Elsevier

Journal of Crystal Growth

Volume 289, Issue 1, 15 March 2006, Pages 102-106
Journal of Crystal Growth

Synthesis and optical properties of nanocrystalline ZnO powders by a simple method using zinc acetate dihydrate and poly(vinyl pyrrolidone)

https://doi.org/10.1016/j.jcrysgro.2005.10.145Get rights and content

Abstract

This paper reports the synthesis and characterization of nanocrystalline ZnO powders by a simple method using zinc acetate dihydrate and polyvinyl pyrrolidone (PVP) as a chelating agent. The polymeric precursor was characterized by TG-DTA to determine the thermal decomposition and crystallization temperature which was found to be at 600 °C. The precursor was calcined at 600 °C for 1 h to obtain nanocrystalline ZnO powders. The morphology and crystalline size of the calcined powders characterized by SEM and TEM revealed that the powders consisted of the mixture of nanoparticles with particle sizes of ∼50–100 nm and nanorods with diameters of ∼100–200 nm and 200–500 nm in length. The XRD and FT–IR results indicated that the synthesized ZnO powders had the pure wurtzite structure with lattice parameters a and c of 0.32344±0.00058 and 0.51843±0.00211 nm, respectively. The synthesized powders exhibited the UV absorption at around 2.99 eV with the estimated direct bandgap (Eg) of 3.10 eV. Room temperature photoluminescence spectrum of the powders showed a strong UV emission band at ∼2.98 eV, a weak blue band at 2.82 eV, a week blue–green band at 2.56 eV, and a weak green band at 2.34 eV, which indicated their high structural and optical quality.

Introduction

Zinc oxide (ZnO), a representative II–VI compound semiconductor, has attracted considerable attention over the last few years. Its many attractive properties, such as the direct wide bandgap (3.37 eV), large exciton binding energy (60 meV at room temperature), good piezoelectric characteristics, chemical stability and biocompatibility, suggest a host of possible practical applications, notably in the area of ultraviolet/blue emission devices [1], [2], [3], [4], [5], [6], [7], [8]. So far, nanocrystalline ZnO with different particle morphologies and sizes have been obtained by several preparation approaches including thermal decomposition, vapor chemical deposition, sol–gel method, wet chemical synthesis, mechanochemical, electrodeposition, gas-phase reaction, hydrothermal synthesis and so on. An excellent review of recent progress on processing, properties and applications of ZnO was recently published elsewhere [9]. Among other established synthesis methods, simple and cost effective routes to synthesize nanocrystalline ZnO by utilization of cheap, nontoxic and environmentally benign precursors are still the key issues.

In this paper, we report the synthesis and optical properties of nanocrystalline ZnO powders prepared by a simple method using zinc acetate dihydrate and polyvinyl pyrrolidone (PVP) as a chelating agent. The synthesized powders were characterized by TG-DTA, XRD, FT-IR, UV-VIS, SEM, and TEM. The photoluminescence properties of the powders were also investigated.

Section snippets

Experimental procedure

In this study, zinc acetate dihydrate (Fluka, ⩾99.5%) and PVP (Mn=1300000, Aldrich) were used as the starting chemicals. In a typical procedure, 7.5 g of PVP was first dissolved into 500 ml de-ionized water under vigorous stir on hot plate stirrer (CERAMAC, Midi, USA) at 27 °C for 30 min. Subsequently, 5 g of zinc acetate was added to the PVP solution under vigorous stir at 60 °C for 30 min to obtain a well-dissolved solution. Then, the solution was evaporated by heating in water bath of 60 °C for a

Results and discussion

The TG curve in Fig. 1 shows a major weight loss step from 400 up to about 550 °C with no further weight loss observed up to 1000 °C. The weight loss is related to the combustion of organic matrix. The clear plateau formed between 550 and 1000 °C on the TG curve indicates the formation of nanocrystalline ZnO as decomposition product, as confirmed by XRD and FT-IR analysis shown in Fig. 1, Fig. 2. On the DTA curve (Fig. 1) a main exothermic effect was observed between 400 and 600 °C with a maximum

Conclusion

Nanocrystalline ZnO powders have been synthesized by a simple method using Zn acetate and PVP. The XRD patterns and FTIR spectra suggested the formation of wurtzite nanocrystals in the synthesized powders after calcination the precursor at 600 °C for 1 h. The powders consisted of the mixture of nanoparticles with particle sizes of ∼50–100 nm and nanorods with diameters of ∼100–200 nm and 200–500 nm in length, obtained by SEM and TEM. The synthesized powders exhibited the UV absorption below 2.99 eV

Acknowledgments

The authors would like to thank the Department of Chemistry for providing TG-DTA and FTIR facilities, the Faculty of Science Electron Microscopy Unit for providing SEM facilities, and the Science and Technology Service Center (Chiang Mai University) for providing TEM facilities. This work is supported by the Postgraduate Education Development (PED) in Physics Program, The Commission on Higher Education, The Ministry of Education, Thailand.

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