Zarei 2013

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In situ growth of Zinc Oxide Nanoparticles on cotton fabric usingSonochemical Method

Leila Zarei 1, a , Sheila Shahidi 2, Seyed Mohammad Elahi 3

and arash Boochani 4 1 Department of Physics, Science and Research branch of Kermanshah, Islamic Azad university,

Kermanshah, Iran 2Department of Textile, Islamic Azad University, Arak Branch, Arak, Iran

3 Plasma Physics Research Center, Science and Research Branch, Islamic Azad University,Tehran, Iran

4 Department of Physics, Science and Research branch of Kermanshah, Islamic Azad university,Kermanshah, Iran

a [email protected]

Keywords: ZnO Nanoparticles; In-Situ; Antibacterial; Fabric.

Abstract. Researches show that properties of semiconductor materials such as electrical, opticaland antibacterial properties can be improved in the nano scale. Among the semiconductor materials, zinc oxide with excellent electronic properties has been considered extremely. Application and

properties of Zno nanoparticles depends on the size and morphology. In the present work, Zno Nanoparticles(NPs) were prepared by sonochemical method at a constant temperature and wereapplied on to the 100% cotton woven fabric using Insitu method. The results show thatnanoparticles with average sizes of 20-100 nm with different morphologies were created on thesurface of samples. Synthesis of ZnO -NPs were varied in the morphological transformation bychanges in zinc acetate concentration. Characterizations were carried out, Scanning electronmicroscopy (SEM) and Spectrophotometery. The antibacterial activities of the fabrics were assessedsemi-quantitatively by the coloneis count method. The results show that the finished fabricdemonstrated significant antibacterial activity against S.aureus in antibacterial test.

Introduction

In recent years, much attention has been paid to creating more comfortable living conditions,especially for health and hygiene. For example, fabrics treated with antimicrobial agents are used tosuppress bacteria, molds, algae and microorganisms that cause some health-concerned problemssuch as corruption, spots, and odor.[1 - 3] Antimicrobial agents are natural or synthetic compoundsthat inhibit microbial growth. Various classes of antimicrobial agents are used in the textileindustry, most of which are biocides. The use of inorganic material has advanced rapidly due to theamount of work done towards the synthesis and modification of particles for biomedicalapplications. Many heavy metals and metal oxides either in their free state, or in compounds at verylow concentrations, are toxic to microbes. These inorganic materials kill bacteria through variousmechanisms, such as by binding to intracellular proteins and inactivating them, generation ofreactive oxygen species and via direct damage to cell walls. [4- 7]

Recently, synthesis of inorganic materials with specific size and morphology has attractedsignificant attention due to their possible use in different fields [ 8- 9]. Of the inorganic materials,metal oxides such as TiO2, ZnO, MgO and CaO are of particular interest as they are not only stableunder harsh process conditions but also generally regarded as safe materials to human beings and

animals.[10 - 12] The application of nanoparticles to textile materials has been the object of severalstudies aimed at producing finished fabrics with different performances [13,17] The use ofnanoparticles of silver and zinc oxide has been seen as a viable solution to stop infectious diseasesdue to the antimicrobial properties of these nanoparticles [10 , 13]. In this nanosized range, they are

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expected to possess interesting physical properties and pronounced coupling quite different fromtheir bulk counterpart.[18] Zinc oxide (ZnO) exhibits several unique properties, such assemiconducting and piezoelectric behavior, and it is consequently used in a wide variety of sensorsand actuators, Zno nanostructures have been explored for a wide range of applications in nanoscaleand microscale devices, such as generators, sensors , field–emission transistors ultraviolet

photodetectors, and in biomedical systems, such as ultrasensitive DNA sequence detectors [18] anddermatological and antibacterial properties[5-6] . Antibacterial effect of ZnO-NP on textiles hasalready been shown by various researchers[19, 20, 21, 30]. Recently, it is aimed to reduce thenumber of production steps , energy and costs required for production. It should also be possible torecycle the majority of the chemicals for reuse in the process rather than disposal. Currently, thesynthesis approaches of nano-ZnO are various, which are mainly divided into three kinds: the solid,the solution and the vapor phase methods [5,22]. Sonochemical method is a green and feasibletechnique [18]. The sonochemical method has been proven to be a useful technique to obtain novelmaterials with interesting properties. It is based on acoustic cavitation resulting from the continuousformation, growth and implosive collapse of bubbles in a liquid. This method has been used forsynthesis of many kinds of nanomaterials so far.[9, 23] In this study, the simple method was used toin-situ grow ZnO nanoparticles on the cellulose fiber. The ease and availability of materials andreaction conditions in this method makes it possible to accomplish mass production. This methodgives rise to advantages such as large deposition area, uniform deposits on the objects, the desiredshapes, and short processing time.

Experimental

Materials zinc acetate (Zn(CH 3COO) 2.2H 2O), ethanol and sodium hydroxide were purchased frommerc. The samples used in this investigation were plain weave 100% cotton fabrics supplied by theBaft Azadi Co. (Tehran, Iran).

Synthesis of ZnO nanoparticles To prepare the ZnO nanoparticles,100 ml of NaOH solutionwith a concentration of 0.1 M were added to 25ml of the 0.05 , 0.1 , 0.2 , 0.4 Mol solutions ofZn(CH 3COO) 2.2H 2O in ethanol, to prepared solutions at room temprature followed by stirring for5 min. The mixtures were sonicated for 1h with 60W ultrasound power. The ultrasonic generatorautomatically adjusted the power level. The wave amplitude in each experiment was adjusted asneeded. All these process were carried out at room temperature without any specific conditions. Thesolutions were heated by 75 for 1 hour until ethanol was evaporated and powders of ZnO-NPs wereobtained. The homogeneous solutions became a milky solution after 1 min. After stirring at 75 0 Cfor 1 h the ethanol was evaporated and ZnO nano particles were obtained.

Characterization of ZnO nanoparticles The morphology and size of the prepared ZnOnanoparticles was observed using a Scanning Electron Microscope (SEM) (KYKY, 3200 EM). Allof the samples were gold coated before conducting the SEM examination .

In-situ growth of ZnO nanoparticles on cotton fabrics All samples of fabrics (10 × 10 cm 2) before treatment were scoured at 80 oC for 30 min by nonionic detergent solution (0.5 g/L) toremove wax, grease and other impurities. Then these samples were rinsed five times by water andcured in a curing oven (Memmert ULE800 Universal Oven, Germany) at 80 oC for 5 min.

Four pieces of prepared fabrics were added to the mentioned solution of ethanol and zinc acetatewith different concentration of 0.05, 0.1, 0.2 and 0.4 M. Then 100 mL of sodium hydroxide with aconcentration of 0.1M were added to prepared solutions at room temperature followed by stirringfor 5 min. The mixtures were sonicated for 1h with 60W ultrasound power.

The cotton fabric was then taken out from the solution, washed three times with DD water. Thefabric was dried in the curing oven at 80 oC for 10 min. The specimen was then conditioned for 24 h

under standard condition (humidity: 65 ± 2%, temperature: 21 ± 1o

C).Characterization of ZnO nanoparticle treated cotton The morphology of the fabrics wasobserved using a Scanning Electron Microscope (SEM) (KYKY, 3200 EM). All of the sampleswere gold coated before conducting the SEM examination . An EDX unit connected to a scanningelectron microscope was used to determine the percentage of the atomic contents of elements

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presented in the treated fabrics. For Bacteria counting test, Luria Bertani media (LB) broth was usedas growing medium for Staphylococcus aurous. Bacteria were dripped in 10 mL of LB broth toreach a cell concentration of 1×10 8 (CFU)/mL. Then it was diluted to a cell concentration of 1×10 5 (CFU)/mL. 1cm×1cm size fabric sample was cut and put into 1mL Bacteria suspension. Allsamples were incubated for 24 h at 37 o C. From each incubated sample, 100 µL of solution was

taken and distributed onto an agar plate. All plates were incubated for 24 h and colonies formedwere counted. The percentage reduction was determined as follows:

Reduction (%) =(C-A)/C (1) where C and A are the colonies counted from the plate of the control and treated sample,respectively.

Results and Discussion

Figure 1 SEM images of ZnO nanoparticles

Figure 2 SEM images of ZnO-NPs on In-situ cotton samplesIn the present work, Zno nanoparticles were prepared by sonochemical method at a constant

temperature and were applied on to the 100% cotton woven fabric using In-situ method. The

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morphology, structure and size of prepared nano particles were observed using a Scanning ElectronMicroscope. The SEM images of prepared ZnO- NPs with different concentration of zinc acetateare shown in Figure 1.

Figure 1 indicates that the original morphology of the particles is approximately spherical withthe diameter varying between 20-100 nm. As it is observed the size of the particular has become

larger by increasing concentration. The average particle size in case of using 0/05 M of zinc acetateis about 24 nm. By increasing the concentration of zinc acetate to 0/2 M and 0.4M, the average

particle size increase to 45nm and 98nm, respectively. The SEM images of in situ ZnO-NPs treatedcotton with different concentration of zinc acetate are shown in Figure 2. As it is seen, by increasingthe concentration of zinc acetate, more amounts of ZnO-NPs are deposited on the surface of cottonfabric.

EDX method was used for the identification of ZnO nanoparticles in the surface of samples. Theresults are shown in Figure 3. As it is seen the amount of ZnO nanoparticles are on the surface of insitu samples. There are a good match between the SEM figures and EDX results.

Figure 3 The EDX results of the In-situ treated samples

Figure 4 Antibacterial activity results of ZnO-NPs for In-situ treated fabric


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For testing the antibacterial activity of the samples, bacterial counting test were used. Fig. 4illustrate the test results for the untreated and In-situ treated fabric. This control test shows that theuntreated fabric does not have any antibacterial properties(fig.4(untreated)), but the ZnO-NP -treated samples have very good antibacterial activity.

A study by Yamamoto et al . [24], stated that the presence of reactive oxygen species (ROS)

generated by ZnO nanoparticles is responsible for their bactericidal activity. Zhang et al ., furthershowed that the antibacterial behaviour of ZnO nanoparticles could be due to chemical interactions

between hydrogen peroxide and membrane proteins, or between other chemical species produced inthe presence of ZnO nanoparticles and the outer lipid bilayer of bacteria. The hydrogen peroxide

produced enters the cell membrane of bacteria and kills them. It was shown in the study that nanosized ZnO particles are responsible for inhibiting bacterial growth [25-27]. Padmavathy andVijayaraghavan, further elucidated the bactericidal activity of ZnO nanoparticles. According tothem, once hydrogen peroxide is generated by ZnO nanoparticles, the nanoparticles remains incontact with the dead bacteria to prevent further bacterial action and continue to generate anddischarge hydrogen peroxide to the medim [28-29]. Our results correspond with the results of theauthors above, showing that ZnO nanoparticles applied on to fabrics have an excellent antimicrobialactivity.

Conclusion

In this research work, cotton fabrics were applied with various concentration of zinc acetate by in-situ method. The SEM images show that particles have spherical shape with the diameter varying

between 20-100 nm . after treatment , some particles appear on the cases of loading samples withZnO-NPs. The antibacterial activity of untreated and treated samples was investigated by bacterialcounting test method. The results show very good antibacterial activity for ZnO-NPs on In-situtreatment samples ; however, the efficiency of antibacterial activity for 0/05mol of In-situ samplewere decreased slightly. Our results shows that ZnO-NPs applied on to fabrics have an excellentantimicrobial activity.

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