Abstract
We present the process of synthesis and characterization of magnetite-maghemite nanoparticles by the ball milling method. The particles were synthesized in a planetary ball mill equipped with vials and balls of tempered steel, employing dry and wet conditions. For dry milling, we employed microstructured analytical-grade hematite (α-Fe2O3), while for wet milling, we mixed hematite and deionized water. Milling products were characterized by X-ray diffraction, transmission electron microscopy, room temperature Mössbauer spectroscopy, vibrating sample magnetometry, and atomic absorption spectroscopy. The Mössbauer spectrum of the dry milling product was well fitted with two sextets of hematite, while the spectrum of the wet milling product was well fitted with three sextets of spinel phase. X-ray measurements confirmed the phases identified by Mössbauer spectroscopy in both milling conditions and a reduction in the crystallinity of the dry milling product. TEM measurements showed that the products of dry milling for 100 h and wet milling for 24 h consist of aggregates of nanoparticles distributed in size, with mean particle size of 10 and 15 nm, respectively. Magnetization measurements of the wet milling product showed little coercivity and a saturation magnetization around 69 emu g−1, characteristic of a nano-spinel system. Atomic absorption measurements showed that the chromium contamination in the wet milling product is approximately two orders of magnitude greater than that found in the dry milling product for 24 h, indicating that the material of the milling bodies, liberated more widely in wet conditions, plays an important role in the conversion hematite-spinel phase.
Similar content being viewed by others
References
Beth M, Cheng Y (1994) Determination of para-and ferromagnetic components of magnetization and magnetoresistance of granular Co/Ag films (invited). J Appl Phys 75:6894–6899
Can MM, Ozcan SC, Ceylan A, Firat T (2010) Effect of milling time on the synthesis of magnetite nanoparticles by wet milling. Mater Sci Eng B 172:72–75
Chang HSW, Chiou C, Chen Y, Sheen SR (1997) Synthesis, characterization, and magnetic properties of Fe3O4 thin films prepared via a sol–gel method. J Solid State Chem 128:87–92
Chiba M, Morio K, Koizumi Y (2002) Microstructure and magnetic properties of iron oxide thin films by solid reaction. J Magn Magn Mater 239:457–460
Chicinas I (2006) Soft magnetic nanocrystalline powders produced by mechanical alloying routes. J Optoelectron Adv Mater 8(2):439–448
De Carvalho JF, De Medeiros SN, Morales MA, Dantas AL, Carric AS (2013) Synthesis of magnetite nanoparticles by high energy ball milling. Appl Surf Sci 275:84–87
Dong C (1999) Powder X: Windows-95-based program for powder X-ray diffraction data processing. J Appl Crystallogr 32:168–173
Escobar DM, Arroyave C, Calderón J, Margarit I, Mattos O (2007) Paintings pigmented with doped magnetite: preliminary evaluation of anticorrosive properties. Revista de la Facultad de ingeniería Universidad de Antioquia 41:21–30
Feng JSY, Pashley RD, Nicolet M (1975) Magnetoelectric properties of magnetite thin films. J Phys C Solid State Phys 8:1010–1022
Globus A, Pascard H, Cagan V (1977) Distance between magnetic ions and fundamental properties in ferrites. Journal de Physique, Colloque C1, supplément au N° 4, 38, C1-163
Iwasaki T, Kosaka K, Yabuuchi T, Watano S, Yanagida T, Kawai T (2009) Novel mechanochemical process for synthesis of magnetite nanoparticles using coprecipitation method. Adv Powder Technol 20(6):521–528
Iwasaki T, Kosaka K, Watano S, Yanagida T, Kawai T (2010) Novel environmentally friendly synthesis of superparamagnetic magnetite nanoparticles using mechanochemical effect. Mater Res Bull 45:481–485
Kaczmarek WA, Ninham BW (1994) Preparation of Fe3O4 and α-Fe2O3 powders by magnetomechanical activation of hematite. IEEE Trans Magn 30:732–734 Preparation of Fe/sub 3/O/sub 4/ and γ-Fe/sub 2/O/sub 3/ powders by magnetomechanical activation of hematite
Meillon S, Dammak H, Flavin E, Pascard H (1995) Existence of a direct phase transformation from hematite to maghemite. Philos Mag Lett 72(2):105–110
Monshi A, Foroughi MR, Monshi MR (2012) Modified Scherrer equation to estimate more accurately nano-crystallite size using XRD. World J Nano Sci Eng 2:154–160
Morales AL, Velásquez AA, Urquijo JP, Baggio E (2011) Synthesis and characterization of Cu2+ substituted magnetite. Hyperfine Interact 203:75–84
National Bureau of Standards (1981) Standard X-ray diffraction powder patterns. Lib Cong Catalog Card N: 53-61386, 37
Özdemir O, Dunlop DJ (1997) Effect of crystal defects and internal stress on the domain structure and magnetic properties of magnetite. J Geophys Res 102(B9):20211–20224
Ramos JA, Martínez AI, Osorio A, Valladares L, León L, Bustamante A (2014) Structural and magnetic properties of monophasic maghemite (γ-Fe2O3) nanocrystalline powder. Adv Nanoparticles 3:114–121
Randrianantoandro N, Mercier AM, Hervieu M, Greneche JM (2001) Direct phase transformation from hematite to maghemite during high energy ball milling. Mater Lett 47:150–158
Sahebary M, Raygan S, Seyed SA, Abdizadeh H (2009) Inception of transformation of hematite to magnetite during mechanical activation: a thermodynamical approach. Iran J Sci Technol Trans B Eng 33(B5):415–424
Štefanić G, Krehula S, Štefanić I (2013) The high impact of a milling atmosphere on steel contamination. Chem Commun 49(81):9245–9247
Štefanić G, Krehula S, Štefanić I (2015) Phase development during high-energy ball-milling of zinc oxide and iron—the impact of grain size on the source and the degree of contamination. Dalton Trans 44(43):18870–18881
Vandenberghe RE (1990) Mössbauer spectroscopy and applications in geology. International training centre for post-graduate soil scientists. State University Gent, Belgium
Vandenberghe RE, De Grave E, De Bakker PMA (1994) On the methodology of the analysis of Mössbauer spectra. Hyperfine Interact 83:29–49
Velásquez AA, Trujillo JM, Morales AL, Tobón JE, Reyes L, Gancedo R (2005) Design and construction of an autonomous control system for Mössbauer spectrometry. Hyperfine Interact 161:139–145
Zdujić M, Jovalekić C, Karanović L, Mitrić M (1999) The ball milling induced transformation of α-Fe2O3 powder in air and oxygen atmosphere. Mater Sci Enf A 262:204–213 The ball milling induced transformation of α-Fe2O3 powder in air and oxygen atmosphere
Author information
Authors and Affiliations
Corresponding author
Ethics declarations
Conflict of interest
The authors declare that they have no conflict of interest.
Electronic supplementary material
ESM 1
(DOCX 27 kb)
Rights and permissions
About this article
Cite this article
Velásquez, A.A., Marín, C.C. & Urquijo, J.P. Synthesis and characterization of magnetite-maghemite nanoparticles obtained by the high-energy ball milling method. J Nanopart Res 20, 72 (2018). https://doi.org/10.1007/s11051-018-4166-x
Received:
Accepted:
Published:
DOI: https://doi.org/10.1007/s11051-018-4166-x