20 Dec 2016 - In addition, precursor powders of Ba3[Cu0.8-xZnx Mn0.2 ]2Fe24O41 hexaferrite (x = 0.0, 0.2, 0.4, 0.6, 0.8) were prepared using ball milling ...
FABRICATION AND CHARACTERIZATION OF POWDER AND THIN FILMS OF Z-TYPE HEXAFERRITE
By Eman Salem H. Al-Hwaitat
Supervisor Dr. Sami Hussein Mahmood, Prof.
Co- Supervisor Dr. Mahmoud Omar Al–Hussein, Prof.
This Dissertation was Submitted in Partial Fulfillment of the Requirements for the Doctor Philosophy Degree in Physics.
School of Graduate Studies The University of Jordan
Dec, 2016
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This Dissertation (Fabrication and Characterization of Powder and Thin Films of Z-Type Hexaferrites) was Successfully Defended and Approved on December 20, 2016.
Examination Committee
Signature
Dr. Sami Hussein Mahmood (supervisor) ------------------------------Prof. of Experimental Solid State Physics Dr. Mahmoud Omar Al –Hussein (Co-supervisor) ------------------------------Prof. of Polymer Physics
Dr. Bashar Ibrahim Lahlouh (Member) ------------------------------Assoc. Prof. of Electronics and Material science
Dr. Yahya Ibrahim Al-Ramadin (Member) ------------------------------Prof. of Molecular physics
Dr. Hasan Mohammed El Ghanem (Member) ------------------------------Prof. of Solid State Physics (Jordan University of Science and Technology)
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FABRICATION AND CHARACTERIZATION OF POWDER AND THIN FILMS OF Z-TYPE HEXAFERRITE
By Eman Salem H. Al-Hwaitat Supervisor Dr. Sami Hussein Mahmood, Prof. Co- Supervisor Dr. Mahmoud Omar Al–Hussein, Prof.
ABSTRACT
In this research, we investigated the influence of preparation methods and experimental conditions on the structural and magnetic properties of Z-type hexaferrite. Precursor powder for Zn2Z system was prepared using ball milling technique. The resulting powder was then preheated at 900° C for 2 h, and then pressed into disks which were subsequently sintered in air at 1250 and 1300° C for 2 h. The structural properties of the prepared samples were carefully investigated using X-ray diffraction, and scanning electron microscopy (SEM). The magnetic properties of the prepared samples were investigated using vibrating sample magnetometry (VSM). XRD patterns revealed the presence of Z-type hexaferrite phase with traces of Y-, and W- type hexaferrite phases. The SEM imaging demonstrated particle stacking in the samples, which could indicate crystallographic texture. Further, the SEM images showed that the particle size increased with increasing the sintering temperature. The magnetic results showed that the saturation magnetization of the samples increased with increasing the sintering temperature, while the value of the coercivity decreased sharply at high sintering temperatures. This sharp decrease is associated with the transformation from the hard BaM magnetic phase to the softer Z-, Y, and W-type phases, and the accompanying growth of the particle size at elevated temperatures. For comparison, precursor powders of Zn2Z system were prepared using sol-gel auto combustion method. The powder, as well as the disks prepared from the precursor powder were then sintered in air at 900, 1100, 1250° C for 2 h. XRD pattern for the disk sample sintered at 1250° C revealed the existence of Zn2Z phase with a trace Zn2Y phase, while for the powder sample sintered at 1250° C showed Zn2Y with BaM, and ZnFe2O4 as secondary phases. The separation of intermediate BaM and Y phases in the powder sample is due to the complexity of Z-type structure which imposes progressive transformation through intermediate ferrites before achieving the final required structure. The sol-gel auto combustion method lowers the sintering temperature, and produces smaller particle size compared with ball milling technique. In addition, the magnetic results showed that the saturation magnetization of the
4 samples increased, while the coercive field decreased with increasing the sintering temperature. In addition, precursor powders of Ba3[Cu0.8-xZnx Mn0.2 ]2Fe24O41 hexaferrite (x = 0.0, 0.2, 0.4, 0.6, 0.8) were prepared using ball milling technique. The samples were sintered at 1200° C for 2h in air. XRD pattern for sample with x = 0.4 and x = 0.6 revealed the presence of a pure Z-type hexaferrite phase. The absence of the secondary phases indicates that the zinc and manganese ions diffuse completely into Cu2Z crystal. SEM images showed that the particle size increase with increasing Zn content, and then decrease for x = 0.6 and 0.8. The magnetic results indicated that the saturation magnetization Ms increase with increasing Zn content, while the coercive field decrease with increasing Zn content, and then increase at x = 0.6 due to reduction of the particle size. Hexaferrite films on Si substrates (S-film) were prepared from solution using drop casting technique. Sol-gel precursor was dissolved in a mixture of ethylene glycol and 2-methoxyethanol solvents. The deposited films were dried at 450° C and then sintered at 1250° C. XRD patterns of the prepared films revealed reflections corresponding to the Z-type hexaferrite, ZnFe2O4 and α-Fe2O3 phases. The corresponding SEM images showed a variety of crystallization habits, which could be associated with solution inhomogeneities. In addition, EDX results confirmed the existence of Z hexaferrite, ZnFe2O4 and α-Fe2O3 phases. The magnetic results demonstrated that the magnetization did not reach saturation up to the maximum applied field of 6 kOe. The hysteresis loops revealed typical characteristics of a soft magnetic material. Also, the magnetic moment in a direction perpendicular to the applied field is significantly lower than that in the parallel direction, which could indicate that the easy direction of magnetization is in the plane of the film Finally, we tried to prepare hexaferrite films with micron-size pores. Micronsize polymer spheres were embedded in the hexaferrite film precursors. To remove the polymer spheres, the films were calcinated at temperatures ranging between 450600° C. Magnetic characterization of the porous films revealed that the increased porosity has no effect on the coercive field.
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