journal article·2021-04-06Open access

Rapid Microwave Method for Synthesis of Iron Oxide Particles under Specific Conditions

Ivana Mitar, Lucija Guć, Željka Soldin, Martina Vrankić, Andrea Paut, Ante Prkić, Stjepko Krehula

Crystals· Volume 11· Issue 4

Abstract

The advantages of microwave technology over conventionally conducted experiments are numerous. Some of them are reduction in reaction time, a higher degree of process control, repeatability, and work safety. Microwave synthesis routes require a complete description of the experimental details, instrumentation, and design program of a microwave oven used in the experiments. In this work, microwave-assisted hydrothermal synthesis of hematite (α-Fe2O3) particles from 0.1 M FeCl3 solution in highly alkaline media with heating in a microwave oven at continuous microwave emission of 800 W at 150 °C, 200 °C, and 250 °C for 20 min are presented. Also, the influence of the percentage of the addition of a cationic surfactant, cetyltrimethylammonium bromide (CTAB) on the composition, size, and shape of the final product was investigated. The samples precipitated at 150 °C formed a final product consisting of goethite (α-FeOOH) and hematite particles in contrast to the those precipitated at 200 °C and 250 °C where pure hematite phase was obtained. In these synthesis routes, the CTAB caused to slow down the rate of the goethite-to-hematite transformation process at temperatures at 200 °C but did not affect the transformation at 250 °C.
Source: crossref · Quality: baseline

Research context

OpenAlex topics: Iron oxide chemistry and applications · Nanomaterials for catalytic reactions · Minerals Flotation and Separation Techniques

SciVX discovery tags are terminology-based. OpenAlex topics are source-provided classifications.

Affiliations

Faculty of Science, University of Split, Ruđera Boškovića 33, 21000 Split, Croatia

University of Split, Ruđera Boškovića 31, 21000 Split, Croatia

Department of Chemistry, Faculty of Science, University of Zagreb, Horvatovac 102a, 10000 Zagreb, Croatia

Division of Materials Physics and Center of Excellence for Advanced Materials and Sensing Devices, Ruđer Bošković Institute, Bijenička 54, 10000 Zagreb, Croatia

Faculty of Chemistry and Technology, University of Split, Ruđera Boškovića 35, 21000 Split, Croatia

Division of Materials Chemistry, Ruđer Bošković Institute, Bijenička 54, 10000 Zagreb, Croatia

Funding

Croatian Science Foundation

References (88)

Show source-provided references
1. Microwave chemistry for inorganic nanomaterials synthesis10.1039/b9nr00377k ↗
2. How to measure reaction temperature in microwave-heated transformations10.1039/c3cs00010a ↗
3. Practical Microwave Synthesis for Organic Chemists.Strategies, Instruments, and Protocols. Edited by C. Oliver Kappe, Doris Dallinger and Shaun Murphree10.1002/anie.200900791 ↗
4. Microwave-assisted synthesis of nanocrystalline binary and ternary metal oxides10.1080/09506608.2017.1402158 ↗
5. Microwave assisted synthesis–a critical technology overview10.1039/B310502D ↗
6. Cornell, R.M., and Schwertmann, U. (2003). The Iron Oxides: Structure, Properties, Reactions, Occurrence, and Uses, VCH.10.1002/3527602097 ↗
7. Buxbaum, G. (1993). Industrial Inorganic Pigments, VCH. [1st ed.].
8. The removal of carbon monoxide by iron oxide nanoparticles10.1016/S0926-3373(02)00297-7 ↗
9. Arsenic removal from contaminated water by natural iron ores10.1016/j.mineng.2003.11.020 ↗
10. Synthesis and applications of nano-structured iron oxides or hidroxides—A review
11. Magnetic nanoparticles: Synthesis, protection, functionalization, and application10.1002/anie.200602866 ↗
12. Rapid preparation of alpha-FeOOH and alpha-Fe2O3 nanostructures by microwave heating and their application in electrochemical sensors10.1016/j.materresbull.2013.09.052 ↗
13. New sensor based on AgCl containing Iron Oxide or Zinc Oxide Nanoparticles for Chloride Determination10.20964/2019.01.71 ↗
14. Schwertmann, U., and Cornell, R.M. (2000). Iron Oxides in the Laboratory: Preparation and Characterization, VCH.10.1002/9783527613229 ↗
15. Magnetic properties improvement in Fe3O4 nanoparticles grown under magnetic fields10.1016/j.jcrysgro.2004.03.034 ↗
16. Magnetic nanoparticles: Preparation, physical properties, and applications in biomedicine10.1186/1556-276X-7-144 ↗
17. Magnetic iron oxide nanoparticles: Synthesis, stabilization, vectorization, physicochemical characterizations, and biological applications10.1021/cr068445e ↗
18. Yue, J., Jiang, X., Kaneti, Y.V., and Yu, A. (2012). Experimental and theoretical study of low-dimensional iron oxide nanostructures. Smart Nanoparticles Technology, InTech.10.5772/33319 ↗
19. Polymorphous transformations of nanometric iron(III) oxide—A review10.1021/cm200397g ↗
20. Magnetic iron oxide nanoparticles: Synthesis and surface functionalization strategies10.1007/s11671-008-9174-9 ↗
21. Synthesis, properties, and applications of magnetic iron oxide nanoparticles10.1016/j.pcrysgrow.2008.08.003 ↗
22. Fe57 Mössbauer, FT-IR and FE SEM investigation of the formation of hematite and goethite at high pH values
23. Structural Properties of Precipitates Formed by Hydrolysis of Fe3+ Ions in Aqueous Solutions Containing NO3- and Cl- Ions10.1007/BF00363442 ↗
24. Mössbauer spectroscopic study of the formation of Fe(III) oxyhydroxides and oxides by hydrolysis of aqueous Fe(III) salt-solutions10.1016/0021-9797(82)90254-5 ↗
25. Microstructural properties of Fe-oxide powders obtained by precipitation from FeCl3 solutions10.1016/S0921-5107(98)00212-8 ↗
26. Fe57 Mössbauer, FT-IR and TEM investigations of Fe-oxide powders obtained from concentrated FeCl3 solutions10.1016/S0925-8388(98)00637-9 ↗
27. Chemical and microstructural properties of iron oxide powders obtained from FeCl3 solutions with decomposing urea
28. Some factors influencing forced hydrolysis of FeCl3 solutions10.1016/S0167-577X(02)00937-0 ↗
29. Effect of HCl additions on forced hydrolysis of FeCl3 solutions10.1016/j.matlet.2004.04.002 ↗
30. Influence of ruthenium ions on the precipitation of α-FeOOH, α-Fe2O3 and Fe3O4 in highly alkaline media10.1016/j.jallcom.2005.09.016 ↗
31. Properties of γ-FeOOH, α-FeOOH and α-Fe2O3 particles precipitated by hydrolysis of Fe3+ ions in perchlorate containing aqueous solutions10.1016/j.jallcom.2005.09.043 ↗
32. Mössbauer, FT-IR and FE SEM investigation of iron oxides precipitated from FeSO4 solutions
33. Influence of aging in an alkaline medium on the microstructural properties of α-FeOOH10.1016/j.jcrysgro.2007.10.072 ↗
34. Microstructural changes in particles detected during the transformation from β-FeOOH to α-Fe2O3 in dense aqueous suspensions10.1016/j.jallcom.2007.10.014 ↗
35. Investigation of factors influencing the precipitation of iron oxides from Fe(II) containing solutions
36. Precipitation of α-Fe2O3 from dense β-FeOOH suspensions with added ammonium amidosulfonate
37. The effect of temperature on the crystallization of α-Fe2O3 particles from dense β-FeOOH suspensions10.1016/j.matchemphys.2009.10.040 ↗
38. Preparation and characterization of hollow alpha-Fe2O3 irregular microspheres10.1016/j.matlet.2010.08.028 ↗
39. Monitoring the hydrothermal precipitation of α-Fe2O3 from concentrated Fe(NO3)3 solutions partially neutralized with NaOH10.1016/j.molstruc.2010.09.048 ↗
40. The synthesis and microstructure of goethite particles precipitated in highly alkaline media10.1016/j.jallcom.2013.01.027 ↗
41. A novel route in the synthesis of magnetite nanoparticles10.1016/j.matlet.2013.03.013 ↗
42. Monitoring of the Forced Hydrolysis of FeCl3 Solutions in the Presence of Sodium Dodecyl Sulphate
43. Forced hydrolysis of FeCl3 solutions in the presence of sodium dextran sulphate10.1007/s00396-018-4450-4 ↗
44. Synthesis and surface engineering of iron oxide nanoparticles for biomedical applications10.1016/j.biomaterials.2004.10.012 ↗
45. Designed synthesis and surface engineering strategies of magnetic iron oxide nanoparticles for biomedical applications10.1039/C6NR07542H ↗
46. Magnetic nanoparticles: Synthesis, stabilization, functionalization, characterization, and applications10.1007/BF03245856 ↗
47. Microwave assisted synthesis and magnetic property of magnetite and hematite nanoparticles10.1007/s11051-005-9051-8 ↗
48. Microwave-assisted one-step hydrothermal synthesis of pure iron oxide nanoparticles: Magnetite, maghemite and hematite10.1007/s10971-011-2579-4 ↗
49. Synthesis of iron oxide nanocubes via microwave assisted solvolthermal method10.1016/j.jallcom.2010.05.020 ↗
50. Microwave-assisted synthesis of Fe3O4 nanorods and nanowires in an ionic liquid10.1016/j.jpcs.2010.09.016 ↗
51. Iron oxide hollow spheres: Microwave–hydrothermal ionic liquid preparation, formation mechanism, crystal phase and morphology control and properties10.1016/j.actamat.2009.01.009 ↗
52. Microwave-assisted Hydrothermal Synthesis of Magnetite Nanoparticles with Potential Use as Anode in Lithium Ion Batteries10.1590/1516-1439.264714 ↗
53. Rapid microwave assisted synthesis of dextran coated iron oxide nanoparticles for magnetic resonance imaging10.1088/0957-4484/23/21/215602 ↗
54. Microwave-hydrothermal synthesis of nanophase ferrites10.1111/j.1151-2916.1998.tb02738.x ↗
55. Microwave hydrothermal synthesis of γ-Fe2O3 nanoparticles and their magnetic properties10.1016/j.materresbull.2006.11.014 ↗
56. Microwave-Hydrothermal Synthesis of Monodispersed Nanophase α-Fe2O310.1111/j.1151-2916.2001.tb01007.x ↗
57. Microwave–hydrothermal synthesis, characterization and properties of rice-like α-Fe2O3 nanorods10.1016/j.matlet.2012.01.065 ↗
58. Microwave hydrothermal preparation of submicron-sized spherical magnetite (Fe3O4) powders10.1016/S0167-577X(02)00554-2 ↗
59. Mössbauer effect studies on the formation of iron oxide phases synthesized via microwave–hydrothermal route10.1007/s10751-006-9458-3 ↗
60. Effect of variation of molar ratio (pH) on the crystallization of iron oxide phases in microwave hydrothermal synthesis10.1016/S0167-577X(02)00811-X ↗
61. Microwave assisted synthesis of iron(III) oxyhydroxides/oxides characterized using transmission electron microscopy, X-ray diffraction, and X-ray absorption spectroscopy10.1016/j.jpcs.2008.12.017 ↗
62. Fast production of self-assembled hierarchical alpha-Fe2O3 nanoarchitectures10.1021/jp073073e ↗
63. A facile method to syntheses monodisperse gamma-Fe2O3 nanocubes with high magnetic anisotropy density10.1016/j.spmi.2014.01.009 ↗
64. Microwave-assisted synthesis and humidity sensing of nanostructured alpha-Fe2O310.1016/j.materresbull.2008.09.044 ↗
65. A biotechnological perspective on the application of iron oxide magnetic colloids modified with polysaccharides10.1016/j.biotechadv.2010.10.003 ↗
66. A one pot green synthesis and characterisation of iron oxide pectin hybrid nanocomposite10.4236/ojcm.2013.32005 ↗
67. Synthesis and characterization of surfactant-coated superparamagnetic monodispersed iron oxide nanoparticles10.1016/S0304-8853(00)01224-5 ↗
68. Synthesis of Fe3O4 Nanoparticles Prepared by Various Surfactants and Studying their Characterizations10.4028/www.scientific.net/DDF.273-276.22 ↗
69. Hydrolysis of Fe(III) in the presence of mixed anions and promoters10.1007/s10967-020-07158-w ↗
70. The influence of CTAB and gum arabic on the precipitation of alpha-FeOOH in a highly alkaline medium10.1016/j.molstruc.2014.11.040 ↗
71. The Effect of Sodium Dodecyl Sulphate On The Forced Hydrolysis Of FeCl3 Solutions10.20903/csnmbs.masa.2017.38.1.101 ↗
72. Experimental and numerical study of cetyltrimethylammonium bromide (CTAB)-directed synthesis of goethite nanorods10.1016/j.solidstatesciences.2010.04.003 ↗
73. Pulsed-Electrochemical Synthesis and Characterizations of Magnetite Nanorods10.1016/S1452-3981(23)13864-8 ↗
74. Surface modification of magnetic nanoparticles using gum arabic10.1007/s11051-006-9084-7 ↗
75. Facile green synthesis of gold nanoparticles with gum arabic as a stabilizing agent and reducing agent10.1007/BF03214993 ↗
76. Fluoride in Drinking Water and Cancer Mortality in Taiwan10.1006/enrs.1999.4018 ↗
77. Polyethylene glycol modified, cross-linked starch coated iron oxide nanoparticles for enhanced magnetic tumor targeting10.1016/j.biomaterials.2010.11.040 ↗
78. Iron hydroxide nanoparticles coated with poly(ethylene glycol)-poly(aspartic acid) block copolymer as novel magnetic resonance contrast agents for in vivo cancer imaging10.1016/j.colsurfb.2006.12.019 ↗
79. Microwave Rapid Synthesis of Nanoporous Fe3O4 Magnetic Microspheres10.2174/157341309789378050 ↗
80. (2020). Origin 2020b, OriginLab Corporation.
81. Structure and magnetic properties of (La1-xFex)FeO3(x = 0, 0.25, 0.50) perovskite10.1016/j.jallcom.2019.01.047 ↗
82. A profile refinement method for nuclear and magnetic structures10.1107/S0021889869006558 ↗
83. (2014). HighScore Plus Program, Version 4.1, PANalytical.
84. Infrared study of goethites of varying crystallinity and particle size 1: Interpretation of OH and lattice vibration frequencies10.1180/claymin.1986.021.2.08 ↗
85. FTIR analysis of well defined α-Fe2O3 particles10.1016/S0927-7757(97)00102-7 ↗
86. Quantitative phase analysis from neutron powder diffraction data using the Rietveld method10.1107/S0021889887086199 ↗
87. Suggested guidelines for the publication of Rietveld analyses and pattern decomposition studies10.1107/S0021889882012138 ↗
88. Hematite iron oxide nano-particles: Facile synthesis and their chemi-resistive response towards hydrogen10.1088/2053-1591/2/5/055901 ↗