WO2017170901A1 - Noyau de poussière recouvert d'un isolant à base de silicium, procédé de fabrication associé et composant de circuit électromagnétique - Google Patents

Noyau de poussière recouvert d'un isolant à base de silicium, procédé de fabrication associé et composant de circuit électromagnétique Download PDF

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WO2017170901A1
WO2017170901A1 PCT/JP2017/013329 JP2017013329W WO2017170901A1 WO 2017170901 A1 WO2017170901 A1 WO 2017170901A1 JP 2017013329 W JP2017013329 W JP 2017013329W WO 2017170901 A1 WO2017170901 A1 WO 2017170901A1
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Prior art keywords
silica
powder
soft magnetic
coated
grain boundary
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PCT/JP2017/013329
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English (en)
Japanese (ja)
Inventor
裕明 池田
五十嵐　和則
Original Assignee
三菱マテリアル株式会社
株式会社ダイヤメット
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Priority claimed from JP2017066237A external-priority patent/JP6832774B2/ja
Application filed by 三菱マテリアル株式会社, 株式会社ダイヤメット filed Critical 三菱マテリアル株式会社
Priority to EP17775435.5A priority Critical patent/EP3441989A4/fr
Priority to US16/089,052 priority patent/US11183321B2/en
Priority to CN201780015882.0A priority patent/CN108701519B/zh
Publication of WO2017170901A1 publication Critical patent/WO2017170901A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/16—Metallic particles coated with a non-metal
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/147—Alloys characterised by their composition
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F27/00—Details of transformers or inductances, in general
    • H01F27/24—Magnetic cores
    • H01F27/255—Magnetic cores made from particles
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets

Definitions

  • the powder magnetic core after forming a phosphate coating on the surface of the soft magnetic powder, a silicone resin is added and mixed as a binder, and then the silicone resin-coated soft magnetic powder is compression-molded and heat-treated.
  • This powder magnetic core (composite soft magnetic material) has a structure in which soft magnetic powder particles are bonded via a silicone resin coating, and the insulation between the soft magnetic powder particles is ensured by the resin coating layer. Loss can be suppressed.
  • the surface of the phosphate-coated iron powder is subjected to a primer treatment, and then the fluororesin powder is added to and mixed with the iron powder after the primer treatment.
  • electromagnetic components for electronic devices are required to have better material properties, and have become necessary to be electromagnetic components that do not cause problems in actual use conditions.
  • the dust core produced by using the mixed powder in which the soft magnetic powder is covered with an insulating resin typified by silicone resin is likely to have insufficient heat resistance,
  • the specific resistance cannot be sufficiently high.
  • the insulating resin deteriorates, so that it is difficult to satisfactorily insulate the soft magnetic powder particles, and there is a problem that the specific resistance is lowered.
  • electromagnetic circuit component of the present invention is characterized by comprising the silica-based insulating coated dust core described above. If it is the electromagnetic circuit component of this invention which consists of the above-mentioned silica type insulation coating powder magnetic core, it can provide the electromagnetic circuit component which is excellent in heat resistance, high intensity
  • the present invention there is a structure in which a plurality of Fe-based soft magnetic powder particles are joined via a grain boundary layer made of a silica-based insulating film, and the grain boundary layer is composed of an oxide of Fe and Si or Fe and Si.
  • the powder magnetic core is composed of a composite oxide and contains Fe diffused from soft magnetic powder particles in the grain boundary layer, so that the grain boundary layer is firmly bonded to the soft magnetic powder particles and has excellent heat resistance.
  • the grain boundary layer covering the soft magnetic powder particles is an individual oxide or composite oxide of Fe and Si, and is excellent in insulation even after being subjected to high-temperature heat treatment. Can provide magnetic core.
  • the expansion schematic diagram which shows the structure
  • the perspective view which shows an example which applied the silica type insulation coating powder magnetic core which concerns on this invention to the reactor core.
  • Explanatory drawing which shows an example of the process for manufacturing the silica type insulation coating powder magnetic core which concerns on this invention.
  • the solvent 15 such as IPA (2-propanol) is heated to a temperature of about 25 to 50 ° C. and the solvent is kept for about 2 to 12 hours.
  • the silicone resin 16 is dissolved in the solvent 15 with stirring (dissolution step).
  • TEOS tetraethoxysilane: Si (OC 2 H 5 ) 4
  • the temperature when TEOS 17 is mixed with the solvent 15 may be room temperature, but it may be heated to a temperature range similar to that when the silicone resin 16 is dissolved.
  • hydrochloric acid 18 and water 19 as acid catalysts are added to the solvent, and then at 25 to 50 ° C., for example, 35 ° C. for 4 hours or more, for example, 4 to 24 Stir for about an hour (catalyst addition step).
  • hydrochloric acid 18 By adding hydrochloric acid 18, the hydrolysis reaction proceeds preferentially and the condensation polymerization reaction proceeds.
  • the acid catalyst used here nitric acid, acetic acid, formic acid, phosphoric acid and the like can be used in addition to hydrochloric acid.
  • the sol-gel coating solution 20 can be obtained as shown in FIGS. 3 and 4D.
  • the sol-gel coating solution 20 is in a state in which fine particles of silicone resin that cannot be visually observed are dispersed in a liquid in which TEOS is added to a solvent.
  • the soft magnetic powder 21 with a phosphate film is put into a fluid mixer such as a Henschel mixer and the outer periphery of the soft magnetic powder has a predetermined thickness.
  • the coating liquid 20 is applied (application step 22).
  • the soft magnetic powder 21 used in the coating step 22 may be the soft magnetic powder 21 not provided with the phosphate coating 13, and the phosphate coating 13 may be omitted.
  • the heating temperature at the time of mixing is set to 85 ° C. to 105 ° C., for example, 95 ° C. After the mixing is completed under reduced pressure, the mixture is heated at a temperature of about 175 to 250 ° C., for example, about 200 ° C.
  • the coating liquid is dried, and a molding coating powder having a structure in which the outer periphery of the soft magnetic powder is covered with a dry film of the coating liquid can be obtained (drying step 23).
  • drying step 23 When drying at a temperature of less than 175 ° C. during the drying, the drying time is long, so the production efficiency is poor, and when drying at a temperature of more than 250 ° C., the film tends to crack.
  • the obtained molded body is subjected to a temperature range of 500 ° C. to 900 ° C., for example, 650 ° C. for several tens of minutes to several hours, for example, 30 minutes in a non-oxidizing atmosphere such as a vacuum atmosphere or a nitrogen gas atmosphere.
  • the target dust core A having a structure in which the soft magnetic powder particles 11 made of a plurality of soft magnetic powders are joined together by the grain boundary layer 12 can be obtained by the heat treatment step 26 in which heating is performed to a certain degree.
  • the powder magnetic core A obtained by the manufacturing method described above is prepared by sufficiently dissolving a silicone resin in the above-described solvent and compacting a dried coating liquid in which TEOS is sufficiently dispersed.
  • a grain boundary layer 12 having a structure in which Fe is diffused in a complex oxide of Si is generated, Due to the grain boundary layer 12, it is possible to obtain a powder magnetic core A having high strength in which the soft magnetic powder particles 11 are firmly joined. In addition, it has confirmed that Fe was diffused inside the grain boundary layer 12 from the analysis of the Example sample mentioned later. Further, if the soft magnetic powder particles 11 are surrounded by the grain boundary layer 12, the periphery of the soft magnetic powder particles 11 can be increased even if the temperature is raised to a high temperature of 500 ° C. to 650 ° C.
  • the grain boundary layer 12 includes a base layer 12a in which C is contained in an individual oxide of Fe and Si or a composite oxide of Fe and Si, and a SiO 2 rich spot-like or non-dispersed material dispersed in the grain boundary layer 12. It is composed of regular fine particles 12b.
  • the SiO 2 rich fine particles 12b are in the C low concentration region from the distribution state of C in FIG. 7 showing the test results of Examples described later.
  • SiO 2 rich particulates 12b as described in detail in the examples below, the grain boundary layer, the acceleration voltage 1 kV, 50000 times the SiO 2 rich patchy or irregular shapes can be seen in SEM reflection electron image of the observation conditions Fine particles.
  • the SiO 2 rich fine particles 12b are preferably included in the range of 0.2 to 50 area% with respect to the entire area of the grain boundary layer 12 in the visual field during observation.
  • the proportion of the SiO 2 rich fine particles 12b existing in the grain boundary layer 12 is less than 0.2 area% (average value)
  • the compact shrinks during the heat treatment process Even if there are few insulation coating defects (Fe exposed portions), there is a possibility that it is impossible to prevent the Fe exposed portions on the surface of the soft magnetic powder particles from contacting and conducting. That is, since the specific resistance of the silica-based insulating coating powder magnetic core A may be lowered, it is not preferable that the ratio of the SiO 2 rich fine particles 12b is less than 0.2 area% (average value).
  • a plurality of SiO 2 rich fine particles 12b are present in the silica-based insulating coating on the surface of the silica-based insulating coated iron powder. Even if the green compact shrinks during the heat treatment in the nitrogen atmosphere between the iron powders in the green compact (compression-molded silica-based insulating iron powder) structure, a proper distance is maintained through the grain boundary layer 12. I keep it. By this, even if there are only a few Fe exposed parts on the surface of the silica-based insulating coated iron powder, it can be estimated that the effect of preventing conduction due to the contact between the iron powders in the Fe exposed parts can be obtained. .
  • the present invention can be applied to various electromagnetic circuit components such as a motor core, an actuator core, a transformer core, a choke core, a magnetic sensor core, a noise filter core, a switching power supply core, and a DC / DC converter core.
  • electromagnetic circuit components such as a motor core, an actuator core, a transformer core, a choke core, a magnetic sensor core, a noise filter core, a switching power supply core, and a DC / DC converter core.
  • An iron phosphate-coated iron powder or a pure iron powder prepared by applying iron phosphate coating to pure iron powder having an average particle size of 50 ⁇ m (D50) was prepared.
  • a molding raw material mixed powder for producing an example was produced according to the following steps.
  • Second embodiment containing 300 g of iron phosphate-coated pure iron powder (soft magnetic powder) with a TEOS-derived SiO 2 film thickness of 33.8 nm and 0.41% by mass as a silicone resin in the coating solution with respect to the soft magnetic powder.
  • a molding raw material mixed powder for production or for production of the third example was produced according to the following steps.
  • Example 4 containing TEOS-derived SiO 2 film thickness of 67.5 nm with respect to 300 g of the iron phosphate-coated pure iron powder (soft magnetic powder) and 0.54% by mass as the silicone resin in the coating liquid with respect to the soft magnetic powder.
  • a molding raw material mixed powder for production was produced according to the following steps.
  • the silicone resin in these silica sol-gel coating solutions is 0.20% by mass (for producing the first example), 0.41% by mass (for producing the second and third examples), 0.54 with respect to the iron powder. It is set to mass% (for manufacturing the fourth embodiment) and 0.41 mass% (for manufacturing the fifth embodiment).
  • a silicone resin having a particle size of 1 mm or less was used.
  • the film thickness of the SiO 2 coating derived from the TEOS sol-gel coating solution is calculated from the following formula using the specific surface area (measured value by the BET three-point method) and SiO 2 density (physical property value of crystal 2.65 g / cm 3 ). did.
  • SiO 2 film thickness (nm) TEOS substance amount (mol) ⁇ SiO 2 atomic weight (g / mol) / SiO 2 density (g / cm 3 ) / specific surface area of soft magnetic powder (m 2 / g) / Soft magnetic powder weight (g) (*)
  • ⁇ (H 2 O mass) (TEOS mass / (208.33 g / mol (TEOS atomic weight))) ⁇ 2 ⁇ 18.016 g / mol (molecular weight of H 2 O)
  • the silica sol-gel coating solution was applied to the iron phosphate-coated iron powder or pure iron powder using a Henschel mixer.
  • Example 3 0.18% by mass of a silicone resin powder is added to the silica sol-gel coated iron powder for production, and 0.6% by mass of a wax-based lubricant is added to the soft magnetic powder. A powder was obtained.
  • Example 4 Addition of 0.03% by mass of silicone resin powder to silica sol-gel coated iron powder for preparation, and addition of 0.4% by mass of wax-based lubricant to soft magnetic powder, mixing raw materials of Example 4 A powder was obtained.
  • Example 5 0.18% by mass of a silicone resin powder is added to the silica sol-gel coated iron powder for preparation, and 0.6% by mass of a wax-based lubricant is added to the soft magnetic powder. A powder was obtained.
  • the magnetic flux density (magnetic field 10 kA / m), specific resistance ( ⁇ m), magnetic flux density 0.1 T, iron loss (W / kg) at a frequency of 10 kHz, and bending strength ( MPa).
  • the average value (at%) of Fe existing in the grain boundary layer was also measured.
  • the magnetic flux density at 10 kA / m was measured with a BH tracer (DC magnetization measuring device B integration unit TYPE 3257 manufactured by Yokogawa Electric Corporation) using a ring-shaped sample.
  • the iron loss at 0.1 T and a frequency of 10 kHz was measured with a BH analyzer (AC magnetic property measuring apparatus SY-8218 manufactured by Iwatatsu Measurement Co., Ltd.) using a ring-shaped sample.
  • the above results are shown in Table 1 below.
  • the value of Fe existing in the grain boundary layer is an average value of the analysis values at 10 locations.
  • the TEM analysis result of Example 3 described later is shown as a specific example, and the values of Fe existing in the grain boundary layers shown in other examples and comparative examples are subjected to elemental analysis at 10 locations. Refers to the average value. Therefore, in Example 3, the (average) value of Fe existing in the grain boundary layer is 0.60 at%. In Examples 1 to 5, the Fe content in the grain boundary layer was in the range of 0.4 to 5.7 at%. Focusing particularly on Examples 3 and 5 with the same magnetic flux density at 10 kA / m and the same coating liquid composition, the bending strength of the dust core tends to improve as the Fe content increases. Was confirmed.
  • FIG. 5 is a photograph showing a result (SEM secondary electron image) of a partial cross-sectional structure of soft magnetic particles including the grain boundary layer of the powder magnetic core of Example 3 described above observed at a low acceleration voltage with a field emission scanning electron microscope. It is. Moreover, FIG. 6 shows the photograph of the SEM reflected electron image about the same visual field of the sample.
  • the SEM was analyzed using Carl Zeiss Ultra 55, EDS software: Noran System Seven, observation conditions: acceleration voltage 1 kV, EDS surface analysis conditions: acceleration voltage 4 kV, current amount 1 nA, WD 3 mm.
  • a thin iron phosphate coating is formed on the peripheral surface of the soft magnetic powder particles, and a grain boundary layer is formed between adjacent soft magnetic powder particles.
  • the grain boundary layer of this embodiment in the visual field of FIGS. 5 and 6 given as an example has a thickness of about 1 to 2 ⁇ m.
  • a substantially elliptical shading pattern having a maximum diameter of about 0.5 ⁇ m is dispersed in the grain boundary layers. 5 and 6, the light and shade pattern substantially elliptical region was a region having a low C concentration and SiO 2 rich fine particles from the analysis results described later.
  • FIGS. 7 to 11 are diagrams showing the results of EDS surface analysis of the SEM observation region of the example sample shown in FIGS. 7 shows the abundance ratio of C
  • FIG. 8 shows the abundance ratio of O
  • FIG. 9 shows the abundance ratio of Si
  • FIG. 10 shows the abundance ratio of Fe
  • FIG. 11 shows the abundance ratio of P.
  • the C concentration in the substantially elliptical region in the grain boundary layer is lower than the other portions. From this, it was found that the substantially elliptical region in the grain boundary layer shown in FIGS. 5 and 6 is a region having a lower C concentration than other portions.
  • FIG. 8 shows no characteristic in the oxygen distribution
  • FIG. 9 shows no particular characteristics in the Si distribution.
  • FIG. 8 shows no characteristic in the oxygen distribution
  • FIG. 9 shows no particular characteristics in the Si distribution.
  • FIG. 12 shows the bright field observation result by STEM (scanning transmission electron microscope) of the magnetic powder particles cut out from the sample of Example 3 described above by the FIB (focused ion beam apparatus) processing and the surrounding grain boundary layer portion.
  • STEM scanning transmission electron microscope
  • a carbon vapor deposition layer for preparing an observation sample is formed above the arrow indicated as the outermost surface.
  • the round black region clearly designated as iron powder is soft magnetic powder particles, and the gray portion surrounding the outer periphery of the soft magnetic powder particles corresponds to the grain boundary layer.
  • EDS analysis was performed on each part of the rectangular region specified by reference numerals 1, 2, 3, 4, and 5.
  • the sample was similarly cut out from the other part of the sample of Example 3, and the result of bright field observation by STEM is shown in FIG.
  • EDS analysis was performed on the rectangular region portions designated by reference numerals 6, 7, 8, 9, and 10.
  • the STEM was analyzed using FTI's Titan G2 ChemiSTEM, EDS software: Quantax Esprit under observation conditions: acceleration voltage 200 kV.
  • FIB SMI3050TB manufactured by Seiko Instruments Inc. was used, and a sample for analysis was prepared under processing conditions: gallium ion 30 kV.
  • FIG. 14 shows the result of analyzing the region indicated by reference numeral 1 of the sample shown in FIG. As a result of dividing the rectangular region on the lower side of FIG. 14 and conducting elemental analysis in this compartment, at%, O: 57.17%, Si: 41.86%, Fe: 0.97%, iron Was confirmed.
  • FIG. 15 shows the result of analyzing the region indicated by reference numeral 2 of the sample shown in FIG. As shown in FIG. 15, most of the rectangular region excluding the upper end portion was partitioned, and as a result of elemental analysis in this partition, O: 65.36%, Si: 33.94%, P: 0.20% at at%. , S: 0.05%, Fe: 0.44%, and the presence of iron could be confirmed.
  • FIG. 20 shows the result of analyzing the region indicated by reference numeral 7 in the sample shown in FIG. As a result of dividing a rectangular region showing about 2/3 of the portion excluding the upper part of FIG. 20 and performing elemental analysis in this partition, O: 68.79%, Si: 29.69%, S: at%. The presence of iron was confirmed by 0.07%, Cl: 0.08%, and Fe: 1.37%.
  • FIG. 21 shows the result of analyzing the region indicated by reference numeral 8 of the sample shown in FIG. As a result of dividing a rectangular region showing a portion of about 2/3 excluding the upper part of FIG. 21 and performing elemental analysis in this compartment, O: 68.26%, Si: 31.36%, Fe: It was 0.38%, and the presence of iron could be confirmed.
  • FIG. 22 shows the result of analyzing the region indicated by reference numeral 9 in the sample shown in FIG. As a result of dividing a rectangular region showing a portion of about 2/3 excluding the upper part of FIG. 22 and performing elemental analysis in this compartment, O: 70.08%, Si: 29.47%, Fe: The presence of iron was confirmed to be 0.44%.
  • FIG. 23 shows the result of analyzing the region indicated by reference numeral 10 in the sample shown in FIG. As a result of dividing a rectangular region showing a portion of about 2/3 excluding the upper part of FIG. 23 and performing elemental analysis in this compartment, O: 70.31%, Si: 29.04%, Fe: The presence of iron was confirmed by 0.58%, Zr: 0.05%, and Sn: 0.02%.
  • FIG. 24 shows silica sol-gel-coated iron powder obtained by heating and drying the iron phosphate-coated iron powder coated with the sol-gel coating solution prepared in Example 4 in the air at 200 ° C. for 0.5 hour. It is a SEM enlarged photograph of. The magnification was set to 2000 ⁇ , and the magnification was such that one silica sol-gel-coated iron powder would fill the SEM image.
  • FIG. 25 shows an SEM image after this silica sol-gel coated iron powder is subjected to a heat treatment of heating to 650 ° C. for 30 minutes in a reduced pressure inert gas atmosphere.
  • FIG. 26 shows a conventional silicone obtained by adding only a silicone resin to a solvent instead of the sol-gel coating solution used in Example 4 and omitting the addition of TEOS, water, and hydrochloric acid, and the other steps were performed through the same steps.
  • Resin-coated iron powder FIG. 27 shows an ESEM image of the coated iron powder after the temperature was raised in a vacuum inert gas atmosphere using the ESEM described above and held at 650 ° C. for 30 minutes. A change appears so that the state of an outer peripheral surface can be discriminate
  • the generation of a large number of fine crystals of iron oxide on the outer peripheral surface of pure iron soft magnetic powder in this way means that there are a large number of defects in the silicone resin film covering the soft magnetic powder of pure iron,
  • the number of iron oxide microcrystals is considered to correspond to the number of defects present in the film before the temperature rise. Since the number of defects present in the film before the temperature rise cannot be analyzed by a general analysis method, the temperature rise can be determined by grasping the number of iron oxide microcrystals produced during the temperature rise process in a vacuum inert gas atmosphere. The number of defects present in the previous film can be estimated.
  • the specific resistance of the powder magnetic core made of soft magnetic powder particles having this film is greatly reduced because the film having a large amount of iron oxide microcrystal precipitates has many defects existing in the film before the temperature rise. it can. For this reason, since almost no precipitation of iron oxide microcrystals is observed in the silica sol-gel coated iron powder after the temperature rise shown in FIG. 25, the silica sol-gel coated iron powder before the temperature rise is compacted to form a grain boundary.
  • the powder magnetic core obtained by firing together with the layer is less likely to cause a decrease in specific resistance even when heated to about 650 ° C. Therefore, the powder magnetic core of the present invention has excellent heat resistance. I understand that.
  • FIG. 28 shows an enlarged photograph of a partial cross-sectional structure of the silica-based insulation-coated powder magnetic core of Example 1, and a part of the grain boundary layer was 50,000 times at a low acceleration voltage (1 kV) using a field emission scanning electron microscope. Shows a backscattered electron image taken at.
  • this sample uses 0.09% of the raw material mixture powder for molding containing 16.9 nm as the thickness of the TEOS-derived SiO 2 film and 0.2% by mass as the silicone resin in the coating liquid with respect to the soft magnetic powder. It is a sample to which silicone resin powder was added afterwards. Presence of small spot-like SiO 2 rich fine particles can be confirmed in a very small part of the grain boundary layer.
  • FIG. 29 shows an enlarged photograph of a partial cross-sectional structure of the silica-based insulating coated powder magnetic core of Example 3, and a part of the grain boundary layer was 50,000 times at a low acceleration voltage (1 kV) using a field emission scanning electron microscope. Shows a backscattered electron image taken at.
  • this sample uses 0.18% of the raw material mixture powder for molding containing 33.8 nm as the thickness of the TEOS-derived SiO 2 film and 0.18% by mass as the silicone resin in the coating liquid with respect to the soft magnetic powder. It is a sample to which silicone resin powder was added afterwards. Presence of various small and large SiO 2 -rich fine particles having an elliptical spot shape can be confirmed in many parts of the grain boundary layer.
  • FIG. 30 shows an enlarged photograph of a partial cross-sectional structure of the silica-based insulating coated powder magnetic core of Example 5, and a part of the grain boundary layer was photographed with a field emission scanning electron microscope at a low acceleration voltage (1 kV). A reflected electron image of 50000 times is shown.
  • this sample uses 0.18% of the raw material mixture powder for molding containing 33.8 nm as the thickness of the TEOS-derived SiO 2 film and 0.41% by mass as the silicone resin in the coating liquid with respect to the soft magnetic powder. It is a sample to which silicone resin powder was added afterwards. Presence of various small and large SiO 2 rich fine particles having an irregular shape so as to occupy a large part of the grain boundary layer can be confirmed.
  • the proportions of the SiO 2 rich fine particles in the grain boundary layer of the samples of Examples 1 to 5 and Comparative Examples 1 and 2 described above were determined by the following method.
  • a reflected electron image obtained by photographing a part of the grain boundary layer with a field emission scanning electron microscope at a low acceleration voltage (1 kV) at a magnification of 50000 times with respect to the cross-sectional structure of the silica-based insulating coated powder magnetic core is binarized to form The area ratio of 2 rich fine particles was calculated.
  • image analysis was performed on 10 fields of the reflected electron images taken at 50000 times.
  • the area ratio of the SiO 2 rich fine particles to the total area of the grain boundary layer was averaged by dividing the area ratio of the SiO 2 rich fine particles by the number of fields of view to obtain the average value of the area ratio of the SiO 2 rich fine particles to the area of the entire grain boundary layer.
  • the average value of the area ratio of the SiO 2 rich fine particles to the total area of the grain boundary layer was as follows. Example 1 (0.26 area%). Example 2 (32.6 area%). Example 3 (26.4 area%). Example 4 (48.4 area%). Example 5 (37.6 area%). Comparative example 1 (0.00 area%). Comparative Example 2 (4.2 area%).
  • ⁇ Left and right can be easily selected using a switch attached to the housing, and can be applied.
  • a Powder magnetic core 11 Soft magnetic powder particles 12 Grain boundary layer 12a Base layer 12b SiO 2 rich fine particles 13 Phosphate coating (undercoat) 14 Reactor (Electromagnetic circuit parts) 14a Reactor door 14b Coil part

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Abstract

La présente invention concerne un noyau de poussière recouvert d'un isolant à base de silice, le noyau de poussière étant caractérisé par une structure dans laquelle des particules de poudre magnétique douce à base de Fe, possédant des surfaces recouvertes de films isolants à base de silice, sont liées par des couches limites de grains composées de la pluralité de films isolants à base de silice, les couches limites de grains contenant du Fe diffusé à partir des particules de poudre magnétique douce à base de Fe et contenant des oxydes de Fe et Si, ou un oxyde composite de Fe et de Si.
PCT/JP2017/013329 2016-03-31 2017-03-30 Noyau de poussière recouvert d'un isolant à base de silicium, procédé de fabrication associé et composant de circuit électromagnétique WO2017170901A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
EP17775435.5A EP3441989A4 (fr) 2016-03-31 2017-03-30 Noyau de poussière recouvert d'un isolant à base de silicium, procédé de fabrication associé et composant de circuit électromagnétique
US16/089,052 US11183321B2 (en) 2016-03-31 2017-03-30 Powder magnetic core with silica-based insulating film, method of producing the same, and electromagnetic circuit component
CN201780015882.0A CN108701519B (zh) 2016-03-31 2017-03-30 二氧化硅系绝缘包覆压粉磁芯及其制造方法和电磁电路部件

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Application Number Priority Date Filing Date Title
JP2016-073636 2016-03-31
JP2016073636 2016-03-31
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CN110828108A (zh) * 2018-08-09 2020-02-21 太阳诱电株式会社 含金属磁性粒子的磁性基体和含该磁性基体的电子部件
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CN110246651A (zh) * 2018-03-09 2019-09-17 Tdk株式会社 软磁性金属粉末、压粉磁芯及磁性部件
CN110246651B (zh) * 2018-03-09 2021-04-06 Tdk株式会社 软磁性金属粉末、压粉磁芯及磁性部件
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