The study of coloration and antibacterial efficiency of corona activated dyed polyamide and...

Fibers and Polymers 2009, Vol.10, No.5, 650-656

650

The Study of Coloration and Antibacterial Efficiency of Corona Activated Dyed

Polyamide and Polyester Fabrics Loaded with Ag Nanoparticles

Vesna Ili , Zoran Šaponji 1, Vesna Vodnik1, Darka Mihailovi , Petar Jovan i ,

Jovan Nedeljkovi 1, and Maja Radeti *

Textile Engineering Department, Faculty of Technology and Metallurgy, University of Belgrade,

Karnegijeva 4, 11120 Belgrade, Serbia1Vin a Institute of Nuclear Sciences, P.O. Box 522, 11001 Belgrade, Serbia

(Received May 10, 2008; Revised March 18, 2009; Accepted March 30, 2009)

Abstract: The aim of this study was to examine the influence of dyeing on antibacterial efficiency of corona activated polya-mide and polyester fabrics loaded with colloidal Ag nanoparticles as well as the influence of the presence of Ag nanoparticleson the color change of dyed fabrics. C.I. Acid Green 25 and C.I. Disperse Blue 3 were used for dyeing of polyamide fabricsand C.I. disperse violet 8 for polyester fabrics. The color change of polyamide fabrics depends on the dye type, which wasgenerally lower compared to polyester fabrics. Antibacterial efficiency of Ag loaded fabrics was tested against Gram-positivebacterium Staphylococcus aureus and Gram-negative bacterium Escherichia coli. Corona activated polyester and polyamidefabrics showed excellent antibacterial efficiency independently of order of dyeing and Ag loading. The morphology of fibersloaded with Ag nanoparticles was assessed by SEM and atomic absorption spectroscopy for elemental analysis.

Keywords: Ag nanoparticle, Polyester, Polyamide, Corona, Color change, Antibacterial efficiency

Introduction

Nanotechnology is increasingly attracting the attention of

textile industry since it opens up new possibilities for

engineering the textile materials with specific end-use

properties [1]. The concept of nanoparticles (NPs) application

to textile materials relies on development of new technology

that should provide desired effects with long term durability

and stability without use of highly toxic organic compounds.

Recently, the major research interests have been focused on

the application of Ag NPs to different textile fibers for

imparting antimicrobial effects [1-15]. Ag is particularly

convenient for prolonged antibacterial treatments since

bacteria do not become resistant to Ag unlike antibiotics [12].

High surface to volume ratio of Ag NPs and consequently

considerable portion of Ag atoms on the surface of the NPs

that are exposed towards surrounding medium provide an

excellent antibacterial efficiency.

Desirable fiber surface tailoring, from the standpoint of its

functionality, in combination with well known surface

characteristics of NPs can contribute to improvement of their

binding to fibers and durability of obtained effects. Polyamide

(PA) and polyester (PES) fibers, which found widespread

application in the manufacturing of medical, healthcare or

apparel products, are hydrophobic in nature. It is well known

that improvement of wettability and thus, accessibility to

water molecules and hydrophilic NPs can be obtained by

low-pressure plasma activation of fiber surface [4,15,16].

The increased hydrophilicity of fibers is attributed to the

formation of new polar functional groups (hydroxyl, carbonyl,

carboxyl, etc.) on the fiber surface during the plasma

treatment and through post-plasma reactions [17]. In this

study, PA and PES fabrics were activated by corona

discharge at atmospheric pressure.

The synergy between antimicrobial finishing and dyeing is

very important from the technological point of view. So far,

it was barely examined [2,18] and thus, this study was aimed

to highlight the influence of dyeing on antibacterial efficiency

of corona activated PA (CPA) and PES fabrics (CPES)

loaded with colloidal Ag NPs as well as the influence of Ag

NPs on the color change of dyed fabrics. Dyes C.I. Acid

Green 25 and C.I. Disperse Blue 3 were used for dyeing of

PA fabrics and C.I. Disperse Violet 8 for PES fabrics.

Bactericidal efficiency of these systems was tested against

Gram-positive bacterium Staphylococcus aureus and Gram-

negative bacterium Escherichia coli.

Experimental

Material

Desized and bleached PET (PES, 165 g/m2) and Nylon 6.6

(PA, 150 g/m2) fabrics were washed as described elsewhere

[19].

Studies on dyeing were performed with C.I. Acid Green

25 and C.I. Disperse Blue 3 for PA fabrics and C.I. Disperse

Violet 8 for PES fabrics. The characteristics of the dyes are

presented in Table 1.

Corona Treatment of Fabrics

Corona treatment of fabrics was carried out at atmospheric

pressure using a commercial device Vetaphone CP-Lab MK

II. Fabrics were placed on the electrode roll covered with

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*Corresponding author: [email protected]

DOI 10.1007/s12221-010-0650-3

Efficiency of Corona Activated Dyed Polyamide and Polyester Fabrics Fibers and Polymers 2009, Vol.10, No.5 651

silicon, rotating at the minimum speed of 4 m/min. The

distance between electrodes was 2 mm. The power was 900

W and the number of passages was set to 30. The samples

were always dipped into the colloid of Ag NPs 2 hours after

corona treatment.

Loading of Fabrics with Ag NPs

AgNO3 (Kemika) and NaBH4 (Fluka) of p.a. grade were

used without any further purification for the synthesis of

colloid of Ag NPs [20,21]. Briefly, 8.5 mg of AgNO3 was

dissolved in 250 ml of water purged by argon for 30 min.

Under vigorous stirring, reducing agent NaBH4 (125 mg)

was added to the solution and left for 1 h in argon atmosphere.

The concentration of Ag colloid was 50 ppm.

One gram of fabric was immersed in 65 ml of Ag colloid

for 5 min and dried at room temperature. After 5 min of

curing at 100 oC, the procedure was repeated. Subsequently,

the samples were rinsed twice (5 min) with deionized water

and dried at room temperature.

Dyeing of Fabrics

The schematic presentation of dyeing procedure for PA

and PES fabrics is shown in Figure 1. PA fabrics were dyed

in the bath containing 2 % (o.w.f.) acid dye and 4 % (o.w.f.)

Na2SO4 at liquor-to-fabric ratio of 60:1 and pH 4. Dyeing of

PA fabrics with disperse dye was carried out in the bath

containing 2 % (o.w.f.) dye at liquor-to-fabric ratio of 60:1

and pH 5. The pH values were adjusted with CH3COOH

(30 %). PES fabrics were dyed in the bath containing 1 %

(o.w.f.) disperse dye, 1 g l-1

CHT dispergator (Bezema) and

0.5 ml l-1 CH3COOH (30 %) at liquor-to-fabric ratio of 25:1

and pH 5. Fabrics were subsequently washed in the bath

containing 0.5 % Felosan RG-N (Bezema) at liquor-to-

fabric ratio of 40:1. After 30 min of washing at 40 oC,

fabrics were rinsed once with warm water (40 oC) for 3 min

and four times (3 min) with cold water. Afterwards, the

fabrics were dried at room temperature.

Methods

The shape and size of Ag NPs were determined using

transmission electron microscope (TEM) Philips EM-440

operating at 100 kV. Samples for TEM measurements were

prepared by placing a drop of Ag colloid onto a holey

carbon-coated standard copper grid (400 mesh) and evaporating

the solvent.

The UV/VIS absorption spectra of the silver colloid and

the UV/VIS reflectance spectra of PA and PES fabrics were

measured using a Thermo Evolution 600 spectrophotometer.

Fiber morphology was observed by scanning electron

microscope (SEM) JEOL JSM 6460 LV. Gold layer was

deposited on the samples before the analysis.

The elemental analysis of CPA and CPES fabrics loaded

with Ag NPs was done using a Perkin Elmer 403 atomic

absorption spectrometer (AAS).

Color coordinates of the dyed fabrics (CIE L*, a*, b*) were

determined with Datacolor SF300 spectrophotometer under

illuminant D65 using the 10o standard observer. On the basis

of measured CIE color coordinates, color difference (∆E*)

was determined as:

∆E* = (1)

where:

∆L*: the color lightness difference between treated (dyed

fabric loaded with Ag NPs) and control (dyed untreated

a*∆( )

2

b*∆( )

2

L*∆( )

2

+ +

Figure 1. Dyeing procedures for (a) PA and (b) PES fabrics.

Table 1. The characteristics of studied dyes

Dye Manufacturer Molecular structure

AG 25

C.I. Acid Green 25

(Ortolgreen B)

BASF

DB3

C.I. Disperse Blue 3

(Colliton blue FFR)

BASF

DV8

C.I. Disperse Violet 8

(Palanil violet 3B)

BASF

652 Fibers and Polymers 2009, Vol.10, No.5 Vesna Ili et al.cé

fabric without Ag) samples, ∆a*: red/green difference

between treated and control samples, ∆b*: yellow/blue

difference between treated and control samples.

The influence of dyeing on antibacterial efficiency of

fabrics was quantitatively evaluated using a Gram-positive

bacterium Staphylococcus aureus ATCC 25923 and Gram-

negative bacterium Escherichia coli ATCC 25922. Bacterial

inoculum was prepared in the trypton soy broth (Torlak,

Serbia), which was used as a growing medium for bacteria,

and potassium hydrogen phosphate buffer solution (pH 7.2)

as a testing medium. Bacteria were cultivated in 3 ml of

trypton soy broth at 37 oC and left overnight (late exponential

stage of growth). 70 ml of sterile potassium hydrogen

phosphate buffer solution was added to sterile Erlenmeyer

flask (300 ml), which was then inoculated with 0.7 ml of a

bacterial inoculum. Time zero counts were made by

removing 1 ml aliquots from the flask which were diluted

with phosphate buffer. 0.1 ml of the solution was placed

onto a trypton soy agar (Torlak, Serbia) and after 24 h of

incubation at 37oC, the zero time counts (initial number of

bacterial colonies) of viable bacteria were made.

One gram of sterile fabric cut into small pieces was put in

the flask and shaked for 1 h. One hour counts were made in

accordance with above described procedure.

The percentage of bacteria reduction (R, %) was calculated

using the equation (2):

R = (2)

where, C0 (CFU-colony forming units) is the number of

bacteria colonies on the control fabric (dyed untreated fabric

without Ag) and C (CFU) is the number of bacteria colonies

on the dyed fabric loaded with Ag NPs.

Results and Discussion

The absorption spectrum of colloidal Ag NPs exhibited a

strong surface plasmon resonance band with maximum at

380 nm (Figure 2). The position of symmetric plasmon

resonance band and its half-width (fwhm, ∆λ=46 nm)

indicate narrow size distribution without undesired aggregation.

TEM analysis of colloidal Ag NPs revealed nearly spherical

Ag NPs with average diameter of about 10 nm (inset in

Figure 2).

In order to enhance the interaction between hydrophilic

colloidal Ag NPs and hydrophobic fibers, PA and PES

fabrics were treated by corona discharge. The deposition of

Ag NPs on CPA and CPES fabrics was followed by

measuring UV/VIS reflectance spectra (Figure 3). The color

of fabrics after Ag loading turned from white to yellow-

beige, which is in accordance with the changes obtained in

reflectance spectra and literature data [4]. The decrease in

reflectance intensity at ~ 415 nm corresponding to plasmon

resonance band of silver particles is noticeable in Figure 3.

C0 C–

C0

-------------- 100×

Figure 2. Absorption spectrum of Ag NPs in aqueous solution;

inset: TEM image of Ag NPs.

Figure 3. Reflectance spectra of control (untreated fabrics that

were not dyed) and corona activated (a) PA and (b) PES fabrics

loaded with Ag NPs.


However, the shift of plasmon resonance band to lower

energies compared to the position of plasmon band of non-

agglomerated Ag NPs in initial aqueous solution (380 nm)

appeared. This is suggested to be due to higher dielectric

constant of the surrounding medium caused by the inter-

particle coupling of Ag NPs agglomerated on the fiber

surface [21]. Plasmon resonance band of Ag NPs deposited

on CPES fabrics is stronger compared to resonance band of

Ag NPs deposited on CPA fabrics. This is in good agreement

with the values of color differences between corona treated

fabrics loaded with Ag NPs and control fabrics (untreated

fabrics that were not dyed) which are expressed via ∆E*,

∆L*, ∆a* and ∆b* values in Figure 3.

The greater color changes induced by loading of Ag NPs

onto CPES fabrics (∆E*=15.663) compared to CPA fabrics

(∆E*=9.405) is in good correlation with Ag contents in

corresponding samples obtained by elemental analysis using

an atomic absorption spectrometry. The elemental analysis

revealed that 4.46 and 8.61 µg of Ag was found per one

gram of CPA and CPES fabrics, respectively [19]. Evidently,

almost double amount of Ag retained onto CPES fabrics

compared to CPA fabrics. The higher content of Ag NPs on

the PES fibers indicates their stronger binding most likely

due to the existence of benzene rings in polymer structure. It

is well known from SERS (Surface-Enhanced Raman

Spectroscopy) studies of benzoic acid and its derivates on

Ag NPs that the strong interaction between Ag surface and

benzene rings can be established [22,23].

The presence of Ag NPs on CPA and CPES fabrics can be

also confirmed by SEM analysis. SEM images of CPA and

CPES Ag loaded fibers are shown in Figure 4. The Ag NPs

aggregated into quite big assemblies on the CPA fabric

(Figure 4(a)). Unlike CPA, the surface of the CPES fibers

was covered with much smaller, uniformly dispersed

aggregates with dimensions mainly ranging from 20-60 nm

(Figure 4(b)). Additionally, almost spherical Ag NPs can be

observed with approximate diameters around 10 nm,

corresponding to results of TEM analysis of colloidal Ag

NPs (Figure 2).

Taking into account a strong impact of fiber surface

modifications on dyeability of textiles, the influence of

loading of colloidal Ag NPs onto CPA and CPES fabrics

before and after dyeing on color change of fabrics was

evaluated by measuring reflectance spectra. The color

changes were expressed via CIELAB color coordinates.

Colorimetric data for control, corona treated (CPA, CPES)

and corona activated fabrics loaded with Ag NPs (CPA+Ag,

CPES+Ag) before and after dyeing are given in Table 2. The

results indicate that corona treatment of PA fabrics dyed

with AG25 and PES fabrics dyed with DV8 caused the color

changes that cannot be visually detected since the values of

color difference (∆E*) were less than one. However, corona

treatment brought about visible color change of PA fabrics

dyed with DB3 (∆E*=1.753).

The color of CPA fabrics dyed with AG25 was slightly

affected by Ag loading independently of the order of the

operations as can be seen from the low ∆E* values (∆E*<1).

In contrast, the loading of Ag NPs onto CPA fabrics before

and particularly after dyeing with DB3 induced a considerable

color change: the fabrics became less red and less blue.

Similar behavior occurred in the case of Ag loaded CPES

fabrics dyed with DV8, which appeared to be darker, less red

and less blue. High value of color difference particularly

when the Ag loading was performed after dyeing of CPES

fabric (∆E*=23.575) indicates also the remarkable change in

the fabric hue. The increased greenness and decreased

blueness are attributed to the presence of Ag NPs on the

fabrics. This change was indicated by the reflectance curves

of PA and PES fabrics that were not dyed (Figure 3), whose

color turned from white to yellow after loading of Ag NPs

and thus, affected the color of dyed fabrics.

Corona treatment itself does not impart any antibacterial

properties to PA and PES fabrics (Table 3), but our previous

studies indicated that CPA and CPES fabrics loaded with Ag

NPs showed excellent antibacterial efficiency and laundering

durability of obtained antibacterial effects [19,24]. However, in

this study the influence of order of operations i.e. dyeing and

loading of Ag NPs onto CPA and CPES fabrics on their

Figure 4. SEM images of Ag loaded (a) CPA and (b) CPES fibers.


antibacterial properties against Gram-positive bacterium S.

aureus and Gram-negative bacterium E. coli were examined.

Antibacterial efficiency of CPA and CPES fabrics loaded

with Ag NPs before and after dyeing is presented in Tables 4

and 5, respectively. Ag loaded CPES fabrics exhibited

extraordinary antibacterial efficiency for both bacteria

independently of the order of the operations. Similar antibacterial

efficiency is noticed for the Ag loaded CPA fabrics dyed

with DB3. However, the importance of order of Ag loading

and dyeing of CPA fabrics with AG25 becomes more

prominent. The Ag loading onto CPA fabrics after dyeing

with AG25 induced good antibacterial efficiency for both

bacteria. The opposite order of operations slightly affected

the bacterial reduction of E. coli while the bacterial

reduction of S. aureus became minor and these fabrics can

be considered inactive.

CPES and CPA Ag loaded fabrics showed excellent

Table 2. Colorimetric data for PA and PES fabrics loaded with Ag NPs before and after dyeing

Dye Sample L* a* b* ∆E* Description

AG25

Control* 30.16 -25.40 -4.72

CPA 29.46 -25.38 -4.71 0.698 Darker

Ag loading before dyeing

CPA+Ag 30.33 -25.50 -4.79 0.213 Lighter, greener

Ag loading after dyeing

CPA+Ag 29.67 -25.25 -4.47 0.567 Darker, less green, less blue

DB3

Control* 34.80 6.15 -44.78

CPA 33.33 6.96 -44.26 1.753 Darker, redder, less blue


CPA+Ag 34.97 4.49 -42.76 2.617 Lighter, less red, less blue


CPA+Ag 33.96 3.00 -38.82 6.789 Darker, less red, less blue

DV8

Control* 43.38 14.55 -39.52

CPES 43.53 14.42 -39.21 0.377 Lighter, less red, less blue


CPES+Ag 42.65 13.28 -37.31 2.654 Darker, less red, less blue


CPES+Ag 40.55 3.92 -18.67 23.575 Darker, less red, less blue

*Dyed untreated fabric without Ag.

Table 3. Bacterial test of corona activated PA and PES fabrics

Sample Bacteria

Initial number of

bacterial colonies

(CFU)

Number of

bacterial colonies

(CFU)

Control PA

S. aureus 1.4×105

5.2×104

CPA 1.0×105

Control PES 2.9×104

CPES 2.8×104

Control PA

E. coli 3.2×105

2.7×105

CPA 2.6×105

Control PES 5.9×104

CPES 7.4×104

Table 4. Antibacterial efficiency of corona activated PA and PES

fabrics loaded with Ag NPs before dyeing

Dye Sample

Initial number

of bacterial

colonies

(CFU)

Number of

bacterial

colonies

(CFU)

R, %

S. aureus

AG25Control PA*

4.9×1052.3×105

CPA+Ag 1.4×105 39.1

DB3Control PA*

1.3×1055.6×104

CPA+Ag 150 99.7

DV8Control PES*

3.0×1052.5×104

CPES+Ag <10 99.9

E. coli

AG25Control PA*

3.9×1052.2×105

CPA+Ag 2.0×103 99.1

DB3Control PA*

3.9×1051.3×105

CPA+Ag 20 99.9

DV8Control PES*

3.0×1058.5×104

CPES+Ag <10 99.9



antibacterial efficiency in the case of dyeing with disperse

dyes. However, with respect to results on color change and

from technological point of view, the Ag loading after

dyeing should be avoided in order to minimize the effect of

increased yellowing. To achieve optimum antibacterial effect,

the loading of Ag NPs onto CPA fabrics is recommended to

be run after dyeing with AG25 and this order of operation

does not have negative influence on color change.

Conclusion

The order of loading of Ag NPs and dyeing affected the

color of corona activated PA and PES fabrics. CIELAB

colorimetric data showed that color of corona activated PA

fabrics dyed with C.I. Acid Green 25 was slightly influenced

by Ag loading independently of the order of the operations.

On the contrary, the loading of Ag NPs onto corona

activated PA fabrics before and particularly after dyeing

with C.I. Disperse Blue 3 induced considerable color

change. The most prominent color change occurred on

corona activated PES fabrics, which were loaded with Ag

NPs after dyeing with C.I. Disperse Violet 8.

The increased greenness and decreased blueness of

studied fabrics can be attributed to the presence of Ag NPs

on the fabrics. Their existence was proved indirectly by

reflectance curves of PA and PES fabrics that were not dyed,

whose color turned from white to yellow after loading of Ag

NPs. This was more pronounced in the case of corona

activated PES fabrics due to higher content of Ag NPs,

which was confirmed by atomic absorption spectrometry.

Antibacterial efficiency of corona activated PA and PES

fabrics against E. coli is independent of the order of dyeing

and loading of Ag NPs. All fabrics exhibited excellent

antibacterial efficiency against S. aureus except corona

activated PA Ag loaded fabric, subsequently dyed with C.I.

Acid Green 25. Taking into account the results on color

change, the Ag loading before dyeing is recommended for

corona activated PA and PES fabrics dyed with disperse

dyes. The opposite order is suggested to be more efficient if

the fabrics are dyed with C.I. Acid Green 25.

Acknowledgements

The financial support for this work was provided by the

Ministry of Science of Republic of Serbia (Eureka project

NANOVISION E! 4043 and project 142066). We gratefully

acknowledge M. Bokorov (University of Novi Sad, Serbia)

for providing SEM measurements.

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Table 5. Antibacterial efficiency of corona activated PA and PES

fabrics loaded with Ag NPs after dyeing

Dye Sample

Initial number

of bacterial

colonies

(CFU)

Number of

bacterial

colonies

(CFU)

R, %

S. aureus

AG25Control PA*

4.9×1052.3×105

CPA+Ag 3.9×102 99.8

DB3Control PA*

2.4×1051.3×105

CPA+Ag <10 99.9

DV8Control PES*

3.0×1052.5×104

CPES+Ag <10 99.9

E. coli

AG25Control PA*

3.6×1059.3×104

CPA+Ag <10 99.9

DB3Control PA*

3.6×1051.9×105

CPA+Ag <10 99.9

DV8Control PES*

3.0×1058.5×104

CPES+Ag <10 99.9



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