Article Sidebar

Download
PDF
Statistic
Read Counter : 349 Download : 329

Downloads

Download data is not yet available.

Main Article Content

Abstract

The present article reports a simple and cost-effective process to prepare the crystalline MgAl2O4 spinel using non-stoichometric amount of magnesium nitrate, aluminium nitrate by solution combustion route. Thiourea was used as a fuel and reducing agent while soaking was carried at 1000ºC with different soaking periods. After slow drying of mixed solutions at 80ºC for 4-5 hours a gel was formed and got characterized by DTA/TGA (Differential Thermal Analysis and Thermal Gravimetric Analysis) to observe the effect of temperature variation and identify the range of temperature where crystalline nature of the powder was noted. Powder sample was prepared from the gel after annealing at 1000ºC followed by soaking for 4 hours, 5 hours, 6 hours to compare the variation of particle size with respect to time. The calcined powders were characterized by XRD (X-ray powder diffraction) to determine the phases and crystal planes present in the sample, FT-IR (Fourier-transform infrared spectroscopy) to study the types of metal oxide or metal-metal bond present in the sample along with M-O coordination studies, FESEM (Field emission scanning electron microscopy) to observe the morphological structure of the sample, EDAX (Energy Dispersive X-Ray Analysis) to observe the percentage of each element present in the sample. Bulk densities were estimated from 2.4156 g/cm3 to 2.8571 g/cm3 and the rapid increase in apparent porosity of samples 7.4289%, 10.3630% and 32.51% for 4 hours 5 hours and 6 hours respectively were also noted. It had been observed that the average crystal size of spinel particles was about 48 nm, 36 nm, and 47 nm respectively. Finally, hardness of spinel was evaluated by Vicker Hardness test and evaluated to be10.52GPa (1073 HV), 4.087GPa (416.7HV) and 5.079 GPa (517.9HV).

Keywords

Magnesium Aluminate Phase analysis Morphology M-O co-ordinations Vicker hardness

Article Details

Creative Commons License

This work is licensed under a Creative Commons Attribution-NoDerivatives 4.0 International License.

Author Biographies

Sathi Banerjee, Department of Metallurgical & Materials Engineering, Jadavpur University, 188, Raja S.C. Mallick Road, Kolkata – 700032, India.

Assistant Professor, Department of Metallurgical & Materials Engineering

Soumya Mukherjee, Kazi Nazrul University

Assistant Professor Department of Metallurgical Engineering
How to Cite
Banerjee, S., Mukherjee, S., & Ghosh, S. R. (2021). EVALUATION OF PROPERTIES OF NON-STOICHOMETRIC ALUMINA MAGNESIA SPINEL USING THIOUREA AS FUEL BY VARYING SOAKING TIME. The Journal of Engineering Research [TJER], 18(1), 44–51. https://doi.org/10.53540/tjer.vol18iss1pp44-51
Download Citation
Endnote/Zotero/Mendeley (RIS)
BibTeX

References

  1. Barj M, Bocquet J.F, Chhor K, Pommier C, (1992), Submicronic MgAl2O4 powder synthesis in supercritical ethanol. Journal of Materials Science 27: 2187-2192.
  2. Bickmore R Clint, Waldner F. Kurt, Treadwell R. David, Laine M. Richard, (1996), Ultrafine Spinel powders by Flame Pyrolysis of a Magnesium Aluminium Double Hydroxide. Journal of the American Ceramic Society 79(5): 1419-1423.
  3. Bratton R.J, (1969), Coprecipitates yielding MgAl2O4 powders. American Ceramic Society Bulletin 83: 759-762.
  4. Domanski Daniela, Urretavizcaya Guillermina, Castro J. Facundo, Gennari C. Fabiana, (2004), Mechanochemical Synthesis of Magnesium Aluminate Spinel Powder at Room Temperature. Journal of the American Ceramic Society 87(11): 2020-2024.
  5. Du Xuelian, Liu Yaqiang, Li Liqiang, Chen Wencong, (2014), Synthesis of MgAl2O4 spinel nanoparticles via polymer-gel and isolation –medium-assisted calcination. Journal of Materials Research 29(24): 2921-2927.
  6. Ghosh Chandrima, Ghosh Arup, Halder Manas Kamal (2015), Studies on densification, mechanical, micro-structural and structure properties relationship of magnesium aluminate spinel refractory aggregates prepared from Indian magnesite. Materials Characterization 99: 84-91.
  7. Ghosh S.R, Mukherjee S, Banerjee S (2018), Solution combustion synthesis of Alumina spinel and its characterization. Interceram 67: 34-41.
  8. Gorshkov V.A, Miloserdov P.A, Yukhvid V. I, Sachkova N.V, Kovalev I.D, (2017), Preparation of magnesium aluminate spinel by self propagating high temperature synthesis metallurgy methods. Inorganic Materials 53: 1046-1052.
  9. Habibi Narges, Wang Yuan, Arandiyan Hamidreza, Rezaei Mehran (2017), Low temperature synthesis of mesoporous nanocrystalline magnesium aluminate (MgAl2O4) spinel with high surface area using a novel modified sol-gel method. Advanced Powder Technology 28: 1249-1257.
  10. Lazau Ioan, Ianos Robert, Pacurariu Cornelia, Savii Cecilia, (2008), Spinel preparation by combustion synthesis: The influence of synthesis conditions on the features of the resulted spinel MgAl2O4 powder. Romanian Journal of Materials 3: 224-232.
  11. Lee P.Y, Suematsu H, Yano T, Yatsui K, (2006), Synthesis and Characterization of nanocrystalline MgAl2O4 spinel by polymerized complex method. Journal of Nanoparticle Research 8: 911-917.
  12. Macêdo Maria laponeide Fernandes, Bertran Celso Aparecido, Osawa Carla Cristiane, (2007), Kinetics of the γ → α-alumina phase transformation by quantitative X-ray diffraction. Journal of Materials Science 42: 2830–2836. https://doi.org/10.1007/s10853-006-1364-1
  13. Marakkar Kutty P V, Dasgupta Subrata (2013), Low temperature synthesis of nanocrystalline magnesium aluminate spinel by a soft chemical method. Ceramics International 39(7): 7891-7894.
  14. Mukherjee Soumya, (2020), Evolution of Spinel Magnesium Aluminate by Combustion route using Glycine as Fuel and its characterization. International Journal of Emerging Trends in Science and Technology 6(1): 24-27.
  15. Nassar Y. Mostafa, Ahmed S. Ibrahim, Samir Ihab (2014), A novel synthetic route for magnesium aluminate (MgAl2O4) nanoparticles using sol-gel auto combustion method and their photocatalytic properties. Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy 131: 329-334.
  16. Păcurariu C, Lazău I, Ecsedi Z, Lazău R, Barvinschi P, Mărginean G, (2007), New Synthesis methods of MgAl2O4 spinel. Journal of the European Ceramic Society 27: 707-710.
  17. Patil Kashinath C, Aruna S. T, Mimani Tanu, (2002), Combustion synthesis: An update. Current Opinion in Solid State and Materials Science 6: 507-512.
  18. Pommier C, Chhor K, Bocquet J.F, Barj M, (1990), Reactions in supercritical fluids, a new route for oxide ceramic powder elaboration, synthesis of the spinel MgAl2O4. Materials Research Bulletin 25(2): 213-221.
  19. Saberi Ali, Golestani-Fard Farhad, Sarpoolaky Hosein, Willert Porada Monika, Gerdes Thorsten, Simon Reinhard (2008), Chemical synthesis of nanocrystalline magnesium aluminate spinel via nitrate-citrate combustion route. Journal of Alloys and Compounds 462: 142-146.
  20. Salem Shiva (2015) Application of autoignition technique for synthesis of magnesium aluminate in nano scale: Influence of starting solution pH on physico-chemical characteristics of particles. Materials Chemistry and Physics 155(1): 59-66.
  21. Torkian Leila, Amini M Mostafa, Bahrami Zohreh, (2011), Synthesis of Nano Crystalline MgAl2O4 powder by Microwave assisted combustion. Journal of Inorganic Materials 26(5): 550-554.
  22. Varnier Olivier, Hovnanian Nadine, Larbot André, Bergez Pierre, Cot Louis, Charpin Jean, (1994), Sol-gel synthesis of magnesium aluminum spinel from a heterometallic alkoxide. Materials Research Bulletin 29(5): 479-488.
  23. Yang Ning, Chang Li, (1992), Structural inhomogenity and crystallization behavior of aerosol reacted MgAl2O4 powders. Materials Letters 15(1-2): 84-88.