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Magnetic Properties and Mechanical Strength of MnZn Ferrite

Y. Matsuo, K. Ono, T. Hashimoto, and F. Nakao

Abstract-- From MnZn ferrite ("6H20" of FDK production), cores having grain size of about 8¡Á10 ¦Ìm were produced by controlling the calcination temperature, after-calcination milling time, and sintering conditions. The ferrite powder production conditions and core microstructure were examined to determine their effects on the magnetic properties and mechanical strength of MnZn ferrite cores. A tendency of core loss to decline with a decrease in grain size was confirmed. Strength increased also with a decrease in grain size. Thus, a relation similar to that between strength and fracture toughness in the Equation of Griffith-Irwin was noted. By these findings, it has become possible to produce MnZn ferrite cores with lower loss and greater strength.

Index Terms-- MnZn ferrite, sintering conditions, magnetic properties, mechanical strength.

I. INTRODUCTION

THE use of MnZn ferrite is spreading from switching power supplies to inductive charging systems for electric vehicles and automated guided vehicles. These inductive charging systems incorporate a connector whose contact transformer has its primary and secondary sides divided in the middle[1]-[3]. The circuit composition of the inductive charging systems adopts a high-frequency switching method of 100 to 370 kHz[4]. Inductive charging systems require lower loss cores for minimizing heat generation during battery charging[1]. They also require cores with a high saturation magnetic flux density to match large current inputs. Moreover, they require cores with greater mechanical strength since electric vehicles are often driven on rough unpaved roads. For these reasons, MnZn ferrite ("6H20" of FDK make) production conditions and core microstructure were examined to determine their effects on the magnetic properties and strength values of MnZn ferrite cores.
II. SAMPLE PREPARATION AND MEASUREMENT

The samples used in this experiment were prepared by the conventional powder metallurgical processes summarized in Fig. 1. ZnO, MnO and Fe2O3 were weighed to the basic formula, and were wet-mixed in a ball mill. Three groups of the mixture, after drying, were calcined at 800¡î, 900¡î and 1000¡î, respectively, in the atmosphere. Then, they were wet-milled in a ball mill under the conditions shown in Table. 1. The resultant ferrite powder, following the addition of PVA, was granulated. The resultant granules were pressed of PVA, was granulated. The resultant granules were pressed into bar and toroidal shapes. Then the bars and toroids were sintered at peak temperatures between 1250 to 1310¡î in an oxygen concentration controlled atmosphere. The sintered samples had the shapes and dimensions shown in Fig. 2. The maximum fracture load of bars was measured under the conditions shown in Fig. 3. Their 3-point bending strength values were calculated, by using Equation (1)/ Fig. 3, from the numerical values of their dimensions, maximum fracture load, and distances between supports. The core loss of toroids (sized 25 mm in outer diameter, 15 mm in inner diameter, 5 mm in thickness) was measured with a B-H analyzer SY-8232 of Iwatsu make at ambient temperatures raised from room temperature to 120¡î. The microstructure of toroidal cores was observed by SEM micrography, and their density by the Archimedean method. Samples of calcinated powder were set aside for measurement. The crystalline phase of this calcinated powder was observed by the powder X-ray diffraction method using Multiflex¡¿XRD (Cu K¦Á, 40 kV, 30 mA) of Rigaku make. For thermal shrinkage measurement, calcinated powder was pressed into ¦Õ4¡ß4 mm shapes of uniform density, and their shrinkages were measured with TMA-8310 equipment of Rigaku make as the applied temperature was raised from 600 to 1400¡î at a rate of 10¡î/min.
Fig. 1
Table 1
Fig. 2
Fig. 3

III. RESULTS AND DISCUSSION

3.1 Properties of Calcinated Powders
At the beginning of the sample preparation process, the weighed raw materials were wet-mixed before calcination. A part of this mixed powder was taken as samples for the examination of their X-ray diffraction patterns at measured temperatures between 25¡î and 1200¡î. It was found that, as the temperature was raised, the peaks of Fe2O3 and ZnO diminished while the spinel phase peaks became more prominent as shown in Fig. 4. At temperatures above 1000¡î, the spinel phase peaks were extremely predominant. The remainder of the above mixed powder was divided into three groups and were calcinated at 800¡î, 900¡î and 1000¡î, respectively. Then, the calcinated powder of each group was milled in a ball mill for 3, 5 and 7 hours, respectively. This milled powder was examined and found to have the relation between its particle size and milling time as shown in Fig. 5. At all the milling periods, the particle size increased with a rise in calcination temperature. This was attributed to the increase of spinel phase by a rise in calcination temperature, as shown in Fig. 4.

Fig. 4
Fig. 5
In other words, because spinel phase causes particles to melt together, it becomes more difficult to mill calcinated powder into small particles. Fig. 6 presents the TMA curves of powder samples calcinated at various temperatures. The temperature at which shrinkage starts was found to go up with an increase in calcination temperature. The amount of shrinkage increased with a drop in calcination temperature. This was attributed to a decrease in particle as shown in Fig. 5. Smaller particle size means a greater number of contact points among the particles so that spinel phase formation is promoted thus resulting in greater shrinkage. Milled powder, after calcinating, was granulated and then pressed into toroidal shapes which were sintered at a peak temperature between 1250¡î and 1310¡î. The grain size of these sintered cores was measured to be between 8¦Ìm and 11¦Ìm as shown in Fig. 7. The relation between their density and grain size is presented in Fig. 8. The density ranged 4.82 ¡Þ 0.04 g/cm3 and indicated a tendency to increase with an increase in grain size.
Fig. 6
Fig. 7
Fig. 8
3.2 Magnetic Properties
Fig. 9 shows the core loss values obtained from sintered toroids in relation to their grain size and calcination temperature. Core loss tended to go up with an increase in grain size. At this measurement frequency level, hysteresis loss (Phv) and eddy current loss (Pev) were dominant; therefore, both of these losses had to be reduced in order to lower the core loss. Fig. 10 gives the results of loss separation in toroidal cores calcinated at 900¡î. Both hysteresis and eddy current losses declined as grain size became smaller, with the former leveling off while the latter indicating a possibility of further decline. This was attributed to an increase in alternating current resistance as smaller grain size works to suppress eddy current. Fig. 11 shows the relation between the core loss and measuring temperature of sintered toroids which calcination temperature was 900¡î. It was found that the core loss (100 kHz, 200 mT, 80¡î) could be reduced by about 30% if grain size was made smaller.
Fig. 9 / Fig.10
Fig.11
3.3 Mechanical Strength
Fig. 12 shows the relation between the 3-point bending strength and grain size of bar cores. The strength tended to decline with an increase in grain size, thus indicating a relation given by the Equation of Griffith-Irwin (Fig. 13). High strength values were obtained from cores (calcinated at 900¡î) having a grain size of about 8 and 9 ¦Ìm. Fig. 14 presents the SEM photographs of fractured surfaces of bar cores calcinated at 900¡î.
Fig.12
The photographs indicate that high strength cores (b) and (c), as compared to low strength cores (a), had smaller grain size and fewer pores. As indicated by the Equation of Griffith-Irwin, porosity is one essential factor for sharply reducing core strength. To obtain strong cores, therefore, it is important to select the production conditions which will minimize pores, crack, defect.

Fig.13
Photo
IV. CONCLUSIONS

By regulating the calcination temperature, milling time and sintering temperature, we produced MnZn ferrite core samples having grain size of around 8 to 10 ¦Ìm. Then, relation between core loss, 3-point bending strength, and milling time was investigated. The conclusions were:
1. The core loss was reduced by 30% under the conditions of longer after-calcination milling time and smaller grain size.
2. The bending strength was confirmed to increase under the condition of small grain size. As a result, strength behavior similar to the one expressed by the Equation of Griffith-Irwin was noted.
3. The lowest core loss and highest strength were obtained under the conditions of 900¡î calcination, 1280¡î sintering, and 9 ¦Ìm grain size. On the basis of the above findings, we plan to develop MnZn ferrite cores of even lower loss and higher strength for use in the inductive charging systems for electric vehicles and automated guided vehicles.

REFERENCES
[1] Y. Matsuo, S. Otobe, F. Nakao, H. Sakamoto, "Development of a Ferrite Material for Inductive Chargers" , EVS-16 (16th International Electric Vehicle Symposium), Beijing, 1999.
[2] H. Sakamoto, K. Harada, S. Washimiya, K. Takehara, Y. Matsuo and F.Nakao, "Large air gap coupler for inductive charger" , IEEE Trans Magn.,vol. 35, no.5, pp.3526-3528, 1999
[3] Y. Matsuo, K.Ono, M.Kondoh, Y. Matsuo, "Die mechanisms affection the forming of super-large ferrite cores, FP-06, Digests of the 2000 Intermag-Conrerence (Toronto).
[4] D. Ouwerkerk, T. Sekimori, H. Satoh, "New Inductive Charging Approach" , JEVA Electric Vehicle Forum, pp.181-187, 1998.

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