H. S. Woon, K. P. Lim, C. K. Ho, C. L. Cheah and N. Riza / IJECCT 2011, Vol. 1 (2) 1 A Study on Waste-derived NiZn Soft Ferrites As EMI Suppressor H. S. Woon1, K. P. Lim2, C. K. Ho1, C. L. Cheah1 and N. Riza1 1 College of Engineering, Universiti Tenaga Nasional (UNITEN), Kampus Putrajaya, Jalan Ikram-UNITEN, 43000 Kajang, Selangor, Malaysia. 2 Physics Department Faculty of Science Universiti Putra Malaysia Serdang 43400 Selangor, Malaysia E-mail: [email protected] Abstract: Nickel-zinc soft ferrites with spinel structure are important electronic components popularly used as EMI suppressor, electromagnet core and transformer core. It contains nickel, zinc or manganese, and the raw material is mainly hematite. The most commonly use soft ferrites are NiZn ferrites and MnZn ferrites. NiZn ferrites exhibit higher resistivity than MnZn ferrites and are therefore more suitable for frequencies above 1 MHz. In this work, iron oxide waste generated from a local cold-rolling steel mill was purified and converted into hematite. The wastederived hematite was used as the raw material in the synthesis of NiZn ferrites. The magnetic properties such as permeability, saturation magnetization and coercivity of the waste-derived NiZn ferrites was analyzed and compared to the industrial grade NiZn ferrites. Our results show that the waste-derived ferrite possesses excellent magnetic properties. The microstructure of the wastederived NiZn ferrite is also discussed. Keywords – soft ferrite; hematite (Fe2O3); cold-roll steel industry I. INTRODUCTION Ferrite cores are commonly used in electronic inductors, transformers, electromagnets and EMI suppressor where the high electrical resistance of the ferrite leads to very low eddy current losses. They are usually seen as a lump in a computer cable, called a ferrite bead. These ferrite beads prevent high frequency electrical noise (radio frequency interference) from exiting or entering the equipment. Nickel-zinc ferrite is produced using conventional ceramic processing method (wet method) in the industry. The process includes wet mixing the raw materials, that are hematite, nickel oxide and zinc oxide, heat treatment, forming and sintering. The NiZn ferrite compound is produced shown by the chemical reaction: NiO + ZnO + 2 Fe2O3 → 2 Ni0.5Zn0.5Fe2O4 Ferrite materials possess good magnetic properties such as high permeability and saturation magnetization but low coercivity[1,2,3]. The Malaysia steel-making industry consists of two major streams; i.e. hot rolling and cold rolling industries. The hot rolling process involves slab-heating (as well as billet and bloom), rolling, and forming operations. Several types of hot forming mills manufacture diverse steel products. Long products are manufactured by hot rolling billets into reinforcement bars, or for further rolling and drawing into wire rods and sometimes coating. To prepare the steel for cold rolling or drawing, acid pickling is performed. The acid pickling chemically remove oxides and scale from the surface of the steel. In continuous pickling processes, the steel is immersed in acid cleaning tanks and then cleaned in a series of water rinsing tanks. The spent acid will normally be re-generated in the acid regeneration plant (ARP) through fluidized-bed process where iron oxide waste is produced.[4] Colormetry is a simple but useful method to identify the presence of hematite in the sample. The L*a*b* color space (also referred to as CIELAB) is one of the most popular color space for measuring object color and is widely used in virtually all fields. In this color space, L* indicate lightness and a* and b* are the chromaticity coordinates. Figure 1 shows the a* and b* chromaticity diagram. +a* is the red direction, -a* is the green direction, +b* is the yellow direction and –b* is the blue direction [5]. H. S. Woon, K. P. Lim, C. K. Ho, C. L. Cheah and N. Riza / IJECCT 2011, Vol. 1 (2) 2 Mixing Fe2O3 : NiO:ZnO Pre-Sintering at 1000°C High Energy Milling Forming Sintering at 1150°C Figure 1. The Color Ball and the L*a*b* Colormetry System Sample Characterizations Figure 2. Schematic Diagram of NiZn Soft Ferrites Synthesis Procedure II. MATERIAL AND METHOD Iron oxide waste produced by acid-regeneration-plant (ARP) in a local cold-rolling steel mill was collected. The factory waste then inspected, cleaned and dried in an oven. A high-energy-blender was employed to mill the waste into ultra-fine powder and high-gradient magnetic separation was performed. The sub-micron powder was then converted into hematite by means of heat treatment. Conventional ceramic preparation process was employed in this work in the synthesis of NiZn soft ferrites. The process includes mixing, pre-sintering, granulation, forming and sintering. The experimental procedure is summarized in Figure 2. III. RESULTS Steel industry waste is generally a rich iron source (> 70% Fe) and consists of three distinct layers of iron oxides; namely wuistite (FeO), magnetite (Fe3O4) and hematite (Fe2O3). During the milling process in this work, the factory waste was grinded into ultra-fine particles and in the form of single-phase-particle. Using magnetic separation, we obtained defective FeO from the factory waste. This defective FeO was further oxidized into useful Fe2O3. The following chemical equation illustrates the process. 4 FeO For sample characterization, a chromameter (Model: Minolta CR-10) was used to study the color property of the waste-derived hematite. The L*, a*, b*values were read by the chromameter and recorded. The microstructure of the sintered samples was analyzed by using a Scanning Electron Microscope (Model: Philips LEO-VSEM). Finally, B-H tracer (Model: Linkjoin MATS-2010S) was employed to analyze the magnetic properties of the samples. Magnetic properties such as permeability, saturation magnetization and coercivity were obtained. O2 2 Fe 2 O 3 Figure 3 shows the raw waste material and the treated waste-derived hematite. The color change is obvious. It changes from light blue to red. The color property was analyzed by a chromameter (Model: Minolta CR-10) and the results is shown in Table 1. After several treatments, the value of a* improved from 1.3 to as high as 9.5. This value is an indication of the reddishness of the samples. Pure hematite always possesses high a* value. Also, the value of b* shows the blue property but it is not our concern in this study. We can conclude that high purity hematite was obtained and the treatments were successful. H. S. Woon, K. P. Lim, C. K. Ho, C. L. Cheah and N. Riza / IJECCT 2011, Vol. 1 (2) Figure 3. Cold-rolling Waste (Up) and Waste-derived Hematite (Down) Table 1. Color Property of Cold-rolling Waste and Waste-derived Hematite Color Property L* a* b* Coldrolling Waste 36.2 1.3 -1.6 Wastederived Hematite 38.9 9.5 3.1 Figure 4 reveals the magnetic properties of the wastederived NiZn ferrite compared to an industrial grade NiZn ferrite. The hysteresis graph shows the magnetic induction of the samples to the external field provided. 3 Figure 4. Hysteresis-graph of Waste-derived NiZn Ferrite (Up) and Industrial Grade NiZn Ferrite (Down) Permeability is an important information to show the ability of the sample to acquire high magnetization in relatively weak magnetic fields. Both the samples possess high permeability (μ) that is 7.731 mH/m and 7.882 mH/m respectively. These high permeability can be explained by the fact that atomic magnetic moments are randomly oriented on the inter-atomic scale and the field gradually aligns them as in the case of paramagnets. Saturation magnetization or saturation remanence of the samples is 2246 Gauss and 2328 Gauss respectively which are high enough to be used as EMI suppressor. Saturation magnetization is the highest magnetic induction possessed by the samples when high external field is supplied. However the coercivity (Hc) of the waste-derived samples that is 0.1024 Oe is considered slightly too high to be categorized as a high-end product. This is because high coercivity may cause high lost in the signal transmission system. Eddy current generated may lead to heat agitation and signal quality will be distorted. The target value for coercivity is usually 0.06 Oe or lower. H. S. Woon, K. P. Lim, C. K. Ho, C. L. Cheah and N. Riza / IJECCT 2011, Vol. 1 (2) 4 from the impurities content, which resided at the grain boundaries. IV. CONCLUSIONS The purifying process which includes milling, magnetic separation and heat treatment is proven successful to convert the cold-rolling waste material into useful hematite. The waste-derived hematite performs the color with high a* value and thus it is an acid test for the presence of hematite. The magnetic properties such as magnetic permeability and saturation magnetization are high and meet the requirement for the sample to be used as EMI suppressor. The only drawback seems to be the high coercivity possessed by the waste-derive NiZn ferrite. The high coercivity may lead to high lost and may eventually have adverse effect to the signal quality. REFERENCES [1] [2] Figure 5. Microstructure of Waste-derived NiZn Ferrite (Up) and Industrial Grade NiZn Ferrite (Down) Figure 5 unveiled the microstructure of the waste-derived NiZn ferrite and the industrial grade NiZn ferrite. From our observation of all the SEM micrographs, the higher impurity in the waste-derived NiZn ferrite sample is detrimental to the reaction between the grains after sintering. This is due to the formation of secondary phases [3] [4] [5] D. Jiles, “ Introduction To Magnetism and Magnetic Material”, Chapman & Hall. pp: 229-323. 1991. H.S.Woon, M.Hashim, N.Yahya, A.Zakaria and K.P.Lim, “The Purification and Conversion of Mill Scale Into Useful Hematite”, Journal of Solid State Science and Technology Letters.Vol 12, No 1 & 2 298-303. 2005. A.Goldman, “Modern Ferrite Technology 2nd Edition”, Springer. pp: 30-41 . 2006. H.S. Woon, K.P.Lim, Puteri.N, Rozaimah.R, and C.Y.Tan, “Synthesis and Characterization of Hot-roll and Cold-roll Byproduct-derived Strontium Hard Ferrites”, American Journal of Engineering and Applied Sciences, 2(4):580-583. 2009. Konica Minolta, “Precise Color Communication”, Unpublished. pp.11-20.2008.
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