WO2009101999A1 - 焼結フェライト材料及び焼結フェライト材料の製造方法 - Google Patents
焼結フェライト材料及び焼結フェライト材料の製造方法 Download PDFInfo
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- WO2009101999A1 WO2009101999A1 PCT/JP2009/052365 JP2009052365W WO2009101999A1 WO 2009101999 A1 WO2009101999 A1 WO 2009101999A1 JP 2009052365 W JP2009052365 W JP 2009052365W WO 2009101999 A1 WO2009101999 A1 WO 2009101999A1
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Definitions
- the present invention relates to a sintered ferrite material used for a core material of a winding component, such as an inductor used for a power circuit or the like, an antenna such as a bar antenna, a transformer, etc., and particularly has a high initial permeability, a high saturation magnetic flux density, and a high
- the present invention relates to a sintered ferrite material satisfying a specific resistance and a method for producing the same.
- ferrite materials used as a core material for winding parts such as inductors, bar antennas, and transformers used for power circuits of DC-DC converters, etc. are used to ensure electrical insulation from the conductor.
- ferrite materials used as a core material for winding parts such as inductors, bar antennas, and transformers used for power circuits of DC-DC converters, etc.
- a Ni-based ferrite material having a high specific resistance has been used.
- Ni-based ferrite materials have high Ni as the main component and a large magnetostriction constant. Therefore, in resin-molded winding parts, when the resin is cured, the soft magnetic characteristics change depending on the stress applied to the core. There was a problem.
- Li-based ferrite materials are known as materials that do not contain expensive Ni. Since the Li-based ferrite material has a small magnetostriction constant, it has a feature that the rate of change in soft magnetic characteristics is small even when used for a resin mold type winding component.
- a high initial magnetic permeability for example, 200 or more
- a high specific resistance for example, 10 6
- the composition formula is (1-x) Li 2 O. (5-2 ⁇ -x) Fe 2 O 3 .4xZnO.4yMnO.4 ⁇ Bi 2 O 3 0 ⁇ ⁇ ⁇ 0.35, 0 ⁇ x ⁇ 0.45, 0 ⁇ y ⁇ 0.2, 0 ⁇ ⁇ ⁇ 0.005, and at least two of x, y, and ⁇ are simultaneously.
- a Li-based ferrite material for non-reciprocal circuit elements having a composition where ⁇ is not zero and ⁇ is not zero when y is zero (Patent Document 1).
- the Li-based ferrite material according to Patent Document 1 improves characteristics such as temperature characteristics and loss characteristics by simultaneously containing at least two of Zn, Mn, and Bi, and further performs repeated heat treatment in oxygen and nitrogen.
- characteristics such as temperature characteristics and loss characteristics by simultaneously containing at least two of Zn, Mn, and Bi, and further performs repeated heat treatment in oxygen and nitrogen.
- the specific resistance is improved by performing heat treatment at least once in nitrogen and finally in oxygen.
- the Li-based ferrite material according to Patent Document 1 has a saturation magnetic flux density of 4000 G (400 mT) or more, but has a low specific resistance of about 10 7 ⁇ cm (10 5 ⁇ m). In order to improve the specific resistance, it is necessary to repeatedly perform heat treatment in oxygen and nitrogen, but there is a problem that the manufacturing cycle becomes longer and the manufacturing cost increases.
- Li-based ferrite materials have a feature of a large squareness ratio, they have been studied for use in memory core materials and the like, but there is a problem that the saturation magnetic flux density is smaller than that of Ni-based ferrite materials. Therefore, it is necessary to improve the saturation magnetic flux density for use in applications such as inductors and antennas that require good DC superposition characteristics.
- the present invention is a series winding type that does not require a bobbin that requires a high specific resistance, a gap type that is used under a DC bias magnetic field that requires high initial permeability and saturation magnetic flux density, and high stress resistance. It satisfies all of high initial permeability, high saturation magnetic flux density, and high specific resistance, which is optimal as a core material for various types of inductor parts such as resin mold types, antennas, transformers, etc.
- An object of the present invention is to provide an inexpensive Li-based sintered ferrite material having a high saturation magnetic flux density even at a relatively high temperature.
- the present inventors have a composition region that can satisfy all of high initial magnetic permeability, high saturation magnetic flux density, and high specific resistance.
- the present inventors have confirmed that a Li-based ferrite material having excellent characteristics can be provided at low cost without performing a complicated heat treatment, and the present invention has been completed.
- the sintered ferrite material of the present invention has the composition formula (1-xyz) (Li 0.5 Fe 0.5 ) O.xZnO.yFe 2 O 3 .zCuO, where x, y, z are 100% by mass of a material satisfying 0.14 ⁇ x ⁇ 0.19, 0.48 ⁇ y ⁇ 0.5, and 0 ⁇ z ⁇ 0.03, and Bi 2 O 3 is 0.5% by mass or more 3
- the initial magnetic permeability is 200 or more
- the saturation magnetic flux density is 430 mT or more at 23 ° C., 380 mT or more at 100 ° C.
- a specific resistance of 10 6 ⁇ m or more is a specific resistance of 10 6 ⁇ m or more.
- the present invention is characterized in that, in the sintered ferrite material having the above configuration, the average crystal grain size is 7.5 ⁇ m or more and 25 ⁇ m or less.
- the present invention is characterized in that, in the sintered ferrite material having the above-described configuration, the rate of change of the initial magnetic permeability when pressed at a pressure of 30 MPa is within ⁇ 5%.
- the present invention is characterized in that in the sintered ferrite material having the above-described configuration, the number of grain boundary pores per 100 crystal grains is 20 or more.
- the present invention is characterized in that, in the sintered ferrite material having the above-described configuration, the rate of change of the initial magnetic permeability when pressed at a pressure of 30 MPa is within ⁇ 3%.
- the present invention is characterized by a winding component using a sintered ferrite material having the above-described configuration.
- the method for producing the sintered ferrite material of the present invention is represented by the composition formula (1-xyz) (Li 0.5 Fe 0.5 ) O.xZnO.yFe 2 O 3 .zCuO, and x, y, a step of preparing a raw material powder satisfying z satisfying 0.14 ⁇ x ⁇ 0.19, 0.48 ⁇ y ⁇ 0.5, and 0 ⁇ z ⁇ 0.03; A step of obtaining a calcined powder, a step of obtaining a second calcined powder by adding 0.5% by mass to 3% by mass of Bi 2 O 3 by setting the first calcined powder to 100% by mass, (2) It is characterized by having a step of pulverizing calcined powder to obtain pulverized powder, a step of forming pulverized powder to obtain a molded body, and a step of firing the molded body to obtain a sintered ferrite material.
- the method for producing the sintered ferrite material of the present invention is represented by the composition formula (1-xyz) (Li 0.5 Fe 0.5 ) O.xZnO.yFe 2 O 3 .zCuO, and x, y,
- the material satisfying z satisfying 0.14 ⁇ x ⁇ 0.19, 0.48 ⁇ y ⁇ 0.5, 0 ⁇ z ⁇ 0.03 is defined as 100% by mass, and Bi 2 O 3 is further included in 0.5% by mass.
- a step of preparing a raw material powder obtained by adding at least 3% by mass or less, a step of calcining the raw material powder to obtain a calcined powder, a step of crushing the calcined powder to obtain a pulverized powder, and a pulverized powder It has the process of shape
- the present invention is characterized in that the calcining temperature when calcining the raw material powder is 800 ° C. to 1200 ° C., preferably 1000 ° C. to 1200 ° C., in the method for producing a sintered ferrite material having the above steps.
- a sintered ferrite material satisfying an initial permeability of 200 or more, a saturation magnetic flux density of 430 mT or more at 23 ° C., 380 mT or more at 100 ° C., and a specific resistance of 10 6 ⁇ m or more can be obtained.
- the sintered ferrite material according to the present invention is directly wound around the core by using it as a core material of an inductor used for a power circuit of a DC-DC converter, an antenna such as a bar antenna, and a winding component such as a transformer. This makes it possible to reduce the manufacturing cost of the winding component and further reduce the size.
- the sintered ferrite material according to the present invention has a high saturation magnetic flux density even at a high temperature, it can be used as an inductor or antenna core material to provide an inexpensive inductor or antenna excellent in DC superposition characteristics.
- the rate of change in magnetic permeability with respect to external stress is small, so that a winding component with reduced variation in soft magnetic characteristics is provided. Can do.
- a Li-based sintered ferrite material that satisfies the above characteristics can be provided at a low cost.
- the calcining temperature is set to 800 ° C. to 1200 ° C., preferably 1000 ° C. to 1200 ° C., the change rate of the initial permeability of the sintered ferrite material to be manufactured can be reduced.
- FIG. 2 is a chart showing a composition and characteristics of a sintered ferrite material in Example 1.
- FIG. It is a graph which shows the relationship between the amount of ZnO in a sintered ferrite material, and initial permeability. It is a graph which shows the relationship between the amount of ZnO in a sintered ferrite material, and the saturation magnetic flux density in 23 degreeC. It is a graph which shows the relationship between the amount of ZnO in a sintered ferrite material, and the saturation magnetic flux density in 100 degreeC. It is a graph which shows the relationship between the amount of ZnO in a sintered ferrite material, and a specific resistance.
- 6 is a chart showing a composition and characteristics of a sintered ferrite material in Example 2.
- 10 is a chart showing the composition and characteristics of a sintered ferrite material in Example 5. It is a figure which shows the structure
- FIG. 10 is a chart showing characteristics of sintered ferrite material in Example 8. It is a graph which shows the relationship between the number of grain boundary pores per 100 crystal grains in sintered ferrite material, and the rate of change of initial permeability. It is a figure which shows the SEM photograph of the ground powder in this invention. It is a figure which shows the SEM photograph of the ground powder in this invention. It is a figure which shows the SEM photograph of the ground powder in this invention. It is a figure which shows the structure
- the sintered ferrite material of the present invention has the composition formula (1-xyz) (Li 0.5 Fe 0.5 ) O.xZnO.yFe 2 O 3 .zCuO, where x, y, z are 100% by mass of a material satisfying 0.14 ⁇ x ⁇ 0.19, 0.48 ⁇ y ⁇ 0.5, and 0 ⁇ z ⁇ 0.03, and Bi 2 O 3 is 0.5% by mass or more 3 It is characterized by being added by mass% or less.
- the composition formula is (1-x) Li 2 O. (5-2 ⁇ -x) Fe 2 O 3 ⁇ 4xZnO ⁇ 4yMnO ⁇ 4 ⁇ Bi 2 O 3 and 0 ⁇ ⁇ ⁇ 0.35, 0 ⁇ x ⁇ 0.45, 0 ⁇ y ⁇ 0.2, 0 ⁇ ⁇ ⁇ 0.005 are satisfied, and at least two of x, y, and ⁇ are not simultaneously zero, and A Li-based ferrite material having a composition in which ⁇ is not zero when y is zero is described.
- Patent Document 1 “at least two of x, y and ⁇ are not simultaneously zero”, so Mn and Zn, Zn and Bi, Mn and Bi, or Mn, Zn and Bi must be contained at the same time.
- Mn and Zn, Zn and Bi, Mn and Bi, or Mn, Zn and Bi must be contained at the same time.
- almost all the examples of Patent Document 1 contain Mn.
- sample number MLF-37 in Table 3 does not contain Mn.
- but y 0, that is, if Mn is not included, the DC resistance becomes extremely small and is not suitable for practical use as a microwave circuit”.
- Fe 2 O 3 0.5
- (Li 0.5 Fe 0.5 ) O 0.3
- ZnO 0.2. It becomes.
- the sintered ferrite material according to the present invention does not contain MnO (except when it is mixed as an inevitable impurity). Further, the upper limit of ZnO is 0.19, and the upper limit of Fe 2 O 3 is less than 0.5 (not including 0.5). Furthermore, as shown in the Example mentioned later, although MnO is not contained in this invention, the high specific resistance of 10 ⁇ 6 > (omega
- the composition of the sintered ferrite material according to the present invention is an intensive study on the composition of the Li-based ferrite material that can satisfy all of high initial permeability, high saturation magnetic flux density, and high specific resistance in view of the conventional Li-based ferrite material. As a result, it was found.
- x is the content of ZnO, and is preferably in the range of 0.14 to 0.19 (0.14 or more and 0.19 or less, meaning of the same applies hereinafter). If it is less than 0.14, the initial permeability becomes smaller and less than 200, and if it exceeds 0.19, the saturation magnetic flux density becomes smaller and becomes less than 430 mT at 23 ° C. and less than 380 mT at 100 ° C., which is not preferable. A more preferable range is 0.16 to 0.17, and characteristics with an initial permeability of 250 or more, a saturation magnetic flux density of 440 mT or more at 23 ° C., 400 mT or more at 100 ° C., and a specific resistance of 10 6 ⁇ m or more are obtained.
- y is the content corresponding to Fe 2 O 3 and excludes Fe in (Li 0.5 Fe 0.5 ) O, preferably in the range of 0.48 or more and less than 0.5, and has an initial permeability of 200
- the saturation magnetic flux density can satisfy 430 mT or more at 23 ° C., 380 mT or more at 100 ° C., and a specific resistance of 10 6 ⁇ m or more.
- the saturation magnetic flux density becomes small, and is less than 430 mT at 23 ° C. and 380 mT at 100 ° C., and more than 0.5 is not preferable because the specific resistance is less than 10 6 ⁇ m.
- y when y is 0.5 or more, the specific resistance rapidly decreases. Accordingly, y is preferably less than 0.5 in order to obtain a stable specific resistance.
- a more preferable range is 0.485 to 0.495, and characteristics such as an initial permeability of 250 or more, a saturation magnetic flux density of 440 mT or more at 23 ° C., 400 mT or more at 100 ° C., and a specific resistance of 10 6 ⁇ m or more are obtained. It is optimal as an inductor or antenna material that requires direct current superposition characteristics. Note that (Li 0.5 Fe 0.5 ) O is the remainder of x, y described above and z described later.
- z is the content of CuO, and when added, it is preferably 0.03 or less.
- excellent properties can be obtained without addition of CuO, but the specific resistance can be further improved by addition of CuO.
- CuO replaces a part of (Li 0.5 Fe 0.5 ) O, and has high characteristics even when the amount of Bi 2 O 3 to be described later is reduced by addition of CuO.
- the sintered ferrite can be provided at low cost by reducing the amount of Bi 2 O 3 .
- z exceeds 0.03, the saturation magnetic flux density decreases, and it is not preferable because it is less than 430 mT at 23 ° C. and 380 mT at 100 ° C. A more preferable range is 0.02 or less.
- the material having the above composition is set to 100% by mass, and Bi 2 O 3 is further added in an amount of 0.5% to 3% by mass.
- Bi 2 O 3 is preferably added after the calcination step and before the sintering step in the production method described later.
- the sintered ferrite material according to the present invention can tolerate inevitable impurities.
- MnO is not an essential element of the sintered ferrite material according to the present invention, but may be used as long as it is mixed as an impurity.
- the sintered ferrite material according to the present invention can be obtained by the following manufacturing method.
- the composition formula is (1-xyz) (Li 0.5 Fe 0.5 ) O.xZnO.yFe 2 O 3 .zCuO, and x, y, and z are 0.14 ⁇ x ⁇ 0. .19, 0.48 ⁇ y ⁇ 0.5, 0 ⁇ z ⁇ 0.03 is taken as 100% by mass, and Bi 2 O 3 is added in an amount of 0.5% by mass to 3% by mass.
- the step of preparing the material may be performed by the firing step described later. That is, the above materials may be prepared in each process from weighing, mixing, calcination, pulverization, and molding. For example, carbonate powders and oxide powders as starting materials for all elements may be weighed and mixed from the beginning and calcined, or only other raw material powders excluding raw material powders such as Bi and Li may be used first. After calcination by weighing and mixing, raw powders such as Bi and Li may be mixed with the calcination powder, and then pulverized and molded. Or you may bake, after mixing with the grind
- the calcination temperature is preferably 800 ° C to 1200 ° C. A more preferred range is 1000 ° C to 1200 ° C.
- the mixed raw material powder is heated, and a ferrite phase is formed by a solid phase reaction (ferritization reaction).
- the calcining time is preferably 2 to 5 hours.
- the calcination atmosphere is preferably in the air or in oxygen.
- the sintered ferrite material of the present invention has excellent initial magnetic permeability, saturation magnetic flux density, and specific resistance, and is characterized by a small change rate of initial magnetic permeability with respect to external stress.
- a sintered ferrite material having an above-described composition range calcining performed at 800 ° C. to 1200 ° C., and passing through the steps described below, a change rate of initial permeability within ⁇ 5% when pressed at a pressure of 30 MPa. Although it can be obtained, by calcining at a relatively high temperature of 1000 ° C. to 1200 ° C., the rate of change of the initial permeability relative to external stress can be further reduced, and the change in the initial permeability when pressurized at 30 MPa. A sintered ferrite material having a rate within ⁇ 3% can be obtained.
- the number of pores formed at the grain boundary can be increased, and the external stress can be relaxed by increasing the grain boundary pores.
- the rate of change of can be further reduced.
- the pulverization is preferably performed in pure water or ethanol.
- the average particle size of the pulverized powder after pulverization is preferably 0.5 ⁇ m to 2.0 ⁇ m.
- the pulverized powder after pulverization is molded by a desired molding means. Prior to molding, the pulverized powder may be granulated by a granulator as necessary.
- the molding pressure is preferably 70 MPa to 150 MPa.
- the sintered body obtained above is fired to obtain a sintered ferrite material.
- the firing temperature is preferably 1000 ° C to 1150 ° C. If it is less than 1000 ° C., the initial magnetic permeability is small, and if it exceeds 1150 ° C., Bi in the molded body may be volatilized and the inside of the furnace may be contaminated. A more preferable range is 1050 ° C. to 1100 ° C.
- the firing atmosphere is preferably in the air or an oxygen atmosphere, and the firing time is preferably 2 to 5 hours.
- the sintered ferrite material according to the present invention can improve the initial magnetic permeability and the saturation magnetic flux density without reducing the specific resistance by adjusting the average grain size after firing to 7.5 ⁇ m or more and 25 ⁇ m or less. .
- the average crystal grain size in order to obtain a high specific resistance, it has been considered preferable to reduce the average crystal grain size and increase the grain boundary resistance.
- the sintered ferrite material according to the present invention it has been found that when the average crystal grain size is made larger than that of the conventional material, the initial permeability and the saturation magnetic flux density can be improved without reducing the specific resistance. This is considered to be caused by the composition range of the sintered ferrite material according to the present invention, and is an effect unique to the present invention.
- the average crystal grain size is preferably 7.5 ⁇ m or more because an effect of improving the initial magnetic permeability and saturation magnetic flux density can be obtained. If it exceeds 25 ⁇ m, the specific resistance decreases, which is not preferable.
- the average crystal grain size can be adjusted by the calcination temperature / time, the pulverized grain size, and the firing temperature / time described above.
- Example 1 This example demonstrates the reason for limiting the composition of x (ZnO).
- the granulated powder has a ring shape of outer diameter 9 mm ⁇ inner diameter 4 mm ⁇ thickness 3 mm, 30 mm ⁇ 20 mm ⁇ thickness 5 mm. And a frame shape of outer frame 9.5 mm ⁇ inner frame 4.7 mm ⁇ thickness 2.4 mm molded at a molding pressure of 150 MPa, and the resulting molded body was fired at 1050 ° C. in the atmosphere for 3 hours, A sintered ferrite material was obtained.
- the obtained frame-shaped sintered ferrite material was wound, and the initial permeability was measured with the same LCR meter as described above. Further, uniaxial pressure was applied at 30 MPa, and the rate of change in initial permeability before and after the pressurization was obtained. The measurement results are shown in FIG.
- FIG. 1 those marked with an asterisk (*) beside the sample number are comparative examples (the meaning of * is the same hereinafter).
- 1 to 5 are graphs showing the results of FIG. In each case, the horizontal axis represents the amount of ZnO, FIG. 2 is a graph showing changes in initial permeability ( ⁇ i), FIG. 3 is a graph showing changes in saturation magnetic flux density (Bs) at 23 ° C., and FIG. 4 is saturation at 100 ° C.
- FIG. 5 is a graph showing a change in specific resistance ( ⁇ ), and a graph showing a change in magnetic flux density (Bs).
- the initial permeability is 200 or more
- the saturation magnetic flux density is 430 mT or more at 23 ° C.
- 380 mT or more at 100 ° C. It can be seen that high characteristics with a resistance of 10 6 ⁇ m or more are obtained.
- the sintered ferrite material of the present invention has a small change in initial permeability due to stress.
- Example 2 This example demonstrates the reason for limiting the composition of y (Fe 2 O 3 ).
- FIG. 7 to FIG. 10 are graphs showing the results of FIG. In each case, the horizontal axis represents the amount of Fe 2 O 3 , FIG. 7 is a graph showing the change in initial permeability, FIG. 8 is a graph showing the change in saturation magnetic flux density at 23 ° C., and FIG. 9 is the saturation magnetic flux density at 100 ° C.
- FIG. 10 is a graph showing a change in specific resistance.
- the Fe 2 O 3 content is in the range of 0.48 to less than 0.5
- the initial permeability is 200 or more
- the saturation magnetic flux density is 430 mT or more at 23 ° C., and 100 ° C. It can be seen that high characteristics of 380 mT or more and a specific resistance of 10 6 ⁇ m or more are obtained.
- the sintered ferrite material of the present invention has a small change in initial permeability due to stress.
- Example 3 This example demonstrates the reason for limiting the composition of z (CuO).
- FIG. 11 graphs of the results of FIG. 11 are shown in FIGS.
- the horizontal axis represents the amount of CuO
- FIG. 12 is a graph showing changes in initial permeability
- FIG. 13 is a graph showing changes in saturation magnetic flux density at 23 ° C.
- FIG. 14 shows changes in saturation magnetic flux density at 100 ° C.
- a graph and FIG. 15 are graphs showing changes in specific resistance.
- the CuO content is 0.03 or less
- the initial permeability is 200 or more
- the saturation magnetic flux density is 430 mT or more at 23 ° C., 380 mT or more at 100 ° C.
- the specific resistance is 10 6 ⁇ m or more. It can be seen that high characteristics are obtained.
- the specific resistance is improved by the addition of CuO.
- the sintered ferrite material of the present invention has a small change in initial permeability due to stress.
- Example 4 This example demonstrates the reason for limiting the amount of Bi 2 O 3 added.
- FIG. 17 to FIG. 20 are graphs showing the results of FIG.
- the horizontal axis represents the amount of Bi 2 O 3
- FIG. 17 is a graph showing the change in initial permeability
- FIG. 18 is a graph showing the change in saturation magnetic flux density at 23 ° C.
- FIG. 19 is the saturation magnetic flux density at 100 ° C.
- FIG. 20 is a graph showing a change in specific resistance.
- the initial permeability is 200 or more
- the saturation magnetic flux density is 430 mT or more at 23 ° C., 100 It can be seen that high characteristics of 380 mT or more and specific resistance of 10 6 ⁇ m or more are obtained at ° C.
- the sintered ferrite material of the present invention has a small change in initial permeability due to stress.
- Example 5 This example demonstrates the reason for limiting the average grain size of sintered ferrite materials.
- the final composition shown in FIG. 21 is used, and the calcination temperature is 800 ° C. (sample number 28), 835 ° C. (sample number 29), 900 ° C. (sample number 30), 1000 ° C. (sample number 31), 1100
- the experiment was performed in the same manner as in Example 1 except that the temperature was within the range of ° C (sample number 32). However, only the sample number 28 set the firing temperature to 930 ° C. The result is shown in FIG. Moreover, the structure
- Example 6 This example demonstrates an application example when a sintered ferrite material is applied to an inductor.
- FIG. 24 shows a sintered ferrite material (sample numbers 33 and 34) having a saturation magnetic flux density of 380 mT or more at 100 ° C. and a sintered ferrite material (sample number 35, saturated magnetic flux density at 100 ° C. of less than 380 mT). 36) was used to produce the inductor drum core shown in FIG.
- L1 ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ is an inductance at the time of DC superposition
- ⁇ L is L1 ⁇ L0 ⁇
- the sintered ferrite material according to the present invention has an excellent saturation magnetic flux density of 380 mT or more at 100 ° C., so that the current value at which 10% L decreases is as high as 0.5 A or more, and direct current It can be seen that the superimposition characteristics are excellent. Therefore, by using it for winding components such as an inductor, an inexpensive inductor excellent in DC superposition characteristics can be provided.
- Example 7 This example demonstrates an application example when a sintered ferrite material is applied to an antenna.
- FIG. 26 shows a sintered ferrite material (sample numbers 37 and 38) having a saturation magnetic flux density at 100 ° C. of 380 mT or more and a sintered ferrite material having a saturation magnetic flux density at 100 ° C. of less than 380 mT (sample numbers 39, 38).
- a prismatic core for a 50 mm ⁇ 4 mm ⁇ 4 mm antenna shown in FIG. 27 was produced, and a coated copper wire of ⁇ 0.29 mm was wound around this core for 70 turns.
- the obtained winding component was measured for DC superposition characteristics at 100 ° C. under measurement conditions of 100 kHz and 0.1 V with an LCR meter (device name: 4285A, manufactured by HEWLETT PACKARD).
- L1 is an inductance at the time of DC superposition
- ⁇ L is L1 ⁇ L0
- the sintered ferrite material according to the present invention has an excellent saturation magnetic flux density of 380 mT or more at 100 ° C., so that the current value at which 10% L decreases is as high as 1.0 A or more, and direct current It has excellent superposition characteristics, and the L temperature change during actual operation is 1.0% or less, and since the L temperature change is extremely small even under high current, it can be seen that it is suitable for winding parts such as antennas. .
- Example 8 Carbonate powder and oxide powder as starting materials are weighed and mixed so as to have the composition shown in sample number 4 in FIG. 1, and calcined at 800 ° C. (sample number 41) and 900 ° C. (sample number) in the air. 42), 950 ° C. (Sample No. 43), 1000 ° C. (Sample No. 44), 1100 ° C. (Sample No. 45), 1200 ° C. (Sample No. 46), and calcined for 3 hours, respectively, and calcined powder (first calcined) Powder).
- the obtained calcined powder (first calcined powder) was taken as 100% by mass, and further 0.75% by mass of Bi 2 O 3 was added to obtain calcined powder (second calcined powder).
- This calcined powder (second calcined powder) was wet pulverized to a size of 1.1 ⁇ m to 1.3 ⁇ m (measured by an air permeation method) with a ball mill and then dried.
- the rate of change in initial permeability when the obtained sintered ferrite material was pressurized at 30 MPa was determined.
- the measurement method was the same as in Example 1.
- the result is shown in FIG.
- FIG. 29 is a graph showing the results of FIG. In FIG. 28, the number of grain boundary pores per 100 crystals is the number of pores present at the grain boundaries in the region where 100 crystals exist in the structure photograph of the cross section of the sintered ferrite material.
- FIGS. 30 to 32 are SEM photographs of the pulverized powder
- FIGS. 33 to 35 are structural photographs of the sintered ferrite material after firing
- FIGS. 30 and 33 are sample number 41 (calcination temperature 800 ° C.)
- FIG. FIG. 34 shows the case of sample number 44 (calcination temperature 1000 ° C.)
- FIGS. 32 and 35 show the case of sample number 46 (calcination temperature 1200 ° C.).
- each pulverized powder has a different particle size distribution even though the average particle size is almost the same (1.1 ⁇ m to 1.3 ⁇ m).
- FIG. 30 (calcination temperature 800 ° C.), it is presumed that the particle size of the powder is relatively uniform and the particle size distribution is sharp
- FIG. 31 (calcination temperature 1000 ° C.) and FIG.
- the calcining temperature of 1200 ° C. it can be estimated that a large number of relatively large powders and relatively small powders are contained, and the particle size distribution is not sharp.
- the number of grain boundary pores per 100 crystal grains is 20 or more, and a sintered ferrite material can be obtained in which the rate of change in initial permeability is as small as ⁇ 3% or less. Also in FIG. 33 (calcination temperature 800 ° C.), the average crystal grain size is 11.5 ⁇ m, which is in the range of the preferable average crystal grain size according to the present invention, and the rate of change of the initial permeability is within ⁇ 5%. is there.
- the sintered ferrite according to the present invention is a direct-winding type that does not require a bobbin that requires a high specific resistance, a gapped type that is used under a DC bias magnetic field that requires initial permeability and high saturation magnetic flux density, and high. It is optimal as a core material for various types of inductors, antennas, transformers, and other types of inductors, such as resin molds that require stress resistance.
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Abstract
Description
本実施例は、x(ZnO)の組成限定理由を実証するものである。
本実施例は、y(Fe2O3)の組成限定理由を実証するものである。
本実施例は、z(CuO)の組成限定理由を実証するものである。
本実施例は、Bi2O3の添加量の限定理由を実証するものである。
本実施例は、焼結フェライト材料の平均結晶粒径の限定理由を実証するものである。
本実施例は、焼結フェライト材料をインダクタへ適用した場合の適用例を実証するものである。
本実施例は、焼結フェライト材料をアンテナへ適用した場合の適用例を実証するものである。
図1の試料番号4に示す組成となるように、出発原料となる炭酸塩粉末と酸化物粉末を秤量、混合し、大気中で仮焼温度800℃(試料番号41)、900℃(試料番号42)、950℃(試料番号43)、1000℃(試料番号44)、1100℃(試料番号45)、1200℃(試料番号46)で夫々3時間仮焼して仮焼粉(第1仮焼粉)を得た。得られた仮焼粉(第1仮焼粉)を100質量%として、更に0.75質量%のBi2O3を添加して仮焼粉(第2仮焼粉)を得た。この仮焼粉(第2仮焼粉)をボールミルで1.1μmから1.3μm(空気透過法による測定)の大きさになるように湿式粉砕した後、乾燥した。
Claims (10)
- 組成式(1-x-y-z)(Li0.5Fe0.5)O・xZnO・yFe2O3・zCuOであり、x,y,zが、0.14≦x≦0.19、0.48≦y<0.5、0≦z≦0.03を満足する材料を100質量%として、更にBi2O3を0.5質量%以上3質量%以下を添加してなり、初透磁率200以上、飽和磁束密度が23℃で430mT以上、100℃で380mT以上、比抵抗106 Ωm以上を満足する焼結フェライト材料。
- 平均結晶粒径が7.5μm以上25μm以下である請求項1に記載の焼結フェライト材料。
- 圧力30MPaで加圧したときの初透磁率の変化率が±5%以内である請求項1または2に記載の焼結フェライト材料。
- 結晶粒100個あたりの粒界ポア数が20個以上である請求項1または2に記載の焼結フェライト材料。
- 圧力30MPaで加圧したときの初透磁率の変化率が±3%以内である請求項4に記載の焼結フェライト材料。
- 請求項1から5のいずれかに記載の焼結フェライト材料を用いた巻線部品。
- 組成式(1-x-y-z)(Li0.5Fe0.5)O・xZnO・yFe2O3・zCuOであり、x,y,zが、0.14≦x≦0.19、0.48≦y<0.5、0≦z≦0.03を満足する原料粉末を準備する工程と、
原料粉末を仮焼して第1仮焼粉を得る工程と、
第1仮焼粉を100質量%として、更にBi2O3を0.5質量%以上3質量%以下だけ添加して第2仮焼粉を得る工程と、
第2仮焼粉を粉砕して粉砕粉を得る工程と、
粉砕粉を成形して成形体を得る工程と、
成形体を焼成して焼結フェライト材料を得る工程と
を有する焼結フェライト材料の製造方法。 - 組成式(1-x-y-z)(Li0.5Fe0.5)O・xZnO・yFe2O3・zCuOであり、x,y,zが、0.14≦x≦0.19、0.48≦y<0.5、0≦z≦0.03を満足する材料を100質量%として、更にBi2O3を0.5質量%以上3質量%以下を添加してなる原料粉末を準備する工程と、
原料粉末を仮焼して仮焼粉を得る工程と、
仮焼粉を粉砕して粉砕粉を得る工程と、
粉砕粉を成形して成形体を得る工程と、
成形体を焼成して焼結フェライト材料を得る工程と
を有する焼結フェライト材料の製造方法。 - 前記原料粉末を仮焼するときの仮焼温度は800℃~1200℃である請求項7または8に記載の焼結フェライト材料の製造方法。
- 前記仮焼温度が1000℃~1200℃である請求項9に記載の焼結フェライト材料の製造方法。
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- 2009-02-13 US US12/867,693 patent/US9434622B2/en active Active
- 2009-02-13 WO PCT/JP2009/052365 patent/WO2009101999A1/ja active Application Filing
- 2009-02-13 CN CN200980105392.5A patent/CN101945836B/zh active Active
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Also Published As
Publication number | Publication date |
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CN101945836A (zh) | 2011-01-12 |
US9434622B2 (en) | 2016-09-06 |
JP5387947B2 (ja) | 2014-01-15 |
EP2258671A4 (en) | 2011-05-25 |
US20110018675A1 (en) | 2011-01-27 |
EP2258671B1 (en) | 2017-01-11 |
JP2009215152A (ja) | 2009-09-24 |
CN101945836B (zh) | 2014-04-09 |
EP2258671A1 (en) | 2010-12-08 |
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