Synthesis and characterization of ZnO nanoparticles by thermal decomposition of a curcumin zinc complex

Mutasim I. Khalil; Maha M. Al-Qunaibit; Aisha M. Al-zahem; Joselito P. Labis

doi:10.1016/j.arabjc.2013.10.025

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Original article

7 (

); 1178-1184

doi:

10.1016/j.arabjc.2013.10.025

Synthesis and characterization of ZnO nanoparticles by thermal decomposition of a curcumin zinc complex

Mutasim I. Khalil^{^a,*}, Maha M. Al-Qunaibit^{^a}, Aisha M. Al-zahem^{^a}, Joselito P. Labis^{^b}

a Chemistry Department, King Saud University, Riyadh 11451, Saudi Arabia

b King Abdullah Institute for Nanotechnology, King Saud University, Riyadh, Saudi Arabia

*Corresponding author. Tel.: +966 1 75973; fax: +966 1 75992 mkhalil@ksu.edu.sa (Mutasim I. Khalil)

Received: 2012-7-15, Accepted: 2013-10-21, Published: 2013-12-01

Disclaimer:
This article was originally published by Elsevier and was migrated to Scientific Scholar after the change of Publisher.

Available online 8 November 2013

Peer review under responsibility of King Saud University.

Abstract

ZnO nanoparticles were generated by thermal decomposition of a binuclear zinc (II) curcumin complex as single source precursor. Thermal behavior of the precursor showed a considerable weight loss at about 374 °C by an exothermic reaction with a maximum weight loss rate of 14%/min. Complete decomposition of precursor was observed within 49 min with a heating rate of 10 °C/min. Synthesized nanoparticles have been characterized by X-ray diffraction, Fourier transform infrared spectroscopy, transmission electron microscopy and selected area electron diffraction microscopy. Results revealed monodispersed hexagonal zincite structure with an average size of 117 ± 4 nm.

Keywords

Binuclear zinc complex

Curcumin

Thermal decomposition

Zinc oxide nanoparticles

X-ray diffraction

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1 Introduction

Metal oxides are particularly attractive with respect to applications in catalysis, sensing, energy storage, conversion optics, electronic devices (Purica et al., 2001; Aoki et al., 2000), memory arrays, biomedical application (Ayudhya et al., 2006; Wu et al., 2006) and acoustic wave devices (Gorla et al., 1999). Zinc oxide nanocrystals are one of the most intensively studied materials because of their versatile optoelectronic applications. Their large band gap of 3.37 eV and large excitation binding energy of 60 meV ensure an efficient UV-blue emission at room temperature (Joo et al., 2005; Vafaee and Ghamsari, 2007; Kim et al., 2005 ). Because of this, ZnO has a great potential in several applications such as room temperature UV-lasers (Huang et al., 2001, Arnold et al., 2003, light emitting diodes (Park et al., 2002; Jo et al., 2003), solar cells (Rensmo et al., 1997) and sensors (Kind et al., 2002; Senoussaoui et al., 2004).

Various synthetic methods have been developed to fabricate ZnO nanocrystals including vapor phase growth (Sun et al., 2004), vapor liquid–solid processes (Gao and Wang, 2004), soft chemical method (Vayssieres, 2003), electrophoretic deposition (Liu et al., 2003), sol–gel processes (Zhang et al., 2003), solvothermal processes (Wang et al., 2006), and thermal decomposition techniques (Baskoutas et al., 2008; Niassari et al., 2005; Liewhiran et al., 2006; Xu et al., 2002 ). For example, ZnO nanocrystals with various shapes were synthesized using a variety of surfactants (Joo et al., 2005), by the thermal decomposition of zinc alginate at 800 and 450 °C (Baskoutas et al., 2008), or by using bis(acetylacetonate) zinc(II) as a precursor (Niassari et al., 2005). Nano-sized ZnO powders (10–60 nm) were synthesized by thermal decomposition of zinc acetate (Liewhiran et al., 2006). Using urea and zinc nitrate as raw materials, Liu et al., 2007, prepared zinc oxide nanocrystals by a homogeneous precipitation method followed by thermal treatment at 500 °C for 10 min. On the other hand, ketones have been used as an oxolation source for the synthesis of titanium-oxo-organo crystals (Steunou et al., 1999; Garnweitner et al., 2004). Analogously, the β-diketone curcumin and curcuminoids (1,7-diaryl-1,6-heptadiene-3,5 diones) which are a group of naturally occurring 1,3-diketones with a good ligating ability for metal ions (Tennesen and Greenhill, 1992; Krishnankutty and John, 2003) is an attractive area for exploring the potential of its metal complexes for the synthesis of metal oxides nanoparticles. Curcumin is a renewable resource, its metal complexes are easily prepared that can be used to prepare metal oxides nanoparticles with low cost. In the mean time, there is no published data over the synthesis of metal oxides nanoparticles using curcumin metal complexes as a single source precursor. In this study, we describe the synthesis of ZnO nanoparticles by the thermal decomposition of a binuclear zinc hydroxido curcumin complex as a precursor prepared by the reaction of Zn(NO₃)₂·6 H₂O and curcumin in a 1:2 mol ratio (Khalil et al., 2013). The thermal behavior of the precursor metal complex was studied by thermogravimetric analysis (TGA), and differential thermal analysis (DTA). The synthesized ZnO nanocrystals were characterized by Fourier transform infrared (FTIR) spectroscopy, powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected area electron diffraction (SAED).

2 Experimental

2.1

2.1 Chemicals and materials

All the chemicals and solvents were of reagents grade and used without further purification as purchased from Sigma–Aldrich, New Jersey, USA. Zinc nitrate (BDH, Poole, England) laboratory reagent was used.

2.2

2.2 Analytical instruments

The FTIR spectrum was recorded on a Shimadzu FTIR-8400S, Prestige-21 spectrophotometer in a KBr matrix. TGA and DTA curves were recorded using a TA instrument model-SDT-Q600. XRD patterns were obtained by an Ultima IV X-ray diffractometer by using monochromatized Cu Kα 1 radiation under the acceleration voltage of 40 kV and a current of 40 mA. The morphology of the ZnO nanocrystals was examined by a JEOL JSM-6380 LA SEM and a JEOL TEM 2100F TEM with an acceleration voltage of 200 kV.

2.3

2.3 Preparation of zinc (II) curcumin complex

(Bis1,7-bis[4-hydroxy-3-methoxyphenyl]-1,6-heptadiene-3,5-dionato)hydroxide zinc(II), [Zn(OH)(curc)] was prepared by a previously reported method (Khalil et al., 2013). An ethanolic mixture solution of zinc nitrate and curcumin in a 1:2 mol ratio was refluxed for 1 h and the resulting product was filtered and washed several times by de-ionized water, dried in vacuum and used as a precursor to synthesize ZnO nanoparticles.

3 Results and discussion

3.1

3.1 Thermal decomposition of zinc (II) curcumin complex precursor

Our investigation revealed that such a complex lends itself as a potential precursor for zinc oxide nanoparticles synthesis through thermal decomposition. The thermal properties of precursor were determined by thermogravimetric analysis (TGA) and differential thermal analysis (DTA). Sample was heated in an aluminum pan from room temperature to 600 °C at a heating rate of 10 °C/min. The TGA and DTA analyses (Fig. 1) revealed that the complex looses 6% of its weight at about 200 °C attributed to desorption or removal of moisture and solvents, and 50% weight loss of its total weight at 374 °C with a maximum weight loss rate of 14% min⁻¹ indicating a fast rate of degradation of curcumin into volatile combustible products. The DTA curve has a large exothermic peak at that temperature which may be attributed to the fact that volatile organic moieties generated by the dissociation of precursor react with O₂ to form CO₂ and H₂O. This is confirmed by the weight loss observed in the temperature region 400–600 °C in the TGA curve.

The morphology of the synthesized micro particles of the zinc complex precursor shown in the SEM image of Fig. 2 was converted into hexagonal nanoparticles upon thermal treatment at 500 °C.

SEM image of [Zn(OH)C21H20O6]2 precursor.

The phase and crystallinity of the synthesized sample were investigated by X-ray diffraction patterns shown in Fig. 3. The patterns are in accord with the typical zincite structure ZnO diffraction (hexagonal phase, space group P6₃mc, with lattice constants a = 3.24982 Å, c = 1.6021 Å, Z = 2, JCPDS No. 361451) (Bigdeli et al., 2010; Liu et al., 2007).

X-ray diffraction pattern of ZnO nanoparticles.

A most intense peak at 2θ = 36.67° is obtained along (1 0 1) orientation. The sharpness, strong intensity and narrow width of ZnO diffraction peaks in the XRD pattern indicate that the synthesized ZnO sample is well crystallized. The FTIR spectrum of ZnO nanoparticles exhibited two strong vibrational bands at 640 and 605 cm⁻¹ assigned to the stretching modes of Zn–O and the weak bands at 3500 and 1040 cm⁻¹ are probably attributed to the presence of water in the KBr matrix (Bigdeli et al., 2010; Chen et al., 2004). The EDS pattern of the ZnO nanoparticles is shown in Fig. 4. The Cu and C signals were from the Cu grid and carbon film coated on the support formvar. No other signals were detected within the detection limits of EDS which confirm the purity of the ZnO nanoparticles.

The scanning electron microscopy (SEM) image of ZnO sample is shown in Fig. 5. This image reveals that the ZnO is in nano scale.

The fine powder of ZnO nanocrystals was dispersed in ethanol on a carbon-coated copper grid and the high resolution transmission electron microscopy (HRTEM) images (Fig. 6) were obtained with ultra high resolution at an accelerating voltage of 200 kV. The selected area electron diffraction (SAED) pattern shown in insert (a) of Fig. 6 has sharp spots indicative of polycrystalline nature with symmetrical orientation of ZnO nanoparticles in the sample. The crystallinity of the synthesized nanoparticles was also supported by the observed lattice fringes of 0.25 nm in HRTEM image shown in insert (b) of Fig. 6. This value is very near the 0.26 ± 0.05 nm spacing for ZnO corresponding to (1 0 1) plane of ZnO (Yan et al., 2000).

TEM image of ZnO nanoparticles, SAED (insert a) and high scanning resolution (insert b).

The average crystal size is estimated by considering the few number of crystals shown in the TEM image, Fig. 6, and found to be about 127 ± 4 nm presented by a histogram in Fig. 7.

Histogram (average size) of ZnO nanoparticles.

4 Conclusion

The synthesis of zinc oxide nanoparticles from a curcumin zinc complex by a thermal decomposition technique was studied in this paper. Low heat energy was applied to degrade the organic moiety. Nanoparticles with an average size of 117 ± 4 nm were obtained from an easily prepared organic moiety containing metal complex precursor. Such a type of precursors have potential for synthesizing metal oxide nanoparticles.

Acknowledgement

This project was supported by the King Saud University, Deanship of Scientific Research, College of Science, Research Center.

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Introduction

Experimental

Chemicals and materials
Analytical instruments
Preparation of zinc (II) curcumin complex

Results and discussion

Thermal decomposition of zinc (II) curcumin complex precursor

Conclusion

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[1] Aoki T., Hatannaka Y., Look D.C., . ZnO diode fabricated by excimer-laser dopping. Appl. Phys. Lett.. 2000;76:3257. Aoki, et al., 2000. reported the fabrication of a ZnO diode by using a laser-doping technique. The surface changes and photoluminescence of three samples were measured. Poor electroluminescence was reported
[Google Scholar]

[2] Arnold M.S., Avouris P., Pan Z.W., Wang Z.L., . Field effect transistors based on single semiconducting oxide nanobelts. J. Phys. Chem. B. 2003;107(3):659. Arnold, et al., fabricated field-effect transistors based on single SnO₂ and ZnO nanobelts of thickness between 10 and 30 nm. Conductance and ultraviolet light sensitivity were reported. The results could be utilized in tuning the electrical performance of the electrical device
[Google Scholar]

[3] Ayudhya S.K.N., Tonto P., Mekasuwandumrong O., Pavarajarn V., Praserthdam P., . Solvothermal synthesis of ZnO with various aspect ratios using organic solvents. Cryst. Growth Des.. 2006;6:2446. Ayudhya, et al., synthesized nanocrystalline ZnO powders by a solvothermal method using various organic solvents as the reaction medium. Products were characterized by XRD, SEM, TEM, and SAED. The work opens a field of investigating the role of dielectric constant of solvents in nanomaterials synthesis
[Google Scholar]

[4] Baskoutas S., Gabournis P., Yannopoulos S.N., Dracopoulos V., Toth L., Chrissanthopoulos A., Bouropoulos N., . Preparation of ZnO nanoparticles by thermal decomposition of zinc alginate. Mater. Lett.. 2008;62:1890-1892. Baskoutas, et al., reported a method of ZnO nanocrystals production based on the thermal decomposition of zinc alginate gels.XRD, SEM and TEM analysis revealed the presence of ZnO hexagonal phase. The temperature and precursor used influenced the crystal size besides the existence of structural defects of nanoparticles
[Google Scholar]

[5] Bigdeli F., Morsali A., Retalleau P., . Synthesis and characterization of different zinc (II) oxide nano-structures from direct thermal decomposition of ID coordination polymers. Polyhedron. 2010;29:801-806. Bigdeli, et al., synthesized different ZnO nano-structures from direct thermal decomposition of ID co-ordination polymers. Their claims were documented by crystallographic measurements of precursors and TGA, IR, SEM, and EDAX measurements of ZnO particles. However, synthesis of precursors involved several chemicals and energy
[Google Scholar]

[6] Chen B.J., Sun X.W., Xu C.X., Tay B.K., . Growth and characterization of zinc oxide nano/micro-fibers by thermal chemical reactions and vapor transport deposition in air. Physica E. 2004;21:103-107. Chen, et al., reported the preparation of ZnO nano/micro crystal fibers on silicon substrate via thermal chemical reactions vapor transport deposition method in air with a mixture of ZnO and carbon powders as reactants. Products were characterized by XRD and SEM techniques. However, very high temperature was used in the method
[Google Scholar]

[7] Gao P.X., Wang Z.L., . Nanopropeller arrays of zinc oxide. Appl. Phys. Lett.. 2004;84(15):2883. Gao and Wang, synthesized ZnO nanopropeller arrays by a two-step high temperature solid-vapor deposition process. They showed the modes of growth along the axes and a wide band gap. The study is of an applied physics nature
[Google Scholar]

[8] Garnweitner G., Antonietti M., Niederberger M., . Nonaqueous synthesis of crystalline anatase nanoparticles in simple ketones and aldehydes as oxygen supplying agent. Chem. Commun. 2004:397-399. Garnweitner, et al., obtained highly crystalline nanoparticles of 5–20 nm size by reacting titanium tetraisopropoxide with ketones and aldehydes as oxygen-supplying agents under solvothermal conditions. The XRD diffraction pattern and TEM image support their claims. The high concentration of the TiO₂ in the system and the potential for the synthesis of other binary and ternary metal oxides are promising aspects for practical applications
[Google Scholar]

[9] Gorla C.R., Emanetoglu N.W., Liang S., . Structural, optical and surface aqoustic wave properties of epitaxial ZnO films grown on (011 over-bar2) sapphire by metalorganic chemical vapor deposition. J. Appl. Phys.. 1999;85(5):2595. Gorla, et al., reported growing high quality epitaxial ZnO films on R-plane sapphire substrates by metalorganic chemical vapor deposition. The properties of ZnO films were studied by TEM and photoluminescence techniques. The work is suitable for application in UV modulator
[Google Scholar]

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Synthesis and characterization of ZnO nanoparticles by thermal decomposition of a curcumin zinc complex

Abstract

Keywords

Binuclear zinc complex

Curcumin

Thermal decomposition

Zinc oxide nanoparticles

X-ray diffraction

1 Introduction

2 Experimental

2.1 Chemicals and materials

2.2 Analytical instruments

2.3 Preparation of zinc (II) curcumin complex

3 Results and discussion

3.1 Thermal decomposition of zinc (II) curcumin complex precursor

4 Conclusion

Acknowledgement

References

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