Functionalization of a Cotton Fabric Surface

with Titania Nanosols: Applications for

ARTICLE
Self-Cleaning and UV-Protection Properties
Noureddine Abidi,* Luis Cabrales, and Eric Hequet
Fiber and Biopolymer Research Institute, Department of Plant and Soil Science, Texas Tech University,
Lubbock, Texas 79403

ABSTRACT In this study, cotton fabric was successfully modified by titania nanosols prepared by means of the sol-gel process with
tetrabutyl orthotitanate [Ti(OC4H9)4] as the active ingredient. The cotton fabric was padded with the nanosol solution, dried at 60 °C,
and cured at 150 °C. Scanning electron microscopy showed the presence of a titania film on the fiber surface. The photocatalytic
properties of titania-nanosol-treated cotton fabric were investigated. The results showed that stains of coffee and red wine were
successfully decomposed by exposure of the stained fabric to UV radiation. Furthermore, titania-nanosol treatment imparted to the
cotton fabric a very good protection against UV radiation. The durability of the treatment was investigated by performing repeated
home laundering, and the results showed no effect of laundering on the UV-protection efficiency.

KEYWORDS: titania nanosol • functionalization • cotton fibers • sol-gel • modification • coatings • UV radiation

INTRODUCTION Daoud and Xin reported the successful nucleation and

I t has been reported that titania coatings exhibit a power- growth of anatase crystallites on cotton fabrics at low
ful photocatalytic activity (1-6). When illuminated, temperature (18-20). The precursor used for TiO2 particle
degradation of various organic compounds could be preparation was titanium tetraisopropoxide. The photocata-
achieved (7-15). This activity is attributed to the fact that lytic activity of the film formed on the fabric surface was
upon exposure to ultraviolet (UV) radiation (wavelength less investigated (2, 18). It was reported that coating with titania
than 385 nm) the photon energy generates an electron hole imparted UV protection, antibacterial performances, and
pair on the TiO2 surface (16, 17). The hole in the valence self-cleaning properties. Room temperature synthesis of
band can react with H2O or hydroxyl ions adsorbed on the rutile nanorods and their applications on cotton fabrics
surface to produce hydroxyl radicals, and the electron in achieved promising bactericidal photocatalytic activity and
the conduction band can reduce O2 to produce superperox- excellent protection against UV radiation (21).
ide ions (O2-). Both hydroxyl radicals and superoxide ions Meilert et al. used chemical spacers (succinic acid, 1,2,3-
are extremely reactive particles, and they can decompose propanetricarboxylic acid, and 1,2,3,4-butanetetracarboxylic
organic compounds upon contact with them. Therefore, acid) to attach TiO2 particles to cotton fabric surfaces (22).
functionalization of the cotton fabric surface with titania In this process, the spacers were attached on the cotton by
nanosols may have efficient antibacterial properties and the formation of ester bonds, which are then used to anchor
may exhibit self-cleaning and disinfecting properties.
TiO2 particles. The results showed that TiO2-coated cotton
Bozzi et al. reported that cotton fabric can be modified fabric possessed stable self-cleaning properties and allowed
by TiO2 at low temperature to impart self-cleaning properties
the partial elimination of the chromophore of the red wine
(1). For this purpose, cotton fabric was first activated by
under daylight radiation.
radio-frequency plasma, microwave plasma, and UV irradia-
Titania coating on cotton fabric also imparts UV-protec-
tion in order to introduce functional groups to anchor TiO2
tion properties (23, 24). This property is largely attributed
particles on the fabric surface. TiO2 colloidal particles were
prepared from titanium tetraisopropoxide (Ti[OCH(CH3)2]4) to the scattering effect of UV radiation by the TiO2 particles.
and titanium tetrachloride (TiCl4). The efficiency of the In previous work, we reported on the cotton fabric surface
treated fabric to decompose organic stains (red wine, coffee, modification to improve the UV-radiation protection using
make up, and grease) when exposed to UV daylight was the sol-gel process (25). Cotton fabrics were treated with
investigated. It was reported that the amount of CO2 gener- titania nanosols or titania-silica nanosols. These nanosols
ated from the organic stains increased with exposure time were prepared from tetraethyl orthotitanate [Ti(OC2H5)4] and
to UV daylight (50 mW/cm2). tetraethyl orthosilicate [Si(OC2H5)4]. The resulting titania-
nanosol-treated cotton fabric exhibited excellent and durable
UV-radiation protection. In this paper, we report on the
* To whom correspondence should be addressed. E-mail: [email protected].
Received for review May 11, 2009 and accepted September 3, 2009 efficiency of titania-nanosol-treated cotton fabric to decom-
DOI: 10.1021/am900315t pose organic stains. Titania nanosols were prepared from
© 2009 American Chemical Society tetrabutyl orthotitanate [Ti(OC4H9)4]. Treated cotton fabrics

www.acsami.org VOL. 1 • NO. 10 • 2141–2146 • 2009 2141

Published on Web 09/21/2009
 were stained with coffee and red wine and exposed to a UV- Scheme 1. Structure of Cibacron Red
radiation source for a specified period of time, and the stain
removal efficiency was evaluated.
ARTICLE

MATERIALS AND METHODS

Materials. The fabric used in this study was desized, scoured,
and bleached 100% cotton. The fabric characteristics were as
follows: 79.4 ends, 65.4 picks, yarn count of 23.4 × 22 tex, and
a weight of 161.98 g/m2 (4.8 oz/yard2). The chemicals used to
prepare the sol were purchased from Fisher Scientific: tetrabutyl
orthotitanate [Ti(OC4H9)4], ethanol (C2H5OH), and hydrochloric
acid (HCl; 37.7%). All chemical reagents were used as received. 4-5, and 5). Grade 5 means that there is no color difference
Titania-Nanosol Preparation. A total of 45 mL of Ti(OC4H9)4 between the sample and the control; while grade 1 means that
was first mixed with 15 mL of absolute C2H5OH. C2H5OH was there is a drastic difference in color between the sample and
added dropwise with stirring. Upon completion of the C2H5OH the control.
addition, HCl was added until the desired pH (1.5, 2, 3.5, and Cibacron Dye Decomposition. Dye decomposition experi-
4.5) was reached, and the solution was stirred for 45 min. The ments were conducted as follows: A 0.1166 mM solution of
sol obtained was clear and homogeneous. Cibacron red (Ciba-Geigy, Greensboro, NC) in water was pre-
Fabric Treatment. Cotton fabric samples were dipped in the pared. The structural formula of Cibacron red is shown in
titania nanosol, soaked for 5 min, and passed through a two- Scheme 1. In a plastic cuvette, 0.05 g of fabric was weighed
roller laboratory padder (BTM 6-20-190) at a speed of 3.66 and 3.5 mL of the dye solution was added. The cuvettes were
m/min and an air pressure of 2.76 × 105 Pa. The padded fabric sealed with a plastic film and were exposed to UV light in a C5
samples were then dried at 60 °C for 10 min by passing through UV chamber (Ultraviolet Products, San Gabriel, CA). A 6 W long-
a Ben Dry-Cure Thermosol Oven (IT500 with 0.45 m working wave Spectroline E series lamp (Westbury, NY) was used. The
width) at 0.27 m/min to evaporate the solvent (C2H5OH) and lamp spectra ranged from 320 to 400 nm. The intensity at
then cured in the same oven at 150 °C for 5 min at a speed of 0.1524 m from the lamp was 9 W/m2 at 365 nm. Samples were
0.64 m/min. The samples were subjected to hydrothermal placed 0.1524 m below the lamp and exposed for a predeter-
treatment by boiling them in water for 1 h. Then, the samples mined amount of time (from 0 to 46 h). The absorption of the
were dried, ironed, and finally conditioned in a laboratory samples was measured using a Lambda 650 UV-vis spectro-
maintained at 65 ( 2% relative humidity and 21 ( 1 °C for at photometer (PerkinElmer, Shelton, CT) at 541 nm.
least 24 h before analysis was performed. Three replications UV-Protection Measurement. The UV-protection factor (UPF)
were performed. The percent add-on on the fabric was calcu- was measured using the SPF-290 analyzer equipped with an
lated as follows: % add-on ) (m - m0)/m0 × 100, where m is integrating sphere (Optometrics, Ayer, MA). This instrument is
the weight of the treated fabric and m0 is the weight of untreated equipped with an automated X-Y stage, allowing automated
control fabric. measurements. The UV transmission measurements were per-
Scanning Electron Microscope. A Hitachi scanning electron formed according to AATCC TM 183 (30). Three specimens (0.1
microscope (TM-1000, Hitachi, Japan) with an accelerating m × 0.1 m each) from each sample were scanned, and 12 scans
voltage of 15 kv was used to visualize the cotton fabrics. Cotton per specimen were acquired. The UPF (average of 12 scans) was
fabrics were placed on a carbon disk, and no coating was computed using the following formula: UPF ) ∑290400EλSλ∆λ/
performed prior to visualization. ∑290400EλSλTλ∆λ. In this equation, Eλ corresponds to the relative
Fabric Staining, Irradiation Procedure, and Evaluation Erythemal effectiveness, Sλ is the solar spectral irradiance, Tλ
of the Stain Removal Efficiency. The control sample and the is the average spectral transmittance, and ∆λ is the measured
titania-treated samples were stained with coffee and red wine wavelength interval in nanometers (290 nm e λ e 400 nm).
following the standard method AATCC TM 130 (26). The same Tests of the Durability of the Treatment to Repeated
procedure was used for the stains of Cibacron red F-B (Ciba- Laundering. The treated fabric samples were subjected to home
Geigy, Greensboro, NC) using a solution of 0.010 g of the dye laundering for up to 18 cycles according to AATCC TM 124 (31).
in 20 mL of water. The area stained on the fabric was marked. AATCC standard detergent without optical brighteners was used
After staining, the samples were conditioned at 65 ( 2% throughout the laundering cycles.
relative humidity and 21 ( 1 °C for at least 24 h and exposed
to simulated sunlight radiation (Q-Sun Xe-3-HS, Q-Lab OH). The RESULTS AND DISCUSSION
light intensity was 0.72 W/m2 at 420 nm. The relative humidity Figure 1 shows the morphological changes induced by
in the chamber was maintained at 50% and the temperature treatment with titania nanosols prepared from Ti(OC4H9)4.
at 47 °C. The samples were conditioned again at 65 ( 2%
relative humidity and 21 ( 1 °C for at least 24 h before analysis. In contrast to the scanning electron microscopy (SEM)
All color measurements were performed using a Macbeth micrograph of untreated cotton fabric (Figure 1A), the
spectrophotometer (EC3000). The untreated and unstained micrograph of the cotton fabric treated with titania nanosols
control fabric was used as the standard for color measurements. shows white particles deposited on the fiber surface (Figure
A white Macbeth reference ceramic tile in reflectance mode was 1B). At higher magnification, the formation of a thin layer
used for the calibration. Measurements were taken from the
marked stained area in a large area view (0.0254 m in diameter) of titania is observed on the fiber surface (Figure 1D). The
with standard illuminant C and at a 2° observer angle. UV light percentage add-on of the titania on the fabric surface was
was excluded, and the specular components were included. 16%.
Color differences between the control sample and the stained The effect of the pH of the nanosol solution was first
samples are reported as ∆Ecmc and AATCC gray scale for staining investigated. Cotton fabrics were treated with different
(GS) (27-29). ∆Ecmc is a single number that represents the
number of Color Measurement Committee (CMC) color differ- nanosol solutions with pH 1.5, 2, 3.5, and 4.5. Stains of
ence units of a trial from a standard. The AATCC GS for color Cibacron red dye were made on the treated cotton fabric
change is composed of 10 grades (1, 1-2, 2, 2-3, 3, 3-4, 4, and exposed to UV radiation (0.72 W/m2) for different

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 ARTICLE
FIGURE 1. SEM images of (A) untreated fabric at 150×, (B) titania-nanosol-treated fabric at 150×, (C) untreated fabric at 3000×, and (D)
titania-nanosol-treated fabric at 3000×.

FIGURE 2. Decomposition of the Cibacron red dye stain: Effect of FIGURE 3. Evolution of ∆Ecmc as a function of the exposure time to
the pH of the nanosol solution on ∆Ecmc. UV radiation: (A) control fabric with no stain; (B) control fabric
stained with coffee; (C) titania-nanosol-treated fabric stained with
periods of time (from 0 to 16 h). A Macbeth spectrophotom- coffee. The pH of the titania-nanosol solution was 2.
eter was used to measure ∆Ecmc as a function of the exposure receive any treatment, was used as a control. The stained
time to UV radiation (Figure 2). The analysis of variance fabrics and the control fabric were exposed to UV radiation
shows significant effects of the pH [F(1,4) ) 948.32, p ) (0.72 W/m2) for different periods of time (from 0 to 46 h). A
0.000 001] and the exposure time [F(1,6) ) 239.97, p ) Macbeth spectrophotometer was used to measure the AATCC
0.000 001] on ∆Ecmc. There is also significant interaction of GS and ∆Ecmc as a function of the exposure time to UV
pH × exposure time. The nanosols prepared with a pH of radiation. The evolution of ∆Ecmc of the coffee stain is shown
1.5 provide the best results (after 16 h of exposure to UV in Figure 3 for a fabric treated with Ti(OC4H9)4 nanosols and
radiation, ∆Ecmc is 1.89). However, some of treated samples the control fabrics. The results presented in this graph are
showed signs of degradation. Therefore, we decided to work the average of three replications. Overall, there is a decrease
with a pH of 2. of ∆Ecmc with increasing exposure time to UV radiation. The
The photocatalytic activity of titania nanosols deposited analysis of variance shows a significant effect of the treat-
on the fabric surface was investigated. For this purpose, ment and exposure time (Table 1). There is also a statistically
stains of coffee and red wine were made on untreated and significant interaction of treatment × exposure time. ∆Ecmc
titania-nanosol-treated fabrics. Cotton fabric, which did not decreased from 28.0 at 0 h to 0.9 after 46 h of exposure to

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 Table 1. Analysis of Variance: Effect of the
Exposure Time to UV Radiation and Treatment on
∆Ecmc: (A) Control Fabric with No Stain; (B) Control
ARTICLE

Fabric Stained with Coffee; (C) Titania-Nanosol-

Treated Fabric Stained with Coffeea
∆Ecmcb

parameter df F probability A B C

intercept 1 12 972.47 0.000 001

treatment 2 2 891.68 0.000 001
treatment × 24 191.62 0.000 001
time FIGURE 4. Decomposition of the coffee stain: (A) nanosol-treated
time (h) 12 314.82 0.000 001 cotton fabric and stained with coffee before exposure to simulated
0 0.0 b 10.9 a 28.0 a sunlight; (B) sample A after exposure to simulated sunlight for 28 h;
2 0.2 ab 9.4 b 17.3 b (C) control white fabric with no treatment and no stain. The pH of
the titania-nanosol solution was 2.
4 0.2 ab 8.7 bc 11.5 c
6 0.2 ab 8.1 cd 9.3 d
8 0.3 ab 7.7 d 7.5 e
10 0.2 ab 7.4 de 6.4 ef
12 0.3 ab 7.2 de 5.5 fg
14 0.2 ab 7.1 de 6.0 f
18 0.4 ab 6.7 ef 4.3 ig
22 0.5 a 6.4 ef 3.1 i
30 0.4 ab 6.0 fg 3.1 i
38 0.6 a 5.5 gh 1.7 hi
46 0.6 a 5.1 h 0.9 j
error 78
a
df ) degrees of freedom; F ) variance ratio. b Values not
followed by the same letter are significantly different with R ) 5% FIGURE 5. Evolution of ∆Ecmc as a function of the exposure time to
(according to Newman-Keuls tests). UV radiation: (A) control fabric with no stain; (B) control fabric
stained with red wine; (C) titania-nanosol-treated fabric stained with
UV radiation. This corresponds to a 97% reduction, while red wine. The pH of the titania-nanosol solution was 2.
for the stained control fabric, ∆Ecmc decreased only slightly
(from 10.9 to 5.1). effect of the treatment with the titania nanosols on ∆Ecmc
It should be pointed out that ∆Ecmc is higher for the (Table 2). ∆Ecmc decreased from 12.6 at 0 h to 0.7 after 46 h
stained and titania-nanosol-treated fabric compared to the of exposure to UV radiation. This corresponds to a 94%
stained and control fabric. This is attributed to some type reduction, while for the untreated fabric, ∆Ecmc decreased
of chemical reaction between the stain and the titania only slightly (from 15.2 to 8.8). The AATCC GS increased
nanosols. The AATCC GS of the fabric stained with coffee from 2 before exposure to UV radiation to 5 after 46 h
before exposure to UV radiation was 2. After 46 h of exposure to UV radiation. These results suggest that the
exposure to UV radiation, the GS increased to 5. This titania nanosol coating prepared from the tetrabutyl orthoti-
indicates that there is no noticeable difference for the human tanate precursor imparts very good photocatalytic activities.
eye between the control (unstained white control fabric) and The change in the color of the white control sample
the titania-nanosol-treated cotton fabric that has been stained exposed to UV radiation was also measured. The result
with coffee and exposed to UV radiation for 46 h. showed a very minimal increase in ∆Ecmc from 0 to 0.6 after
Figure 4 shows the changes in color of the titania-nanosol- 46 h of exposure. This change in color could be due to the
treated cotton fabric stained with coffee. The picture in oxidation of cellulosic chains by UV radiation (32, 33).
Figure 4A shows the coffee stain on the titania-nanosol- Figure 6 shows the changes in color of the titania-nanosol-
treated cotton fabric before exposure to UV radiation. ∆Ecmc treated cotton fabric stained with red wine. The picture in
was 33.4, and the GS was 2. This level of coloration is very Figure 6A shows the red wine stain on the titania-nanosol-
dark and easily noticeable on the white cotton fabric. The treated cotton fabric before exposure to UV radiation. ∆Ecmc
picture in Figure 4B shows the fabric after 28 h of exposure was 13, and the GS was 2. This level of coloration is very
to UV radiation (0.72 W/m2). The values of ∆Ecmc ) 0.6 and dark and easily noticeable on the white cotton fabric. The
GS ) 5 mean that the human eye cannot distinguish picture in Figure 6B shows the fabric after 28 h of exposure
between this fabric and the control white fabric (the picture to UV radiation (0.72 W/m2). The values of ∆Ecmc ) 1.6 and
in Figure 4C). GS ) 5 mean that the human eye cannot distinguish
The evolution of ∆Ecmc of the red wine stain is shown in between this fabric and the control white fabric (the picture
Figure 5 as a function of the exposure time to UV radiation. in Figure 6C).
The results presented in this graph are the average of three To further test the efficiency of the photocatalytic proper-
replications. The analysis of variance shows a significant ties of treated fabric with titania nanosols, a Cibacron red

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Table 2. Analysis of Variance: Effect of the
Exposure Time to UV Radiation and Treatment on
∆Ecmc: (A) Control Fabric with No Stain; (B) Control

ARTICLE
Fabric Stained with Red Wine; (C) Titania-Nanosol-
Treated Fabric Stained with Red Winea
∆Ecmcb

parameter df F probability A B C

intercept 1 25 113.80 0.000 001

treatment 2 8 785.41 0.000 001
treatment × 24 145.38 0.000 001
time
time (h) 12 410.99 0.000 001
FIGURE 7. Decomposition of Cibacron red dye: (A) Cibacron red dye
0 0.0 b 15.2 a 12.6 a solution with no fabric; (B) Cibacron red dye solution containing
2 0.2 ab 11.2 b 7.1 b control white fabric; (C) Cibacron red dye solution containing cotton
4 0.2 ab 8.7 c 4.8 c fabric treated with titania nanosols and kept in the dark; (D)
Cibacron red dye solution containing cotton fabric treated with
6 0.2 ab 6.9 de 3.5 d
titania nanosols and exposed to UV radiation for different periods
8 0.3 ab 6.4 e 2.7 e of time.
10 0.2 ab 6.3 e 2.3 ef
12 0.3 ab 6.4 e 2.0 fg
14 0.2 ab 6.7 de 1.8 gh
18 0.4 ab 7.1 de 1.5 hi
22 0.5 a 7.5 d 1.2 ij
30 0.4 ab 8.7 c 1.7 gh
38 0.6 a 8.7 c 0.8 jk
46 0.6 a 8.8 c 0.7 k
error 78
a
df ) degrees of freedom; F ) variance ratio. b Values not
followed by the same letter are significantly different with R ) 5% FIGURE 8. Decomposition of Cibacron red dye: (A) Cibacron red dye
(according to Newman-Keuls tests). solution; (B) Cibacron red dye solution containing control white
fabric with no treatment and no stain; (C) Cibacron red dye solution
containing cotton fabric treated with titania nanosols and kept in
the dark: (D) Cibacron red solution containing cotton fabric treated
with titania nanosols and exposed to UV radiation for different
periods of time.

FIGURE 6. Decomposition of the red wine stain: (A) nanosol-treated

cotton fabric stained with red wine before exposure to simulated
sunlight; (B) sample A after exposure to simulated sunlight for 28 h;
(C) control white fabric with no treatment and no stain. The pH of
the titania-nanosol solution was 2.

dye solution was prepared and the titania-nanosol-treated

fabric was cut into small pieces and introduced into the dye FIGURE 9. Evolution of the UPF as a function of the laundering
cycles.
solution. The solution was then exposed to a source of UV
radiation for different periods of time as detailed in the
Materials and Methods section. A Cibacron dye solution and When the nanosol-treated fabric is immersed in the dye
a Cibacron dye solution containing a control fabric (un- solution and kept in the dark, the concentration of the dye
treated) were also exposed to UV radiation at the same time. did not change with time (Figure 7C). However, the concen-
The concentration of the dye in the solution was measured tration of the dye decreased when the solution containing
with a UV-vis spectrophotometer. The evolution of the nanosol-treated cotton fabric was exposed to UV radiation.
concentration of the dye in the solution as a function of the After 80 h of exposure, the concentration of the dye de-
exposure time is exhibited in Figure 7. The concentration creased by 83%. Figure 8 shows pictures of dye solutions
of the dye in the solution containing the control fabric (Figure after 80 h of exposure to UV radiation. The dye molecules
7A) did not show any change with the exposure time to UV in the solution containing titania-nanosol-treated fabric were
radiation. This is also true for the dye solution (Figure 7B). decomposed, resulting in a clear solution.

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 Finally, the efficiency of the titania-nanosol-treated fabric (10) Hsiao, C.-Y.; Lee, C.-L.; Ollis, D. F. J. Catal. 1983, 82, 418 –423.
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The UPF was measured. The analysis of variance showed a
ARTICLE
(12) Pelizzetti, E.; Minero, C.; Maurino, V.; Sclafami, A.; Hidaka, H.;
significant effect of the treatment on the UPF [F(1,1) ) Serpone, N. Environ. Sci. Technol. 1989, 23, 1380 –1385.
925.02, p ) 0.000 001]. The UPF increased by 571% (from (13) Pruden, A. L.; Ollis, D. F. Environ. Sci. Technol. 1983, 82, 404 –
417.
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by performing repeated home laundering (Figure 9). The (15) Xu, Y. M.; Menassa, P. E.; Langford, C. H. Chemosphere 1988, 17,
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CONCLUSION 1438.
A cotton fabric surface was successfully modified with (18) Daoud, W. A.; Xin, J. H. J. Sol-Gel Sci. Technol. 2004, 29, 25–29.
(19) Daoud, W. A.; Xin, J. H. Chem. Commun. 2005, 2110 –2112.
titania nanosols prepared from Ti(OC4H9)4. SEM images (20) Daoud, W. A.; Xin, H. J. Am. Ceram. Soc. 2004, 87 (5), 953–955.
showed the formation of a film on the fiber surface at (21) Fei, B.; Deng, Z.; Xin, J. H.; Zhang, Y.; Pang, G. Nanotechnology
relatively low treatment temperature (150 °C). The photo- 2006, 17, 1927–1931.
(22) Meilert, K. T.; Laub, D.; Kiwi, J. J. Mol. Catal. A: Chem. 2005, 237,
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101–108.
imparted self-cleaning properties to the cotton fabric. In- (23) Xin, J. H.; Daoud, W. A.; Kong, Y. Y. Text. Res. J. 2004, 74 (2),
deed, stains of coffee and red wine on the treated cotton 97–100.
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Acknowledgment. The authors thank the Texas Depart- (27) AATCC 173-2005. Technical Manual 2006; American Association
ment of Agriculture, Food and Fibers Research Grant Pro- of Textile Chemists and Colorists: Research Triangle Park, NC,
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(28) AATCC EP 7. Technical Manual 2006; American Association of
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