Structural and Magnetic properties of α-Fe 2 O 3 Nanoparticles د.محمد عبد الله ولد محمد الأمين قسم الفيزياء كلية العلوم جامعة الإمام محمد بن سعود الإسلامية SPS 4th annual meeting November Riyadh
Introduction Experimental Results Conclusions Outline
Introduction Maghemite (γ-Fe 2 O 3 )Hematite (α-Fe 2 O 3 )Magnetite (Fe3O4) Magnetic iron oxides nanoparticles have attracted an increasing interest in the fields of nanoscience and nanotechnology. Sol–gel process Microemulsion technique Forced hydrolysis method Chemical precipitation Ball milling :has been used by several groups : the phase transformations of α-Fe2O3 to γ-Fe2O3 or vice versa. Recently L.C.Sanchez et al Physica B 389 (2007) : by milling in ethanol and in air (the jars were opened to the atmosphere) Rhombohedrally centered hexagonal structure R3c space group a= Å c= Å T<T M = 260 K: antiferromagnetic 260 K<T<950 K: weak ferromagnetic (spin canting) T>T N = 950 K: paramagnetic Aim of this work Production of hematite nanoparticles without phase transformation by dry milling (the jars were closed) ? - Structural and magnetic properties
Mechanical Alloying Magnetic Properties Mössbauer Spectrometry Hysterisis Loops Structure and Morphology XRD, SEM and FT-IR Experimental
Mössbauer Spectrometry Information obtained from Mössbauer : - Magnetic hyperfine characteristics of iron oxide phases. - Information concerning the valence state of iron atoms. - Relative abundance of each component Samples preparation - Commercial α-Fe2O3 powder - Fritsch-P6 – Intensity 250rpm - Stainless steel balls(10 and 15 mm in diameter). - The sample to balls weight ratio 1:10 - Different milling times Information obtained from Mössbauer : Mössbauer effect is the recoil-free emission and resonant absorption of gamma ( γ) rays from the nuclei of certain radioactive isotopes such as 57Fe emission
Results X-ray diffraction All Bragg peaks were only assigned to the presence of α-Fe 2 o 3. The diffraction peaks became broader and their relative intensity decreases. The peak broadening can be caused by both a reduction in crystallite size and an increase in lattice strain ??? In order to obtain these parameters (particles size and strain), a qualitative and quantitative phase analyses using the Rietveld method have been performed. Visual observation : the color of the samples remains red (no new phase).
Rietveld Analysis Δa/a0 and Δc/c0 were found to be positive for all milled samples indicating a lattice expansion. -The variation have the same tendancy indicating anisotropic expansion. The average grain size decreases The microstrain increase with milling time -Using FullProf program -The fitting is performed by a least square method. - Information given by Rietveld : lattices parameteres, microstrain average particle size
FT-IR measurements to access at possible structural changes of the hematite particle during the milling process ? No new peaks in the milled spectra Important changes in the relative intensities and broadening, In agreement with XRD results
Magnetic properties Mössbauer Spectrometry Hysterisis Loops
Mössbauer at room temperature Only one sextet = 0.37 mm/s Q = -0.2 mm/s H = 51.3 T Bulk -Fe 2 O 3 Micrometric (100%) First sextet = 0.37 mm/s Q = -0.2 mm/s H = 50.2 T Micrometric -Fe 2 O 3 (52%) second sextet = 0.35 mm/s H = 45 T Nanometric -Fe 2 O 3 (48%) Hysteresis loops -- The magnetic hysteresis loops for both samples are typical of ferromagnet; - Increase of saturation with decreasing size
Conclusions - Mechanical alloying of hematite micrometric powder processing can be used for the synthesis of hematite nanoparticles without phase transformation after milling from 1 up to 48h. - An expansion of lattices parameters due to the increasing of microstrain induced by ball milling - Mössbauer spectra show that are two component for the milled sample one attributed to the hematite nanoparticles and other due to micrometric hematite. - XRD, FT - IR and Mössbauer : show that are no phase changing during the milling Mohamed Alameen et al, (Submitted to International Journal of Nanosciences)
Perspective - Thermal analysis are in progress - Particle size obtained by XRD ??? Furthers measurement of nanoparticles size will be conducted with others methods such as TEM and Brunauer – Emmett- Teller method (BET). - Magnetic measurements (I will do more analysis on VSM measurements). New project :Gamma irradiation preparation of magnetite(Fe 3 O 4 ) nanoparticles for MRI diagnosis. Maghemite (γ-Fe 2 O 3 )Hematite (α-Fe 2 O 3 )Magnetite (Fe3O4)
Acknowledgments This work was supported financially by King Abdulaziz City for Sciences and technology (KACST). Collaborations : Dr A.Alyemani, R. Msalam and S. Mufti (KACST) Pr M.Sajieddine, Materials sciences group (Sultan Moulay Slimane University,Béni-Mellal (Morroco). Pr K.Ziq, Physics department, KFUPM Dr M.Bououdina,Physics department, University of Bahrain, Kingdom of Bahrain
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