Abstract
The synthesis for a series of ferrite (MIIFe2O4) and cobaltite (MIICo2O4) spinels was investigated where MII is Mg, Co, Ni, Cu or Zn. The ferrites were prepared at a calcination temperature of 800 °C; the cobaltites at 500 °C. TG–MS indicated that reduction of CoIII to CoII occurs at ca. 800 °C, hence, the lower calcination temperature. For both the ferrites and the cobaltites, the evolution of water and CO2 during the calcination suggests the presence of both species in the precipitates. The observed mass losses indicated that the precursor basic carbonate precipitates for the cobaltite synthesis were predominantly carbonate, while the precursor basic carbonate precipitates for ferrite synthesis were predominantly hydroxide in character. XRD data showed successful synthesis of the ferrites with minimal contamination from the parent oxides, while the cobaltites were observed to be predominantly of the spinel structure.
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References
Hyeon T. Chemical synthesis of magnetic nanoparticles. Chem Commun. 2003;(8):927–34.
Hirai P, Sengupta S. Spinel ferrites as catalysts: a study on catalytic effect of coprecipitated ferrites on hydrogen peroxide decomposition. Can J Chem. 1991;69:33–6.
Konvička T, Mošner P, Šolc Z. Investigation of the non-isothermal kinetics of the formation of ZnFe2O4 and ZnCr2O4. J Therm Anal Calorim. 2000;60(2):629–40.
Paike VV, et al. Synthesis of spinel CoFe2O4 Via the co-precipitation method using tetraalkyl ammonium hydroxides as precipitating agents. J Am Ceram Soc. 2007;90(9):3009–12.
Klissurski DG, Uzunova EL. Synthesis of high-dispersity zinc cobaltite from coprecipitated hydroxycarbonate precursor. J Mater Sci Lett. 1990;9(5):576–9.
Klissurski DG, Uzunova EL. Synthesis of nickel cobaltite spinel from coprecipitated nickel-cobalt hydroxide carbonate. Chem Mater. 1991;3:1060–3.
Zümreoglu-Karan B, Yilmazer E. Preparation of spinel-type cathode materials from carbonate/oxalate powder mixtures. A solid-state experiment for advanced undergraduate inorganic chemistry laboratory. J Chem Educ. 2000;77(9):120.
Berger P, et al. Preparation and properties of an aqueous ferrofluid. J Chem Educ. 1999;76(7):943.
Suchow L. A detailed, simple crystal field consideration of the normal spinel structure of Co3O4. J Chem Educ. 1976;53(9):560.
Weller MT. Inorganic materials chemistry. Oxford: Oxford University Press; 1994.
Szczygiel I, Winiarska K. Low-temperature synthesis and characterization of the Mn–Zn ferrite. J Therm Anal Calorim. 2011;104:557–83.
Bordeneuve H, Rousset A, Tenailleau C, Guillemet-Fritsch S. Cation distribution in manganese cobaltite spinels Co3-xMnxO4 (0 ≤ x ≤ 1) determined by thermal analysis. J Therm Anal Calorim. 2010;101:137–42.
Pacurariu C, et al. New synthesis methods of MgAl2O4 spinel. J Eur Ceram Soc. 2007;27(2–3):707–10.
Thang PD, Rijnders G, Blank DHA. Spinel cobalt ferrite by complexometric synthesis. J Magnet Magnet Mater. 2005;295(3):251–6.
Gawas UB, Verenkar V/M/S, Mojumdar SC. Synthesis and characterisation of Ni0.6Ni0.4Fe2O4 nano-particles obtained by autocatalytic thermal decomposition of carboxylato-hydrazinate complex. J Therm Anal Calorim. 2011;104:879–83.
Gonsalves LR, Mojumdar SC, Verenkar VMS. Synthesis of cobalt nickel ferrite nanoparticles via autocatalytic decomposition of the precursor. J Therm Anal Calorim. 2010;100:789–92.
Waqas H, Qureshi AH. Influence of pH on nanosized Mn–Zn ferrite synthesized by sol–gel auto combustion process. J Therm Anal Calorim. 2009;98:355–60.
Waqas H, Qureshi AH. Low temperature sintering study of nanosized Mn–Zn ferrites synthesized by sol–gel auto combustion process. J Therm Anal Calorim. 2010;100:529–35.
Sen A, Pramanik P. Preparation of nano-sized calcium, magnesium & zinc chromite powder through metalo-organic precursor solutions. J Mater Synth Process 2002;10(3):107–11.
Šepelák V, Heitjans P, Becker K. Nanoscale spinel ferrites prepared by mechanochemical route. J Therm Anal Calorim. 2007;90(1):93–7.
Turkin AI, Drebushchak VA. Synthesis and calorimetric investigation of stoichiometric Fe-spinels: MgFe2O4. J Cryst Growth. 2004;265(1–2):165–7.
Turkin AI, et al. Low temperature heat capacity of magnesioferrite, MgFe2O4. J Therm Anal Calorim. 2008;92(3):717–21.
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Angus, K., Thomas, P. & Guerbois, JP. Synthesis and characterisation of cobaltite and ferrite spinels using thermogravimetric analysis and X-ray crystallography. J Therm Anal Calorim 108, 449–452 (2012). https://doi.org/10.1007/s10973-011-1863-4
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DOI: https://doi.org/10.1007/s10973-011-1863-4