Effect of Capping Agent on Structure, Composition, and Optical Properties of Low-Cost Chemically Deposited Zinc Oxide Thin Films and Their Antibacterial Activities

Thanikaikarasan, S.; Amutha, C.; Natarajan, B.; Dhanasekaran, D.; Rajkumar, S.

doi:https://doi.org/10.1155/2023/7187387

Bioinorganic Chemistry and Applications

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Abstract Introduction Results and Discussion Conclusions Data Availability Conflicts of Interest Acknowledgments References Copyright Related Articles

Research Article | Open Access

Volume 2023 | Article ID 7187387 | https://doi.org/10.1155/2023/7187387

Effect of Capping Agent on Structure, Composition, and Optical Properties of Low-Cost Chemically Deposited Zinc Oxide Thin Films and Their Antibacterial Activities

S. Thanikaikarasan,¹C. Amutha,²B. Natarajan,²D. Dhanasekaran,³and S. Rajkumar⁴

Academic Editor: Chun Xu

Received24 Dec 2022

Revised16 Apr 2023

Accepted07 Oct 2023

Published23 Oct 2023

Abstract

In the present report, pure zinc oxide and albumen-capped zinc oxide thin films were deposited on a glass substrate by a simple chemical method. The growth rate of the deposited film increases by means of number of dipping linearly. The films deposited were subjected to XRD, SEM, EDX, and UV-visible spectroscopy to analyze the crystal structure, morphology, composition, and optical properties. Structural feature reported that the deposited films were found to be a wurtzite structure. The degree of crystallinity depends on film thickness with deposition time per cycles. The parameters related to film structure, such as stress, strain, dislocation density, lattice constant, and bond length, were determined. The values of the fundamental absorption edge were at 3.28 and 3.06 eV for the deposited films of pure zinc oxide and albumen-capped zinc oxide, respectively. Photoluminescence measurements indicated that the peaks of emission were found to be 375 and 340 nm for zinc oxide and albumen-capped zinc oxide. The effects of an antibacterial activity against different positive and negative bacteria sources were determined.

1. Introduction

Transparent conducting oxides found extensive application in liquid crystal displays, transducers, and solar cells. The efficiency of the devices strongly depends upon materials, important key properties, high electrical conductivity with its transparency [1–3]. The materials such as cadmium oxide, indium oxide, and tin oxide plays a vital role in view of the fact that high transmission above wide spectral range have interesting characteristics such as moderately low cost and stability in the environment of chemistry [4–6]. Zinc oxide (ZnO) found to exist in wurtzite structure with band gap, binding energy values 3.3 eV, 60 meV attracted researchers to fabricate efficient optoelectronic devices [7, 8]. ZnO is predicted as an interesting candidate for devices such as gas sensors, solar cells, and photodiodes, and varistors and its different structure with physical, chemical, optical, and biological properties has attracted ZnO for medical and biological applications. ZnO thin films are mostly crystallized in wurtzite and cubic structures. Besides, it is a transparent material with different structures that could be synthesized in different forms of nanostructure [7, 8]. Several physical and chemical methods were employed for the preparation of ZnO thin films with cubic and hexagonal structures [9–14]. The method of SILAR is simply a two-step process for film preparation in which the substrate is immersed in a precursor that consists of sources of cation with anion. The growth of the film deposition takes place consequently when it is dipped in precursors number of times [15]. The continuous reaction at optimized precursor concentration with solution pH values results on the formation of films on the substrate. The ZnO thin film was prepared by dipping the substrate in zinc acetate complex followed by dipping in a hot water bath at the boiling temperature of 95°C. Number of zinc complexes viz., sodium zincate, ammonium zincate prepared from zinc acetate, zinc sulphate, and zinc chloride were used as precursors for cation in film deposition by the SILAR method. The present work focused on the formation of ZnO thin films from ammonium zincate obtained from zinc chloride. The advantages and highlight of the technique is its simplicity of the equipment, ease to control the deposition rate with precursor concentration, and solution of pH values. SILAR is a simple wet chemical route for thin film synthesis in which the formation of film as a building block by ions instead of atoms, where the preparative parameters are controlled easily [16–19]. ZnO doped with individual elements such as Ag, Al, Bi, Cd, Co, Eu, and Mn which has been reported earlier [11, 12, 20–24]. By the comparison of a number of works for ZnO thin films with metallic dopants, few reports highlighted the growth and characterization of ZnO thin films mediated with bio-template such as silk [25], albumen [26], orange juice [26], and pea starch [27].

In the present report, ZnO and albumen-mediated (capped) ZnO thin films were deposited on a glass substrate made from zinc chloride, sodium hydroxide (NaOH), and liquid ammonia (NH₄OH) in addition with albumen as the capping agent by the simple SILAR method. The influence of the capping agent (albumen) on structure, composition, morphology, optical properties, FTIR, and photoluminescence measurement of the deposited films were reported. The effect of antibacterial activity against different bacteria sources was reported.

2. Experimental Details

The chemicals ZnCl₂, NaOH, liquid ammonia were purchased from Sigma Aldrich with 99.99% purity. The commercially purchased microscopic slides were cleaned using chromic acid followed by distilled water and ultrasonic cleaning with acetone and alcohol. The commercially purchased egg white layer (albumen) was used as a capping agent. The substrate was dipped in sodium zincite bath which was kept at temperature around 35°C for a well-known standardized time followed by the immersion process in boiled water for the same time of hydrogenation in which the water is maintained at temperature in the range between 90 and 95°C. Thin films of ZnO grown by the process of two-step chemical bath deposition method from a solution consist of 0.3 M ZnCl₂ and 0.3 M NaOH with a pH value maintained at 9.0 ± 0.1 and bath temperature 90°C under optimized condition. In the first dipping process, the ions in the solution get adsorbed over the substrate produced sodium zincite. Also, by following the same procedure with few number cycles by the incorporation of albumen as the capping agent with 0.3 M ZnCl₂ and 0.3 M NaOH. The prepared films were subjected to the process of annealing by keeping them in a muffle furnace at 300°C for 1 hour, thereafter taking them out to determine structure, morphology, composition, and optical properties. Figure 1 shows the experimental setup used for the preparation of pure and albumen-capped ZnO thin films. Structural feature of the prepared films was determined by an X-ray diffractometer (XPERTPRO PANalytical) with CuKα target radiation (λ = 1.5406 Å). Microscopic view with film composition was analyzed using a JEOL JSM 840 scanning electron microscope. The optical absorbance and transmittance of the deposited films was determined using a SHIMADZU 2000 ultra-violet-visible spectrophotometer. Photoluminescence measurement for the prepared samples was analyzed by PERKIN ELMER LS55 spectrofluorometer. Also, the appearance of bonds in the deposited films was determined using a SHIMADZU 8400S FTIR spectrometer. The effect of antibacterial activity for Gram (+) and Gram (−) sources was determined by disc diffusion method.

3. Results and Discussion

3.1. Film Thickness

The growth rate, deposition of ZnO, and albumen-capped ZnO on glass substrates were controlled by separate variables thickness and surface morphology [28–30]. The zinc chloride complex was prepared by dissolving 3.344 g ZnCl₂ in 250 cc demineralized water to attain a chemical solution of 0.3 M ZnCl₂. The solubility of zinc chloride is difficult leads to produce precipitation of the solution which is dissolved by the incorporation of few drops of acetic acid produces a transparent solution. The transparent solution has the solution pH value of 4.5 ± 0.1 as estimated by digital pH meter (HANNA instruments). The concentration of ZnCl₂ was found to be higher than 0.3 M in addition with 0.075 M NaOH, and particulate absorption takes place on the substrate surface that leads to produce films with poor quality. The molarity of ZnCl₂ was found to be 0.3 M ZnCl₂ and higher amount of 0.075 NaOH was added which leads to increase the pH value upto 9.0 ± 0.1, producing films with higher thickness and well-defined crystallinity. The higher value of NaOH with 0.3 M ZnCl₂ increases the pH value above 9.0 ± 0.1, and there is detachment of film from the substrate not from the layers on the substrate. The dependency of deposition time with films thickness and number of dipping for the deposited films on substrate is shown in Figure 2. Thickness of the deposited films was estimated by the measurement of weight difference for films deposited before and after certain intervals of time deposition on the substrate and the film thickness was determined using the following equation:

It is noted that the film thickness increases linearly with rate of 5 more dippings for both ZnO and albumen-capped ZnO. The observation reflects a small variability in the deposition process arising probably from small experimental scattered in deposition parameters bath concentration, temperature as well as due to the nonuniformity of film from the substrate handling procedure as the deposition is carried out manually. The process has been carried out for ZnO and albumen-capped ZnO thin films.

3.2. Structural Properties

XRD pattern was obtained to identify the nature, structure, and phase of the deposited ZnO and albumen-capped ZnO thin films (Figure 3(a)). Several researchers reported that the ZnO thin films have cubic and hexagonal structures. Figure 3(a) revealed that the prepared films possess polycrystalline nature with a wurtzite structure. There are no additional secondary peaks in the XRD pattern, which denoted the films were devoid of impurities. The position of XRD pattern confirmed that the observation of diffraction angles at 36.32, 47.56, 56.52, 62.23, 66.42, 68.06, and 69.14 corresponds to the planes (100), (002), (101), (102), (110), (103), (200), (112), and (201) with prominent reflection along (101) for the films of pure ZnO with hexagonal crystal symmetry. The observed results were found to be in close agreement with standard file for hexagonal ZnO [30]. The peak intensity of (101) plane is found to be higher when compared with intensities of the all other planes, respectively. The diffraction pattern of albumen-capped ZnO thin films deposited on glass substrate is shown in Figure 3(b). It is evidenced that there is a slight shift in 2θ value when compared with results of pure ZnO. The intensity of (002) plane is maximized, which denoted the ZnO thin films with orientation along c axis when it is deposited additionally with albumen as the capping agent with pure ZnO. The observed characteristic results reported that any peaks corresponding to secondary elements as capping agent not present in EDX pattern as shown in Figure 3(b). There is observation of slight shift in 2θ value of ZnO thin films in addition with albumen as capping agent which produces films with slight difference in 2θ values as shown in Figure 3(b). The growth of ZnO thin films along c axis orientation is greatly favoured by the polar structure of ZnO, and it consists of Zn²⁺ and anion O²⁻ with its high polarity [31]. The observed peak intensity (002) along c axis is found to be a film with higher thickness value which has been measured using weight difference method. The intensity of (002) and (101) plane is found to be higher for films have higher thickness around 1000 nm for ZnO, 960 for albumen-capped ZnO. As the time increases, the thickness of the deposited films tends to increase and thereafter decreases for higher deposition time, due to the overgrowth of the film [31]. The value of average crystallite size with grain sizes was obtained from X-ray line broadening analysis using the Scherrer equation assuming Gaussian-shaped peaks [15]. It is evident that the capping of albumen with ZnO produces variation of structural properties which are peaks of FWHM data, the peak position of diffraction angle 2θ, the crystallite size, lattice constant (c), the dislocation density (δ), and strain (ε) were determined. It is seen from the Table 1 that the lattice constant is found to increase by the addition of lesser amount of the capping agent. The crystallite size of the deposited films is calculated using the following equation: [32]:

The value of force acting on the deposited films to restrict the formation of crystallites on the substrate is calculated using equation (3). Dislocation density and bond length for the ZnO and albumen-capped ZnO thin films were determined using the following equations [15, 29, 31, 33]:

The value lattice constants (“a” & “c”), unit cell volume, c/a ratio, atomic packing factor, and bond length were determined according to the following equations [28]:

The stress value present in ZnO and albumen-capped ZnO has been determined using the following equation:

The estimated value of lattice parameters for ZnO and albumen-capped ZnO thin films is given in Table 1.

3.3. Morphology and Film Composition

Morphological feature along with film composition for ZnO and albumen-capped ZnO was analyzed by EDX with SEM. The SEM image of ZnO and albumen-capped ZnO deposited on glass substrate is shown in Figure 4. It is found that albumen added as a capping agent there is no change in surface morphology for deposited films. A number of crystallites were grouped together to form a grain. The sizes of the grains were found to be between 0.7 and 0.9 μm. The average sizes of the grains were found to be 760 nm. Similar observation for albumen-mediated ZnO thin films reported earlier [34]. EDX spectra recorded for ZnO and albumen-capped ZnO thin films are denoted in Figures 5(a) and 5(b). The observation of emission lines Zn and O present in the investigated energy range indicated the formation of ZnO thin films as EDX spectra as in Figure 4(a). Similarly, the EDX spectra of albumen-capped ZnO thin films represent the Zn and O emission lines in the investigated energy range, but there are no impurities excluding albumen that can be acted as a capping agent in the deposited films. The capping agent added produces a slight change in stoichiometric ratio of Zn and O of the deposited films on the substrate (Figure 5(b)).

(a)

(b)

(a)

(b)

3.4. Ultraviolet Visible Spectroscopy

The investigation of semiconductors by the route of optical absorption provides scientific explanation, concerning the band structure and the energy gap value of the deposited films. The percentage of absorption, transmittance for the deposited ZnO, and albumen-capped ZnO films was estimated using a SHIMADZU spectrophotometer. The band gap value of the deposited films was determined using the following equation:

The absorbance spectra recorded for ZnO and albumen capped ZnO thin films are shown in Figure 6. It is noted that the deposited films had less absorption in the visible region. The behavior of absorption spectra which may be dependent upon film thickness deposited and also, there is a correlation between transmittance and absorbance of the deposited films. The band gap value of the deposited films was obtained by the extrapolation of linear portion of the energy axis at zero absorption coefficient (Figure 7). The band gap value was found to be 3.28 and 3.61 eV for ZnO and albumen-capped ZnO, respectively [34, 35]. There is a shift in the band gap value which can be due to the thickness value of the deposited films. Similar behavior was exhibited by albumen-capped ZnO films that were reported earlier [35].

3.5. FTIR Spectroscopy

FTIR spectroscopy is an important analytical tool to categorize the chemical bonds, composition, and element present in the deposited ZnO and albumen-capped ZnO thin films. The spectroscopic observation was carried out in between the wave number 400 and 4000 cm⁻¹. Figure 8 shows the FTIR spectra recorded for ZnO and albumen-capped ZnO thin films deposited on glass substrate. The peak appearance at 848 cm⁻¹ responds to stretching mode of Zn-O bond present in the deposited films. The peak appeared at 1450 cm⁻¹ which is responsible for asymmetric, symmetric stretching modes of C=O bonds in addition with associated with present in the deposited films after certain intervals of time as indicated in Figure 7(a) [36]. The FTIR spectra recorded for albumen-capped ZnO thin films deposited on glass substrate is shown in Figure 7(b). The observed peak intensity at 1585, 1018 cm⁻¹ which may be attributed to C=C, Zn-O bands indicates capping effect of albumen with ZnO. The transformation of OH⁻ organic phase takes place due to the abovementioned process. The appearance of broad absorption peak at 3400 cm⁻¹ is probably due to superimposition of N-H stretching of amide group at 3450 cm⁻¹ by the bio-template and O-H stretching mode of water molecules. Besides, the appearance of some of the absorption bands in the range between 1316 and 1585 cm⁻¹ may be due to C=O and C=C stretching modes of albumen as well as the new peak observed at 2900 cm⁻¹ due to symmetric and asymmetric C-H bonds, respectively. The observed results are in close agreement with the results reported earlier [37]. The observed bands at 1557 and 3452 cm⁻¹ may be due to stretching frequency of OH group absorbed at ambient atmosphere [38].

3.6. Photoluminescence

Photoluminescence measurements were taken out to identify the observation of peak shift emission for films of ZnO and albumen capped ZnO. The photoluminescence spectra of for ZnO and albumen-capped ZnO thin films obtained by the SILAR technique are shown in Figure 8. It is noted that there is strong that peak emission at 440 nm corresponding to blue emission has been observed due to the process of surface defect in ZnO mainly due to Zn vacancy and weak green emission band approximately at 500 nm known as a deep level emission related to the states of defect in the deep level [16]. The oxygen vacancy present in single ionized level which is responsible for this green emission in the ZnO [17]. It may result from the process of recombination of photo-generated hole with an electron occupying the oxygen vacancies with interstitials of zinc. The albumen capped ZnO thin films denoted peak emission at wavelength 380 nm, and they also have a weak blue emission peak located at 420 nm (Figure 8(b)). The ultraviolet emission is known as a near-band emission, originating from the recombination of free exciton through an exciton-exciton collision process [18]. In all the samples, the emission of ultraviolet was found to be most prominent. But the albumen capped with ZnO thin films sample a dramatic change in emission spectrum was observed. The observation of ultraviolet emission peaks at 440–500 nm (Z₃g and Z₆g) (with the blue shift of single emission peak), which is considered as a signature of charge transfer reaction [19].

3.7. Antibacterial Activity

The efficiency of antibacterial activity for ZnO and albumen-capped ZnO thin films were tested by disc diffusion method. The samples such as ZnO and albumen-capped ZnO deposited on glass substrate were taken out from the substrate by the process of scratching method and the powder sample with diameter of zone of inhibition around the membranes after 24 hours were measure as 12, 10, 5, 3, 5, and 14 mm for Escherichia coli, Pseudomonas aeroginosa, Streptococcus agalactiae, Staphylococcus auereus, Salmonella typhimurium, and Klebsiella pneumonia, respectively. Pure ZnO and capped ZnO powder taken out from the substrate and the sample diameters of the zone of inhibition around the membranes after 24 hours were measured as 12, 10, 5, 3, 5, and 14 mm for E coli, Paerogi-nosa, Sagalactiae, Staphylococcus auereus, Salmonella typhimurium, and Klebsiella pneumonia, respectively. After 48 hours of incubation, the diameter of the zone of inhibition was found to increase as shown in Figure 9. Pure ZnO have low antibacterial activity against E. coli was investigated. The albumen capped ZnO sample diameters of the zone of inhibition around the membrane after 24 hours were measured at 18, 9, 12, 5, and 8 mm for E. coli, P. aeroginosa, S. agalactiae, S. auereus, S. typhimurium, and K. pneumonia, respectively. The zone inhibition diameter of samples found to increase after 48 hours which is shown in Figure 10. As a result, the samples influence strong influence against sources such as E. coli than S.auereus, and such observation found to close agreement with value reported earlier [25–27, 39]. The cell nature with structure is one the favourable reason for difference in sensitivity. The formation zone of inhibition has clearly indicated the antibacterial activity against ZnO nanostructure. The value of zone inhibition of different bacteria sources for ZnO and albumen capped ZnO thin films at 24 and 48 hours is given in Table 2. We have concluded that albumen capped ZnO found to exhibit higher value antibacterial activity for E. coli and S. auereus bacterial than ZnO (see Figure 11).

4. Conclusions

The aim of this research report was to explain the effect of albumen as capping agent with ZnO thin films prepared by the simple SILAR method. Structural properties reported that the prepared films exhibited hexagonal structure with orientation along (101) and (002) for ZnO and albumen capped ZnO. Microscopic observation reported that the films have grain such as structure with low density. EDX analysis reported that the replacement of capping agent in addition with the presence of elements as stoichiometry (Zn:O) in the deposited films. The shift in energy gap was determined as 3.28, 3.61 eV for the deposited ZnO and albumen-capped ZnO with different film thickness values. FTIR results indicated that the appearance stretching mode at 848 cm⁻¹, 1018, cm⁻¹ corresponding to Zn-O, whereas the band in present at 1585 cm⁻¹ corresponding C=C response to effect of capping agent albumen with ZnO. The appearance of band absorbance in between 1316 and 1585 cm⁻¹ corresponding stretching modes of albumen also the new observed peak at 2900 cm⁻¹ corresponding to symmetric, asymmetric modes of C–H, respectively. The broad absorption peak at 3400 and 1325 cm⁻¹ is probably due to superimposition of N-H stretching of amide group with water molecules. Photoluminescence measurements reported that the peaks of emission of ultraviolet blue are at 375 and 340 nm, respectively. The films of ZnO capping with albumen were found to possess higher value of activity than ZnO corresponding to change in surface morphology with increase in surface of the deposited films. Due to the reason of nontoxicity and intense antibacterial activity with some other noble properties of ZnO, capping ZnO with albumen found to exhibit antibacterial activity effect against bacteria sources in nanotechnology. [40, 41].

Data Availability

The data used to support the findings of this study are included in the paper. Further information or data are available from the corresponding author upon request.

Conflicts of Interest

The authors declare that there are no conflicts of interest regarding the publication of this paper.

Acknowledgments

The authors acknowledge the Saveetha School of Engineering, Saveetha Institute of Medical and Technical Sciences, provided to carry out this kind of research work and publication in the journal. The authors thank Management of Saveetha School of Engineering, Saveetha Institute of Medical And Technical Sciences, India, for their appreciation and encouragement to complete this research work with in-house research facilities.

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Copyright © 2023 S. Thanikaikarasan et al. This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

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