The Effects of Calcination Temperatures in the Synthesis of Nanocrystalline Magnesium Oxide via Sol-Gel Technique

Abstract:

This study highlights on a convenient and optimised method for the preparation of nanocrystalline magnesium oxide (MgO) catalyst via sol-gel combustion method. Nanocrystalline MgO was prepared by using polyvinyl alcohol (PVA) as a complexing agent and metal nitrate (Mg (NO ₃ )₂.6H₂O) as a precursor. The obtained MgO powder was calcined at 200 °C, 400 °C, 600 °C and 800 °C. All the MgO calcined samples including commercial MgO were characterised using Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), X-Ray diffraction (XRD) and N₂ adsorption-desorption Brunauer–Emmett–Teller (BET). From FTIR analysis, the appearance of a peak at 3700 cm^-1 represent the O-H stretching bonded with Mg and the broad absorption peak at 3421 cm^-1 indicates O-H stretching band which is due to the absorption of moisture from the surrounding. (BET) results indicate the MgO sample that has been calcined at 400 °C shows the largest surface area. SEM images show there is porosity in all MgO powder. While XRD patterns revealed that higher temperature of calcination gives higher crystallinity of the MgO samples.

• Periodical: Applied Mechanics and Materials (Volume 865)
• Pages: 36-42
• DOI: https://doi.org/10.4028/www.scientific.net/AMM.865.36
• Online since: June 2017
• Authors: Hanis Mohd Yusoff*, Faridatul Akmar Rafit, Fatin Izwani Mohamad, Norhafiefa Hassan, Adibah Izzati Daud
• Keywords: Catalyst, Magnesium Oxide, Nanocrystalline, Sol-Gel

References

[1] G. Singh, I. P. S. Kapoor, S. Dubey, P. F. Siril, Preparation, Characterization and Catalytic Activity of Transition Metal Oxide Nanocrystals. J. Sci. Conf. Proc. 1 (2008) 7-14.

DOI: 10.1166/jcp.2009.002

[2] Y. C. Sharma, B. Singh, K. J. Korstad, Latest developments on application of heterogenous basic catalysts for an efficient and eco-friendly synthesis of biodiesel: A review. Fuel. 90(4) (2011) 1309-1324.

DOI: 10.1016/j.fuel.2010.10.015

[3] N. A. Harun, M. J. Benning, B. R. Horrocks, D. A. Fulton, Gold nanoparticle-enhanced luminescence of silicon quantum dots co-encapsulated in polymer nanoparticles. Nanoscale. 5 (2013) 3817-3827.

DOI: 10.1039/c3nr00421j

[4] H. Li, R. Xiao, Y. Zhan, H. D. Bian, B. Nie, Z. Chen, J. Lu, Y. Y. & Li, Efficient ternary ChSSe quantum-dot-sensitized solar cells based on MgO-coated TiO2 nanoparticles. Energ. Tech. 2(6) (2014) 526-530.

DOI: 10.1002/ente.201400003

[5] M. S. Mastuli, N. Kamarulzaman, M. A. Nawawi, A. M. Mahat, R. Rusdi, N. Kamarudin, Growth mechanisms of MgO nanocrystals via a sol-gel synthesis using different complexing agents. Nano. Res. Lett. 9 (2014) 134.

DOI: 10.1186/1556-276x-9-134

[6] M. Babaie, H. Sheibani, Nanosized magnesium oxide as a highly heterogeneous base catalyst for the rapid synthesis of pyranopyrazoles via a tandem four-component reaction. Arabian J. Chem. 4 (2011) 159-162.

DOI: 10.1016/j.arabjc.2010.06.032

[7] B. Nagappa, G. T. Chandrappa, Mesoporous Nanocrystalline Magnesium Oxide for Environmental Remediation. Microp. Mesop. Mater. 106 (2007) 212-218.

DOI: 10.1016/j.micromeso.2007.02.052

[8] M. Y. Hanis, U. H. Nuur, H. Norhafiefa, I. Fatin, Comparison of Sol-gel and Dehydration Magnesium Oxide as a Catalyst in Michael Addition Reaction. Int. J. Integr. Eng. 7(3) (2015) 43-50.

[9] R. Wahab, S. G. Ansari, M. A. Dar, Y. S. Kim, H. S. Shin, Synthesis of magnesium oxide nanoparticles by sol-gel process. Mater. Sci. Forum. 558-559 (2007) 983-986.

DOI: 10.4028/www.scientific.net/msf.558-559.983

[10] S. Balamurugan, L. Ashna, P. Parthibani, Synthesis of nanocrystalline Mgo particles by combustion followed by annealing method using hexamine as a fuel. J. Nanotech. (2014) 2014 841803.

DOI: 10.1155/2014/841803

[11] A. R. Beuno, R. F. M. Oman, P. M. Jardin, N. A. Rey, R. R. Avillez, Kinetics of nanocrystalline MgO growth by the sol-gel combustion method. Microp. Mesop. Mater. 185 (2014) 86-91.

DOI: 10.1016/j.micromeso.2013.10.021

[12] A. Hunyek, C. Sirisathikul, Variation In Magnetic Properties of Sol-Gel-Synthesized Cobalt Ferrites. Mater. Tech. 47(6) (2013) 845–848.

[13] H. Jeon, D. J. Kim, J. H. Kim, Synthesis of mesoporous MgO catalyst templated by a PDMS-PEO comb-like copolymer for biodiesel production. Fuel Proc. Tech. 116 (2013) 325-331.

DOI: 10.1016/j.fuproc.2013.07.013

[14] A. R. Yacob, M. K. Asyraf, N. S. Samadi, Calcination Temperature of Nano MgO Effect on Base Transesterification of Palm Oil. World Academy of Science, Eng. Tech. 3(1) (2009) 408-412.

[15] S. S. Chang, B. Clair, J. Ruelle, J. Beauchêne, F. D. Reuno, F. Quignard, G. J. Zhao, H. Yamamoto, J. Gril, Mesoporosity as a new parameter for understanding tension stress generation in trees. J. Exp. Botany. 60(11) (2009) 3023-3030.

DOI: 10.1093/jxb/erp133