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Green Synthesis of ZnO Nanoparticles, its Characterization and Application

Tushar Shamba Anvekar,* Vrajeshwari Rajendra Chari and Hari Kadam

Department of Chemistry, St. Xavier’s College, Mapusa, Goa – 403507, India

Corresponding Author Email: tsanvekar@yahoo.co.in

DOI : http://dx.doi.org/10.13005/msri/140211

Article Publishing History
Article Received on : 9 Sept 2017
Article Accepted on : 20 Sept 2017
Article Published : 16 Oct 2017
Plagiarism Check: Yes
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ABSTRACT:

Nano ZnO was synthesised by green approach employing aqueous extract of Adulsa and Lemongrass leaves. XRD suggested hexagonal wutzite structure for these prepared ZnO. Synthesised nanoparticles efficiently catalysed Biginelli reaction.

KEYWORDS: Biginelli reaction; FTIR; XRD; Green Synthesis; ZnO nanoparticles

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Anvekar T. S, Chari V. R, Kadam H. Green Synthesis of ZnO Nanoparticles, its Characterization and Application. Mat.Sci.Res.India;14(2)

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Anvekar T. S, Chari V. R, Kadam H. Green Synthesis of ZnO Nanoparticles, its Characterization and Application. Mat.Sci.Res.India;14(2). Available from: http://www.materialsciencejournal.org/?p=6100

Introduction

Nanoparticles are gaining importance in various fields such as health, biomedical science, chemicals industries, food & feed, cosmetics, environmental, drug and gene delivery, energy science, electronics mechanics and space industries.1-2

Design of processes that reduces or eliminates generation of hazardous substances is the key principle for sustainable chemistry. Developing green methods for synthesising nanoparticles is a major focus of present research scenario.3-7

Available literature forecasts that the nanoparticle synthesis using medicinal plants, micro-organisms and algae and other as source has been unexplored and underexploited.8-16

Materials and Methods

Preparation of Extract: A fresh leaf of Adulsa or Lemongrass leaves were collected and washed several times with deionized water, grinded and boiled for 30 min. till the colour of solution changes from watery to light yellow and filteres to get the extract. The filtrate is used as a stabilizing (capping) agent.

Experimental procedure: For the synthesis of naoparticles, Adhatoda/Lemongrass leaves extract (50 mL) was taken and heated to 80 °C with vigorous stirring. ZnNO3.6H2O (5 g) was added to the solution under heating. The paste thus obtained was heated in ceramic crucible at 400 °C for 3 h in air. Nano ZnO was obtained as white powder.17-18

Characterisation: XRD analysis was performed on Philips XPert Pro diffractometer. JEOL JSM-6360LV Scanning Electron Microscope was used to study surface morphology of nanoparticles. FTIR were recorded on ThermoFischer FTIR instrument with KBr.21-22

Catalytic Application

Urea (15 mmol, 0.90 g), Ethylacetoacetate (13 mmol, 1.69 g), Benzaldehyde (10 mmol, 1.06 g), prepared ZnO catalyst (0.2 g), Ethanol (10 mL) were refluxed for 3 hr. (Scheme 1) Mixture was then filtered in crushed ice and crude solid product as separated by filtration and washed with water. Product was purified by recrystallisation with Ethylacetate and structure was confirmed by comparing melting point and IR data.23-25

Scheme 1: Biginelli reaction

Scheme 1: Biginelli reaction
Click on image to enlarge

 

Results and Discussion

X-ray Diffraction (XRD)

The technique provides valuable information of structure, different phases and preferred crystal orientation. The pallets sintered at 400 C were finely powdered and used for XRD analysis. Inter-atomic spacing (d), lattice parameter (a), and particle size (D) were calculated for the highest intensity peak having miller indices as (hkl) for the above sample.

Figure 1: XRD pattern of ZnO (Adulsa)

Fig. 1: XRD pattern of ZnO (Adulsa)
Click on image to enlarge

 

Figure 2: XRD pattern of ZnO (Lemongrass)

Fig. 2: XRD pattern of ZnO (Lemongrass)
Click on image to enlarge

 

Fig. 1 shows XRD pattern for ZnO prepared using adulsa leaves extract. The peaks are indexed as 34.45º (100), 31.78º (002), 36.235º (101), 56.55º (102), 47.51º (110), 62.84º (103), 66.06° (200), 67.95º (112), 69.01° (201) and 78.82° (202). These peaks correlate to the hexagonal wurtzite structure of ZnO without any impurity peaks. The average crystallite / particle size as calculated by Debye-Scherrer equation was found to be 28 nm.

Fig. 2 shows XRD pattern for ZnO prepared using Lemongrass leaves extract. These peaks are indexed as 31.74° (100), 34.40° (002), 36.23° (101), 47.52° (102), 56.59° (110), 62.82° (103), 66.30° (200), 67.88° (112), 69.00° (201) and 76.93° (202). This pattern also correlates to the Hexagonal wurtzite structure of ZnO. The average crystallite / particle size was found to be 50 nm.

Scanning Electron Microscopy (SEM):

Fig. 3 and 4 shows SEM images depicting the morphologies of nano ZnO obtained by Adulsa and Lemongrass resp.

Figure 3: SEM Images of ZnO (Adulsa)

Fig. 3: SEM Images of ZnO (Adulsa)
Click on image to enlarge

 

Figure 4: SEM Image of ZnO (Lemongrass)

Fig. 4: SEM Image of ZnO (Lemongrass)
Click on image to enlarge

 

Figure 3 shows the formation of irregular spherical ZnO nanoparticles, and change of the morphology of the nanoparticles. This SEM image indicates irregular morphology. Some particles are in the range of 85-95 nm.

Figure 4 shows the formation of spherical ZnO nanoparticles, and changes of the small granular size of zinc oxide nanoparticles are formed. Spherical morphology of the nanoparticles, mixed with some chunky particles due to agglomeration. It is seen from the image that the zinc oxide nanoparticles range from 85-98 nm and there are also some nanoparticles are formed in the range of 500 nm.

Figure 5: FTIR spectra of ZnO (Adulsa)

Fig. 5: FTIR spectra of ZnO (Adulsa)
Click on image to enlarge

 

Figure 6: FTIR spectra of ZnO (Lemongrass)

Fig.6: FTIR spectra of ZnO (Lemongrass)
Click on image to enlarge

 

Figure 5 and 6 shows the FTIR spectrum of the ZnO nanoparticles synthesized by green method, this spectrum shows accordance with the literature spectrum. IR graph depict that the adhatoda (adulsa) extract acts a stabilization (capping agent). Adhatoda sample is rich in alkaloids, tanins, saponins, phenolic, and flavonoids. The chemical constituents of lemongrass extract are terpene associated to aldehyde, alcohol and ketones. All these constituent promote these lemongrass extract as a stabilizing agent. These biomolecules helped in stabilization (capping) of the synthesized ZnO NPs.

Table 1 presents the performance of prepared ZnO catalyst for Biginelli reaction giving dihydropyrimidinone product. (M.P. 207 °C, Lit. 206-208 °C)23-25

Catalytic Activity

Table 1: Catalytic activity

Catalyst

Time (Min)

% Yield

ZnO (ADULSA)

180

64

ZnO(LEMONGRASS)

180

75

COMMERCIAL ZnO

180

66

 

Fig. 7 displays the IR spectrum of dihydropyrimidinone product obtained from Biginelli reaction while Table 2 correlates its characteristic absorption peaks with probable vibrational modes.

Figure 7: FTIR spectrum of dihydropyrimidinone

Fig. 7: FTIR spectrum of dihydropyrimidinone
Click on image to enlarge

 

Table 2: Characteristics bands

Observed Peak cm-1

Stretching mode

3245

N-H asymm

3115

N-H symm

2979

C-H

1725

C=O  Ester

1701

C=O Amide

1645

C=C

1089

Monosubstituted Aromatic Ring

 

Conclusion

In this study we report a simple, biological and low cost approach for nano Zinc oxide using various leaves extract asadhatoda (adulsa), lemongrass as the reducing agent. They are employed as stabilizing agents. The prepared Zinc oxide nanoparticles were characterized by XRD, SEM and FTIR. XRD patterns of ZnO nanoparticles prepared with the green synthesis method using leaves extracts of adhatoda (adulsa), lemongrass, neem, meethi, tulsi, shows average particles size calculated as in the range of 25-50 nm by using Scherer formula. SEM image indicate irregular morphology with particles are in the range of 85-100 nm. Also, the synthesized ZnO catalyst was used in Biginelli reaction to prepare 3,4-Dihydropyrimidinones from ethylacetoacetate, benzaldehyde and urea with around 75 % product yield.

Acknowledgement

Authors thank National Institute of Oceanography, Goa for analysis.

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