SYNTHESIS AND CHARACTERIZATION OF ZINC OXIDE (ZNO

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1Assistant Professor, Department of Bio-Medical Engineering, Rajiv Gandhi Institute ... In this paper, we discuss the Synthesis of Zinc oxide using Leaf Extract of .... S. Ambika, K. Bharathi “Plant-extract mediated synthesis of ZnO nanoparticles.
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SYNTHESIS AND CHARACTERIZATION OF ZINC OXIDE (ZNO) NANOPARTICLES USING MANGO (MANGIFERA INDICA) LEAVES Ashwath Narayana B S1, Kushal Pandey2, Nasehuddin Azmi2, Tejashwini M2, Umang Shrestha2, S V Lokesh* Assistant Professor, Department of Bio-Medical Engineering, Rajiv Gandhi Institute of Technology, Cholanagar, R.T Nagar, Hebbal, Bengaluru, India 2 B. E, Department of Bio-Medical Engineering, Rajiv Gandhi Institute of Technology, Cholanagar, R.T Nagar, Hebbal, Bengaluru, India Assistant Professor, Department of Nanotechnology, Centre for PG Studies- Bangalore Region, Visvesvaraya Technological University, Muddenahalli, Chikkaballapur, Karnataka, India.

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Abstract: ZnO is commercially used in wide range of application ranging from gas detection, cosmetics, painting, glass industry, packaging materials, etc. The versatile use of ZnO can be attributed to its various features like low cost, anti-bacterial, high corrosion resistance, wide energy gap. Various methods already exists for synthesis of ZnO nanoparticles like high temperature evaporation, gas spraying, pulsed laser deposition, sputtering, sol-gel, wet chemical and electrochemical methods. But they have high toxicity level. In this paper, we discuss the Synthesis of Zinc oxide using Leaf Extract of Mangifera Indica to overcome this problem. Here we use Zinc Nitrate (Zn(No3)2.6H2O) as a precursor, Ethanol (C2H5OH) as a solvent and Leaf extract as a reducing agent. The method used is SolutionCombustion method for synthesizing ZnO nanoparticles using green approach and the material so obtained is then characterized by X-ray Diffraction (XRD), Scanning Electron Microscope (SEM), Ultraviolet-Visible (UV-Vis) Spectroscopy, Fourier transform infrared spectroscopy (FTIR). The obtained ZnO nanoparticles are then compared with commercial ZnO. The size of ZnO nanoparticles so obtained from green approach is 26nm with Zincite structure, which falls under commercial range of 1540nm.

Keywords: Zinc Oxide [ZnO], Green synthesis, Mango leaves [Mangifera Indica]

1. Introduction In the last decade synthesis of metal oxide nanoparticles has received great attention due to their potential properties such as optical, electronic, mechanical, magnetic, and chemical properties and hence has incredible applications in the field of physics, chemistry, medicine, biology, agriculture, food processing, and so forth [1, 11-16]. A synthesis of zinc oxide nanoparticles has wide varieties of methods and is reported [2, 17-23]. However, these methods are energy consuming, using hazardous solvents and expensive reagents in their preparation [3-8]; therefore the rising needs to develop eco-friendly green method for nanoparticle preparation [9]. Researchers have started working on green synthesis approach using green

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leaves for reduction of Zinc nitrates and chlorides into Zinc Oxide nanoparticles instead of using chemical ways synthesis the nanoparticles. Zinc Oxide (ZnO) is commonly used metal oxide for gas sensing. It has large binding energy of 60meV. [1]

It has a wide band polycrystalline semiconductor energy band gap in the range of 3.2 to 3.5 eV. Large

surface area of ZnO particles provides it with good sensitivity and fast response time. These advantages of ZnO Nps have increased its application towards various operations like gas sensing, paints, transducers, as well as various biomedical application including therapeutic procedures. The figure 1 shows crystal lattice structure of Zinc Oxide with lattice spacing a = 0.325 nm and c = 0.521 nm, having stable wurtzite structure [24].

Fig. 1: - Wurtzite structure model-tetrahedral coordination of ZnO.

Various methods like chemical reduction, laser ablation, solvo-thermal, inert gas condensation and sol-gel method are generally used for synthesis of ZnO oxide. These methods are expensive, require special equipment and needs attention to maintain parameter. We use green synthesis method for synthesis of ZnO as it is cost effective, uses less toxic chemicals, it is ecofriendly and requires only one step for synthesis of nanoparticles. This procedure requires Zinc nitrate as precursor (Zn(NO₃)₂.6H₂O) and leaf extract as precipitating agent.

2. Experimental

2.1 Materials Zinc Oxide nanoparticles Synthesis (ZnO-Np) involves the use of zinc nitrate (Zn(NO₃)₂.6H₂O) as precursor from Sigma-Aldrich. Ethanol from Merck, DI water and Mango (Mangifera Indica) leaves were collected in rural areas around Muddenahalli, Chikkaballapur.

2.2 Preparation of Leaf extract The Zinc Oxide nanoparticles were produced by reducing the precursor salt of zinc nitrate using the leaf extracts of mango (Mangifera Indica) tree. In order to do so, the leaves with the best conditions were selected from local trees, avoiding those that were exposed to urban pollution. The mango leaves

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(Mangifera Indica) of 100g weight were collected and the leaves were then rinsed and washed with tap water followed by DI water for 2-4 times. The thoroughly cleaned leaves were then placed in 250ml beaker with100ml of DI water and the beaker was then kept on top of the hot plate for 30minutes stirring using magnetic stirrer (Rim) by maintaining the temperature of hotplate at 80oC during this process. As the solution turned green giving the confirmation of green extract the solution was then filtered using Whattman filter paper and leaves were separated from the beaker. The so obtained green extract was then used for synthesis of ZnO nanoparticles. The complete process flow is as shown in figure2.

Fig 2. Leaf extracts process flow

2.3 Green synthesis of ZnO using leaf extract The green synthesis approach of ZnO nanoparticles using mango leaves by solution combustion method is the cost effective and simple way to synthesis nanoparticles under normal conditions. Initially, 20ml of an aqueous solution of Zinc nitrate (Zn(NO₃)₂.6H₂O) (0.1M) were prepared and mixed with 2ml of concentrated leaf extract. The mixture was then magnetically stirred for 15 minutes and the resultant was then transferred to 20ml silicon crucible which was later heated at 70oC using electric heater (heating mantle) until the solution is converted into ZnO nanoparticles in powder form which usually takes 10minutes for this process. The so obtained ZnO nanoparticles were further calcinated in hot-air oven for 1 hour at 110oC and later the fine powder of ZnO nanoparticles were obtained by grinding using mortar.

3. Results and Discussion 3.1 X-Ray Diffraction The X-Ray Diffraction (XRD) pattern of the as-synthesized ZnO nanoparticles was obtained using Rigaku Ultima IV is as shown in Fig.3.1 The peaks were obtained at 2 θ values of 31.750°, 34.407°, 36.232°, 47.523° and 56.565° are associated with (100), (002), (101), (110), and (102) respectively and all the peaks of diffraction are well indexed to the Zincite structure of hexagonal ZnO (DB card number:

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-1011258). The average particle size was calculated using XRD pattern by applying Scherer formula is about 26 nm. D = 0.9 λ/ (β COS θ) --------------- [1]

Fig. 3.1: - XRD of ZnO Nano particles.

3.2 Scanning Electron Microscope (SEM) SEM analysis is used to determine the external morphology (structure) and size of the crystal particles. Mixed surface morphology is determined by the obtained SEM images using Hitachi VP-SEM SU1510. The ZnO NPs so formed were agglomerated with mixed morphology structures with irregular shapes. The structure and morphology of SEM images are shown in fig 3.2 which clearly states that the obtained SEM image of ZnO nanoparticles is of mixed morphology [19-22]. The hexagonal structures of ZnO nanoparticles can be clearly observed with magnification of 1 μm as shown in fig 3.2(b).

Fig. 3.2: - Surface morphology of the sensing film at the specified magnification (a)3 μm (left), (b)1 μm (right).

3.3 Fourier-transform infrared spectroscopy (FTIR) FTIR of Zinc oxide nanoparticles with the green synthesis approach were obtained from Perkin Elmer as shown in figure 3.3. The as synthesized zinc oxide nanoparticles from leaf extract were analyzed by FTIR spectroscopy technique in order to find out the functional groups present in the particles. Bandwidth of 1500–600 cm−1 exhibited the fingerprint region of zinc oxide nanoparticles. Strong peak observed at the frequency of 1650 cm−1 indicates the N-H bending and weak peaks were found at 1623 cm-1 and 1510 cm-1 Indicates Diketones C=O stretch. The broad peak around 3329 cm-1

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Indicates Amide N-H stretch bond vibration which was due to the water adsorption on the surface of zinc oxide nanoparticles while the peak at 440 cm−1 was attributed to the Zn-O stretching vibration.

Fig. 3.3: - Absorption Spectra of ZnO

3.4 Ultraviolet-Visible (UV-Vis) Spectrophotometry ZnO nanoparticles were characterized using UV-visible spectrometer LAMBDA 750, and the results were shown in Figure 3.4. Absorption spectra of ZnO nanoparticle dispersions as thin films on a glass substrate were recorded. A high absorption coefficient in the UV region was revealed by the spectra of ZnO, whereas they are transparent in the visible region. From the Tauc relation, the optical band gap (Eg) of the semiconductor was calculated [23, 24]. A plot of (αhυ)2 versus hυ shows intermediate linear region, the extrapolation of the linear part can be used to calculate the Eg from intersect with h axis. The resultant value of Eg for ZnO synthesized using a green process was found to be about 3.75 eV as shown in Figure 3.4 and is in good consensus with the earlier published values. [24, 25]

Fig 3.4: -UV Spectroscopy. 4. Conclusion The synthesis of zinc oxide nanoparticles from a solution combustion method was studied in this paper. Nanoparticles with an average size of 26 nm were obtained from an easily prepared Zinc nitrate precursor. Green synthesis is highly economical and less toxic method for synthesis of ZnO NPs, especially in case of medical and biological applications. Toxicity level was greatly reduced using green

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synthesis method. Best nanoparticle size was obtained at temperature of 80 °C and based on SEM analysis, morphology ZnO-NP has a spherical, hexagonal shape as well as irregular shapes which confirms the mixed morphology structure of ZnO NPs.

Acknowledgement We are grateful to Visvesvaraya Technological University (VTU) for providing us a good working environment with necessary resources to carry out our research work.

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