cotton fabric by increasing the number of washes. This fully confirms the concept
that the nanoparticles get bound to the fibre (and thus the fabric) surface on their
own because of their high surface energy. The large size nanoparticles possess less
surface energy than the small size nanoparticles and hence, the large nanoparticles
get released after less number of washes. T1 (water) fabric sample exhibits a better
value of antimicrobial activity compared to T2 (ethanol) fabric sample.
The FORECAST function is used to predict the number of washes for which
the fabrics will be completely devoid of any microbial activity. The details of the
prediction are given in the Table 3.

Functional testing of UV protection (UPF)

Figure 7 shows the values of UPF for the fabric sample (treated with the nano-
particles of TiO2) for UV-A (315–400 nm) and UV-B (280–315 nm) radiations.
These results show that the UPF values of the treated fabric had better UV pro-
tection than the untreated fabrics.
The 100% cotton fabrics treated with TiO2 nanoparticles of T1 shows lower
UPF values than the same fabrics treated with TiO2 nanoparticles of T2. According
to Raleigh’s scattering theory, the scattering of light is inversely proportional to the
fourth power of wavelength. The optimum particle size for scattering the radiation
is calculated as 15–40 nm. This clearly indicates that nanoparticles nearer to the

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Figure 7. Ultraviolet protection factor (UPF) values for the fabric samples.

Figure 8. Ultraviolet protection factor (UPF) values after a number of washes.

range of 15–40 nm exhibit better scattering of UV rays. Out of T1 (7 nm) and T2

(12 nm), T2 is closer to the above said range. And hence the UPF value for T2 is
more than T1.
Functional testing of UV protection after a repeated of washes. The test results of
the UV-protection testing for the first use, after 5th, 10th, 15th, and 20th washes
are shown in Figure 8. The results show that the UPF values of all the treated
fabrics had better UV protection, when compared to the untreated fabric. The
results indicate that the efficiency of finish were gradually reduced with the increase
in number of washes.

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Sundaresan et al. 15

Table 4. Number of washes predicted using the forecast statistical analysis for UPF values

Particulars No. of washes 1% 1.5% 2%

UPF value for fabrics treated Untreated 1.6 1.6 1.6

with TiO2 (T1) nanoparticles 0 43.3 44.5 44.8
5 42.6 43.7 44.0
10 36.8 38.5 38.9
15 26.3 28.5 28.8
20 17.5 18.5 18.8
Predicted number of washes for T1 32 33 33
UPF value for fabrics treated Untreated 1.6 1.6 1.6
with TiO2 (T2) nanoparticles 0 47.7 49.1 49.6
5 47.0 47.4 48.1
10 41.5 42.9 43.6
15 31.5 32.6 33.4
20 22.4 23.1 24.2
Predicted number of washes for T2 35 36 36
UPF: ultraviolet protection factor, TiO2: titanium dioxide.

From Table 4, it is clear that the predicted number of washes for (to reach
untreated UPF value of 1.6) TiO2 (T1) nanoparticles treated fabrics are found to
be 32, 33, and 33 for 1%, 1.5%, and 2% concentration levels. And TiO2 (T2)
nanoparticles treated fabrics are found to be 35, 36, and 36 for 1%, 1.5%, and
2% concentration levels.

Functional testing of self-cleaning activity

The self-cleaning property of TiO2-coated cotton textile is based on the highly
oxidative intermediates generated at the cotton surface. The mechanism of photo-
catalysis reaction in presence of these particles is well established and is reported by
many researchers. The K/S values (absorption to scattering coefficient) of exposed
and unexposed parts of the samples were measured after 0, 12, 24, and 48 hours. The
comparison of K/S values of different test sample are shown in Figure 9. The per-
centage decrease in K/S value for the exposed samples in comparison to unexposed
sample is measured to quantify the self-cleaning activity. The rate of degradation of
coffee stain is faster in first 12 hours of exposure. In the nanoparticles-coated
samples, no visual deterioration in the properties of cotton fabric is observed up
to 48 hours of exposure. The nanoparticles of smaller size have more surface area
and exhibits superior self-cleaning action. The smaller nanoparticles of T1 (7 nm)
show better self-cleaning activity than T2 (12 nm).The TiO2, which has a particle size
below 10 nm, was found to have higher self-cleaning activity. The sample coated with
nano-sol T1 shows a better photocatalytic activity then T2. As shown in Figure 9,

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Figure 9. Percentage decrease in K/S values of coffee-stained cotton fabric.

after the first 12 hours of exposure of the sample, it was observed that the decrease in
K/S value was nearly 68%.

Physical properties
The physical properties of cotton fabrics such as fabric weight, thickness, crease
recovery, drape coefficient, abrasion resistance, tensile strength, elongation, air
permeability, stiffness, and tearing strength of the untreated and TiO2-treated
cotton fabrics were analyzed as per AATCC and ASTM standard methods and
their test results are given in Table 5. The mechanical properties of cotton fabrics
do not detetoriate after finished with TiO2.

Conclusions
The nano TiO2-treated cotton fabrics were tested the important functional properties
viz. antimicrobial activity, UV protection, and self-cleaning activity. The durability
characteristics of the multifunctional treatments of the cotton treated fabrics were
studied. The influences of the surface treatment of nanoparticles on the mechanical
properties of the treated fabrics were examined.
The following conclusions have been drawn from the test results:

. In the synthesis of TiO2, water medium at 30 C yields nanoparticles of size 7 nm,
whereas ethanol medium at 75 C yields nanoparticles of size 12 nm.
. The FTIR analysis was carried out to analyze the presence of TiO2 on the cotton
fabric. The presence of an IR signature in the region 432 cm1 in the finished
product indicate the presence of TiO2 in the treated fabric. The PSA was used to
analyze the nanoparticles, which conforms that water medium give nanoparticles
of size 7 nm and ethanol medium of size 12 nm. The XRD spectra of the TiO2

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Table 5. Physical properties of untreated and TiO2-treated cotton fabrics

100% Cotton woven fabric

Treated cotton fabric

Sundaresan et al.

Untreated TiO2 (7 nm) T1 TiO2 (12 nm) T2

(JIT)

cotton
S.No Properties fabric 1.0% 1.5% 2.0% 1.0% 1.5% 2.0%
[27.8.2011–8:05am]

2
1 Fabric weight (g/m ) 118  2.68 119  3.12 119  3.14 120  2.94 119  3.10 120  2.98 120  2.98
2 Fabric 0.168  0.005 0.175  0.004 0.176  0.004 0.176  0.004 0.176  0.003 0.176  0.003 0.178  0.003
thickness (mm)
3 Crease recovery Warp 68.5  2.05 71.5  1.82 71.5  1.84 71.5  1.84 71.0  1.78 71.0  1.80 71.0  1.82
(angle) Weft 62.0  1.86 65.0  1.79 65.5  1.62 65.5  1.60 65.0  1.64 65.0  1.58 65.5  1.66
[1–19]
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4 Drape 50.4  1.50 59.2  1.68 59.2  1.62 59.4  1.70 58.8  1.61 59.0  1.66 59.0  1.70
coefficient (%)
5 Abrasion 6.1  0.18 5.8  0.16 5.8  0.16 5.62  0.12 6.0  0.18 5.9  0.19 5.8  0.17
resistance (%)
6 Tensile Warp 29.66  0.98 30.12  0.98 30.12  0.92 30.12  0.94 30.12  0.94 30.12  0.94 30.12  0.92
strength (kg) Weft 25.41  0.83 25.78  0.76 25.78  0.76 25.78  0.76 25.78  0.74 25.78  0.74 25.78  0.76
7 Elongation (%) Warp 11  0.34 11  0.33 11  0.33 11  0.33 11  0.34 11  0.33 11  0.32
Weft 13.30  0.39 13.30  0.38 13.30  0.39 13.30  0.39 13.30  0.40 13.30  0.39 13.30  0.39

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8 Air permeability 37.42  1.14 37.12  1.08 37.08  1.10 36.84  1.12 36.98  1.02 36.2  1.06 36.10  1.06
(cm3/cm2/sec)
9 Stiffness (cm) Warp 2.10  0.06 2.2  0.06 2.2  0.04 2.2  0.05 2.2  0.05 2.2  0.05 2.2  0.06
Weft 2.2  0.06 2.3  0.08 2.3  0.08 2.4  0.08 2.3  0.07 2.3  0.08 2.3  0.08
10 Tearing Warp 17  0.52 17.5  0.52 17.5  0.54 17.5  0.51 17.5  0.52 17.5  0.52 17.5  0.51
strength (kg) Weft 18  0.54 18.5  0.52 18.5  0.52 18.5  0.53 18.5  0.51 18.5  0.52 18.5  0.53
TiO2: titanium dioxide.
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nanoparticle were analyzed and the presences of well-defined peaks indicate the
crystalline structure.
. The particle size plays a primary role in determining their adhesion to the fibers.
It was observed that the larger particle agglomerates and were easily removed
from the fabric surface, while the smaller particle penetrate deeper and adhere
strongly into the fabric matrix.
. In the case of antimicrobial activity, the fabrics treated with smaller sized TiO2
nanoparticles (T1) 7 nm show better results than the fabrics treated with slightly
large sized (12 nm) TiO2 nanoparticles (T2). These results are due to the fact that
a decrease in the size of particles increases the surface area.
. In the case of UV-protection function, it was interesting to find that the fabrics
treated with slightly larger sized (12 nm) TiO2 nanoparticles (T2) have higher
UPF values than the fabrics that were treated with smaller sized (7 nm) TiO2
nanoparticles (T1).
. In the case of self-cleaning activity, the smaller nanoparticle size in situ coating of
TiO2 derived using sol-gel technique; nano-sol TiO2 (T1) show better self-cleaning
activity as compared to large nanoparticles of nano-sol TiO2 (T2).
. The UPF and antimicrobial activity increases enormously after TiO2 finishing
on cotton, when compared to untreated fabric and is retained until 10 washes;
beyond 15 washes there was deterioration in UPF values and antimicrobial
value. The durability of the imparted functions was in the range of 32–36
washes for antimicrobial activity and UPF value.

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Mr K Sundaresan The author is a postgraduate in tex-

tile technology from PSG College of Technology,
Coimbatore, Tamilnadu, India. He is having a teaching
experience of over 26 years in the areas of textile and
apparel technology for undergraduate students.
Presently, he is working as Head of the Department of
Textile and Apparel Technology, PSG Polytechnic
College, Coimbatore, Tamilnadu, India.

So far, he has published 20 technical research articles

in national journals and presented 5 technical articles
in the national- and international-level technical confer-
ences. He has also organized various national-level con-
ferences and workshops. His areas of specialization are weaving, fabric structure
and designing, and textile mill planning.

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