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Fabrication of photocatalytic TiO2 nanoparticle film on PET fabric by hydrothermal method

Hui Zhang, Hong Zhu and Runjun Sun
Textile Research Journal 2012 82: 747 originally published online 19 October 2011
DOI: 10.1177/0040517511424526
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Original article
Fabrication of photocatalytic TiO2

nanoparticle film on PET fabric
by hydrothermal method
Textile Research Journal

82(8) 747754
! The Author(s) 2012
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DOI: 10.1177/0040517511424526
trj.sagepub.com
Hui Zhang, Hong Zhu and Runjun Sun
Abstract
A layer of TiO2 nanoparticle was immobilized on PET fiber using titanium sulfate and urea under hydrothermal condition.
The TiO2-loaded fiber was characterized by scanning electron microscopy, X-ray diffraction, infrared spectroscopy,
thermal gravimetry and differential scanning calorimetry analysis, respectively. PET fabric before and after treatment
was also examined for the reflectance spectrum, tensile properties, water absorption and degradation of methyl orange
dye under UV irradiation. The results show that pure anatase nanocrystalline TiO2 is precipitated in the presence of PET
fabric and deposited on the surface of fiber via the hydrothermal process. The thin film is constituted of sphere
nanoparticles of an average size 3.0 nm, which is grafted onto the fiber surface by chemical reaction. For the TiO2coated fiber, the onset decomposition temperature decreases, but the exothermic temperature increases as compared
with the untreated fiber. Owing to the shrinkage of fabric size, the breaking load and tensile strain in warp and weft
directions increase. The TiO2-loaded PET fabric can absorb more ultraviolet radiation even after being washed for 30
times. The water absorbency is also slightly increased. The capability of photocatalytic degradation of methyl orange dye
is obtained.
Keywords
PET fabric, hydrothermal method, TiO2 nanoparticle
Introduction
Among various methods for the preparation of titanium dioxide (TiO2) photocatalyst, including the thermal hydrolysis, the sol-gel, the template process, the
chemical-precipitation, the thermal oxidation and the
microemulsion process, the hydrothermal processing
is a simple and eective synthesis technique.1,2 The
resulting TiO2 particles have the desired size and
shape with homogeneity in composition as well as a
high degree of crystallinity.3 Its most important feature
is that it favors a decrease in agglomeration among
particles, narrow particle size distribution, phase homogeneity and controlled particle morphology.4 It has
been reported that the structure and morphological
characteristics of TiO2 particles are markedly inuenced by the process conditions. The shape, size, crystalline form, photocatalytic activity and some relevant
properties of TiO2 particles can be controlled by altering the reaction temperature and time, the pH, the ratio
of reactants and so on.5 The precursors for the fabrication of TiO2 particles are mainly focused on titanium
trichloride (TiCl3), titanium tetrachloride (TiCl4), titanium metal, organic titanate, titanium sulfate
(Ti(SO4)2) etc.2 The common crystalline forms of
TiO2 include anatase, rutile and brookite. Rutile is
the only stable form and has a high dielectric constant
and refractive index. The anatase phase has high photocatalytic activities. Both anatase and brookite are metastable and transform to rutile when they are heated.6
Some researchers have carried out the synthesis of TiO2
by the hydrothermal method. For instance, nanosized
School of Textile and Materials, Xian Polytechnic University, China.

Corresponding author:
Hui Zhang, School of Textile and Materials, Xian Polytechnic University,
Xian 710048, China
Email: hzhangw532@xpu.edu.cn
748
Textile Research Journal 82(8)
TiO2 catalysts with high photocatalytic activity under

visible light irradiation were obtained by using acetone,
alcohol and pyridine as the solvent under the hydrothermal conditions.7,8 They could also be obtained by
using titanium sulfate and urea as the raw materials and
EDTA as the control agent,9 or titanium oxysulfate as
the precursor and urea as the precipitation agent,10
or the low-cost meta-titanic acid as the starting reactant and the monacid as the dressing agent.11
Nanocrystalline TiO2 particles co-doped with N, Fe
or Si were prepared using tetrabutyl titanate as the precursors,12,13 or using titanium oxysulfate as the precursor.14 The pH conditions had a great eect on the
quantity of the surface hydroxyl absorbed by the synthesized powders.15 The dispersion of the prepared
nanoparticles could be greatly improved by using tetraethylammonium hydroxide as the solvent.16
Although nanocrystalline TiO2 shows a wide range
of applications in gas sensors, photovolatic cells and
photocatalysis, the dispersion of nanoparticles with a
narrow size distribution is very important for producing the advanced functional materials.17,18 Nanosized
particles are liable to agglomerate among them due to
their large surface area per unit mass and high specic
surface energy. The recovery and reuse of waste nanoparticles are usually restricted in the practical application. Therefore, development of TiO2 based
photocatalysts anchored to supporting materials with
large surface areas would be of great signicance. It can
not only avoid the disadvantages of ltration and suspension of ne photocatalyst particles, but also lead to
high photodecomposition eciency.19 More recently,
TiO2 has been extensively explored as a coating material for textiles to provide functions such as antibacterial activity, UV protection, and self cleaning.
Immobilization of TiO2 (or Au/TiO2) clusters on dierent textiles has been currently realized showing the formation of rutile or anatase crystals of small dimensions,
stably grafted onto ber surfaces.19,2023 For example,
in order to obtain the self-cleaning activity eect under
visible light irradiation, cotton textiles were rstly activated by RF plasma, MW plasma and UV irradiation
respectively, and then (or directly) were immersed in the
TiO2 colloidal suspension, followed by heating at high
temperatures in air. It has been demonstrated that the
contamination from dirt, stains, and harmful microorganisms attached on cotton bers can be eectively
removed upon daylight irradiation. Nanosized TiO2
was prepared by hydrothermal method at rst, and
then the woven glass fabric was dipped in the TiO2
suspension solution. Finally, the coated fabric was calcined at dierent temperatures. It was found that the
TiO2 particle lms coated on glass fabric, with high
photocatalytic activity for the NO oxidation, were
achieved.4 Dierent layers of TiO2 were also
immobilized on polypropylene fabric by the hydrothermal method so as to obtain the highly active buoyant
photocatalysts. It was conrmed that the degradation
of methyl orange dye solution under UV and visible
lights could be greatly improved compared with one
layer of anatase TiO2.24
Unfortunately, relatively little research is found in
the literature related to the TiO2-coated fabric with
photocatalytic activity prepared by the hydrothermal
method. In this paper, we synthesized TiO2 nanoparticles immobilized on a polyethylene terephthalate (PET)
ber surface to evaluate the potential applicability to
functional fabrics. Nanosized TiO2 was deposited in the
presence of PET fabric using titanium sulfate and urea
in the sealed aqueous solution. The morphology, microstructure, thermal stability and optical properties of
PET fabric before and after treatments were characterized by scanning electron microscopy (SEM), X-ray
diraction (XRD), Fourier transform infrared spectroscopy (FT-IR), thermal gravimetry (TG), dierential
scanning calorimetry (DSC) and UV-Vis reectance
spectroscopy. The properties of tensile, water absorption and photocatalytic degradation of methyl orange
were also investigated.
Experimental
Materials
The undyed plain woven PET fabric was used for precipitating TiO2 nanoparticles. The linear densities of
ends and picks were identical (7.3 tex). The numbers
of ends and picks were 410 and 290 per 10 cm, respectively. Chemicals including titanium sulfate (Ti(SO4)2),
urea ((NH2)2CO), acetone, anhydrous ethanol, methyl
orange dye, and distilled water were all of analytical
reagent grade.
Preparation of TiO2 nanoparticle film on PET fabric

The PET fabric was rst scoured with an aqueous solution of 200 g/L NaOH for 30 min at 60 C prior to use,
followed by rinsing with acetone and anhydrous ethanol solution at room temperature for 15 min, and then
was repeatedly washed, three times, with distilled water
at 60 C. The hydrothermal process was employed to
modify PET fabric in the laboratory. First, 19.2 g of
titanium sulfate was added to 160 mL of distilled
water, with vigorous stirring, at a temperature of
60 C. Subsequently, 9.6 g of urea was dissolved in the
above solution completely. At last, 2.4 g of pretreated
PET fabric was dipped in the mixture for 30 min, and
then was transferred to a 200 mL PTFE sealed can,
which was put into the stainless steel autoclave.
The autoclave was then placed in a furnace for the
Zhang et al.
749
hydrothermal treatment. The temperature was heated

to 200 C at a speed of 2 C/min. After treatment for 3 h,
the PTFE sealed can was cooled down to room temperature. The PET fabric was dried at 80 C for 5 min in
an oven, and then was dipped in the acetone and ethanol solution twice for 10 min, respectively, followed by
washing with distilled water for 10 min, and dried at
ambient condition. The weight of PET fabric before
and after treatment was measured by an AL54 analytical balance. The pick-up of TiO2 nanoparticles deposited on PET fabric, in weight, relative to the untreated
one was calculated.
Characterization and measurement

The surface morphologies of the samples were observed
with a JEOL JSM-6700 eld emission scanning electron
microscope. XRD patterns were obtained by using Cu
Ka1 radiation ( 1.540562 A), using a 7000 S diractometer at 40 kV and 40 mA with the angle of 2 from
10 to 80 at a scan speed of 8 deg/min. The mean crystallite size of the TiO2 crystallite formed on the surface
of PET fabric was determined by the Scherrer equation.
FT-IR spectra of the samples were recorded using KBr
pellets in the range of 4004000 cm1, using a Bruker
TENSOR 27 spectrometer. The thermogravimetric
analyses were carried out on a TGA/SDTA851e thermogravimetric/dierential thermal analyzer (TG-DTA)
instrument according to GB/T 13464-2008. Percentage
weight change versus temperature was evaluated at a
heating rate of 10 /min with a nitrogen ush rate of
10 mL/min over the range of 30550 C. DSC analyses
were performed in a Sapphire apparatus at a rate of
10 /min in owing nitrogen gas at 10 mL/min from
30 C to 600 C.
The reectance spectra of the samples in the 200
800 nm wavebands were tested at room temperature on
a U-3010 UV-VIS-NIR spectrometer with an integrating sphere (150 mm) at a scanning speed of 120 nm/
min. The tested sample was overlapped so that the
light could not transmit through the fabric sample.
The tensile properties of the samples were measured
on the YG(B)026D-500 electromechanical test instrument according to GB/T3923.1-1997. The initial
gauge length was 200 mm and the width was 50 mm.
The testing rate was 100 mm/min and the pre-tension
was 5 N.
The water absorption measurements were conducted
according to GB/T23320-2009 and were calculated
from equation (1).
Aw
mw mc
100%
mc
Where Aw is the water absorption (%), mw is the wet

fabric weight (g), and mc is the dry fabric weight (g).
Five samples were tested and the average of the measurements was given.
Photocatalytic experiments
The photocatalytic activities of PET fabric before and
after treatment were evaluated after exposure to UV
irradiation based on the decomposition of methyl
orange dye. The irradiation was carried out using
20 W (main wavelength 254 nm) quartz ultraviolet
lamp. 1.5 g of the fabric sample were dipped into
30 mL of methyl orange solution at a concentration of
20 mg/L at natural pH. The lamp was hung above the
solution at a distance of 10 cm. The absorbance of the
characteristic peak of methyl orange at the maximum
absorption wavelength (464 nm) was measured using a
UV-Vis
spectrophotometer
(Beijing
Rayleigh
Analytical Instrument Corp. UV-1600) at specic time
intervals. The degradation rate was calculated from
equation (2).
D
A0 At
100%
A0
Where D is the degradation rate (%), A0 is the initial

absorbance of the methyl orange solution, and At is the
absorbance of the methyl orange solution irradiated for
t minutes.
Results and discussion

SEM analysis
Figure 1 shows the scanning electron pictures of PET
bers before and after treatment with titanium sulfate
and urea. It can be seen that the surface of the
untreated PET ber is clean and smooth. A few small
particles are induced by the attached substances
(Figure 1a). When PET fabric was treated with titanium sulfate and urea by hydrothermal processing,
the surface of as-obtained ber is covered with a layer
of homogeneous granular materials. Some large particles in the micrometer scale are formed on the ber
surface because of the adhesion of agglomerated particles. The pick-up of TiO2 nanoparticle is 1.1% (w/w). A
number of pits can also be observed on the ber surface, which is etched by the caustic solution (Figure 1b).
From the high resolution SEM picture of PET ber, the
surface of the untreated PET ber is compact (Figure
1c). For the TiO2-coated ber, many irregular tiny particles are distributed on the ber surface. The average
particle size is larger than 100 nm in given growth condition (Figure 1d).
750
(a)
(b)
(c)
(d)
Figure 1. SEM pictures of the surface of PET fiber. (a) 5000 and (c) 30000 before treatment; (b) 5000 and (d) 30000 after
treatment with titanium sulfate and urea.
XRD analysis
FT-IR analysis
Figure 3 shows the FT-IR spectra of PET fabric before
and after treatment with titanium sulfate and urea. It is
(a) Untreated PET fabric

(101)
Intensity
Figure 2 illustrates the XRD patterns of PET fabric

before and after treatment with titanium sulfate and
urea. It is clear that the intense diraction peaks at
2 17.9 , 23.0 and 26.3 are due to the typical PET
phase. A series of characteristic peaks are observed in
the XRD pattern of the TiO2-coated PET fabric at 2
of 25.2 , 37.5 , 48.8 , 53.7 , 55.5 , 62.4 , 68.6 , 70.6
and 75.5 . These are related to the {101}, {004},
{200}, {105}, {211}, {204}, {116}, {220} and {215}
planes of TiO2 anatase structure (see Figure 2c).
From the width of the peaks at 2 25.2 , 37.5 and
48.8 , the crystallite sizes of the TiO2 particle are calculated to be 2.4 nm (101), 3.5 nm (004) and
3.1 nm (200) using Scherrers equation D K/cos
(where D is the diameter of the particle, is the Xray wavelength, is the FWHM (full width at half
maximum) of the diraction line, is the diraction
angle, and K is a constant 0.89), respectively. These
data imply that the shape of the TiO2 nanoparticle is
spherical and is quite dierent from the particle size
estimated in SEM observation because of the agglomerating of nanoparticles.
(b) PET fabric treated with

Ti(SO4)2 and Urea
(004)
(200) (105) (211) (204)
(116) (220) (215)
(c) Anatase TiO2

10
20
30
40
50
60
70
80
2q /
Figure 2. X-ray patterns of PET fabric (a) before and (b) after
evident that compared with the spectrum of the

untreated PET fabric (line (a)), the peaks at
3432 cm1 (C-H stretching vibration in benzene ring)
and 2966 cm1 (C-H stretching vibration of -CH2) are
negligible. The O-H band for the TiO2-coated fabric at
3129 cm1 is observed, which is attributed to the surface absorbed water induced by TiO2 nanoparticles.
Zhang et al.
751
a. Untreated PET fabric

1456
501
1577
1505
(b) TiO2coated PET fabric
2966
1341
Tsmittanceran/%
1410
1716
b. PET fabric treated with

Ti(SO4)2 and urea
1016
1236 1093
1505
1234
723
1017
1659
45.9C
4.13 mW
2000
1500
1000
500
100
Figure 3. FT-IR spectra of PET fabric (a) before and (b) after
120
Relative Mass/%
80
60
40
(c) TiO2 nanoparticle
(b) TiO2-coated PET fabric

Onset: 379.7C
Endset: 422.1C
Step: -81.6%
(c)

Onset: 376.7C
Endset: 416.5C
Step: -80.8%
20
0
100
200
300
(b)
(a)
400
endo
3.00 mW
250.8C
6.30 mW
Wavenumbers/cm-1
100
exo
618
1116
3000
463.4C
1.38 mW
418.5C
722
4000
251.2C
4.67 mW
1401
3129
532.8C
0.36 mW
872
Heat Flow/mW
3432
437.4C
0.46 mW
500
Temperature/C
Figure 4. TG curves of (a) untreated, (b) TiO2-coated PET

fabrics and (c) TiO2 nanoparticles.
The corresponding bending band at 1659 cm1 is identied. The peak at 1410 cm1 caused by the benzene
skeleton vibration is intensied and shifted to
1401 cm1. The peak at 1093 cm1 (COC anti-symmetrical stretching vibration) is also intensied and
shifted to 1116 cm1. At the same time, the new absorption band at 618 cm1 is observed, which is assigned to
the characteristic stretching vibration of Ti-O-Ti band
around 650 cm1.25,26 So this result proves that the
TiO2 nanoparticle is grafted onto the PET ber.
TG analysis
Figure 4 displays the TG curves of PET fabric before
and after treatment with titanium sulfate and urea. The
200
300
400
Temperature/C
500
600
Figure 5. DSC curves of (a) untreated and (b) TiO2-coated

PET fabrics.
TG curve of TiO2 nanoparticle is also given, which is

prepared by using the same method but without adding
the PET sample. This result agrees with that displayed
by Mohamed et al.28 It is obvious that there is only one
onset of decomposition temperature at 376.7 C for the
untreated PET fabric. The weight loss is 80.8% between
339.7 C and 455.5 C. For the TiO2-coated fabric, the
onset of decomposition temperature is increased to
379.7 C, but not distinctly. The corresponding weight
loss changes only a little (81.6%). This is ascribed to the
coating of TiO2 nanoparticles. So the hydrothermal
processing has little eect on the thermal properties
of PET ber.
DSC analysis
Figure 5 exhibits the DSC curves of PET fabric before
and after treatment with titanium sulfate and urea. It is
clear that a small endothermic peak at 45.9 C for the
TiO2-coated fabric is observed, which is mainly due to
the dehydration of absorbed water caused by TiO2
nanoparticle. Compared with the untreated PET
fabric, the endothermic peak at 250.8 C changed only
a little (251.2 C) when the PET fabric was treated with
titanium sulfate and urea. The melting enthalpies of
PET ber before and after treatment calculated by integration of the DSC curve in the temperature range
250 10 C are 10.2 J/g and 14.8 J/g, respectively. The
exothermic peaks at 418.5 C and 463.4 C are increased
to 437.4 C and 532.8 C, respectively. This signies the
thermal pyrolysis of PET ber and phase transition of
anatase TiO2 to rutile.27
752
Reflectance spectrum analysis
Tensile property analysis
Figure 6 represents the diuse reectance spectra of

untreated, TiO2-coated and washed (30 times) PET fabrics. The absorption peak at 304 nm for the untreated
PET fabric is assigned to the p!p* electronic transition in the benzene ring. The enhancement of UV
absorption capability for the TiO2-coated PET fabric
suggests that the TiO2 nanoparticle lm can absorb UV
irradiation and visible light to some extent. As compared with the untreated fabric, the average absorptances of the TiO2-coated fabric are increased by
10.0% in the UV (200400 nm) region, and 16.4% in
the Vis (400800 nm) region, respectively. This is due to
the band gap transition of TiO2 nanoparticles. When
the TiO2-coated fabric was washed for 30 times according to IWS TM31 standard, the average reectances are
slightly increased 3.6% in UV (200400 nm) region, and
9.3% in Vis (400800 nm) region with respect to the
TiO2-coated one. This implies that some TiO2 nanoparticles are washed o from the ber surface.
The fabric densities and tensile properties of PET fabric

before and after treatment are given in Table 1 in accordance with GB/T3923.1-1997. Because PET fabric was
treated at high temperature for a long time, the densities are increased from 410 to 436 per 10 cm in warp
direction, from 290 to 321 per 10 cm in weft direction,
respectively. The corresponding shrinkages are about
6.3% and 10.7% in warp and weft directions. The
breaking loads and tensile strains in both directions
are increased to some extent due to the shrinkage of
fabric size.
Water absorption analysis

The water absorption data indicates that as compared
with the untreated PET fabric, the water absorption of
the TiO2-coated fabric is slightly increased from 11.7%
to 13.9%. This is attributed to the TiO2 nanoparticle
lm loaded onto the surface of the PET ber. The
decreased distance between adjacent yarns also makes
a substantial contribution to the water absorption.
100
100
Degradation rate/%
80
Reflectance/%
80
60
(c) Washed PET fabric 30 times
40
20
0
200
60
40
20
0
0
300
400
500
600
Wavelength/nm
700
20
800
Figure 6. Reflectance spectroscopy of (a) untreated and (b)

TiO2-coated PET fabrics.
40
60
80
Irradiation time/min
100
120
Figure 7. Effect of irradiation time on the degradation rate for

(a) untreated and (b) TiO2-coated PET fabrics.
Table 1. The results of density and tensile properties of PET fabric before and after treatment with titanium sulfate and urea
Density/thread10 cm1
Breaking load/N
warp
weft
warp
weft
warp
weft
410
436
290
321
583.3
593.0
362.3
373.3
19.6
20.1
19.5
22.5
Tensile strain/%
PET fabric
Untreated
TiO2-coated
Zhang et al.
753
Photodegradation effect
Figure 7 shows the eect of UV irradiation time on the
degradation rate of methyl orange dye for PET fabric
before and after treatment. It is found that the degradation rate of methyl orange is gradually increased by
increasing the irradiation time for both fabric samples.
The TiO2-coated fabric possesses higher photocatalytic
activity than that of the untreated one. The degradation
rate of methyl orange is 87.8% for the untreated fabric
and 93.6% for the TiO2-coated fabric after being irradiated for 90 min. The experimental results demonstrate
that the TiO2 nanoparticles precipitated onto PET ber
accelerate the degradation of methyl orange under the
UV irradiation. Consequently, the preparation can be a
low-cost way of producing photocatalytic fabric loaded
with TiO2 nanoparticles, which provides a great opportunity for the treatment of industrial dye euents.
Conclusions
A thin layer of TiO2 nanoparticles was well precipitated
onto the surface of PET ber by the hydrothermal
method, using titanium sulfate and urea. From the
results of SEM and XRD, it is found that the lm of
TiO2 nanoparticles has the anatase phase. The TiO2
particle is constituted of the agglomerated nanoparticles with an average size of 3.0 nm or so. FT-IR results
show that the TiO2 nanoparticles are grafted onto PET
ber. TG and DSC results indicate that the thermal
stability of PET ber is decreased after being treated
with titanium sulfate and urea by the hydrothermal
process. The PET fabric loaded with the TiO2 nanoparticles exhibits an excellent UV absorption ability. Due
to the shrinkage of fabric size in warp and weft directions, the breaking load and tensile strain are increased
to some extent. The water absorption is slightly
increased. As far as the photocatalytic performance is
concerned, the TiO2-coated PET fabric has the prospect
for decontamination of dye in waste water.
Acknowledgement
This study was supported by the key discipline construction
of higher education of Shaanxi province (the special fund) in
China.
Funding
This research received no specic grant from any funding
agency in the public, commercial, or not-for-prot sectors.
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Textile Research

Fabrication of photocatalytic TiO2 nanoparticle film on PET fabric by hydrothermal method

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Fabrication of photocatalytic TiO2