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Sonochemical coating of silver nanoparticles on textile fabrics (nylon,

polyester and cotton) and their antibacterial activity

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Sonochemical coating of silver nanoparticles on textile fabrics (nylon, polyester and cotton)

and their antibacterial activity

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2008 Nanotechnology 19 245705

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IOP PUBLISHING NANOTECHNOLOGY
Nanotechnology 19 (2008) 245705 (6pp) doi:10.1088/0957-4484/19/24/245705

Sonochemical coating of silver

nanoparticles on textile fabrics
(nylon, polyester and cotton) and
their antibacterial activity
Ilana Perelshtein1, Guy Applerot1, Nina Perkas1 ,
Geoffrey Guibert2, Serguei Mikhailov2 and Aharon Gedanken1,3
1
Department of Chemistry, Kanbar Laboratory for Nanomaterials,
Institute of Nanotechnology and Advanced Materials, Bar-Ilan University,
Ramat-Gan 52900, Israel
2
Haute Ecole Arc Ingénierie IMA-Arc, NEODE, 17 Eplatures-Grise,
CH-2300 La Chaux-de-Fonds, Switzerland

E-mail: gedanken@mail.biu.ac.il

Received 3 March 2008, in final form 18 March 2008

Published 12 May 2008
Online at stacks.iop.org/Nano/19/245705

Abstract
Silver nanoparticles were synthesized and deposited on different types of fabrics using
ultrasound irradiation. The structure of silver–fabric composites was studied by
physico-chemical methods. The mechanism of the strong adhesion of silver nanoparticles to the
fibers is discussed. The excellent antibacterial activity of the Ag–fabric composite against
Escherichia coli (gram-negative) and Staphylococcus aureus (gram-positive) cultures was
demonstrated.

1. Introduction in their cell walls. Recent research has demonstrated that

The development of new clothing products based on the
immobilization of nanophased materials on textile fibers has
recently been of increasing interest to both the academic
and the industrial sectors [1, 2]. Today, a wide range of
nanoparticles with various structures can be immobilized on
the fibers, bringing new properties to the final textile product.
Silver ions, which have been used throughout history
as an antimicrobial agent, have recently received renewed
interest [3, 4]. The reason for this is because some bacterial
strains have demonstrated an increasing resistance toward
antibiotics. At the same time, the powerful antimicrobial
activity of silver is known to be effective against nearly 650
types of bacteria.
Several investigations have been carried out on the mech-
anism of the bactericidal activity of silver nanoparticles [5–7].
Experiments showed that, upon silver treatment, Escherichia
coli cells were damaged, showing the formation of ‘pits’
3 Author to whom any correspondence should be addressed.
the antibacterial activities of silver nanoparticles depend on
chemisorbed Ag+ , which is readily formed on the surface of
silver nanoclusters due to their extreme sensitivity to oxy-
gen [8–10]. However, the mechanism of the delivery of sil-
ver ions from silver nanoclusters to the bacteria needs further
investigation.
Nanostructured silver deposited on textile substrates can
be used to make smart functional textiles, which have great
potential for applications ranging from antibacterial materials
to conductive shields and electronic sensors [11].
Different methods have been used for the deposition of
silver nanoparticles on fabrics. For example, a poly(ethylene
terphthlate) fabric (meadox double velor) was coated with
metallic silver using a patented ion-beam-assisted deposition
process developed by the Spire Corporation (Bedford,
MA) [12]. Other methods were constant pressure padding [13]
and the reduction of silver ions by ethanol or isopropanol [14].
Some of the methods are based on reactions in the liquid
medium and require surfactants, reducing agents or templates
for the synthesis of silver nanoparticles, resulting in the

0957-4484/08/245705+06$30.00 1 © 2008 IOP Publishing Ltd Printed in the UK

Nanotechnology 19 (2008) 245705 I Perelshtein et al

presence of impurities in the final products. This method has

some disadvantages with regard to the environment.
Sonochemical irradiation has been proven as an effective
method for the synthesis of nanophased materials [15], as well a b
as for the deposition and insertion of nanoparticles on/into
the mesoporous ceramic and polymer supports [16–18]. Our
previous work [19] was based on coating nylon chips with
nanosilver. The silver–nylon nanocomposite was used as a
master batch for the production of nylon yarn by a melting and
spinning process. Antibacterial tests of the final silver–nylon
fabrics show very promising results. Our further aim was to
avoid the fiber production stage and to develop a direct method
for coating commercial fabrics with silver nanoparticles.
Figure 1. Cotton fabric before (a) and after (b) coating with silver
In this paper, we report on a new method for preparing nanoparticles.
fabrics such as nylon, polyester and cotton with antibacterial
(This figure is in colour only in the electronic version)
properties by coating them with silver nanoparticles. This
process was carried out by ultrasound radiation in a one-step
reaction procedure, a process that did not involve any toxic
enabling the creation of many seeds which eventually lead to
chemicals. To the best of our knowledge, this is the first report
the formation of silver nanoparticles.
on the deposition of silver nanoparticles on fabrics using the
The sonication flask was placed in a cooling bath at a
sonochemical method.
constant temperature of 30 ◦ C during the sonication. At the
The resulting sonochemically deposited silver fabrics
end of the reaction, the color of the fabric changed from white
were characterized by x-ray diffraction (XRD), high resolution
to gray (figure 1). The product was first washed thoroughly
scanning electron microscopy (HR-SEM) and Raman spec-
with water to remove traces of ammonia, then with ethanol, and
troscopy. The thickness of the Ag coating was characterized
dried under vacuum. The adhesion of the deposited silver was
by Rutherford backscattering spectrometry (RBS) and particle-
checked by washing the coated fabric for at least 20 washing
induced x-ray emission (PIXE). The mechanical properties of
cycles. Each cycle lasts 2 h and is conducted in hot (40 ◦ C)
the silver-coated materials and the untreated materials were
water.
also measured and compared. Finally, the antimicrobial ac-
tivity of the particles deposited on fabrics was tested against
gram-negative (E. coli) and gram-positive (Staphylococcus au- 2.2. Characterization
reus) bacteria. The silver content in the fabrics was determined by volumetric
titration with KSCN according to the Folgard method [20]
2. Experimental details after dissolving the sonicated product in HNO3 . The x-
ray diffraction (XRD) patterns of the product were measured
2.1. Synthesis with a Bruker D8 diffractometer (Karlsruhe, Germany) with
Cu Kα radiation. The particle morphology and the size of the
All the chemical reagents, of chemical grade, were purchased noble metal nanoparticles were studied with a high resolution
from Aldrich and used without further purification. The scanning electron microscope, HR-SEM (JEOL-JSN 7000F).
concentration of the precursor was changed in order to obtain The Raman spectra were collected with a JY Horiba Olympus
the best conditions for coating silver nanoparticles on the Bx41 spectrometer (Longjumeau, France) with a 514 nm
fabrics, and the antibacterial activity was measured at different Ar+ ion laser excitation source. The mechanical tests were
Ag concentrations. performed on a mechanical testing machine, ZWICK 1445
In a typical reaction, a 0.002 M solution of water and (Zwick GmbH & Co., Germany).
ethylene glycol (EG) (10:1 v/v) of AgNO3 was purged under
Ar for 1 h in order to remove traces of O2 /air. The purging
2.3. Bactericidal test
was done in the presence of the fabric (∼0.7 g of cotton 4 ply,
gauze of 13 threads cm−2 ). In the next stage, the solution was The antibacterial activity was tested against gram-negative E.
irradiated for 1 h with a high intensity ultrasonic horn (Ti horn, coli (strain 1313) as well as for gram-positive Staphylococcus
20 kHz, 600 W at 70% efficiency) under a flow of Ar. A 25% aureus (strain 195) bacteria. Both strains were obtained
aqueous solution of ammonia (molar ratio NH3 :AgNO3 = 2:1) from the Bacteriology Laboratory of the Meir Hospital, Kfar-
was added to the reaction slurry during the first 10 min of Saba, Israel. A typical procedure was as follows: cultures
sonication. EG was used as a polyol reducing agent. The of the bacteria were grown on nutrient agar (Difco, Detroit,
EG reduces the silver ions to metallic silver. The addition of MI) overnight. These cultures were then transferred into
ammonia forms the [Ag(NH3 )2 ]+ complex. The equilibrium a nutrient broth (NB) at an initial optical density (OD) of
constant for the formation of [Ag(NH3 )2 ]+ is large ≈107 , 0.1 at 660 nm and allowed to grow at 37 ◦ C with aeration.
which dictates a small amount of Ag+1 in equilibrium with When the cultures reached an optical density of 0.3 OD at
the complex. Thus the reduction process is slowed down, 660 nm (the beginning of the logarithmic phase), they were

2
Nanotechnology 19 (2008) 245705
Table 1. Silver content in the fabrics.
Type of fabric Silver content (wt%)
Nylon 1.4
Polyester 1.2
Cotton 1.1
centrifuged and washed twice with saline at pH 6.5 to yield a
final bacterial concentration of approximately 108 CFU ml−1 .
4.5 ml of a saline solution containing the impregnated fabric
(2 cm2 in size) at 1 and 6 wt% concentration of coating
was poured into a vial with an inner diameter of 2.5 cm.
500 μl of the strain cells was then pipetted into the vial. The
initial bacterial concentration in the vial was approximately
107 CFU ml−1 . To ensure that any decrease in bacterial
number was likely to be due to exposure to a coated bandage
treatment, two controls were included in the experiment: the
first, with saline (without the fabric), and the second with
saline with an uncoated fabric. Bacterial suspensions were
incubated and shaken at 170 strokes min−1 at 37 ◦ C for up to
4 h. Samples of 100 μl each were taken at a specified time,
diluted tenfold in saline and then transferred onto nutrient agar
plates (Difco). The plates were allowed to grow for 24 h at
37 ◦ C and then counted for viable bacteria. The viable bacteria
were monitored by counting the number of colony-forming
units from the appropriate dilution on nutrient agar plates.
3. Results and discussion
In this research, we coated textile substrates with silver
nanoparticles by a sonochemical method. The images of the
uncoated and silver-coated cotton are presented in figure 1.
One of the aims of this study was to investigate the interaction
between the fiber’s surface and the metallic silver as a result
of sonochemical irradiation: the options that can result from
the sonication are the formation of a chemical bond between
the silver and the functional groups of the substrate, and the
physical adsorption of the silver nanoparticles on the surface
of the fabric. We performed experiments on three types of
fabrics: nylon, polyester and cotton. These fabrics differ in
their functional groups, which are amide, ester and alcohol,
respectively. All these fabrics were exposed to the same
reaction conditions, i.e. reagent concentration, reaction time,
temperature and sonication power. The silver content in the
fabrics was determined by volumetric titration and the results
are presented in table 1.
The amount of silver deposited on the three different
fabrics is almost the same. This indicates that the amount of
deposited silver is independent of the nature of the substrate.
This also indicates that most probably the mechanism of
coating by ultrasound irradiation is not involved in the creation
of new bonds between the silver and the functional groups of
the substrate. We can therefore conclude that the coating is, in
fact, a physical adsorption of the nanoparticles on the substrate
as a result of the sonication. The sonochemical irradiation
of a liquid causes two primary effects, namely cavitation and
heating. When the microscopic cavitation bubbles collapse
near the surface of the solid substrate, they generate powerful
3
I Perelshtein et al
shock waves and microjets that cause effective stirring/mixing
of the adjusted layer of the liquid. The after-effects of the
cavitation are several hundred times greater in heterogeneous
systems than in homogeneous systems [21]. In our case, the
ultrasound waves promote the fast migration of the newly
formed silver nanoparticles to the fabric’s surface. This fact
might cause a ‘specific melting’ of the substrate surface, which
may be the reason why the particles strongly adhere to the
fabric’s surface, regardless of its properties. This phenomenon
occurs in spite of the free floating of the fabric. The reason is
that the speed of the jets is so much faster than the movement
of the fabric that it can be considered as standing still.
The characterization measurements of the three types
of fabrics sonochemically coated with silver nanoparticles
indicated that the fabrics exhibited similar properties. This is
the reason why we present results for only one coated fabric,
namely cotton.
3.1. Structure and morphology of the silver–fabric composite
The XRD patterns (figure 2) of sonochemically deposited Ag
nanoparticles on a cotton fabric demonstrate that the silver
is crystalline in nature, and the diffraction peaks match a
face-centered cubic (fcc) phase of Ag (PDF: 4–783). The
peaks at 2θ = 38.03◦ , 44.23◦ , 64.39◦ and 77.32◦ are assigned
to the (111), (200), (220) and (311) reflection lines of fcc
Ag particles, respectively. No peaks characteristic of any
impurities were detected. The particle’s size estimated by the
Debye–Scherrer (DS) equation is 80 nm.
The HR-SEM micrographs of cotton fibers before and
after the deposition of Ag nanoparticles are shown in figure 3.
The image in figure 3(a) demonstrates the smooth structure
of the cotton fabric before coating with silver nanoparticles.
After the sonication, the homogeneous deposition of silver
nanoparticles on the cotton yarn is observed (figure 3(b)).
Figure 3(c) is a higher magnification image measured in order
to obtain a particle size distribution. The calculated average
size of the silver nanoparticles deposited on the surface of the
cotton fibers is 80 nm, and it matches well the XRD results.
However, some aggregates consisting of small particles are
also observed.
3.2. Spectroscopy studies
Raman spectroscopy has been applied for the characterization
of a silver–cotton composite and to provide knowledge about
the structure, bonding nature and changes in the material’s state
upon its sonochemical reaction. The Raman spectrum of the
coated cotton fabric is presented in figure 4(b). The spectrum
closely resembles the spectrum of amorphous diamond-like
carbon, and can be resolved into the G (graphitic) and D
(disordered) Raman bands near 1600 cm−1 and 1350 cm−1 ,
respectively. In the Raman spectrum of the pristine cotton,
these bands are not found (figure 4(a)). Obviously, here
we observe the effect of surface-enhanced Raman scattering
(SERS), typical for silver nanoparticles deposited on pure
carbon and widely used for the characterization of carbon-
containing material [22–24].
Nanotechnology 19 (2008) 245705
Figure 2. XRD pattern of Ag nanoparticles deposited sonochemically on a cotton fabric.
a b
c
Figure 3. (a) HR-SEM images of pristine fibers, (b) fabrics coated
with Ag nanoparticles at a low magnification, (c) fabrics coated with
Ag nanoparticles at a high magnification.
Similar Raman spectra are observed for other fabrics after
silver deposition by ultrasound irradiation. From this data
we can assume that the temperature and speed of the silver
nanoparticles thrown to the fabric’s surface by sonochemical
microjets are high enough to cause melting and carbonization
of the fibers at the points of their contact with the silver nuclei.
These ‘hot spots’ become the center of fusion of the silver
nanoparticles and the fabric’s substrate. As a result, the silver
nanoparticles are strongly adhered to the fabric, and the coated
4
I Perelshtein et al
Figure 4. (a) Raman spectra of pristine cotton fabric, (b) fabric
coated with Ag nanoparticles.
material stays on the fabric for at least 20 washing cycles
without a reduction in the silver content. The washing process
is conducted in hot (40 ◦ C) water for 2 h per cycle. The silver
content in the fabrics was determined by volumetric titration
with KSCN according to the Folgard method [20].
3.3. RBS–PIXE measurements
RBS analysis is based on elastic collisions between ions and
the atomic nucleus. The slowing down of ions in matter
provides depth information. The PIXE analysis is based on
ionization of the inner shells of atoms. These techniques
are non-destructive and allow absolute quantitative analysis.
Scanning micro-PIXE–RBS analysis, where the ion probe is
focused to a micrometer level and scanned over the sample,
allows us to obtain the lateral distribution of elements [25].
Nanotechnology 19 (2008) 245705
2
Figure 5. Distribution of Ag on the textile fiber in selected regions 1
and 2 from PIXE cartography, 1 mm2 area.
Table 2. Estimation of the Ag thickness layer (at cm−2 ) coating on
the two cotton fibers by RBS analysis in selected regions 1 and 2.
Thickness (at cm−2 ) Region 1 Region 2
Cotton sample 134.3 ± 9.4 98.5 ± 6.8
Figure 6. Ag profile as a function of depth in region 1 as deduced
from RBS analysis.
Two kinds of area were selected for RBS analysis: (1) Ag
intensity high and (2) Ag intensity low. In these two regions the
Ag thickness profile and the Ag depth profile were estimated
and presented in figure 5. The different thickness layers are
summarized in table 2.
For Ag thickness layer it was found that, whatever the
region, an Ag coating layer was present, but some variations
in the Ag thickness are observed. For example, in region 1
a thickness layer of 134.3 ± 9.4 at cm−2 is measured, while
the silver thickness in region 2 is 98.5 ± 6.8 at cm−2 . Thus a
thickness variation of 30% was detected.
The Ag profile distribution was as follows: in region 1,
scanning the Ag profile from the outer surface to the cotton
fiber showed that, after the pure Ag surface layer, some traces
of Ag were present inside the fiber (figure 6). A few atomic
per cent, i.e. 3–4 at.%, were measured. In region 2, no Ag was
detected deeper than the pure Ag layer.
In conclusion, all the fibers are covered with a pure Ag
layer. The thickness of this layer can vary by approximately
30%. Some traces of Ag (3–4 at.%) were sometimes detected
locally in the fiber as deep as several hundred nanometers.
5
I Perelshtein et al
Figure 7. Mechanical properties of the cotton fabric before and after
the deposition of Ag nanoparticles.
3.4. Mechanical properties
The tensile mechanical properties of a common impregnated
fabric were studied on a universal testing machine, Zwick
1445. Fabric samples folded four times with a gauge length
of 60 mm and a width of 40 mm were placed in special
grips. The silver-coated samples showed a rather more brittle
behavior compared to the pristine fabric. Ultimately, the
tensile force for the coated sample was ∼10% less than that
of the non-impregnated one (figure 7). The observed changes
in the mechanical behavior of the yarn is in a range that is
acceptable for standard cotton fabrics. According to this result,
we conclude that the sonochemical treatment of the fabric did
not cause any significant damage to the structure of the yarn.
3.5. Bactericidal tests
The antibacterial activity of the coated cotton fabric could be
traced at very low concentrations of coating. Cultures of the
bacteria were eradicated completely after 1 h of treatment with
the 6% (wt%) coated fabric, and after approximately 1.5 h for
the 1 wt% sample. The results are presented in table 3.
The antimicrobial activity of the silver-coated cotton
fabric containing 1 and 6 wt% of silver corresponds to the
maximal possible silver concentration in the saline solution,
0.13 or 0.78 mg ml−1 , respectively. However, the diffusion of
silver ions from the deposited silver nanoclusters to the saline
is very slow, and only a small part of the total amount of silver
can participate in antibacterial activity. Nevertheless, even the
total possible amount of silver is much less than the minimum
inhibitory concentration (MIC) in a solution that is commonly
used in commercial preparations (10 mg ml−1 ) [10]. More
likely, the observed required time window of 1.5 h to reduce
the initial amount of CFU to zero is due to the velocity
of Ag+ ions, which are responsible for the antibacterial
activity. Thus, the sonochemically prepared silver-coated
fabrics exhibit excellent antibacterial properties, probably due
to the high association of the Ag nanoparticles with the
membrane.
4. Conclusions
Silver nanoparticles were deposited onto the surface of
different fabrics (nylon, polyester and cotton) by ultrasound
Nanotechnology 19 (2008) 245705 I Perelshtein et al

Table 3. Antibacterial activity test using E.coli 1313 and Staph. aureus 195. The viable bacteria were monitored by counting the number of
colony-forming units (CFU); N/No : survival fraction. Results for the control experiment of saline without a fabric were the same as for the
blank.
Duration of treatment
1h 2h
% reduction % reduction
Treatment CFU ml−1 N/N0 in viability CFU ml−1 N/N0 in viability
E. coli
Blank (clean fabric) 1.76 × 107 1 — 1.76 × 107 1 —
6% sample 0 ∼10−8 100 0 ∼10−8 100
1% sample 2.50 × 106 1.43 × 10−1 85.7 0 ∼10−8 100
Staph. aureus
Blank (clean fabric) 1.54 × 107
1 — 2.11 × 107 1 —
6% sample 0 ∼10−8 100 0 ∼10−8 100
1% sample 1.17 × 106 7.60 × 10−2 92.4 0 ∼10−8 100

irradiation. The advantage of the process that is described
in this paper is a simple, efficient, one-step synthesis. The
process produces a uniform coating of silver nanoparticles on
surfaces with different functional end groups. The physical
and chemical analysis has shown that nanocrystalline pure
silver, 80 nm in size, is finely dispersed on the fabric’s surface
without no significant damage to the structure of the yarn. The
coating is stable on the fabric for at least 20 washing cycles
in hot (40 ◦ C) water. The mechanism of the strong adhesion
of silver nanoparticles to the fibers was discussed herein. It is
based on the point melting of the substrate due to the high rate
and temperature of the silver nanoparticles thrown to the solid
surface by sonochemical microjets.
The performance of coated fabrics with nanosilver as an
antibacterial agent was investigated, and the excellent killing
effect of bacteria was demonstrated. The coated fabrics can
have potential applications in wound dressing, bed lining
and as medicinal bandages. The coated fabrics can also
be recommended for the purification of medical and food
equipment, domestic cleaning, etc. Furthermore, the materials
involved in the preparation are cheap, non-toxic and are
commonly available.
Acknowledgment
This research was supported by an EC grant to the LIDWINE
Consortium through contract no. NMP2-CT-2006-026741 of
the 6th EC Program.
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