TW201243873A - Compressed powder magnetic core and manufacturing method thereof - Google Patents

Abstract

The goal of the present invention is to provide a compressed powder magnetic core to enhance thermal stability of initial magnetic permeability, and the manufacturing method thereof. The compressed powder magnetic core according to the present invention is characterized by forming through compressing mixture containing soft magnetic powder 5 and insulating bonding material 6 and obtained after applying heat treatment. The said insulating bonding material 6 contains binder resin and glass, wherein the glass transition temperature (Tg) of the glass is lower than the temperature of heat treatment. The compressed powder magnetic core and the manufacturing method thereof according to the present invention can enhance the thermal stability of initial magnetic permeability. Furthermore, by adding not only glass but also magnetic micro particles with particle diameter less than that of soft magnetic powder in the insulating bonding material, the initial magnetic permeability (initial stage) may be increased, and not only the thermal stability of initial magnetic permeability, but also the thermal stability of iron loss can be enhanced.

Description

201243873 VI. Description of the Invention: [Technical Field] The present invention relates to a powder magnetic core comprising a soft magnetic powder and an insulating bonding material, a choke coil, and the like, and a method of manufacturing the same. [Prior Art] For a powder magnetic core used in a booster circuit for a hybrid vehicle or a reactor for power generation, substation, a transformer, a choke coil, etc., it is assumed that it is in a high temperature state for a long time. In the environment, it is required to have thermal stability of magnetic properties. The powder magnetic core can be obtained by subjecting a mixture comprising a soft magnetic powder and a binding material (adhesive resin) to powder compaction and further applying heat treatment. This heat treatment is a process necessary for improving the magnetic properties of the soft magnetic powder. Therefore, the industry has designed a resin which is excellent in thermal stability as a binder resin. However, according to the experiment, it was found that the heat resistance test caused the deterioration of the magnetic permeability and the thermal stability of the inductance to be lowered under the constitution of the prior powder magnetic core. [Prior Art Document] [Patent Document 1] Japanese Patent Laid-Open Publication No. 2010-251600 (Patent Document 2) Japanese Patent Laid-Open Publication No. 2010-232223 (Patent Document 3) [Patent Document 4] Japanese Laid-Open Patent Publication No. 2004-143554 [Patent Document 5] Japanese Patent Laid-Open Publication No. 2010-27854 No. 161851.doc 201243873 [Draft] [Problems to be Solved by the Invention] The invention of the patent document 1 relates to a powder for a powder magnetic core which is obtained by dispersing a glass powder in an alkoxide layer coated with a soft magnetic metal powder, and further comprising an insulating layer covering the alkoxide layer. Further, the object of the invention described in Patent Document 1 is to obtain a high-strength powder magnetic core. The invention of the patent document 2 relates to an insulating coated soft magnetic powder comprising a core portion of a soft magnetic material and a coating layer β obtained by fixing particles of an insulating material covering the core portion. Further, Patent Document 2 The object of the invention described is to provide a powder magnetic core having a small eddy current loss. The invention of Patent Document 3 relates to a composite soft magnetic material comprising a soft magnetic powder and an insulating bonding material, and Patent Document 3 discloses that the insulating bonding material is lead-free glass, and a polyfluorene can be added to the composite soft magnetic material. Any of the oxy-resin or stearate. Further, the object of the invention described in Patent Document 3 is to maintain the performance of the powder magnetic core for a long period of time. Here, performance is listed as iron loss and strength. The invention of Patent Document 4 relates to a coated iron-based powder obtained by coating a surface of an iron-based powder with a coating material, and Patent Document 4 contains the above-mentioned coating material comprising glass, a binder, and glass and an adhesive. Insulating and thermally stable substances other than those. Further, the object of the invention described in Patent Document 4 is to obtain a powder magnetic core which can ensure insulation and which is improved. Patent Document 5 discloses a powder magnetic core in which an amorphous four-alloy powder and a glass powder are mixed with a binder resin, and the like; 16185I.doc 201243873, a molded body, 19 amorphous The soft magnetic alloy card 10 5 is formed by heat treatment at a temperature at which the crystal temperature is low. Further, the purpose of the invention described in the special purpose is to obtain a powder magnetic core having a low loss. As described above, in each of the patents, there is no literature for achieving permeability stability. In addition, there is no such thing as the material composition of the improved bonding material, and the relationship between the material and the heat treatment. The history of the history recorded in Patent Document 5 contains iron loss and magnetic properties. Experiment of the conductivity. However, Patent Document 5 improves the relationship between the I-junction material and the heat treatment, etc., from the viewpoint of reducing the eddy current loss as the first objective, and not from the magnetic permeability, and the inventors believe that the patent document Under the experimental conditions of 5, the addition amount of the bonding material (adhesive resin) is too large to ensure the strength of the powder magnetic core. Therefore, the present invention has been made to solve the above-mentioned problems, and the object thereof is particularly Provided is a powder magnetic core capable of improving thermal stability of magnetic permeability and a method of manufacturing the same. [Technical means for solving the problem] The powder magnetic core of the present invention is characterized in that it comprises a soft magnetic powder and A mixture of an insulating bonding material obtained by compression molding and heat treatment, wherein the insulating bonding material contains a binder resin and glass, and a glass transition temperature (Tg) of the glass Further, the method for producing the powder magnetic core of the present invention is characterized by comprising the steps of: mixing a soft magnetic powder with an adhesive resin as an insulating bonding material and glass powder 161851.doc 201243873 a mixture; and subjecting the mixture to compression molding, and thereafter heat-treating at a heat treatment temperature higher than a glass transition temperature (Tg) of the glass powder. It is considered that the glass contained in the insulating bonding material is pressed by powder magnetic according to the present invention. The heat treatment in the manufacturing step of the core is deformed or the glass is bonded to each other, whereby the expansion or contraction due to thermal deterioration of the adhesive resin can be alleviated (it is considered that the mechanical strength of the insulating bonding material can be improved), that is, the glass is not considered as The simple filler is dispersed in the insulating bonding material, and is also responsible for preventing the expansion or contraction of the adhesive resin layer in the insulating bonding material. Here, the magnetic permeability of the powder magnetic core can be 〇llendrof expression indicating the DC permeability of a collection of ferromagnetic powders. Soft magnetic powder The packing ratio η, the effective demagnetizing factor of the soft magnetic powder is N, the function of the soft magnetic powder μι the inherent permeability as follows: [Equation 1]

Among them, μ〇 is the magnetic permeability of vacuum 4πχ 1〇-7. It is conceivable that, for the effective demagnetization coefficient N, the effective demagnetization coefficient > 1 becomes smaller than the soft magnetic property by the shape of the soft magnetic powder or the magnetic interaction between the soft magnetic powders in the state of filling the soft magnetic powder. N of the powder in a single state. As described above, in the present invention, a glass is mixed in an insulating bonding material 161851.doc 201243873 At this time, 'by selecting a glass having a glass transition temperature (Tg) of a heat treatment temperature in a manufacturing step of a powder magnetic core ( By heating at a temperature higher than the glass transition temperature, the glass becomes a wedge member for preventing the expansion or contraction of the adhesive resin layer, and it is considered that the powder magnetic core is used even in a long-term exposure to a high temperature. The interval between the soft magnetic powders is also not easily changed, and the change in the effective demagnetization coefficient N is small. Therefore, the change in the initial magnetic permeability can be reduced. By the above manner, the thermal stability of the initial magnetic permeability of the powder magnetic core can be improved as compared with the prior art. In the present invention, the content of the glass is preferably in the range of 0 丨 mass% or more and 〇 6 〇 mass% or less based on the mass of the soft magnetic powder. Thereby, the initial magnetic permeability (initial) which is equivalent to the previous (without glass) can be obtained and the thermal stability of the initial magnetic permeability can also be improved. Further, in the invention, the glass preferably comprises at least p2〇5, Β2〇3 and BaO, and the composition ratio 3 of 卩2〇5 is 4〇~6〇m〇i%, and the composition of B2〇3 The ratio b is 2~20 mol. /. , the composition ratio of BaO. 5~45 m〇i〇/0, the composition ratio d of SnO is 0~45 mol%, and the composition ratio e of Ai2〇3 is 〇~15 mol%, and satisfies a+b+c+d+eS100 m〇 The relationship between i〇/0. When the glass 2 and the glass 3 were obtained in the experiment described later, the initial magnetic permeability (initial) which is substantially the same as that of the previous example in which no glass was added was obtained, and the thermal stability of the initial magnetic permeability was improved. Further, in the present invention, the composition ratio e of 'Al2〇3 is preferably 2 to 15 mol% 0. In addition, in the present invention, the composition ratio f of Li2 is preferably 16I851.doc 201243873 mol% 'Ce02 composition The ratio g is 〇~ι 〇m〇i% 'the composition ratio of Ti〇2 is 0 to 1 mol% ' and satisfies a+b+c+d + e+f+g+h+i=100 mol% relationship. Further, in the present invention, the glass transition temperature (Tg) of the above glass is preferably from 280 °C to 470. Further, the glass transition temperature (Tg) of the above glass is more preferably 36 CTC or more and less than 470 ° C. Further, in the present invention, the glass has a thermal expansion coefficient of preferably 60 to 11 Å (X10) 7/° C). The thermal expansion coefficient of the above glass is more preferably 60 to 90 (χ1〇·7/°〇〇 by adjusting the glass composition 'control glass transition temperature (Tg)' as described above and further controlling the thermal expansion coefficient, Further, in the present invention, the insulating bonding material preferably contains the glass and magnetic fine particles having a particle diameter smaller than that of the soft magnetic powder. In the case where magnetic fine particles are present between the soft magnetic powders, the effective demagnetization coefficient N can be reduced, so that the initial magnetic permeability (initial) can be improved. In addition, the heat of iron loss can be improved by adding magnetic fine particles. Stability. Here, the iron loss (core loss) of the powder magnetic core can be generally divided into hysteresis loss proportional to the measured frequency and eddy current loss proportional to the square of the measured frequency. Above The effect of demagnetizing the magnetic coefficient n, or the insulating bond, the hysteresis caused by the residual stress of the soft magnetic powder, and the like, becomes larger. Therefore, it is considered to be insulated by the present invention.磁性 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 161 161 161 161 161 161 161 161 161 161 161 161 161 161 161 161 161 161 161 161 161 161 161 161 161 161 161 161 161 161 161 161 161 161 161 161 161 161 The high mechanical strength of the insulating bonding material can effectively suppress the variation of the residual stress, and can improve the thermal stability of the iron loss together with the initial magnetic permeability. In the present invention, the content of the magnetic fine particles is preferably relative to The mass of the soft magnetic powder is in a range of more than 〇% by mass and not more than 60% by mass. In this case, the magnetic fine particles are oxide magnetic materials, and specifically 5 is preferably ΝιΖη ferrite or MnZn ferrite. At least one of them can increase the initial magnetic permeability (initial), and can also effectively improve the initial magnetic permeability and the thermal stability of the iron loss. [Effect of the Invention] According to the present invention The powder magnetic core of the invention and the manufacturing method thereof can improve the thermal stability of the initial magnetic permeability. Further, by adding not only glass to the insulating bonding material but also adding magnetic particles having a smaller particle size than the soft magnetic powder, the magnetic particle can be improved. The initial magnetic permeability (initial), in addition, not only can improve the thermal stability of the initial magnetic permeability, but also improve the thermal stability of the iron loss. [Embodiment] FIG. 1 is a perspective view of a powder magnetic core (iron core), Figure 2 is a plan view of a coil-sealed powder core. Figure 3 is a partially enlarged cross-sectional view (schematic diagram) of the powder core. The powder magnetics shown in Figure 1 can be made by containing soft magnetic powder and insulation. The mixture of the bonding materials is subjected to compression molding and heat treatment. The symbol 5 shown in Fig. 3 is a soft magnetic powder, and the symbol 6 is an insulating bonding material. As shown in Fig. 3, the insulating insulating material 6 surrounds the surface of the soft magnetic powder 5, 16185I.doc 201243873, and exists between the soft magnetic powders 5 to hold (support) the plurality of soft magnetic powders 5. Further, as shown in Fig. 3, a void 7 is formed everywhere in the insulating bonding material 6. It should be noted that, in Fig. 3, all of the soft magnetic powder 5 and the pores 7 are not labeled. The coil-sealed powder magnetic core 2 shown in Fig. 2 is composed of a powder magnetic core 3 and a coil 4 covered by the powder magnetic core 3. The internal structure of the powder magnetic core 3 is the same as that of Fig. 3. The soft magnetic powder 5 is, for example, an amorphous soft magnetic powder produced by a water atomization method. The above amorphous soft magnetic powder (Fe-based metallic glass alloy powder) has, for example, a composition formula represented by Fe 丨00-a-b_dyztNiaSnbCrcPxCyBzSit, and 〇at%<a<10 at%. 〇at%<b<3 at% > 0 at%<c<6 at% . 6.8 at%<x<l〇.8 at% , 2.0 at%<y<9.8 at% > 0 at%<z<8.0 at% » 0 at%St£5.0 at%. The average crystal grain size (D5〇) of the soft magnetic I1 raw uncle 5 is the degree of i〇. Here, in the present embodiment, the soft magnetic powder 5 is not limited to a non-dimorphic material, but the powder magnetic core and the use of the amorphous soft magnetic powder and the insulating bonding material are used for pressing and forming. Compared with the case of the 4-ferrite ferrite, it has a large saturation magnetic flux density, and thus is advantageous for miniaturization. The insulating bonding material 6 which is not shown in Fig. 3 is composed of a binder resin and glass. The binder resin is a polysulfide resin, an epoxy resin, a (tetra) resin, a urea resin, a melamine resin or the like. It is particularly preferred to use a polyoxymethylene resin as a heat-stable resin for the adhesive resin. 16185I.doc 201243873 The adhesive resin is added to the extent of 0.5 to 5.0% by mass based on the mass of the soft magnetic powder 5 contained in the powder magnetic core. In the present embodiment, as described above, the insulating adhesive material 6 contains glass. Here, it is considered that the glass is dispersed in the adhesive resin layer. The glass is first mixed with the soft magnetic powder 5 or the binder resin in a powder form, and the heat treatment after compression molding into the shape of the powder magnetic cores 1 and 3 shown in Fig. 1 or Fig. 2 is high in the present embodiment. It is carried out at the temperature of the glass transition temperature (Tg) of the glass. Therefore, in the present embodiment, it is considered that the glass is deformed from the initial powder form, or the glass is bonded to each other, a part is diffused into the resin, and the resin is fused. In the present embodiment, it is possible to form a plurality of soft magnetic powders 5 by an adhesive resin layer having a small Young's modulus, and further heat treatment by a glass transition temperature (Tg) in a manufacturing step of the powder magnetic core. The glass having a low temperature is introduced into the insulating bonding material 6 to alleviate the structure of expansion and contraction due to thermal deterioration of the adhesive resin layer. It is considered that the glass (powder) is deformed after being exposed to heat treatment higher than the glass transition temperature (Tg), or the glass is bonded to each other, etc., thereby acting as a wedge for preventing expansion and contraction of the adhesive resin layer. One of the factors determining the magnetic permeability of the powder magnetic cores 1, 3 is the effective demagnetization coefficient N. With respect to the effective demagnetization coefficient n, it is considered that, as shown in FIG. 3, in the state in which a plurality of soft magnetic powders 5 are filled, 'the magnetic demagnetization coefficient 1 becomes changed by the magnetic interaction between the soft magnetic powders 5 and the like. It is smaller than the value of the effective demagnetization coefficient N in the single state of the soft magnetic powder 5. 161851.doc 201243873 In the use environment exposed to high temperature for a long time, if the change of the interval between the soft magnetic powders 5 is small, the change of the effective demagnetization coefficient N is also small, as described above, in the present embodiment. In the form, it is considered that the glass having a glass transition temperature (Tg) lower than the temperature of the heat treatment performed in the manufacturing step of the powder magnetic core can alleviate the expansion or contraction due to thermal deterioration of the adhesive resin layer, even for a long time. In the environment in which the ground is exposed to high temperatures, the change in the interval between the soft magnetic powders 5 and 5 in the powder magnetic cores 1, 3 can be made smaller than the previous one, so that the change in the effective demagnetization coefficient N can be reduced. Based on the above, it can be seen that according to the present embodiment, the thermal stability of the initial magnetic permeability of the powder magnetic cores 1, 3 can be improved as compared with the prior art. Therefore, the thermal stability of the inductance can be improved. In the present embodiment, the content of the glass is preferably relative to the soft magnetic powder; the mass of 5 is 0.1 mass. /0 (wt%) or more, 〇.6〇 mass% (wt%) or less. It is considered that if the amount of addition of glass is too high, the interval between the soft magnetic powders 5 and 5 becomes large when the powder magnetic core is formed, and the effective demagnetization coefficient is the value of ^; the body becomes large', so the initial magnetic permeability is easy. reduce. In the present embodiment, by limiting the amount of glass added as described above, the initial magnetic permeability (initial) equivalent to the previous (excluding glass) can be obtained and the thermal stability of the initial magnetic permeability can be improved. Here, the initial magnetic permeability! (Initial Μ refers to the initial permeability before the formation (initial) and exposure to high temperature use (1).

Further, the glass preferably contains at least a composition ratio of β, 〇3, and Ba0 to form 2〇5, and a composition ratio of 40 to 6 〇mol%, and a composition ratio b of b2〇3 is M 161851.doc *12-201243873 mol %, the composition ratio of BaO is 5 to 45 mol%, the composition ratio d of SnO is 0 to 45, and the composition ratio of Al2〇3 is 0 to 15 m〇i%, and satisfies a+b+c + d+ eS100 mol% relationship. In the composition range of the glass, the initial magnetic permeability (initial) and the previous glass are not added by containing the glasses 2 and 3 in the experiment described later and appropriately controlling the glass transition temperature (Tg) according to the glass. The examples are approximately equal and the thermal stability of the initial permeability can be improved. In addition, the content of the glass of the above composition is in the range of 0 to 1% by mass or more (% by mass) or less in terms of the mass of the soft magnetic powder 5, and it is known from the experiment described later. The thermal stability of the initial magnetic permeability can be improved, and the iron loss (initial) can be further reduced to the previous (without glass). Further, in the present embodiment, the composition ratio 6 of the barium 2〇3 is preferably 2 to 15 mol%. Further, the composition ratio a of 'P2〇5' is preferably 41 to 55 m〇m. Further, the composition ratio b of ΒΖ〇3 is preferably 2 to 15 mol%. Further, the composition of Ba〇 is preferably 5 to 30 mol%. The composition ratio d of SnO is preferably 〇~3〇 m〇i%, more preferably 25 to 30 mol%. Further, the composition ratio of Al2〇3 is more preferably 2 to 1% mol%. Further, in the present embodiment, at least one of U2〇, Ce02, and Ti〇2 may be contained in addition to the above. In this case, it is preferable that the composition ratio f of 〇 is 0 to 1 mol%, the composition ratio g of 〇02 is 〇10 10 〇1%, and the composition ratio i of Ti〇2 is 0 to 1 mol%. And the relationship of a+b+c+d+e+f+g+h+i=l()() mol% is satisfied. The heat treatment performed by compressing the mixture containing the soft magnetic powder 5 and the insulating bonding material 6 into a shape of 161851.doc •13·201243873 is important in eliminating the strain of the soft magnetic powder 5 and obtaining good magnetic properties. Step, therefore, the most suitable temperature for the heat treatment depends on the soft magnetic powder 5'. In the present embodiment, the glass transition temperature having a lower temperature than the (most suitable) heat treatment performed in the manufacturing step of the powder magnetic core is selected ( Tg) glass. The glass transition temperature (Tg) of the glass in the present embodiment is preferably about 280 ° C to 470 ° C. Further, the glass transition temperature (Tg) is preferably 36 Å or more and less than 470 Torr. Further, the glass transition temperature (Tg) is more preferably 44 Å (t or more and less than 470 ° C. By the glass having the above composition, the glass transition temperature (Tg) can be controlled within the above range. In the case where the (heat treatment temperature and glass transition temperature (Tg)) is not very large, both the initial magnetic permeability and the thermal stability of the initial magnetic permeability can be effectively improved. In addition, the initial iron loss (iron) can also be used. The core loss is set to be equal to or less than the previous example in which the glass is not added. Here, the "early iron" refers to the iron loss before the powder magnetic core is formed (initial) and exposed to a high-temperature use environment. The heat treatment temperature-glass transition temperature (Tg) is 2 to 1 〇〇, to the extent of 2 to 28 ° C. Further, it is considered that the glass thermal expansion coefficient (Tg) is controlled together with the glass transition temperature (Tg). (X can improve the thermal stability of the initial magnetic permeability, and is preferable. As the coefficient of thermal expansion α, it is preferably 60 to 11 〇 (xl (rVc), more preferably 6 〇 to 9 〇 (χ 10'7 / ° 〇 Further, in the present embodiment, it is preferable that the insulating bonding material 6 is divided into 1 6l851.doc 14 201243873 Magnetic particles having a particle size smaller than that of the soft magnetic powder 5 "The particle control system of the magnetic fine particles can enter the interval between the soft magnetic powders 5 and 5 shown in Fig. 3 and hardly enlarge the interval. The small particle diameter, specifically, the magnetic fine particles are nano particles, which are sufficiently smaller than the soft magnetic powder 5. The magnetic fine particles may be selected from materials different from the soft magnetic powder 5. For example, the magnetic fine particles are oxidized. The magnetic powder is, in particular, preferably at least one of a NiZn ferrite or a MnZn ferrite. Thus, it is considered that the insulating fine bonding material 6 contains not only glass but also magnetic fine particles. Existing between the soft magnetic powders 5 and 5, the value of the effective demagnetization coefficient N can be reduced. Thereby, the initial magnetic permeability of the powder magnetic cores 1, 3 can be improved. Further, by adding magnetic fine particles, The thermal stability of the iron loss can be improved. As one of the factors for reducing the iron loss, the stress (residual stress) which the soft magnetic powder 5 receives can be reduced. Here, it is considered that the insulating adhesive material 6 is used. By adding the magnetic fine particles, and by combining the magnetic fine particles with the glass, the mechanical strength of the insulating bonding material 6 can be improved not only in the use environment exposed to high temperature for a long period of time, but also the soft magnetic powder 5 can be effectively suppressed. The variation of the residual stress 'by this' can increase the thermal stability of the iron loss with the initial magnetic permeability. ^ In the present embodiment, the content of the magnetic fine particles (4) is greater than 0% by mass with respect to the mass of the soft magnetic powder 5. And in the range of 0.6 〇 mass% or less, the amount of the glass and the magnetic granules added to the rim bond material 6 is adjusted as described above, and is adjusted according to the following. 161851.doc -15- 201243873 It can be seen that 'the initial magnetic permeability and the thermal stability of iron loss can be effectively improved. In addition, the initial magnetic permeability (initial) can be set to be equal to or higher than the previous example (excluding glass and magnetic fine particles). Although the initial iron loss is slightly higher than the previous example (excluding glass and no magnetic particles), it is also within the usable range. In the following, a method for producing a powder magnetic core according to the present embodiment will be described. First, a soft magnetic powder, a binder resin, a glass powder, a lubricant, and a coupling agent produced by a water atomization method are stirred and mixed with a solvent. Mud slurry. Further, magnetic particles such as 211 ferrite or ΜηΖη ferrite may be further mixed. Here, as the lubricant, zinc stearate, stearic acid or the like can be used. Further, as the coupling agent, a decane coupling agent or the like can be used. The slurry is placed in a conventional granulation apparatus, and the solvent of the slurry is instantaneously dried to form a granular mixture containing the soft magnetic powder and the insulating bonding material. Then, the above mixture was filled into a forming mold and compression-molded into the shape of a powder magnetic core. Then, the powder magnetic core is subjected to heat treatment. The heat treatment at this time is carried out at a temperature higher than the glass transition temperature (Tg) of the glass. At this time, since the heat treatment temperature which is most suitable for eliminating the strain of the soft magnetic powder is previously determined and the heat treatment temperature is set to a temperature higher than the glass transition temperature (Tg), it is necessary to select a glass transition temperature (Tg) lower than the heat treatment temperature. ) the glass. It is considered that by this heat treatment, most of the lubricant is vaporized and disappears, and the portion where the H-point resin is formed with the adhesive resin is also vaporized and disappeared. In the present embodiment, the glass and the binder resin are present as a part of the insulating bonding material 6 between the soft magnetic powders. The glassy ray is also mixed in a powder form at the stage of slurry formation as described above. However, after compression molding and heat treatment, the glass is deformed from powder or formed into a state in which the glass is bonded to each other. Therefore, it is considered that the glass is not a simple filler. It is also responsible for the wedge member that prevents the adhesive resin layer from expanding or contracting in the insulating material. The powder magnetic core of the present embodiment is excellent in initial magnetic permeability and thermal stability of iron loss. Therefore, it is particularly suitable for a booster circuit such as a hybrid vehicle or a reactor, a transformer, a choke coil, etc. used in power generation and substation equipment, and is required to have thermal stability in a long-time high temperature environment. [Examples] (Experiment for determining the relationship between the amount of glass 1 and the characteristics and thermal stability of the powder magnetic core) Fe74.43 at% Cri.96 at%P9 Q4 at% prepared by water atomization method C2 16 at% B7.54 at%Si4.87 at% is a mixture of amorphous soft magnetic powder, polyoxynoxy resin, zinc stearate, and phosphoric acid glass powder (glass crucible). The phosphoric acid glass was KF9® 79 powder manufactured by AGC TECHNO GLASS. The glass transition temperature (Tg) of the glass} is 28 〇t. In addition, the blending amount of the polyoxyl resin in the above mixture is 丨4 wt% with respect to the mass of the soft magnetic powder, and the blending amount of zinc stearate is 〇3 wt% with respect to the mass of the soft magnetic powder, and the blending of the glass powder 1 The mass relative to the soft magnetic powder is 〇wt%, 〇3 wt〇/〇, 0.6 wt%, 1.2 wt%, 2.4 wt%, 4.2 wt%, and 6.1 wt%. Then, the above mixture was filled in a mold, and pressure-molded at a carrying pressure of 147 MPa. A ring-shaped sample having an outer diameter of 2 mm mm x an inner diameter of 12 mm x a thickness of 6.8 161851.doc -17 - 201243873 m was produced. The obtained ring-shaped sample was subjected to a heat treatment at 470 ° C for 1 hour in a nitrogen gas atmosphere to thereby form a powder magnetic core. Using a super megohmmeter (SM-8213 manufactured by DKK-TOA), the intrinsic resistance of the obtained annular powder magnetic core was measured 'on the annular powder magnetic core wound copper wire' using an impedance analyzer (HP) 4192 A) The initial magnetic permeability was measured, and the iron loss (initial) was measured using a BH Analyzer (manufactured by Iwasaki Communications) at a frequency of 100 kHz and Bm = l〇〇mT. In the heat resistance test, the annular powder core was used. The initial magnetic permeability and iron loss were measured after being placed in a drying oven at 180 ° C and 250 ° C in the atmosphere for 1 00 hours. The results of each measurement are shown in Table 1. [Table 1] Table 1

Powder magnetic core No. Phosphoric acid glass Tg Phosphoric acid glass added Dong 100 kHz under the beginning # 导牟100 kHz' 100 mT under the iron loss (kW/m5) Surface resistance (Π·αη) 18〇Ί〇χ1〇 Change in initial magnetic permeability after 〇〇 hour heat resistance test 初始 2501 〇 1000 hours change of initial magnetic conductance after heat resistance test 变化 Change rate of iron loss after Woiooo hour heat test 25 〇·〇χΐ〇〇〇 After the heat test, donate «Chemistry 1 - CMt% machine 4 ± 0.4 2 « 4 士 13 t75EM0, · -3 Κ -22% 18K 127 Κ 1 280% ASwtS 45-β 士 05 330±4 8.52EX10* · 2P% 3 ¢ 803⁄4 〇 L6wtK 370±11 fl.23EX10** -2Ϊ ιβχ 8fiK 4 2803⁄4 40.910.4 513±16 1.94ΕΧ10" _τΆ. •16« -ax 5 280*0 2.4wt& 402±8.2 t. «ExtnM -4Χ -UK sx 6 28013⁄4 33·3±0.β 586±22 1.S1EX10" -5Χ 7 6.1wrt ^&.Q±0l4 ί.ε〇ΕχιοΜ -5Κ -!ί« -2Κ (6X 4 is a graph showing the relationship between the amount of addition of the glass 1 of each of the powder magnetic cores shown in Table 1 and the initial magnetic permeability (initial) and iron loss (initial). As shown in Table 1 and FIG. 4, Glass The addition amount of 1 increases, the initial magnetic permeability decreases, but on the other hand, the iron loss increases. When the amount of glass added exceeds 〇·6 wt°/〇, the initial magnetic permeability is the same as that without adding glass (previous example) In comparison with the decrease of 1% or more, the iron loss is increased by 40% or more. Therefore, in order to prevent the magnetic properties of the powder magnetic core from being lowered, it is necessary to increase the glass addition amount to 0.6 wt% or less. The inherent resistance of the powder magnetic core shows an increasing tendency as the amount of glass 1 is increased by -18-161851.doc 201243873, and any sample is shown as 1〇6 Q.cmw. The intrinsic t resistance of the dust powder rn is sufficient as a powder magnetic core. Fig. 5 shows that the heating temperature of each of the powder magnetic cores of the watch is set to 丨8 and 250. (:, heating time is set to 1) The relationship between the amount of addition of the glass crucible and the rate of change (%) of the initial magnetic permeability after the heat resistance test and the amount of iron loss (%) in the heat resistance test of the hour. Rate of change of conductivity" [(Initial permeability after heat resistance test - Initial permeability of initial initial permeability) ] X 1〇〇 (%) indicates. "Initial initial permeability" refers to the initial magnetic permeability before the powder core is formed (initial) and exposed to a high temperature use environment. In addition, the "iron loss change rate" is represented by [(iron loss after heat resistance test - initial iron loss) / initial iron loss] x 100 (%). "Initial iron loss" refers to the iron loss before the powder core is formed (initial) and exposed to high temperature use. As a target of thermal stability, the rate of change of the initial magnetic permeability is set to be within ±15% after 180 to 200 ° 〇 1000 hours, preferably within ±1%, after 00 hours at 250 ° C x H) Within 25%, preferably within 2% of the soil, and the rate of change of iron loss is set to within ±40%, preferably within ±30% after 18〇~2〇〇〇Cxl〇〇〇 It is within ±70% after χ1〇〇〇, preferably ±50%. According to Table 1 and Figure 5, as the amount of glass enamel added increases, the initial after heat resistance test Although the rate of change in magnetic permeability (❶/.) is a negative value, the absolute value tends to decrease. The rate of change in iron loss (%) also tends to decrease. The amount of addition of glass 1 is set to 1 2 . When the wt% or more is more effective, 161851.doc •19·201243873 satisfies the above-mentioned heat stability stability target, but as shown in Table 丨 and FIG. 4, the initial amount of the glass is set to 1.2 wt% or more. The conductivity (initial) is low and the iron loss (initial) becomes large. On the other hand, it is understood that the amount of glass 1 added is 〇6 wt% or less. Although the rate of change of initial permeability after 000 hours of 250 °C XI is slightly more than •20%, it is 18〇. The rate of change of initial permeability after 1000 hours is maintained at -2%~-3%. In addition, for the iron loss, the addition amount of the glass summer is also set to 0.6 wt 〇 /. Below 18, the iron loss change rate after 1000 hours of TCx can be maintained within 30%. (Glass 2, 3 Production) The glasses 2 and 3 are produced by the following production methods: Commercially available orthophosphoric acid, boron oxide powder, strontium carbonate powder, tin oxide powder, and alumina powder are used as the glass raw material to achieve a specific blending amount. The raw materials are metered, charged into a platinum crucible for premixing, and then melted in an atmosphere using an electric furnace. The set temperature of the electric furnace is 1 〇〇〇 to 1300. (:. Then, the platinum iridium is taken out from the electric furnace, The glass melt was cast in an iron mold to obtain glass. The glass was coarsely pulverized in a mortar, and then pulverized using a ball mill to obtain a glass powder. Further, a glass piece of 3 mm x 3 mm x 2 mm was cut out from one part of the cast glass. , cancel After the annealing treatment of the strain, the glass transition temperature, the yield temperature and the thermal expansion coefficient were measured using a thermomechanical analysis device (TMA 8 3 10 manufactured by Rigaku Motor Co., Ltd.) The ratio of each of the prepared glass 2, 3 and the glass transition temperature and yield temperature was determined. And the coefficient of thermal expansion is shown in Table 2. 1618Sl.doc -20- 201243873 [Table 2] Table 2 Glass P205 (mo IX) B203 (motX) AI203 CmoIX) BaO (mol%) SnO (moIX) Glass transition temperature Tg (•C) Yield temperature (•c) Thermal expansion coefficient (i〇rc) Specific gravity (g/cc) Glass transition temperature ro 2 55 15 __e_ 30 0 46Θ .611 113 3.13 1250 3 AQ 7 10 10 25 442 iii~ 88 3.25 1100 (Experiment to determine the relationship between the amount of glass 2 and 3 and the characteristics of the powder magnetic core and thermal stability) Fe77 at%Cn at%P9.23 at%c2.2 at which water atomization method is used %B7, 7 at% Sim at% is a mixture of amorphous soft magnetic alloy powder, polyoxin, zinc stearate, powdered glass 2 or powdered glass 3 to form a mixture. Here, as shown in Table 2, the glass transition temperature (Tg) of the glass 2 (phosphoric acid glass) is 468 ° C, which is 2 ° lower than the temperature (470 ° C) of the heat treatment performed in the manufacturing process of the powder magnetic core. C. Further, the glass transition temperature of the glass 3 (phosphoric acid glass) was 442 ° C, which was lower than the temperature (470 ° C) of the heat treatment performed in the manufacturing step of the powder magnetic core. (In addition, the blending amount of the polyoxyl resin in the mixture is 2.0 wt% with respect to the mass of the soft magnetic powder, and the blending amount of zinc stearate is 0.3 wt% with respect to the mass of the soft magnetic powder. The blending amount of 3 is 0 wt%, 0.1 wt%, 0.3 wt%, 0.6 wt% with respect to the mass of the soft magnetic powder. Then, the above mixture is filled into a mold, and pressure forming is carried out under a bearing pressure of 147 MPa. A ring-shaped sample having an outer diameter of 20 mm x an inner diameter of 12 mm x a thickness of 68 mm was prepared, and the obtained ring-shaped sample was heat-treated at 470 ° C for 1 hour in a nitrogen gas atmosphere to prepare a powder magnetic core. 16I851.doc 201243873 Calculate the density of the magnetic core according to the mass and external dimensions of the obtained annular powder core. The calculation of the occupancy of the soft magnetic powder is carried out using the value of the blending amount. The calculation formula of the soft magnetic powder is as follows [Formula 2] The possession of soft magnetic powder Bi = __ powder core density after heat treatment _ soft magnetic powder density X < l + 0.02xa + glass mass + NiZn iron 氡 at mass a - = - powder magnetic powder before heat treatment Core quality _ heat-treated powder core y amount of zinc stearate 5·_ heat Pre-treatment powder core quality><_Breakfast zinc quality _ soft magnetic powder»Quantity + vitreous 4+NiZn ferrite "Quality + zinc stearate quality and then use super insulation meter (DKK-TOA manufacturing) SM-8213) Measure the intrinsic resistance of the ring-shaped powder core, wind the copper wire on the ring-shaped powder core, and measure the initial permeability using an impedance analyzer (HP 4192A), using BH Analyzer (made by Iwasaki Communications). The iron loss was measured under the conditions of frequency 1 〇〇 kHz and Bm = 100 mT. In the heat resistance test, the annular powder magnetic core was placed in a drying oven at 200 ° C and 250 ° C for 1000 hours in the atmosphere. After that, the initial magnetic permeability and the iron loss were measured. The results of the respective measurements are shown in Table 3. [Table 3] Table 3 Powder Core No. Phosphate Phosphate Tg Phosphate Phosphate Added Initial Magnetic Permeability at 100 kHz 100 kHz '100 mT T donation (kW/m>) Intrinsic resistance (Ω-cm) Magnetic powder is estimated to have a string (°/〇) 200·〇1000 hours After the heat test, the initial magnetic 4 牟 changes 牟250β初始200hCx)000 after the 1000-hour resistance test, the iron loss after the heat test is completed 250*0x1000 Variation of iron loss after heat resistance test 8 - ΟΜΧ 4θ.&10ι4 405i14 4.47Xlrf 80 -ex -12» SO% 60K 9 468^ aiwtx 4θ^ΐα4 ΕΠΤ57Ί mtm 492X1^ 80 -ex -m 49% 66X 10 4β8*0 aswtx ftBflXlrf 80 •m -13% 69« 68X Π 4 oil” aewt& 47,β士αε rrvmn nrnri 1t.1X1〇P 79 -4% 80% m% 12 442ΧΪ aiwtx 47.9±ae 78 -Μ - W ma〇K 13 Ai2X> Q3wtX mrrri mrem 4A1X10* 80 -e% (10) 6〇x 14 λΑίΧ) aewtx txnxicfi 78 -2Χ -a* 44« 50% It should be noted that the powder core No. shown in Table 3 9 to 11 using glass 2, powder magnetic core No 12 to 14 using glass 3 » powder magnetic core No. 8 is a previous example of no added glass. Figure 6 shows the initial magnetic permeability (initial) and iron loss (initial) and glass 2, 3 of the powder magnetic core shown in Table 3 with the glass transition temperature (Tg) shown in Table 3 as -22-161851.doc 201243873 A diagram of the relationship between the added quantities. It can be seen that in the case of using any kind of glass, the initial magnetic permeability tends to decrease slightly as the amount of glass added increases. 'The initial magnetic permeability when the glass addition amount is 〇·6 wt% and the No. 8 (previous example) decreased by about 2 to 4%. Further, as shown in Table 3 and FIG. 6, when the iron loss (initial) is 2, it is reduced as the amount of addition of the glass 2 is increased, and in the case of using the glass 3, The amount of addition of the glass 3 is increased to show a substantially fixed value. By using the glass transition temperature (Tg) as compared with the manufacturing process of the powder magnetic core, the heat treatment temperature is 2 to 28 tons lower than that of the glass 2, 3, when wt% ~ 〇 6 wt / is added. In the case of glass 2 and 3, the initial magnetic permeability of the powder magnetic core is equal or slightly lower than that in the case where no glass is added, and the iron loss is equal or slightly increased (may be reduced) compared with the case where no glass is added. . The increase in the specific resistance shown in Table 3 with respect to the increase in the amount of addition of the glasses 2 and 3 is small, and any sample is shown to be 1〇6 Ω·επι or more, and it is understood that the inherent resistance of the powder magnetic body is A sufficiently high value as a powder magnetic core. In addition, the occupation rate of the amorphous soft magnetic powder occupying the powder magnetic core is 78 to 80%. FIG. 7 is not separately added with the glass transition temperature (Tg) of Table 3 as the glass 2, and the glass transition temperature ( 1^) is 442. Each of the powder cores of the glass 3 is at 200. A graph showing the relationship between the amount of addition of the glasses 2 and 3 and the rate of change (%) of the initial magnetic permeability after 1000 hours & 25 〇〇 Cxl 〇〇〇 hours. The initial magnetic permeability after adding 20 〇t:x looo hours of glass powder of glass 16185I.doc -23· 201243873 glass 2 is reduced to about -11% when the addition amount of glass 2 reaches 0.3 wt%. However, when the addition amount of the glass 2 is set to 0.6 wt°/〇, the rate of change of the initial magnetic permeability is _4%e, and the powder magnetic core of the glass 2 is added after 25 〇 ° CX for 1 hour. The rate of change of the initial magnetic permeability shows a substantially fixed value of about 丨3% regardless of the amount of addition of the glass 2. On the other hand, the rate of change of the initial magnetic permeability of the powder magnetic core to which the glass 3 is added decreases as the amount of glass added increases. When the glass of 3 wt% is added, the rate of change of the initial magnetic permeability is 2〇〇 It is _2% after X1 〇〇〇 hours, and -80/〇 after 250° 〇 1000 hours. Fig. 8 shows each of the powder magnetic cores of the glass 2 having a glass transition temperature (Tg) of 468 〇c and the glass 3 having a glass transition temperature (Tg) of 442 ° C added thereto at 200 ° C for 1,000 hours. A graph showing the relationship between the amount of addition of the glasses 2 and 3 and the rate of change in iron loss (%) after 1000 hours at 250 ° C. As shown in Table 3 and FIG. 8, the iron loss change rate after the addition of the powder magnetic core of the glass 2 at 200 ° C < 1000 hours and after 250 ° 〇 1000 hours is uniform as the amount of the glass 2 is increased. The increase in the iron loss rate when adding 0.6 wt% of glass 2 was +80% and +138%, respectively. On the other hand, 200 of the powder magnetic core of the glass 3 was added. 〇 1000 hours later and 250. The change rate of iron loss after 1000 hours is smaller than the increase of the addition amount of glass 3, which is +44% and +58%, respectively. From this, it can be seen that the initial magnetic permeability (initial) can be set to the same extent as in the case where no glass is added (N〇.8) by adding the amounts of the glasses 2 and 3 to 〇1 to 0.6 wt%. And can improve the thermal stability of the initial magnetic permeability (heat-resistant special 1618Sl.doc -24- 201243873). In addition, the iron loss (initial) is approximately equal to the previous example (No. 8). Small is below the previous example (No. 8). The paired glass 1 is compared with the glasses 2 and 3, and the glass transition (Tg) of the glass 1 is 280 ° C, which is 200 低 lower than the heat treatment a temperature (470 ° C) which is carried out in the manufacturing process of the powder magnetic core. C or so, but the glass transition temperature (Tg) of the glass furnaces 2 and 3 is only 2 to 28 ° C lower than the heat temperature (470 ° C) implemented in the manufacturing steps of the powder magnetic core. In addition, when the glass 1 is used for a powder magnetic core, the rate of change of the initial magnetic permeability after 1000 hours of 1000 ° C can be suppressed to be low, but the initial magnetic permeability is likely to be greatly reduced. tendency. In addition, when the glass 2 and 3 are used for the powder magnetic core, the initial magnetic permeability (initial) can be equivalent to the case where no glass is added, and not only 18 (Γ(>ι〇) After 〇〇 hours, the rate of change of the initial magnetic permeability after 250 ° 〇 1000 hours can also be suppressed to be low. It is understood that as the glass for the powder magnetic core, glass 2, 3 is used as compared with the glass 1 It is preferable in terms of thermal stability of high initial magnetic permeability. (Experiment of composite addition of glass and magnetic microparticles) Fe77 at%Cn at%P9 23 at%c2 2 at%B7 7 at % Sh.87 at% is an amorphous soft magnetic alloy powder, a polyoxynized resin 'zinc stearate, and a NiZn ferrite powder (magnetic fine particles) are mixed to form a mixture. The NiZn ferrite powder is made of Kawasaki iron. The manufactured kN1-106GMs was dried by a ball mill for 30 hours and then dried. Further, Fe77 at%Cri at%P9 23 at%C2 2 heart B7.7 at%Si2.87 at which was produced by water atomization method % amorphous soft magnetic alloy powder, polyoxynoxy resin, 161851.doc -25· 201243873 Zinc stearate, NiZn ferrite The bulk powder and the glass 2 or the glass 3 are separately mixed to form a mixture. In addition, the blending amount of the polyoxyl resin in the mixture is 2.0 wt% with respect to the mass of the soft magnetic powder, and the amount of stearic acid is relatively soft. The mass of the magnetic powder is 〇·3 wt%, and the amount of the NiZn iron strontium powder is 0.3%, 0.6%, 1.2 wt% with respect to the mass of the soft magnetic powder, and the blending amount of the glass 2, 3 is relative to the soft magnetic powder. The masses are 〇%, 0.1% '0.3%, 0.6 wt0/〇. Then 'fill the mixture into the mold' and pressurize the pressure 丨47〇MPa to make the outer diameter 20 mmx inner diameter 12 mmx thickness a ring-shaped sample of 6.8 mm. The obtained ring-shaped sample was heat-treated at 47 ° C for 1 hour in a nitrogen gas flow environment to make a powder magnetic core. According to the quality of the obtained annular powder core And the outer dimensions of the core are calculated, and the occupancy of the amorphous soft magnetic alloy powder is calculated using the value of the blending amount (see Equation 2). In addition, a superinsulator (SM-8213 manufactured by dkk t〇a) is used. Determination of the inherent resistance of the annular powder core, on the ring powder Copper wire wound core, initial permeability was measured using an impedance analyzer (Hp 4192A), using BH Analyzei • (manufactured by Iwasaki Communications) frequency 1〇〇 let out,

The iron loss was measured under the condition of Bm = 100 mT. In the heat resistance test, the annular powder magnetic core was placed in the atmosphere (in a drying oven of TC, 25 〇t) to measure the initial magnetic permeability and iron loss after 1000 hours. The results of the measurements are shown in Table 4. Shown in. 161851.doc • 26 - 201243873 [Table 4] Table 4

Calendar powder magnetic name Να phosphoric acid glass 瑀Tg phosphoric acid glass addition 〇 Ni NiZn ferrite initial magnetic permeability at 100 kHz 100 kHz '100 ml T iron fingers; kW / m3) inherent resistance (Ω · αη) magnetic powder Occupancy (%) 200β〇χ1〇〇〇hour change rate of initial magnetic permeability after heat test 250°〇1〇〇〇Change of initial magnetic enthalpy after heat resistance test 200eC><1000 hours Change rate of paper loss after heat resistance test 1 250eCx1000, change of iron loss after heat resistance test 牟15 - (MX 4β stone soil 0.4 <06±14 4.47Xltf 80 -βχ -12Jt 60X m 16 - Owts ( X3你祖0土05 472±Π 2.00Xttf 79 -ex -Η»他BOX 17 - (XwtX 0.6'AtX 60.0±0A 497±H £30X10* 79 -m -m 41X 78» 18 - OwtX l^wtX 503 ±07 C59±25 eBBXltf 70 -m -m $X 94λ 19 468% OilwtX 0.6KtX 士04 4βθ±2ύ 232X10® I 79 -11« -ΙδΧ \ 45X S7X 20 aswtx o.ewtv 47.0 ± 0.2 I 4.10X16* 79 ! -« -15« m 6dX 21 Shed aewtK a6wt% mrm <75 士15 SMX\& 70 t* -11* m 133X 77 arvrtK Ο,ΰνΜ rnran mm Γδ2&±9 7β -7* •12% " 2 43( 23 OjOlhtX mtrm usxtrf 78 -m ZA% 11%. 24 «2*0 0.6MX O.0MK rfxnm ΠΤΠΠΙ 1ΛβΧ1^ 78 •ΛΑ% 29% T6S Figure 9 shows the powder core No. 15~18 (add The relationship between the amount of addition of NiZn ferrite in NiZn ferrite and non-added glass, initial permeability (initial) and iron loss (initial). Powder core No. 15 does not contain glass and The previous examples of both NiZn ferrites show that the initial magnetic permeability (initial) and iron loss (initial) of the powder magnetic core increase as the amount of NiZn ferrite added increases. Fig. 10 shows the pressure. When the powder core No. 15~18 (with NiZn ferrite added, no glass added) is exposed to heat resistance test at 200 ° C and 25 ° C for 1 〇〇〇 hours, the amount of NiZn ferrite added is A graph of the relationship between the rate of change of initial permeability and the rate of change in iron loss. As the addition amount of NiZn ferrite increases, the rate of change of the initial magnetic permeability is negative and the absolute value gradually becomes larger. When the amount of NiZn ferrite added is 1.2 wt%, after 200 ° 〇 1000 hours, 250 ° C >< -12%, -18% after 1 hour. The rate of change of iron loss monotonously decreases in the heat resistance test at 200 ° C. In the heat resistance test at 250 ° C, the rate of change in iron loss begins to decrease after the maximum value of 0.3 wt % of NiZn ferrite is added, when NiZn iron When the amount of the oxygen added was 1.2 wt%, it was +6% and +34%, respectively. -27- 161851.doc 201243873 The diagram shows the amount of glass 2, 3 added to the powder core No. 19~24 (with NiZn ferrite, glass 2, 3) and the initial permeability of the powder core. A graph of the relationship between the rate (initial) and the iron loss (initial). Glass 3 is added to the powder magnetic core N〇. i 9 to 21, and glass 3 is added to the powder magnetic core Νο· 21 to 24. Further, as shown in Table 4, in the powder magnetic core ν 〇 19 to 24, the addition amount of NiZn ferrite was 0.6 wt%. In addition, the initial magnetic permeability (initial) and the iron loss (initial) when the amounts of the glasses 2 and 3 added in FIG. 11 are 〇wt% are the powder magnetic cores in which the NiZn ferrite is set to 〇6 wt%. The value of 17. As can be seen from Fig. 11 and Table 4, the initial magnetic permeability tends to decrease slightly as the amount of addition of the glasses 2, 3 increases, but the amount of addition of the glass 2'3 is 0.1 wt. /. Then, the initial magnetic permeability can be improved as compared with the powder core No. 15 (previous example) in which no glass is added and ferrite is used. On the other hand, the iron loss (initial) does not depend on the addition amount of the glass 2, 3, and shows a substantially solid value, but by adding the glass 2, with respect to the powder magnetic core 17 (the glass addition amount is 0 wt%), There is a tendency that the iron loss (initial) is slightly decreased by the addition of the glass 3' with respect to the powder magnetic core N〇17 (the glass addition amount is 〇Wt%). Figure U shows the 20 〇txl〇〇〇 and 25〇β (: χΐ〇〇〇 hour heat resistance test) for the powder magnetic core N〇19~24 (with Nizn ferrite and glass 2, 3 added) Figure f, the relationship between the amount of glass added and the rate of change of the initial permeability. Furthermore, the amount of glass 2 and 3 added in Figure 12 is the initial permeability of 〇wt%;;"The history rate is NlZn The ferrite is set to a value of 6·6 wt% of the powder magnetic core N〇j 7. 161851.doc •28· 201243873 According to Fig. 12 and Table 4, 20 (rCxi〇〇〇 hour initial magnetic) The rate of change of the conductivity is negative, but the absolute value decreases as the amount of glass 2 increases. Wherein, when the glass 3 is added, the initial permeability is when the amount is 0.3 to 0.6 wt%. The rate of change of the rate remains almost unchanged at 3%. Then, according to the circle 12 and Table 4, the rate of change of the initial permeability after 25 〇tx 1 〇〇〇 is negative, but In the case of the glass 2, as the amount of glass added increases, the rate of change of the initial magnetic permeability (absolute value) gradually decreases. On the other hand, although the addition of the glass 3 is at the beginning The rate of change of the initial permeability is also shown to be negative, but the rate of change of the initial permeability C is absolute compared to the case where no glass is added (the powder core N〇17). The rate of change of the initial magnetic permeability at 3 o'clock does not change much even if the amount of glass added changes. Fig. 13 shows that the powder magnetic core Νο· 19~24 (added state ferrite, glass 2, 3) is implemented 200t. And 25 (TCxl000 hours of heat resistance test, the relationship between the amount of glass added and the rate of change of iron loss. In addition, the change rate of iron loss when the addition amount of glass 2 and 3 in Fig. 13 is 〇wt% is NiZn iron. The oxygen content is set to a value of 0.6 wt% of the powder magnetic core N 〇 17. The iron loss change rate is 2 在 at the heat resistance test temperature. (: and 25 (the rc shows substantially the same tendency. In the case, even if the addition amount is increased to 0.3 wt%, the iron loss change rate is substantially the same, and when the addition amount is increased to 0.6 wt%, the rate of change of iron loss increases. On the other hand, it is known that the case of adding glass 3 is added. When the amount of addition is 〇1 wt%, the rate of change of iron loss can be minimized. If the amount of addition is further increased, iron I6 L851.doc • 29· 201243873 The rate of change of loss increases. According to Table 4 and Figure! i $圃咖铁氧, it is relatively clear that 'by adding composite glass and one, it can ensure the initial permeability of the south. Rate (initial), and the thermal stability of the conductivity, seven can also reduce the rate of change of iron loss T: Ask the thermal stability of the iron loss. Especially the glass with the glass transition temperature g · '', 442 C 3 powder magnetic core (especially powder magnetic core No. 22, medium 'can effectively reduce the rate of change of iron loss, from the heat of the loss of heat. As described above, in the case where the amount of f of the soft magnetic powder is greater than or equal to the amount of Glf, and the mass of the soft magnetic powder is added, the amount of magnetic fine particles added is set. It is not the first time relative to the soft magnetic powder < Buy 1 is greater than 〇 mass % 〇 · 6 mass% or less. (Experimental experiment on the characteristics of each of the powder magnetic cores of the respective glass compositions) The production of various types of glass having the following glass compositions was produced. [Table 5] Table 5

-, 77. There is no shortage of specific adjustments. Pre-mixing the amount of raw materials in the rabbit's hanging ’. Put it into platinum. 16l85I.doc -30· 201243873 Then use an electric stove to smear it in the atmosphere. The temperature of the electric furnace was set to 1000 to 1300 ° C. Then, the platinum was taken out from the electric furnace, and the glass melt was cast in an iron mold to obtain glass. The glass was coarsely pulverized in a mortar, and then pulverized using a ball mill to obtain a glass frit powder. In addition, a glass piece of 3 mm x 3 匪 x 20 mm was cut out from one part of the cast glass, and after annealing to eliminate the strain, the glass transition temperature and the glass softening temperature (yield) were measured using a thermomechanical analysis device (TMA831Q manufactured by Rigaku Motor Co., Ltd.). Temperature) and coefficient of thermal expansion. The blending amount of each of the produced glass 4 18 and the glass transition temperature, the glass softening temperature (yield temperature), and the thermal expansion coefficient are shown in Table 5. In addition, the specific gravity and the glass transition temperature are also included in Table 5. Then, each of the glass 'amorphous soft magnetic alloy powders shown in Table 5, the polyoxynium tree day, and hard hard zinc citrate or the like were mixed to prepare a mixture. The non-magnetic magnetic alloy powder used was F one produced by a water atomization method.丨(4) P9_23 at%C2'2 at%B7 7 “%” (10) is an amorphous soft magnetic alloy powder. In addition, the blending amount of the polyoxyl resin in the mixture is 2% by weight based on the mass of the soft magnetic powder, and the amount of zinc stearate is 0.3 wt% relative to the mass of the soft magnetic powder. The blending amount was 0.6 wt% with respect to the mass of the soft magnetic powder. Then, the mixture was filled into a mold and subjected to a pressure of 1470 MPa to form a ring-shaped sample having an outer diameter of 20 mm x an inner diameter of 12 mm x a thickness of 6·8 mm. The obtained ring-shaped sample was heat-treated at 470 C for 1 hour in an on-line air flow environment to prepare a powder magnetic core. 161851.doc •31 · 201243873 In the experiment, the copper wire was wound around a ring-shaped powder core, and the initial permeability was measured using an impedance analyzer (HP 4192A) using a BH Analyzer (made by Iwasaki Communications) at a frequency of 1 kHz. Iron loss was measured under conditions of Bm = 100 mT. In the heat resistance test, the annular powder magnetic core was placed in a drying oven at 2 ° C or 250 ° C in the atmosphere, and the initial magnetic permeability and iron loss after 1 hour were measured. Further, the compressive force is applied to the powder magnetic core, and the compressive force when the powder magnetic core is damaged is taken as the maximum strength of the iron core. The results of each measurement are shown in Table 6. [Table 6] Table 6 2003⁄4 250®C No. Break 4: 0.6 wtH Tg (3⁄4) or (x 10- 7/^) (IQOkH z) αα : 100 kHz 100 mT) After 1000H μ. After 1000h « α 200*1: · 1000 h after the change of μ· half 200X, lOOOMft «MX 9 Φ max OOOkH z) AH ; 100 kHz 100 mT) 1000 h After the implant I·I000h iron loss 230*C * 1000h After the W's rate of 150 Χ, «1000 卜后铁«的8化毕25 to add 0 0 46.S 399 46.2 014 -4.7% 54« 0.112 46.3 414 43.5 703 -9.S* 70% 26 4 526 02 46.2 420 4S.1 Θ18 -2.4% 47« 0.104 4β>5 469 42.9 715 -7.6X 56« 27 δ 376 ”0 45.8 435 4S.0 644 -2.0R 48« o.tu 43.7 46Q 41.4 ate 77% 28 6 427 111 47.6 399 46.0 577 -3.4% m 0.0Θ5 4fi.O 420 42.5 792 -11.5% β9Χ 20 7 446 92 47.7 390 4β.1 614 -3.4% 58% 0.100 47.6 421 42.2 &1& -11.4% d4X 30 β 87 4S.Q AZS 46.6 589 -2.ΘΧ 38» 0.092 AB2 460 42.8 785 -11.3% 71Χ 31 9 401 95 ΑΊΑ 423 4β·1 698 -3.2» 41X 0.090 47Λ 435 42.1 βοο -11.8* 84Χ 32 10 441 94 48.6 397 47.1 5βθ ·3_Μ m 0.094 4δ·5 423 43.0 790 -11.4* 87Χ 33 1t 2 9a 46.9 391 47Λ 567 -3.6Χ 4S% 0.100 48.7 414 42.7 787 -\2Ά 90Κ $4 12 410 ΘΘ 385 47.7 57Β -ao« 601⁄4 0Ό8Θ Α6Λ 419 43.0 799 91Χ 35 13 437 63 47.8 379 4θ·3 6β& -2.7 1⁄4 50% 0,101 48.0 387 41.8 821 1121⁄4 36 14 443 101 48.4 381 4β.7 549 -3.4% 44% 0.095 4Θ·3 3&3 42.7 S03 -13.6% 110% 37 16 86 4β.7 360 47J 545 -2. W 51% 0.0 4 4β^ 372 42.4 7Θ3 -13·2« 38 16 45^ ee 4β.7 425 462 5Θ8 -1.1« 41% 0.085 46.6 433 41.4 787 -11 Λ* 82« 39 17 463 137 47.4 431 4β. 7 602 -1.4« AO% 0^87 47Λ 445 42.8 771 -10.0* 733⁄4 40 18 513 124 47.6 451 46丨Θ42 -1.6« ΛΆ 0.113 472 468 __4Μ 799 -ΠΛ 711⁄4 The glass barrier shown in Table 6 and Table 5 The glass No corresponds. In addition, in Table 6, the values of "μ' (1 〇〇 kHz)" and "iron loss (100 kHz, 100 mT)" at 200 ° C and 25 0 ° C are initial values. In Table 6, the values of the initial values of the same powder magnetic core No. are slightly different. They are measured by using other powder magnetic cores produced under the same conditions, and each of the powder magnetic cores is used for measurement. The rate of change of each value after maintaining for 1 hour at each temperature of 200 ° C and 250 ° C. Fig. 14 is a graph showing the initial magnetic conductance of each of the powder magnetic cores shown in the column of 200 °C of Table 6. • 32·161851.doc 201243873 Rate (initial). In Fig. 14, the glass transition temperature of the glass added to each of the powder magnetic cores is taken as the horizontal axis, and the thermal expansion coefficient α of the glass is taken as the vertical axis. Therefore, the experimental results of the powder magnetic core of the prior example in which no glass was added were excluded from Fig. 14. Further, Fig. 15 is a graph showing the iron loss (initial) of each of the powder magnetic cores shown in the block of 200 °C. In Fig. 15, the glass transition temperature Tg of the glass added to each of the powder magnetic cores is taken as the horizontal axis, and the thermal expansion coefficient α of the glass is taken as the vertical axis. Therefore, Fig. 15 does not contain the results of the inspection of the powder magnetic core of the prior art in which no glass was added. In addition, Fig. 16 shows the rate of change of the initial magnetic permeability of each of the powder magnetic bodies shown in Table 6 (200 C, 1000 hours). Fig. 17 shows the rate of change of iron loss with each of the powder magnetic cores (2〇〇t , 1 hour) diagram of the relationship. In Fig. 16 and Fig. 17, the glass transition temperature Tg of the glass added to each of the powder magnetic cores is defined as the horizontal axis, and the thermal expansion coefficient of the glass (1 is the vertical axis. Therefore, FIG. 16 and FIG. Experimental results of the powder magnetic core of the previous example in which no glass was added. First, since the heat treatment temperature of each of the powder magnetic cores of the compression molding table 6 was set to 470 ° C, a glass transition temperature higher than 4701 was added ( The glass powder cores of T g) are all comparative examples. In Fig. 14 to Fig. 17, a line of glass transition temperature (Tg) of 470 ° C is drawn. The portion on the right side of the line is a comparative example. 6. The experimental results of FIG. 14 and FIG. 16 show that by making the glass transition temperature (Tg) of the glass lower than 470 ° C, a relatively high initial magnetic permeability (initial) can be obtained and the previous example (not added) The glass) can effectively reduce the rate of change (absolute value) of the initial magnetic permeability. Thus, according to the present embodiment, I61851.doc • 33-201243873 can effectively improve the thermal stability of the initial magnetic permeability. The glass transition temperature (Tg) of the glass is preferably 360 ° C or higher. 'The thermal expansion coefficient α of glass (χ1〇·7厂C) is preferably 6〇~11〇, or 60~90. By this, the absolute value of the rate of change of the initial permeability can be more effectively reduced. It is known that in the present embodiment, the rate of change (absolute value) of the initial magnetic permeability after 200 hours (in 1000 hours) can be suppressed to 4% or less, preferably 3% or less. Further, it is within 2%, and more preferably within 1.5%. Further, for the iron loss, the glass transition temperature (Tg) of the glass is 36 〇t: or more and less than 470 t, whereby the thermal stability can be improved. BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a perspective view of a powder magnetic core (iron core) Fig. 2 is a plan view showing a coil-sealed powder magnetic core. Fig. 3 is a partially enlarged sectional view showing a powder magnetic core according to an embodiment of the present invention ( Fig. 4 is a graph showing the correlation between the initial magnetic permeability (initial) and the iron loss (initial) of the powder magnetic core to which the glass transition temperature (Tg) is 28 (rc) is added and the amount of glass added. Fig. 5 is a view showing heating of a powder magnetic core to which glass 1 having a glass transition temperature (Tg) of 28 〇t > Degree is set to i 8 〇. 〇 and 25 〇 1. When the heating time is set to 1000 hours in the heat resistance test, 'the rate of change (%) of the initial magnetic permeability after the thermal test and the amount of change in iron loss (%) and glass Fig. 6 shows the initial 161851.doc -34· 201243873 magnetic powder (initial) and iron loss (initial) and broken glass added with the addition of glass 2 and glass 3 respectively. Fig. 7 is a graph showing the heat-heating test in which the heating temperature is set to 200X: and 250t for the powder magnetic core to which the glass 2 and the glass 3 are respectively added, and the heating time is set to 〇〇〇 〇〇〇 hours. , a graph showing the correlation between the rate of change (%) of the initial magnetic permeability after the heat resistance test and the amount of glass added. Fig. 8 is a view showing the heat resistance test when the heating temperature is set to 200t: and 250t, and the heating time is set to 1 hour for the powder magnetic core to which the glass 2 and the glass 3 are respectively added. Fig. 9 shows the initial magnetic permeability (initial) of the powder magnetic core to which the NiZn ferrite is added (but no glass is added). And the correlation between the iron loss (initial) and the amount of ferrite added in Fig. 211. Fig. 10 shows that the heating temperature is set to 2 for the powder magnetic core to which the NiZn ferrite is added (but no glass is added). (TC and 250 ° C, heating time set to 1000 hours of heat resistance test, the rate of change (%) of the initial permeability after the thermal test and the rate of change of iron loss (%) and the amount of NiZn ferrite added Fig. 11 is a graph showing the relationship between the initial magnetic permeability (initial) and the iron loss (initial) and the amount of glass added in the powder magnetic core of the NiZn ferrite composited with glass 2 and glass 3 added in combination. Figure 12 shows the powder core with glass 2 and glass 3 and NiZn ferrite added to the composite. A graph showing the correlation between the rate of change (%) of the initial magnetic permeability after the heat resistance test and the amount of glass added in the heat resistance test in which the heating temperature is 2 〇〇 ° c and 250 ° C and the heating time is 1000 hours. 161851.doc •35- 201243873 Fig. 13 shows that the powder magnetic core to which the glass 2, the glass 3 and the NiZn ferrite are added is heated to 200 ° C and 250 ° C, and the heating time is set to 1000 hours. In the heat resistance test, the relationship between the rate of change in iron loss (°/〇) after the heat resistance test and the amount of glass added. Fig. 14 is a graph showing the glass transition temperature of glass in a plurality of powder magnetic cores containing glass. Fig. 15 is a graph showing the relationship between the thermal expansion coefficient of glass and the initial magnetic permeability (initial). Fig. 15 is a graph showing the relationship between the glass transition degree of glass, the thermal expansion coefficient of glass, and the iron loss (initial) in a plurality of powder magnetic cores containing glass. Fig. 16 shows that the glass transition temperature of the glass is the horizontal axis and the thermal expansion coefficient of the glass is the vertical axis. The heating temperature of the plurality of powder magnetic cores containing glass is set to 200 ° C, and the heating time is set to 1. Hourly hour of heat test Figure 17 is a graph showing the rate of change (%) of the initial permeability after the heat resistance test. Fig. 17 shows the glass transition temperature of the glass as the horizontal axis and the thermal expansion coefficient of the glass as the vertical axis. A diagram showing the rate of change (%) of the iron loss after the heat resistance test in the heat resistance test in which the heating temperature is set to the surface time and the heating time is set. [Main component symbol description] 1. 3 Powder magnetic core 2 Coil sealed powder Core 4 Coil 5 Soft magnetic powder 6 Insulation bonding material 7 Pore 161851.doc -36·

Claims (1)

201243873 VII. Patent application scope: 1. A powder magnetic core, which is obtained by compression-molding a mixture containing a soft magnetic powder and an insulating bonding material and performing heat treatment. The above insulating bonding material Containing a binder resin and glass, the glass transition temperature (Tg) of the above glass is lower than the temperature of the above heat treatment. 2. The powder magnetic core of claim 1, wherein the content of the glass is greater than or equal to or greater than the mass of the soft magnetic powder. / 〇 below the range. 3. The powder magnetic core of claim 2, wherein the glass system comprises at least P2〇5, B2〇3 and BaO, and the composition ratio of p2〇5 is 40~60 mol% 'B2〇3 composition ratio b is 2 to 20 mol%, and the composition ratio of BaO is 5 to 45 mol. /. The composition ratio d of SnO is 0 to 45 mol%, and the composition ratio of Al2〇3 is 0 to 15 mol% ' and satisfies the relationship of a+b+c+d+e$100%. 4. The powder magnetic core of claim 3, wherein the composition ratio e of Al2〇3 is 2 to 15 mol%. 5. The powder magnetic core of claim 3 or 4, wherein the composition ratio f of Li20 is 0 to 1 mol ° /. , the composition ratio of Ce02 is 0~10 mol%, the composition ratio i of Ti02 is 0~1 mol%, and the relationship of a+b+c + d+e+f+g+h+i=100 mol% is satisfied. . 6. The powder magnetic core of claim 3 or 4, wherein the glass transition temperature (Tg) of the glass is in the range of 280 ° C to 470 ° C. 7. The powder magnetic core of claim 3, wherein the glass transition temperature of the glass is 161851.doc 201243873 (Tg) is above 36 ° C and below 47 〇 t. 8. The powder magnetic core of claim 3, wherein the glass has a thermal expansion coefficient of 60 to 110 (χ 1 〇 * 7 / ° c ) 〇 9 · The powder magnetic core of claim 3, wherein the thermal expansion of the glass The coefficient is 60~90 (χ 1 ο·7/.). 10. The powder magnetic core of claim 1, wherein the insulating adhesive material comprises the glass and magnetic fine particles having a particle diameter smaller than the soft magnetic powder. 11. The powder magnetic core of claim 10, wherein the content of the magnetic fine particles is in a range of more than 〇% by mass and not more than 〇6 〇% by mass relative to the mass of the soft magnetic powder. 12. The powder magnetic core of claim 10, wherein the magnetic fine particles are oxide magnetic materials. 13. The powder magnetic core of claim 1 wherein said oxide magnetic material is at least one of NiZn ferrite or MnZn ferrite. A method for producing a powder magnetic core, comprising: a step of mixing a soft magnetic powder, a binder resin as an insulating bonding material, and a glass powder to form a mixture; and compressing the upper (tetra) compound into %, The heat treatment step is carried out at a heat treatment temperature higher than the glass transition temperature (Tg) of the above glass powder. 1618Sl.doc