Textile Research

http://trj.sagepub.com/
Journal

The preparation and antibacterial activity of polyester fabric loaded with silver nanoparticles
Hong Xu, Xue Shi, Yihang Lv and Zhiping Mao
Textile Research Journal 2013 83: 321 originally published online 27 November 2012
DOI: 10.1177/0040517512454187

The online version of this article can be found at:

http://trj.sagepub.com/content/83/3/321

Published by:

http://www.sagepublications.com

Additional services and information for Textile Research Journal can be found at:

Email Alerts: http://trj.sagepub.com/cgi/alerts

Subscriptions: http://trj.sagepub.com/subscriptions

Reprints: http://www.sagepub.com/journalsReprints.nav

Permissions: http://www.sagepub.com/journalsPermissions.nav

Citations: http://trj.sagepub.com/content/83/3/321.refs.html

>> Version of Record - Jan 11, 2013

OnlineFirst Version of Record - Nov 27, 2012

What is This?

Downloaded from trj.sagepub.com at UNIV OF NEW HAMPSHIRE on March 8, 2013

Original article
Textile Research Journal
83(3) 321–326

The preparation and antibacterial activity ! The Author(s) 2013

Reprints and permissions:
sagepub.co.uk/journalsPermissions.nav
of polyester fabric loaded with silver DOI: 10.1177/0040517512454187
trj.sagepub.com
nanoparticles

Hong Xu, Xue Shi, Yihang Lv and Zhiping Mao

Abstract
A facile procedure for binding silver nanoparticles on polyester fabrics was reported. In this paper, the multifunctional
polymer films were firstly formed through simple dip-coating of polyester fabrics in an aqueous solution of dopamine.
Then the silver nanoparticles were in situ generated on the surface of dopamine-modified polyester fabrics in an aqueous
solution of silver nitrate under room temperature. X-ray diffraction, scanning electron microscopy and inductively
coupled plasma optical emission spectrometry were used to characterize the structure and the content of silver
nanoparticles. The antibacterial efficiencies of treated samples were quantitatively estimated. The results indicated
that the dopa-polyester fabrics loaded with silver nanoparticles showed durable antibacterial activity.

Keywords
polyester fabrics, dopamine, silver nanoparticles, antibacterial activity

Nanoparticles can endow fabrics with improved per-
formance and functionality. The application of nano-
particles to textile materials relies on development of
new technology that should provide desired effects for
materials with long-term durability and stability with-
out use of highly toxic organic compounds. Silver
nanoparticles (AgNPs) can endue different textile fab-
rics with an antimicrobial effect.1–7 Although the mech-
anism of this action is still inexplicit, it was widely
thought that AgNPs can interact with the constituents
of the outer membrane of bacteria, causing structural
change and degradation.8–10
Recently, the manufacturing of sportswear, medical
and protective textiles based on polyester fabrics has
continually increased. Most of these fabrics are
expected to be antibacterial. However, the hydrophobic
behavior and low surface energy of polyester make
surface treatment extremely difficult.11 Most reported
methods that were used to treat fabrics with nano-
structured silver, such as electroless plating,12–14
vacuum deposition15 and so on, require multiple steps
or complex reagents to prepare silver nanoparticles on
the fabrics. Therefore, it is necessary to develop a facile
route for the formation of robust silver nanoparticle
coatings on the textile fiber surface. Dopamine
(3,4-dihydroxyphenethylamine), a kind of low-
molecular-weight catecholamine that mimics the adhe-
sive protein, can spontaneously self-polymerize on vari-
ous inorganic and organic surfaces and form uniformly
films under mild conditions.16–19 Furthermore, the
catechol groups in dopamine were redox active and
therefore could perform as metal reducing agents.16,20
In this paper, a facile procedure for binding AgNPs
on polyester fabrics was reported. The polyester fabrics
were modified with dopamine at first and then treated
with AgNO3 in an aqueous medium under room tem-
perature. Dopamine was utilized as the binding agent
and reductant. Silver ions (Ag+) were reduced to
AgNPs and distributed homogeneously on the surface
of dopamine-modified polyester fabrics. The polyester
fabrics with AgNPs showed a highly antibacterial activ-
ity even after being washed 30 times.
Key Lab of Science and Technology of Eco-textile, Ministry of Education,
College of Chemistry, Chemical Engineering and Biotechnology, Donghua
University, China
Corresponding author:
Zhiping Mao, Key Lab of Science and Technology of Eco-textile, Ministry
of Education, College of Chemistry, Chemical Engineering and
Biotechnology, Donghua University, Shanghai 201620, China.
Email: zhpmao@dhu.edu.cn

Downloaded from trj.sagepub.com at UNIV OF NEW HAMPSHIRE on March 8, 2013

322
Materials and methods
Materials
Polyester fabrics supplied by Esquel Group (Gaoming,
China) were cleaned by diethyl ether anhydrous before
used. Dopamine hydrochloride was purchased from
Webb Chemical Co., Ltd (Guangzhou), which was
imported from Acros Organics, USA. Silver nitrate,
Tris(hydroxymethyl) aminomethane (Tris), potassium
phosphate monobasic (KH2PO4), sodium phosphate
dibasic (Na2HPO4) and hydrochloric acid (HCl) were
purchased from Sinopharm Chemical Reagent Co.,
Ltd. All chemicals were used without further
purification.
The modification of polyester fabrics
Dopamine with a concentration of 0.01 mol/l was dis-
solved in the buffer solution, which was prepared
by Tris.16 Then the pH value of the solution was regu-
lated to a typical marine environments (pH ¼ 8.5)
with HCl. The polyester fabrics were dipped directly
into dopamine solution with stirring for 24 h at
room temperature, then were taken out and rinsed
with deionized water until the solution turned clear.
The polyester fabrics treated by dopamine will be
called dopa-polyester fabrics in the subsequent
discussion.
The in situ reduction of silver nanoparticles on the
surface of dopa-polyester fabrics
The polyester fabrics and dopa-polyester fabrics were
immersed into silver nitrate solution (0.29 mol/l) at
room temperature for 8 h. Then the samples were
rinsed with flowing deionized water for 10 min and
dried at 40 C in the vacuum oven for 6 h. The obtained
samples were respectively designated as polyester/Ag
and dopa-polyester/AgNPs fabrics in the subsequent
discussion.
Scanning electron microscope
The surface morphologies of the dopamine functiona-
lized and silver metalized dopa-polyester were investi-
gated in a JEOL JSM 5600 scanning electron
microscope (SEM). The SEM measurements were per-
formed at an accelerating voltage of 15 kV.
X-ray diffraction
X-ray diffraction (XRD) characterization was per-
formed by a D/max-2550PC diffractometer with Cu
Ka radiation (wavelength 1.54056).
Downloaded from trj.sagepub.com at UNIV OF NEW HAMPSHIRE on March 8, 2013
Textile Research Journal 83(3)
Inductively coupled plasma optical emission
spectrometry
The content of silver was determined by inductively
coupled plasma optical emission spectrometry
(ICP-OES) using the prodigy spectrometer (Teledyne
Leeman Labs, USA). The wavelength ranged from
165 to 800 nm.
Before ICP measurements, the sample needed to be
digested according to the following procedure.
The sample was digested using a Multiwave 3000
microwave digestion system (Anton-Paar, courta-
boeuf, France), equipped with a rotor for eight 80 ml
type quartz vessels (operating pressure, 80 bar). Before
use, quartz vessels were decontaminated in a bath of
10% nitric acid (67%, v/v), then were rinsed with
ultrapure water and dried in a 40 C oven. Samples
were weighed precisely to 0.01 g in the quartz diges-
tion vessels and wet-oxidized with 1 ml H2SO4 (98%,
v/v) and 4 ml HNO3 (67%, v/v). One randomly
selected vessel was filled with regents only and taken
through the entire procedure as a blank. The digestion
procedure had previously been optimized. After
cooling at room temperature, sample solutions were
quantitatively transferred into 100 ml polyethylene
flasks. The digested samples were then filled with
ultrapure water to the final volume before analysis
by ICP-OES.
Washing fastness testing
The washing fastness testing of polyester/Ag and dopa-
polyester/AgNPs fabrics was performed according to
the ISO105-C10:2006 standard using the SW-12A II
Launder-O-Meter Standard Instrument.21 The liquid
ration was 50:1 and the washing temperature was
40 C. The samples were washed for 30 min in a solution
of soap with a concentration of 5 g/l for one cycle,
rinsed with deionized water and dried at 40 C in the
vacuum oven for 6 h.
Antibacterial activity
The antibacterial efficiencies of treated samples were
quantitatively estimated using Gram-negative bacteria
E. coli according to the American Association of
Textile Chemists and Colorists (AATCC) 100-2004
standard.
Before the microbiological experimentation, all glass
wares and samples were sterilized by autoclaving at
121 C for 15 min. Finished fabrics (0.4 g), which were
cut up into chips, were put into a 150 ml Erlenmeyer
flask and inoculated with 35 ml phosphate buffer solu-
tion (pH ¼ 7.4) and 1.0 ml of a nutrient broth culture
containing 1–2  105 CFUs (colony forming units)
Xu et al. 323

of bacteria. The samples were then incubated at 37 C

for 24 h. The polyester fabrics were used as a control.
After serial dilutions with phosphate buffer solu-
tion were made, the bacterial suspensions were
spread on nutrient agar plates and incubated at 37 C
for 24 h. Then the number of CFUs was counted.
The reported data were the average value of three par-
allel runs.
The percentage of microbe reduction (R%) was cal-
culated using the following equation:
R ¼ ðB  AÞ=B  100%
where A (CFUs) is the number of microbial colonies of
the finished fabrics after inoculation for 24 h, and
B (CFUs) is the number of microbial colonies of the
finished fabrics that was immediately eluted after inocu-
lation (at ‘‘0’’ contact time).
Results and discussion
The modification of the polyester fabrics with
dopamine
Figure 1 shows the images of polyester and dopa-polye-
ster fabrics. It can be seen that the color of the polyester
fabrics turned from white to dark brown after they were
treated by dopamine. It suggested that poly(dopamine),
the structure and color are similar to that of melanin, was
formed by the polymerization of dopamine monomers.16
The surface morphology of the samples was further
characterized using a SEM (Figure 2). SEM images
showed that the polyester had a slick surface
(Figure 2(a)), whereas the polyester fabrics modified
by dopamine showed a quite different pattern; that is,
a rough coating was observed on the surface
(Figure 2(b)), which indicated that the polydopamine
membrane had formed on the surface of the polyester.

Figure 1. Images of the polyester fabrics: (a) polyester fabrics and (b) dopa-polyester fabrics.

Figure 2. Scanning electron microscope images showing (a) the polyester fabric and (b) the dopa-polyester fabric.

Downloaded from trj.sagepub.com at UNIV OF NEW HAMPSHIRE on March 8, 2013

324 Textile Research Journal 83(3)

The reduction and binding of AgNPs on the surface

According to Lee et al.,16 the catechol of the dopa-
mine structure was easily oxidized and formed a
of dopa-polyester fabrics
quinine structure in the alkaline conditions.11 The pri- After the polyester fabrics and dopa-polyester fabrics
mary roles of both catechol and o-quinone forms were treated by silver nitrate solution, XRD (Figure 3)
of dopamine can be assigned to adhesive bonding was conducted to identify the formation of metallic
and cross-link formation, respectively.10–14 The pos- silver. It can be seen that three major peaks found at
sible reaction mechanism of dopamine is shown in 37.96, 44.28 and 64.82 on the 2y scale correspond to the
Scheme 1. (111), (200) and (220) crystal planes, respectively.

n
H2N
NH NH NH

oxidation polymerization
rearrangement

HO OH HO OH HO OH n HO OH

dopamine 5,6 - dihydroxyindole polydopamine (PDA)

Scheme 1. The possible polymerization mechanism of dopamine.

(a) (b) (c)

Intensity/cps
intensity/cps

Intensity/cps

(111)
(200)
(220)

0 10 20 30 40 50 60 70 80 0 10 20 30 40 50 60 70 80 0 10 20 30 40 50 60 70 80
2θ/degree 2θ/degree 2θ/degree

Figure 3. Wide-angle X-ray diffraction pattern: (a) polyester; (b) polyester/Ag fabrics; and (c) dopa-polyester/AgNPs fabrics.

Figure 4. Scanning electron microscope images of the dopa-polyester/silver nanoparticle fabrics: (a) unwashed; (b) washed 30 times.

Downloaded from trj.sagepub.com at UNIV OF NEW HAMPSHIRE on March 8, 2013

Xu et al. 325

However, no corresponding peaks appear on the spec- The content of silver on the polyester/Ag and dopa-
trum of polyester fabrics and the polyester/Ag fabrics polyester/AgNPs fabrics was determined by ICP-OES
shown in Figures 3(a) and (b). It was confirmed that analysis. From the results of ICP-OES (Figure 5), it was
metallic silver has formed only on the surface of the evident that the content of silver adsorbed by the dopa-
dopa-polyester fabrics. polyester fabrics was much higher than that adsorbed
Figure 4 shows the SEM images of dopa-polyester/ by the polyester fabrics, as expected. According to
AgNPs fabrics. Figure 4(a) indicated that many silver reports, it was mainly attributed to adhesion of the
particles with different size dispersed on the surface of poly(dopamine) on the surface of polyester fabrics.16
dopa-polyster fabrics. However, when the samples were On the other hand, it can be seen that the amount of
washed 30 times, it was noticed that there were rela- AgNPs decreased quickly during washed 1–10 times. It
tively few particles remaining on the surface of the was considered that some AgNPs with large size or
fabric, because the aggregated silver particles adsorbed aggregation adsorbed just onto the surface of dopa-
only onto the surface of dopa-polyester fabric were polyester fabrics were easily washed away. However,
washed away (Figure 4(b)). This confirms that polydo- the content of AgNPs decreased slowly and sustained
pamine membranes own a strong metal-binding ability relatively steadily after washing 10 times. The content of
and adhesion property to the monodispersed silver AgNPs on the dopa-polyester/AgNPs samples remained
nanoparticles. The possible Ag+ in situ reduction 1.38 mg/g even if the fabrics were washed 30 times, which
mechanism for polydopamine has been discussed in was in agreement with the results of Figure 4. However,
our previous research.21 the content of silver on the unmodified polyester fabrics
was nearly zero after washing 30 times.

Antibacterial activity
5 dopa-polyester/AgNPs The bactericidal effects of the samples were investigated
polyester/Ag
against E. coli, as shown in Table 1. To determine the
Content of AgNPs (mg/g)

4 antibacterial activity, the growth of E. coli was per-

formed in the different polyester fabrics. The dopa-
3 polyester fabrics showed a weak antibacterial activity
with the rate of reduction only 20.7% (Table 1(a)). It
2 clearly showed that the polyester only treated with
dopamine had little antibacterial activity. From the
1 data of Table 1(b) and (c), we can conclude that the
fabric that was simply dipped in the AgNO3 solution
0 had poor durable antibacterial activity. However, the
0 5 10 15 20 25 30 growth of E. coli was completely inhibited by the silver
Wash times loaded on dopa-polyester fabrics (Table 1(d)). The per-
cent reduction of E. coli seeded on the dopa-polyester/
Figure 5. The content of silver nanoparticles (AgNPs) on the AgNPs was 99.99% after 24 h incubation. This con-
polyester/Ag and dopa-polyester/AgNPs fabrics washed different firmed that AgNPs were indeed responsible for the bac-
numbers of times. tericidal activity. Table 1(e) showed that the bacterial

Table 1. Reduction (R%) of bacteria E. coli. according to the AATCC 100-2004 standard method

Average Average of viable

of viable E. coli count after E. coli count after
Sample ‘‘0’’ contact time 24 h incubation R (%)
3 3
Original polyester fabrics 2.1  10 1.9  10
(a) Unwashed dopa-polyester fabrics 2.9  102 2.3  102 20.7
(b) Unwashed polyester/AgNPs fabrics 3.3  102 1.3  102 60.6
(c) Polyester/AgNPs fabrics washed 30 times 2.8  102 2.4  102 14.3
(d) Unwashed dopa-polyester/AgNPs fabrics 2.6  102 <1 99.99
(e) Dopa-polyester/AgNPs fabrics washed 30 times 3.0  102 <1 99.99
AgNPs: silver nanoparticles.

Downloaded from trj.sagepub.com at UNIV OF NEW HAMPSHIRE on March 8, 2013

326
colonies of E. coli were also completely inhibited by the
dopa-polyester/AgNPs fabrics that were washed
30 times. Compared with Table 1(d), it could be con-
cluded that the washing process caused no considerable
effect on the antibacterial activity. It was clearly sug-
gested that dopa-polyester/AgNP fabrics could sustain
durable antibacterial activity.
Conclusions
Polydopamine coatings could be formed on the surface
of polyester fabrics after treating with dopamine in the
Tris buffer solution. The catechol groups in the poly-
dopamine coatings could in situ reduce the Ag+ to Ag0
without adding any further reducing agent. AgNPs can
be generated and distributed homogeneously on the
surface of dopamine-modified polyester fabrics. The
polyester fabrics coated with AgNPs show excellent
durable antibacterial activity for at least 30 washes.
Funding
This work was supported by grants from the National
Natural Science Foundation of China (Grant No.
21074021), the National High Technology Research and
Development Program of China (863 Program) (No.
2007AA03Z336) and the Program for New Century
Excellent Talents in University (No. NCET-07-0174).
References
1. Lee HJ, Yeo SY and Jeong SH. Antibacterial effect of
nanosized silver colloidal solution on textile fabrics.
J Mater Sci 2003; 38: 2199–2204.
2. Yeo SY, Lee HJ and Jeong SH. Preparation of nanocom-
posite fibers for permanent antibacterial effect. J Mater
Sci 2003; 38: 2143–2147.
3. Yuranoa T, Rincon AG, Bozzi A, et al. Antibacterial tex-
tiles prepared by RF-plasma and vacuum-UV mediated
deposition of silver. J Photochem Photobiol A 2003; 161:
27–34.
4. Jeong SH, Hwang YH and Yi SC. Antibacterial properties
of padded PP/PE nonwovens incorporating nano-sized
silver colloids. J Mater Sci 2005; 40: 5413–5418.
5. Dubas ST, Kumlangdudsana P and Potiyaraj P. Layer-by-
layer deposition of antimicrobial silver nanoparticles on
textile fibers. Colloid Surf A 2006; 289: 105–109.
6. Hadad L, Perkas N, Gofer Y, et al. Sonochemical depos-
ition of silver nanoparticles on wool fibers. J Appl Polym
Sci 2007; 104: 1732–1737.
Downloaded from trj.sagepub.com at UNIV OF NEW HAMPSHIRE on March 8, 2013
Textile Research Journal 83(3)
7. Ki HY, Kim JH, Kwon SC, et al. A study on multifunc-
tional wool textiles treated with nano-sized silver.
J Mater Sci 2006; 42: 8020–8024.
8. Gogoi SK, Gopinath P, Paul A, et al. Green Fluorescent
protein-expressing escherichia coli as a model system for
investigating the antimicrobial activities of silver nano-
particles. Langmuir 2006; 22: 9322–9328.
9. Kim JS, Kuk E, Yu KN, et al. Antimicrobial effects of
silver nanoparticles. Nanomed Nanotechnol Biol Med
2007; 3: 95–101.
10. Lok CN, Ho CM, Chen R, et al. Silver nanoparticles:
partial oxidation and antibacterial activities. J Biol
Inorg Chem 2007; 12: 527–534.
11. Hossain MM, Herrmann AS and Hegemann D. Plasma
hydrophilization effect on different textile structures.
Plasma Process Polym 2006; 3: 299–307.
12. Jiang SQ, Newton E, Yuen CWM, et al. Chemical silver
plating on polyester/cotton blended fabric. J Appl Polym
Sci 2006; 100: 4383–4387.
13. Jiang SQ, Newton E, Yuen CWM, et al. Chemical silver
plating on cotton and polyester fabrics and its application
on fabric design. Textil Res J 2006; 76: 57–65.
14. Jiang SQ, Newton E, Yuen CWM, et al. Chemical silver
plating and its application to textile fabric design. J Appl
Polym Sci 2005; 96: 919–926.
15. Wang H, Wang J and Hong J. Preparation and charac-
terization of silver nanocomposite textile. J Coat Technol
Res 2007; 4: 101–106.
16. Lee H, Dellatore SM, Miller WM, et al. Mussel-inspired
surface chemistry for multifunctional coatings. Science
2007; 19: 318–426.
17. Yu M, Hwang J and Deming TJ. Role of L-3,4-dihydrox-
yphenylalanine in mussel adhesive proteins. J Am Chem
Sci 1999; 121: 5825–5826.
18. Xi ZY, Xu YY, Zhu LP, et al. A facile method of surface
modification for hydrophobic polymer membranes based
on the adhesive behavior of poly(DOPA) and poly(dopa-
mine). J Membr Sci 2009; 327: 244–253.
19. Lee H, Scherer NF and Messersmith PB. Single-molecule
mechanics of mussel adhesion. Proc Natl Acad Sci 2006;
103: 12999–13003.
20. Lee H, Lee Y, Statz AR, et al. Substrate-Independent
layer-by-layer assembly by using mussel-adhesive-
inspired polymers. Adv Mater 2008; 20: 1619–1623.
21. Xu H, Shi X, Ma H, et al. The preparation and antibac-
terial effects of dopa-cotton/AgNPs. Appl Surf Sci 2011;
257: 6799–6803.