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Abstract
In the present article spinel phase magnesium aluminate was synthesized using Magnesium nitrate, Al-nitrate precursors in 1:2 molar ratio using urea and thiourea as fuel and reducing agent. Nitrate salts were mixed in a stoichiometric ratio in distilled water with three different molar ratios of two different fuels: urea and thiourea. The temperature of crystallization was obtained after thermal analysis followed by annealing at a fixed temperature, fixed soaking period for urea as fuel while variable temperature and soaking period were required for thiourea as fuel. FTIR analyses were carried out of the samples to verify the M-O co-ordinations for the phase formation. Prominent octahedral M-O stretching was noted at about 609 cm-1 while that of Al-Mg-O stretching was noted at about 1100 cm-1 for thiourea based samples. Using Urea as fuel Al-O stretching was noted at about 539cm-1 while that of Al-Mg-O vibration was noted at about 677cm-1. Morphological features of the synthesized samples were observed by SEM. Agglomeration was noted for both urea and thiourea as fuel having irregular polygon shape. Using thiourea as fuel, a bit of porous structure was noted while for urea as fuel negligible porosity was noted.
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References
- Barj M, Bocquet J.F, Chhor K, Pommier C, (1992), Submicronic MgAl2O4 powder synthesis in supercritical ethanol. Journal of Materials Science 27: 2187-2192.
- 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.
- Bratton R.J, (1969), Coprecipitates yielding MgAl2O4 powders. American Ceramic Society Bulletin 83: 759-762.
- 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.
- 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.
- 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.
- Ghosh S.R, Mukherjee S, Banerjee S (2018), Solution combustion synthesis of Alumina spinel and its characterization. Interceram 67: 34-41.
- 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.
- 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.
- 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.
- 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
- 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.
- 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.
- 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.
- 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.
- 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.
- 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.
- 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.
- 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.
- 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.
- Yang Ning, Chang Li, (1992), Structural inhomogenity and crystallization behavior of aerosol reacted MgAl2O4 powders. Materials Letters 15(1-2): 84-88.
References
Barj M, Bocquet J.F, Chhor K, Pommier C, (1992), Submicronic MgAl2O4 powder synthesis in supercritical ethanol. Journal of Materials Science 27: 2187-2192.
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.
Bratton R.J, (1969), Coprecipitates yielding MgAl2O4 powders. American Ceramic Society Bulletin 83: 759-762.
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.
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.
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.
Ghosh S.R, Mukherjee S, Banerjee S (2018), Solution combustion synthesis of Alumina spinel and its characterization. Interceram 67: 34-41.
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.
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.
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.
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
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.
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.
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.
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.
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.
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.
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.
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.
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.
Yang Ning, Chang Li, (1992), Structural inhomogenity and crystallization behavior of aerosol reacted MgAl2O4 powders. Materials Letters 15(1-2): 84-88.