Mira Ristić, Jasenka Štajdohar, Ivana Opačak, Svetozar Musić


Precipitations by the forced hydrolysis of 0.2 M FeCl3 aqueous solutions between 2 and 72 hours in the presence of 1% sodium dodecyl sulphate (SDS) were investigated. In the absence of SDS a direct phase transformation ß-FeOOH → α-Fe2O3 via dissolution/recrystallization occured in the precipitation system. In the presence of SDS, α-FeOOH as an intermediate phase precipitated and, with a prolonged time of forced hydrolysis, also transformed to α-Fe2O3 via the dissolution/recrystallization mechanism. On the basis of Mössbauer spectra it was concluded that in the presence of SDS, α-Fe2O3 phase possessed a lower degree of crystallinity. In this precipitation process the competition between the stability of Fe(III)-dodecyl sulphate, on one side, and the formation of iron oxide phases, on the other, also played an important role. FE SEM revealed that the big α-Fe2O3 particles possessed the substructure. The elongation of primary α-Fe2O3 particles produced in the presence of SDS was noticed. This effect can be assigned to the preferential adsorption of dodecyl sulphate groups on nuclei and crystallites of FeOOH and α-Fe2O3 phase during the forced hydrolysis of FeCl3 solutions.


FeCl3 hydrolysis; sodium dodecyl sulphate; α-Fe2O3; Mössbauer; FT-IR; XRD; FE SEM

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J. R. Freyer, A. Gildawie, R. Paterson, High resolution studies of the initial stages of precipitation of hydrous iron oxides, Eight Int. Congress on Electron Microscopy, Canberra, 1974, Vol. 1, pp. 708–709.

J. M. Gonzáles-Calbet, M. A. Alario-Franco, M. Gayoso-Andrade, The porous structure of synthetic akaganeite, J. Inorg. Nucl. Chem., 43 (1981), pp. 257–264.

S. Musić, A. Vértes, G. W. Simmons, I. Czakó-Nagy, H. Leidheiser Jr., Mössbauer spectroscopic study of the formation of Fe(III)-oxyhydroxides and oxides by hydrolysis of aqueous Fe(III) salt solu-tions, J. Coll. Interface Sci., 85 (1982), pp. 256–266.

E. Matijević, P. Scheiner, Ferric hydrous oxide sols. III. Preparation of uniform particles by hydrolysis of Fe(III)-chloride, -nitrate, and -perchlorate solutions, J. Coll. Interface Sci., 63 (1978), pp. 509–524.

S. Hamada, E. Matijević, Ferric hydrous oxide sols. IV. Preparation of uniform cubic hematite particles by hydrolysis of ferric chloride in alcohol-water solutions, J. Chem. Soc. Faraday Trans., I 78 (1982), pp. 2147–2156.

E. K. De Blanco, M. A. Blesa, S. J. Liberman, Comments on the mechanism of the akageneitehematite phase transformation in hydrothermal solutions, Reactivity of Solids, 1 (1986), pp. 189–194.

S. Musić, M. Ristić, S. Krehula, 57Fe Mössbauer spectroscopy in the investigation of the precipitation of iron oxides, Chapter in the book Mössbauer Spectroscopy: Applications in Chemistry, Biology and Nanotechnology, Edited by V. K. Sharma, G. Klingelhofer and T. Nishida, Publ. by John Wiley & Sons, 2013, pp. 470–504.

H. Katsuki, S. Komarneni, Role of -Fe2O3 morphology on the color of red pigment for porcelain, J. Am. Ceram. Soc., 86 (2003), pp. 183-185.

T. Sugimoto, Y. Wang, H. Itoh, A. Muramatsu, Sys-tematic control of size, shape and internal structure of monodisperse -Fe2O3 particles, Colloids Surfaces A: Physicochem. and Eng. Aspects, 134 (1998), pp. 205–279.

B. Mao, Z. Kang, E. Wang, C. Tian, Z. Zhang, C. Wang, Y. Song, M. Li, J. Solid State Chem., 180 (2007), pp. 489–495.

K. Kandori, N. Hori, T. Ishikawa, Preparation of mesoporous hematite particles by a forced hydrolysis reaction accompanying a peptide production reaction, Colloids Surfaces: Physicochem. Eng. As-pects, 290 (2006), pp. 280–287.

K. Kandori, I. Hori, A. Yasukawa, T. Ishikawa, Effect of surfactants on the precipitation and properties of colloidal particles from forced hydrolysis of FeCl3-HCl solutions, J. Mater. Sci., 30 (1995), pp. 2145–2152.

M. Žic, M. Ristić, S. Musić, Microstructural changes in particles detected during the transfor-mation from -FeOOH to -Fe2O3 in dense aqueous suspensions, J. Alloys Comp., 464 (2008), pp. 81–88.

M. Žic, M. Ristić, S. Musić, Precipitation of -Fe2O3 from dense -FeOOH suspensions with added ammonium amidosulfonate, J. Mol. Struct. 924–926 (2008), pp. 235–242.

S. Musić, A. Šarić, S. Popović, Effects of urotropin on the formation of -FeOOH, J. Mol. Struct. 410-411 (1997), pp. 153–156.

A. Šarić, S. Musić, K. Nomura, S. Popović, Microstructural properties of Fe-oxide powders obtained by precipitation from FeCl3 solutions, Mater. Sci. Eng., B56 (1998), pp. 43–52.

B. Weckler, H. D. Lutz, Lattice vibration spectra. Part XCV. Infrared spectroscopic studies on the iron oxide hydroxides goethite (a), akageneite (b), lepidocrocite (d) and feroxyhite (d), Eur. J. Solid State Inorg. Chem., 35 (1998), pp. 531–544.

E. Murad, J. L. Bishop, The infrared spectrum of synthetic akageneite, -FeOOH, Am. Mineral., 85 (2000), pp. 716–721.

Y. Wang, A. Muramatsu, T. Sugimoto, FTIR analysis of welldefined -Fe2O3 particles, Colloid Surf. Sci. A: Physicochem. Aspects, 134 (1998), pp. 281–297.

S. Krehula, S. Musić, Influence of ageing in an alkaline medium on the microstructural properties of -FeOOH, J. Cryst. Growth, 310 (2008), pp. 513–520.

D. Peak, R. G. Ford, D. L. Sparks, An in situ ATR-FTIR investigation of sulfate bonding mechanisms on goethite, J. Coll. Interface Sci., 218 (1999), pp. 289–299.

M. Ocaňa, M. P. Morales, C. J. Serna, Homogeneous precipitation of uniform -Fe2O3 particles from iron salts solutions in the presence of urea, J. Coll. Interface Sci. 212 (1999), pp. 317–323.

S. Musić, S. Krehula, S. Popović, Effect of HCl additions on forced hydrolysis of FeCl3 solutions, Ma-ter. Lett. 58 (2004), pp. 2640–2645.

W. Wang, J. Y. Howe, B. Gu, Structure and morphology evolution of hematite (-Fe2O3) nanoparticles in forced hydrolysis of ferric chloride, J. Phys. Chem., C 112 (2008), pp. 9203–9208.

E. Murad, J. H. Johnston, Iron oxides and oxyhydroxides, in: G. J. Long (Ed.), Mössbauer Spectroscopy Applied to Inorganic Chemistry, Vol. 2, Ple-num Pub. Corp. 1987, pp. 507–582.



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