MgO nanoparticles via a simple solid-state reaction

MgO nanoparticles via a simple solid-state reaction Norlida Kamarulzaman, Nor Fadilah Chayed, and Nurhanna Badar Citation: AIP Conference Proceedings 1711, 040004 (2016); doi: 10.1063/1.4941626 View online: http://dx.doi.org/10.1063/1.4941626 View Table of Contents: http://scitation.aip.org/content/aip/proceeding/aipcp/1711?ver=pdfcov Published by the AIP Publishing Articles you may be interested in Enhancement of anisotropic magnetoresistance in MgO/NiFe/MgO trilayers via NiFe nanoparticles in MgO layers J. Appl. Phys. 111, 123903 (2012); 10.1063/1.4729273 Fe nanoparticles embedded in MgO crystals J. Appl. Phys. 105, 064906 (2009); 10.1063/1.3086265 Preparation of actinide boride materials via solid-state metathesis reactions and actinide dicarbollide precursors AIP Conf. Proc. 532, 127 (2000); 10.1063/1.1292229 Solid‐state reactions in high‐temperature superconductor‐ceramic interfaces; Y‐Ba‐Cu‐O on Al2O3 versus yttria‐ stabilized ZrO2, and MgO J. Appl. Phys. 67, 2524 (1990); 10.1063/1.345506 Matrix reactions of magnesium atoms with ozone. Infrared spectra of MgO, MgO2, and MgO3 in solid nitrogen J. Chem. Phys. 69, 556 (1978); 10.1063/1.436646

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MgO Nanoparticles via a Simple Solid-state Reaction Norlida Kamarulzaman1,2,a), Nor Fadilah Chayed1, 3 and Nurhanna Badar1,3 1

Centre for Nanomaterials Research, Institute of Science, Universiti Teknologi MARA, 40450 Shah Alam, Selangor, Malaysia 2 School of Physics and Materials Studies, Faculty of Applied Sciences, Universiti Teknologi MARA, 40450 Shah Alam, Selangor, Malaysia 3 School of Chemistry and Environment, Faculty of Applied Sciences, Universiti Teknologi MARA, 40450 Shah Alam, Selangor, Malaysia a)

Corresponding author: [email protected]

Abstract. Normally, nanoparticles were obtained by complex and tedious methods. In this work, magnesium oxide (MgO) nanoparticles were prepared by a simple solid-state reaction method without assistance of any other additives. Magnesium acetate tetrahydrate was used as the starting material and directly annealed at 800 ˚C for 6 h, 12 h and 24 h. All the samples were characterized using X-Ray Diffraction (XRD) and Field Emission Scanning Electron Microscopy (FESEM). All the annealed samples obtained were pure, single phase of cubic structure with space group Fm-3m. SEM results show that all the samples have rounded shape with crystallite size is between 20 to 135 nm. Thus, nanoparticles of MgO can be easily obtained via a simple solid-state reaction method.

INTRODUCTION Nanostructured materials have attracted extensive attention and a number of researchers have explored novel and new methods to obtain the low dimensional materials. Nanostructured materials can exhibit unique properties which have motivated researchers to develop methods to produce important technological materials for various applications. Amongst them, MgO nanostructures is one of the important materials with widespread applications in the chemical and physical fields. Some of the more important characteristics of MgO are chemical inertness, high thermal stability, wide band gap, high thermal conductivity and secondary electron emission. MgO can be used as catalysts, insulators, a component superconductor, in refractory ceramics and substrates for thin film growth [1-4]. In recent years, many synthesis methods have been developed to produce MgO nanostructured materials with different kinds of morphologies such as chemical precipitation, thermal evaporation, hydrothermal, chemical vapor deposition (CVD) and thermal decomposition [5-10]. All these methods require complex procedures. This study was carried out with the aim to synthesize MgO nanoparticles by using a simple and cost effective solid-state reaction method. The solid-state reaction method presented here is used without any surfactants or catalysts. This study also investigates the influence of annealing time employed on the morphology and crystallite size of MgO nanostructure.

EXPERIMENTAL METHODS The solid-state reaction method used in the synthesis of MgO nanostructures employs magnesium acetate tetrahydrate, Mg(CH3COO)2.4H2O (99.5 % purity) as a starting material. Magnesium acetate tetrahydrate was grounded and annealed at 800 °C for 6 hours, 12 hours and 24 hours and then labeled as M6, M12 and M24 respectively. The phase purity of the annealed samples was checked by PANalytical X’pert Pro MPD X-Ray diffractometer. The Bragg-Brentano optical configuration and CuK α radiation were used during data collection. The

International Symposium on Frontier of Applied Physics (ISFAP) 2015 AIP Conf. Proc. 1711, 040004-1–040004-4; doi: 10.1063/1.4941626 © 2016 AIP Publishing LLC 978-0-7354-1358-0/$30.00

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diffraction data were analyzed using the X’pert HighScore Plus software. The crystallite size and morphology of MgO were determined using Field Emission Electron Microscope (FESEM), JEOL JSM-7600F. The specific surface area of the samples was measured using Brunauer-Emmett Teller (BET) method based on N2 absorptiondesorption isotherms that obtained from BELSORP-mini II analyzer.

RESULTS AND DISCUSSIONS Figure 1 indicates the XRD patterns for M6, M12 and M24 samples. XRD patterns represent the diffraction peaks of (111), (200), (220), (311) and (222) corresponding to the MgO cubic structure and matches the ICDD pattern of MgO (ICDD No. 01-087-0651) with space group Fm-3m. From the patterns, no impurity peaks could be observed and it was confirmed that the samples are pure and single phase. On the examination of (200) peak in Figure 2, the full width at half maximum (FWHM) of M6, M12 and M24 samples are 0.30°, 0.28° and 0.26° respectively. The small FWHM value of M24 sample revealed that it is highly crystalline and implies that the crystallite size is also larger compared to M6 and M12 samples. This is supported by SEM results as discussed below.

FIGURE 1. XRD patterns of MgO samples (M6, M12 and M24)


FIGURE 2. XRD peak of (200) plane of MgO samples (M6, M12 and M24)

Figure 3 shows the SEM micrographs of all samples at 50k times magnification using secondary electron imaging. From the SEM results, the morphology for all the samples has agglomeration of crystals of rounded shapes. It can be seen that the crystallite size of M6 sample is the smallest of about less than 100 nm even though the agglomerated particles are larger. The crystallite size of M12 sample is between 50 to 70 nm while for M24 sample, it is between 60 to135 nm as given in Table 1. It is observed that, as the annealing time is increased, the crystallites give larger and better dispersion. The specific surface area of the samples is given in Table 2. From the results, the specific surface area of the macroporous MgO nanoparticles increases as the annealing time increases due to better dispersion of the crystallites. Even though the crystallite size is smaller for the M6 sample, the agglomeration is very strong leaving no spaces in between the crystals, therefore the specific surface area to volume ratio will also be smaller. This is confirmed by the smaller pore volume for M6 sample even though pore size is larger.

FIGURE 3. FESEM images of (a) M6 (b) M12 (c) M24 samples at magnification of 50k times TABLE 1. Crystallite size of MgO samples

Sample M6 M12 M24

Crystallite size range (nm) 20 - 70 50 - 80 60 - 135

Average crystallite size (nm) 53.3 70.8 86.9


TABLE 2. Surface area and pore volume of MgO samples

Sample M6 M12 M24

Specific surface area (m2/g) 6.6952 7.4823 8.6024

Pore volume (cm3/g) 0.0974 0.1074 0.1144

Average pore diameter (nm) 58.17 57.42 53.19

CONCLUSION Pure and single phase MgO nanoparticles have been successfully synthesized by using the simple solid statereaction method. The crystallite size of the samples was very small and affected by the annealing time. The longer annealing time will give larger crystallite size and better dispersion of crystallites. However, even though M6 sample has the smallest crystallite size the specific surface area is smaller due to the strong agglomeration of the crystallites.

ACKNOWLEDGMENTS The authors would like to thank Institute of Science and Faculty of Applied Sciences, Universiti Teknologi MARA, Shah Alam, Malaysia for the financial support for this research work.

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