Abstract
In the present study, manganese oxide (Mn3O4) was synthesized sonochemically by considering manganese sulphate monohydrate as precursor. Initially, 0.1 M of manganese sulphate monohydrate dissolved in 60 ml of doubly distilled water; subsequently, 400 μl of ammonia solution (30% GR) is added to prepare the solution. The experimental variables selected in this study are sonication, sonication with oxygen bubbling, sonication with argon bubbling, adding H2O2 and butanol externally with mechanical stirring. The obtained samples characterized with XRD, FTIR, SEM and TEM to determine the phase purity, morphology and size of the particles. Yield of the end product is determined by weighing the sample obtained after drying. Yield of the product increased with external addition of H2O2 and oxygen bubbling. Morphology studies show that the product obtained is spherical and cubical in shape. The TEM image shows that particle size lies in the range of 20–50 nm in sonication applied experiments. Particle size reduced with applying sonication when compared to mechanical stirring. XRD studies show that the product obtained is Mn3O4.
![](http://media.springernature.com/m312/springer-static/image/art%3A10.1007%2Fs40033-019-00193-2/MediaObjects/40033_2019_193_Fig1_HTML.png)
![](http://media.springernature.com/m312/springer-static/image/art%3A10.1007%2Fs40033-019-00193-2/MediaObjects/40033_2019_193_Fig2_HTML.png)
![](http://media.springernature.com/m312/springer-static/image/art%3A10.1007%2Fs40033-019-00193-2/MediaObjects/40033_2019_193_Fig3_HTML.png)
![](http://media.springernature.com/m312/springer-static/image/art%3A10.1007%2Fs40033-019-00193-2/MediaObjects/40033_2019_193_Fig4_HTML.png)
![](http://media.springernature.com/m312/springer-static/image/art%3A10.1007%2Fs40033-019-00193-2/MediaObjects/40033_2019_193_Fig5_HTML.jpg)
Similar content being viewed by others
References
A.E. Fischer, A.P. Katherine, R.R. Debra, M.S. Rhonda, W.L. Jeffrey, Incorporation of homogeneous, nanoscale MnO2 within ultraporous carbon structures via self-limiting electroless deposition: implications for electrochemical capacitors. Nano Lett. 2, 281–286 (2007)
Y. Zeheng, Z. Yuancheng, Z. Weiin, W. Xue, Q. Yitai, W. Xiaogang, Y. Shine, Nanorods of manganese oxides: synthesis, characterization and catalytic application. J. Solid State Chem. 179, 679–684 (2006)
J.B. Fei, Y. Cui, X.H. Yan, W. Qi, Y. Yang, K.W. Wang, Q. He, J.B. Li, Controlled preparation of MnO2 hierarchical hollow nanostructures and their application in water treatment. Adv. Mater. 20, 452–456 (2008)
Z.Y. Yuan, Z. Zaolo, D. Gaohui, T.-Z. Ren, B.-L. Su, A simple method to synthesize single-crystalline manganese oxide nanowires. Chem. Phys. Lett. 378, 349–353 (2003)
M. Kang, E.D. Park, J.M. Kim, J.E. Yie, Manganese oxide catalysts for NOX reduction with NH3 at low temperatures. Appl. Catal. A Gen. 327, 261–269 (2007)
Y.-F. Han, F. Chen, Z. Zhong, K. Ramesh, L. Chen, E. Widjaja, Controlled synthesis, characterization and catalytic properties of Mn2O3 and Mn3O4 nanoparticles supported on mesoporous silica SBA-15. J. Phys. Chem. B 110, 24450–24456 (2006)
G. Laugel, J. Arichi, M. Moliere, A. Kiennemann, F. Garin, B. Louis, Metal oxides nanoparticles on SBA-15: efficient catalyst for methane combustion. Catal. Today 138, 38–42 (2008)
E.J. Grootendorst, Y. Verbeek, V. Ponec, The role of the mars and van krevelen mechanism in the selective oxidation of nitrosobenzene and the deoxygenation of nitrobenzene on oxidic catalysts. J. Catal. 157, 706–712 (1995)
L. Sanchez, J. Farcy, J.P.P. Ramos, L. Hernan, J. Morales, J.L. Tirado, Low-temperature mixed spinel oxide as lithium insertion compounds. J. Mater. Chem. 6, 37–39 (1996)
Z.W. Chen, S.Y. Zhang, S. Tan, J. Wang, S.Z. Jin, Dependence of electronic structure on the grain size in Mn2O3 nanocrystals. Appl. Phys. A 78, 581–584 (2004)
S.-N. Masoud, F. Davar, M. Mazaheri, Synthesis of Mn3O4 nanoparticles by thermal decomposition of a [bis(salicylidiminato)manganese(II)] complex. Polyhedron 27, 3467–3471 (2008)
E. Finocchio, G. Busca, Characterization and hydrocarbon oxidation activity of coprecipitated mixed oxides Mn3O4/Al2O3. Catal. Today 70, 213–225 (2001)
Z.W. Chen, J.K.L. Lai, C.H. Shek, Shape-controlled synthesis and nanostructure evolution of single-crystal Mn3O4 nanocrystals. Scripta Mater. 55, 735–738 (2006)
H. Dhaouadi, A. Madani, F. Touati, Synthesis and spectroscopic investigations of Mn3O4 nanoparticles. Mater. Lett. 64, 2395–2398 (2010)
L.-X. Yang, Y. Liang, H. Chen, Y.-F. Meng, W. Jiang, Controlled synthesis of Mn3O4 and MnCO3 in a solvothermal system. Mater. Res. Bull. 44, 1753–1759 (2009)
A. Askarinezad, A. Morsali, Direct ultrasonic-assisted synthesis of sphere-like nanocrystals of spinel Co3O4 and Mn3O4. Ultrason. Sonochem. 16, 124–131 (2009)
V. Ganesh Kumar, D. Aurbuch, A. Gedanken, A comparison between hot-hydrolysis and sonolysis of various Mn(II) salts. Ultrason. Sonochem. 10, 17–23 (2003)
V. Ganesh Kumar, D. Aurbuch, A. Gedanken, Influence of pH on the structure of the aqueous sonolysis products of manganese (III) acetylacetonate. J. Mater. Res. 17, 1706–1710 (2002)
I.K. Gopalakrishnan, N. Bagkar, R. Ganguly, S.K. Kulshreshtha, Synthesis of superparamagnetic Mn3O4 nanocrystallites by ultrasonic irradiation. J. Cryst. Growth 280, 436–441 (2005)
T.R. Bastami, M.H. Entezari, Sono-synthesis of Mn3O4 nanoparticles in different media without additives. Chem. Eng. J. 164, 261–266 (2010)
J.P. Park, S.K. Kim, J.-Y. Park, C.H. Hwang, C. Myung-ho, E.K. Jee, M.O. Kang, K. Ho-Young, W. Shim-II, Synthesis of Mn3O4 and LiMn2O4 nanoparticles by a simple sonochemical method. Mater. Lett. 63, 2201–2204 (2009)
D. Chen, B. Yang, Y. Jiang, Y.-Z. Zhang, Synthesis of Mn3O4 nanoparticles for catalytic application via ultrasound-assisted ball milling. Chem. Select 3, 3904–3908 (2018)
A.B. Pandit, A. Badnore, Effect of pH on sonication assisted synthesis of ZnO nanostructures: process details. Chem. Eng. Process. 122, 235–244 (2017)
M. Ashokkumar, R. Hall, P. Mulvaney, F. Grieser, Sonoluminescence from aqueous alcohol and surfactant solutions. J. Phys. Chem. B 101, 10845–10850 (1997)
S.W. Seo, H.H. Jo, K. Lee, B. Kim, S.J. Oh, T.J. Park, Size-dependent magnetic properties of colloidal Mn3O4 and MnO nanoparticles. Angew. Chem. 43, 1115–1117 (2004)
X. Hao, J. Zhao, Y. Li, Y. Zhao, D. Ma, L. Li, Mild aqueous synthesis of octahedral Mn3O4 nanocrystals with varied oxidation states. Colloids Surf. A 374, 42–47 (2011)
Acknowledgements
Authors gratefully acknowledge IIT Guwahati and VFSTR Deemed to be University for providing facilities to carry the work.
Author information
Authors and Affiliations
Corresponding author
Additional information
Publisher's Note
Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.
Dr. Venkata Swamy Nalajala is an assistant professor in the Department of Chemical Engineering, Vignan’s foundation for Science, Technology and Research, Vadlamudi (Deemed to be University).
Rights and permissions
About this article
Cite this article
Nalajala, V.S., Khan, A.A., Tondepu, S. et al. Influence of process parameters on the yield of Mn3O4 through sonochemical route. J. Inst. Eng. India Ser. D 100, 211–215 (2019). https://doi.org/10.1007/s40033-019-00193-2
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s40033-019-00193-2