Low temperature synthesis of Co3O4 and (Co1−xMnx)3O4 spinels nanoparticles

• Published in: Advanced powder technology : the international journal of the Society of Powder Technology, Japan Vol. 28; no. 5; pp. 1325 - 1331
• Main Authors: Giovannelli, F., Marsteau, V., Zaghrioui, M., Autret, C., Delorme, F.
• Format: Journal Article
• Language: English
• Published: Elsevier B.V 01.05.2017
• Subjects: Co3O4; Mn3O4; Precipitation; Solid solution; Spinel; Mn3O4; Precipitation; Spinel; Solid solution; Co3O4
• ISSN: 0921-8831; 1568-5527
• DOI: 10.1016/j.apt.2017.02.022

[Display omitted] •(Co1−xMnx)3O4 solid solution is synthesized in water at 60°C by soda addition.•The particles are well crystallized and exhibit a size close to 50nm.•Each particle is composed by several crystallographic domains of about 10nm.•Precipitation is a simple, fast and safe process. The (Co1−xMnx)3O4 solid solution have been synthesized in water at 60°C by soda addition to a cationic solution. XRD patterns show that spinel oxide has been obtained except for pure cobalt composition which exhibits also the presence of hydroxide and oxy-hydroxide. Therefore, to reach this composition, a different synthesis route has been developed: the cationic solution is added to the soda and for the first time Co3O4 nanoparticles have been synthesized by a direct precipitation in aqueous solution at low temperature. For each composition, the particles are well crystallized and exhibit a size close to 50nm. Each particle is composed by several crystallographic domains of about 10nm. The cubic to tetragonal transition reported in the literature for x=0.46 is observed in between x=0.33 and x=0.50. Raman spectra show that substitution of Co by Mn, in the cubic phase, introduces a random high disorder. In the tetragonal phase, occupation of the octahedral site remains a random occupation, while the tetrahedral site seems to be preferentially occupied by Co ions. All these results show that the precipitation is a simple, fast and safe process to synthesize pure phase of (Co1−xMnx)3O4 spinel solid solution in aqueous media at low temperature.