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DOI: 10.1177/00405175114245262012 82: 747 originally published online 19 October 2011Textile Research Journal

Hui Zhang, Hong Zhu and Runjun Sunnanoparticle film on PET fabric by hydrothermal method2Fabrication of photocatalytic TiO

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Original article

Fabrication of photocatalytic TiO2nanoparticle film on PET fabricby hydrothermal method

Hui Zhang, Hong Zhu and Runjun Sun

Abstract

A layer of TiO2nanoparticle 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 treatmentwas 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 TiO2is precipitated in the presence of PETfabric and deposited on the surface of fiber via the hydrothermal process. The thin film is constituted of spherenanoparticles of an average size 3.0 nm, which is grafted onto the fiber surface by chemical reaction. For the TiO2-coated fiber, the onset decomposition temperature decreases, but the exothermic temperature increases as comparedwith the untreated fiber. Owing to the shrinkage of fabric size, the breaking load and tensile strain in warp and weftdirections increase. The TiO2-loaded PET fabric can absorb more ultraviolet radiation even after being washed for 30times. The water absorbency is also slightly increased. The capability of photocatalytic degradation of methyl orange dyeis obtained.

Keywords

PET fabric, hydrothermal method, TiO2 nanoparticle

Introduction

Among various methods for the preparation of tita-

nium dioxide (TiO2) photocatalyst, including the ther-

mal hydrolysis, the sol-gel, the template process, the

chemical-precipitation, the thermal oxidation and the

microemulsion process, the hydrothermal processing

is a simple and effective 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 homo-

geneity and controlled particle morphology.4 It has

been reported that the structure and morphological

characteristics of TiO2 particles are markedly influ-

enced by the process conditions. The shape, size, crys-

talline form, photocatalytic activity and some relevant

properties of TiO2particles can be controlled by alter-

ing the reaction temperature and time, the pH, the ratio

of reactants and so on.5 The precursors for the fabrica-

tion of TiO2 particles are mainly focused on titanium

trichloride (TiCl3), titanium tetrachloride (TiCl4), tita-

nium 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 photo-

catalytic activities. Both anatase and brookite are meta-

stable and transform to rutile when they are heated.6

Some researchers have carried out the synthesis of TiO2by 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: [email protected]

Textile Research Journal

82(8) 747754

! The Author(s) 2012

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TiO2 catalysts with high photocatalytic activity under

visible light irradiation were obtained by using acetone,

alcohol and pyridine as the solvent under the hydro-

thermal 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 reac-

tant 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 pre-

cursors,12,13 or using titanium oxysulfate as the precur-

sor.14 The pH conditions had a great effect on the

quantity of the surface hydroxyl absorbed by the syn-

thesized powders.15 The dispersion of the prepared

nanoparticles could be greatly improved by using tetra-

ethylammonium 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 produc-

ing 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 specific

surface energy. The recovery and reuse of waste nano-

particles are usually restricted in the practical applica-

tion. Therefore, development of TiO2 based

photocatalysts anchored to supporting materials with

large surface areas would be of great significance. It can

not only avoid the disadvantages of filtration and sus-

pension of fine photocatalyst particles, but also lead to

high photodecomposition efficiency.19

More recently,TiO2 has been extensively explored as a coating mate-

rial for textiles to provide functions such as antibacter-

ial activity, UV protection, and self cleaning.

Immobilization of TiO2(or Au/TiO2) clusters on differ-

ent textiles has been currently realized showing the for-

mation of rutile or anatase crystals of small dimensions,

stably grafted onto fiber surfaces.19,2023 For example,

in order to obtain the self-cleaning activity effect under

visible light irradiation, cotton textiles were firstly acti-

vated 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 microor-

ganisms attached on cotton fibers can be effectively

removed upon daylight irradiation. Nanosized TiO2was prepared by hydrothermal method at first, and

then the woven glass fabric was dipped in the TiO2suspension solution. Finally, the coated fabric was cal-

cined at different temperatures. It was found that the

TiO2 particle films coated on glass fabric, with high

photocatalytic activity for the NO oxidation, were

achieved.4 Different layers of TiO2 were also

immobilized on polypropylene fabric by the hydrother-

mal method so as to obtain the highly active buoyant

photocatalysts. It was confirmed 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 inthe literature related to the TiO2-coated fabric with

photocatalytic activity prepared by the hydrothermal

method. In this paper, we synthesized TiO2 nanoparti-

cles immobilized on a polyethylene terephthalate (PET)

fiber surface to evaluate the potential applicability to

functional fabrics. Nanosized TiO2was deposited in the

presence of PET fabric using titanium sulfate and urea

in the sealed aqueous solution. The morphology, micro-

structure, thermal stability and optical properties of

PET fabric before and after treatments were character-

ized by scanning electron microscopy (SEM), X-ray

diffraction (XRD), Fourier transform infrared spec-

troscopy (FT-IR), thermal gravimetry (TG), differential

scanning calorimetry (DSC) and UV-Vis reflectance

spectroscopy. The properties of tensile, water absorp-

tion and photocatalytic degradation of methyl orange

were also investigated.

Experimental

Materials

The undyed plain woven PET fabric was used for pre-

cipitating TiO2 nanoparticles. The linear densities of

ends and picks were identical (7.3 tex). The numbersof ends and picks were 410 and 290 per 10 cm, respec-

tively. 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 first scoured with an aqueous solu-

tion of 200 g/L NaOH for 30 min at 60C prior to use,

followed by rinsing with acetone and anhydrous etha-

nol solution at room temperature for 15 min, and then

was repeatedly washed, three times, with distilled water

at 60C. The hydrothermal process was employed to

modify PET fabric in the laboratory. First, 19.2 g of

titanium sulfate was added to 160 mLof distilled

water, with vigorous stirring, at a temperature of

60C. 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 mLPTFE sealed can,

which was put into the stainless steel autoclave.

The autoclave was then placed in a furnace for the

748 Textile Research Journal 82(8)



4/9

hydrothermal treatment. The temperature was heated

to 200C at a speed of 2C/min. After treatment for 3 h,

the PTFE sealed can was cooled down to room tem-

perature. The PET fabric was dried at 80C for 5 min in

an oven, and then was dipped in the acetone and eth-

anol solution twice for 10min, respectively, followed by

washing with distilled water for 10 min, and dried atambient condition. The weight of PET fabric before

and after treatment was measured by an AL54 analyt-

ical balance. The pick-up of TiO2nanoparticles depos-

ited 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 field emission scanning electron

microscope. XRD patterns were obtained by using Cu

Ka1 radiation ( 1.540562 A ), using a 7000 S diffrac-tometer at 40 kV and 40 mA with the angle of 2from

10 to 80 at a scan speed of 8 deg/min. The mean crys-

tallite size of the TiO2crystallite 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 ther-

mogravimetric/differential 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 flush rate of10 mL/min over the range of 30550C. DSC analyses

were performed in a Sapphire apparatus at a rate of

10/min in flowing nitrogen gas at 10 mL/min from

30C to 600C.

The reflectance 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 integrat-

ing 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 instru-ment according to GB/T3923.1-1997. The initial

gauge length was 200 mmand 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

mc 100% 1

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 mea-

surements 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 specific time

intervals. The degradation rate was calculated from

equation (2).

D A0 At

A0 100% 2

Where D is the degradation rate (%), A0 is the initial

absorbance of the methyl orange solution, andAtis 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

fibers before and after treatment with titanium sulfate

and urea. It can be seen that the surface of the

untreated PET fiber is clean and smooth. A few small

particles are induced by the attached substances

(Figure 1a). When PET fabric was treated with tita-

nium sulfate and urea by hydrothermal processing,

the surface of as-obtained fiber is covered with a layer

of homogeneous granular materials. Some large parti-

cles in the micrometer scale are formed on the fiber

surface because of the adhesion of agglomerated parti-

cles. The pick-up of TiO2nanoparticle is 1.1% (w/w). A

number of pits can also be observed on the fiber sur-

face, which is etched by the caustic solution (Figure 1b).

From the high resolution SEM picture of PET fiber, the

surface of the untreated PET fiber is compact (Figure

1c). For the TiO2-coated fiber, many irregular tiny par-

ticles are distributed on the fiber surface. The average

particle size is larger than 100 nm in given growth con-

dition (Figure 1d).

Zhang et al. 749



5/9

XRD analysis

Figure 2 illustrates the XRD patterns of PET fabric

before and after treatment with titanium sulfate and

urea. It is clear that the intense diffraction peaks at

2 17.9, 23.0 and 26.3 are due to the typical PETphase. 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 cal-

culated to be 2.4nm(101), 3.5nm(004) and

3.1 nm (200) using Scherrers equation DK/cos

(where D is the diameter of the particle, is the X-

ray wavelength, is the FWHM (full width at half

maximum) of the diffraction line, is the diffraction

angle, and K is a constant 0.89), respectively. These

data imply that the shape of the TiO2 nanoparticle is

spherical and is quite different from the particle size

estimated in SEM observation because of the agglom-

erating of nanoparticles.

FT-IR analysis

Figure 3 shows the FT-IR spectra of PET fabric before

and after treatment with titanium sulfate and urea. It is

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 sur-

face absorbed water induced by TiO2 nanoparticles.

(b)(a)

(d)(c)

Figure 1. SEM pictures of the surface of PET fiber. (a) 5000 and (c) 30000 before treatment; (b) 5000and (d) 30000after

treatment with titanium sulfate and urea.

10 20 30 40

2q/

50 60 70 80

Intensity

(215)(204)(211)(105)(200)

(004)

(101)

(b) PET fabric treated with

Ti(SO4)2and Urea

(a) Untreated PET fabric

(116) (220)

(c) Anatase TiO2

Figure 2. X-ray patterns of PET fabric (a) before and (b) after





6/9

The corresponding bending band at 1659 cm1 is iden-

tified. The peak at 1410 cm1 caused by the benzene

skeleton vibration is intensified and shifted to

1401 cm1. The peak at 1093cm1 (COC anti-sym-

metrical stretching vibration) is also intensified and

shifted to 1116 cm1. At the same time, the new absorp-

tion 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 fiber.

TG analysis

Figure 4 displays the TG curves of PET fabric before

and after treatment with titanium sulfate and urea. The

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 376.7C for the

untreated PET fabric. The weight loss is 80.8% between

339.7C and 455.5C. For the TiO2-coated fabric, the

onset of decomposition temperature is increased to

379.7C, but not distinctly. The corresponding weightloss changes only a little (81.6%). This is ascribed to the

coating of TiO2 nanoparticles. So the hydrothermal

processing has little effect on the thermal properties

of PET fiber.

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 45.9C 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 250.8C changed only

a little (251.2C) when the PET fabric was treated with

titanium sulfate and urea. The melting enthalpies of

PET fiber before and after treatment calculated by inte-

gration of the DSC curve in the temperature range

250 10C are 10.2 J/g and 14.8 J/g, respectively. The

exothermic peaks at 418.5C and 463.4C are increased

to 437.4C and 532.8C, respectively. This signifies the

thermal pyrolysis of PET fiber and phase transition of

anatase TiO2 to rutile.27

100 200 300 400 500 600

endo

45.9C

4.13 mW463.4C1.38 mW

418.5C

3.00 mW

250.8C

6.30 mW

HeatFlow

/mW

Temperature/C


(b) TiO2coated PET fabric

251.2C

4.67 mW

437.4C

0.46 mW

532.8C

0.36 mW

exo

Figure 5. DSC curves of (a) untreated and (b) TiO2-coated

PET fabrics.

501

723

872

1016

10931236

13411410

1456

1505

1577

1716

29663432

618

722

1017

1116

1234

1401

1505

1659

4000 3000 2000 1500 1000 500

Tsmittanceran/%

Wavenumbers/cm-1

3129

a. Untreated PET fabric

b. PET fabric treated with Ti(SO4)2and urea

Figure 3. FT-IR spectra of PET fabric (a) before and (b) after


100 200 300 400 500

0

20

40

60

80

100

120

(c)

(b)

(c) TiO2nanoparticle

(b) TiO2-coated PET fabric

Onset: 379.7C

Endset: 422.1C

Step: -81.6%


Onset: 376.7

CEndset: 416.5C

Step: -80.8%

Temperature/C

RelativeMass/%

(a)

Figure 4. TG curves of (a) untreated, (b) TiO2-coated PET

fabrics and (c) TiO2 nanoparticles.

Zhang et al. 751



7/9

Reflectance spectrum analysis

Figure 6 represents the diffuse reflectance spectra of

untreated, TiO2-coated and washed (30 times) PET fab-

rics. The absorption peak at 304 nm for the untreated

PET fabric is assigned to the p!p* electronic transi-

tion in the benzene ring. The enhancement of UVabsorption capability for the TiO2-coated PET fabric

suggests that the TiO2nanoparticle film can absorb UV

irradiation and visible light to some extent. As com-

pared with the untreated fabric, the average absorp-

tances 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 accord-

ing to IWS TM31 standard, the average reflectances are

slightly increased 3.6% in UV (200400nm) region, and

9.3% in Vis (400800 nm) region with respect to the

TiO2-coated one. This implies that some TiO2nanopar-

ticles are washed off from the fiber surface.

Tensile property analysis

The fabric densities and tensile properties of PET fabric

before and after treatment are given in Table 1 in accor-

dance with GB/T3923.1-1997. Because PET fabric was

treated at high temperature for a long time, the densi-

ties are increased from 410 to 436 per 10 cm in warpdirection, 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

film loaded onto the surface of the PET fiber. The

decreased distance between adjacent yarns also makes

a substantial contribution to the water absorption.

0 20 40 60 80 100 120

0

20

40

60

80

100

Irradiation time/min

Degradationrate/%


(b) TiO2-coated PET fabric

Figure 7. Effect of irradiation time on the degradation rate for

(a) untreated and (b) TiO2-coated PET fabrics.

200 300 400 500 600 700 8000

20

40

60

80

100

(c) Washed PET fabric 30 times

(b) TiO2-coated PET fabricReflectance/%

Wavelength/nm


Figure 6. Reflectance spectroscopy of (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

PET fabricDensity/thread10cm1 Breaking load/N Tensile strain/%

warp weft warp weft warp weft

Untreated 410 290 583.3 362.3 19.6 19.5

TiO2-coated 436 321 593.0 373.3 20.1 22.5




8/9

Photodegradation effect

Figure 7 shows the effect of UV irradiation time on the

degradation rate of methyl orange dye for PET fabric

before and after treatment. It is found that the degra-

dation 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 irra-

diated for 90 min. The experimental results demonstrate

that the TiO2nanoparticles precipitated onto PET fiber

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 TiO2nanoparticles, which provides a great oppor-

tunity for the treatment of industrial dye effluents.

Conclusions

A thin layer of TiO2nanoparticles was well precipitated

onto the surface of PET fiber by the hydrothermal

method, using titanium sulfate and urea. From the

results of SEM and XRD, it is found that the film of

TiO2 nanoparticles has the anatase phase. The TiO2particle is constituted of the agglomerated nanoparti-

cles with an average size of 3.0 nm or so. FT-IR results

show that the TiO2nanoparticles are grafted onto PET

fiber. TG and DSC results indicate that the thermal

stability of PET fiber is decreased after being treated

with titanium sulfate and urea by the hydrothermalprocess. The PET fabric loaded with the TiO2nanopar-

ticles exhibits an excellent UV absorption ability. Due

to the shrinkage of fabric size in warp and weft direc-

tions, 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) inChina.

Funding

This research received no specific grant from any funding

agency in the public, commercial, or not-for-profit sectors.

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