WO2017022594A1 - 軟磁性材料およびその製造方法 - Google Patents
軟磁性材料およびその製造方法 Download PDFInfo
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- WO2017022594A1 WO2017022594A1 PCT/JP2016/072053 JP2016072053W WO2017022594A1 WO 2017022594 A1 WO2017022594 A1 WO 2017022594A1 JP 2016072053 W JP2016072053 W JP 2016072053W WO 2017022594 A1 WO2017022594 A1 WO 2017022594A1
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- soft magnetic
- magnetic powder
- alloy
- heat treatment
- powder
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Images
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Definitions
- the present invention relates to a soft magnetic material and a manufacturing method thereof.
- Soft magnetic powder having an amorphous structure is widely used in applications such as magnetic core (core) materials for coil parts used in electronic equipment.
- core magnetic core
- a method for producing a soft magnetic powder for example, by rapidly cooling a molten alloy to form a ribbon-like or powder-like quenching body having an amorphous phase as a main phase, the quenching body is subjected to a heat treatment to be crystallized.
- a method for producing an Fe-based soft magnetic alloy in which fine grains are formed by precipitating crystal grains having an average crystal grain size of 50 nm or less containing at least Fe, wherein the quenching body is higher than the crystallization start temperature and substantially contains the compound phase.
- Patent Document 1 A method for producing an Fe-based soft magnetic alloy is known in which a heat treatment for heating to a temperature at which it is not formed is performed at least twice (Patent Document 1).
- Patent Document 1 when producing a microcrystalline alloy (nanocrystalline alloy), the influence of self-heating is reduced by optimizing the heat treatment conditions for precipitating the microcrystals.
- the present invention provides a soft magnetic alloy having excellent characteristics, low loss, and low coercive force.
- An object of the present invention is to provide a soft magnetic powder in which small-sized nanocrystals are formed at a high density, which has excellent soft magnetic properties, and a method for producing the same.
- the inventors have subjected the alloy powder obtained by cooling the molten metal of the mother alloy to at least two heat treatments, and the highest temperature in the first heat treatment and the highest in the second heat treatment. It is found that by setting the temperature to an appropriate value, small-sized nanocrystals can be formed at high density, and a soft magnetic powder having excellent soft magnetic properties can be obtained, and the present invention is completed. It came.
- a soft magnetic powder comprising particles having a plurality of crystallites and an amorphous phase existing around the crystallites,
- the average particle size of the crystallites is 30 nm or less
- the average thickness of the amorphous phase is 30 nm or less
- the average Fe concentration in the amorphous phase is lower than the average Fe concentration in the crystallite in a region where the depth from the particle surface is 0.2 r or more and 0.4 r or less.
- the maximum temperature T1 in the first heat treatment is a temperature at which the Avrami constant is 1.7 or more, and the maximum temperature T2 in the second heat treatment is a temperature lower than T1
- a method is provided wherein the degree of crystallinity as measured by powder X-ray diffraction is less than 20% in the alloy powder after the first heat treatment and greater than 20% in the soft magnetic powder after the second heat treatment.
- a magnetic core formed of a composite material containing the above-mentioned soft magnetic powder and a resin.
- the above-mentioned soft magnetic powder and a resin are mixed, and the resulting mixture is molded to obtain a molded body; And a step of heating the molded body.
- a coil component including the above-described magnetic core and a coil conductor wound around the magnetic core.
- a coil component including a magnetic body portion including a composite material containing the above-described soft magnetic powder and a resin as a main component, and a coil conductor embedded in the magnetic body portion.
- the soft magnetic powder according to the present invention has excellent soft magnetic properties due to the above configuration.
- the method for producing a soft magnetic powder according to the present invention can produce a soft magnetic powder in which small-sized nanocrystals are formed at a high density, and can obtain a soft magnetic powder having excellent soft magnetic properties. it can.
- the soft magnetic powder according to the present invention as a magnetic core material, a coil component having excellent magnetic characteristics can be obtained.
- FIG. 1 is a diagram schematically showing a crystallite and an amorphous phase in a soft magnetic powder according to an embodiment of the present invention.
- FIG. 2 is a diagram for explaining an X-ray diffraction pattern analysis method.
- the soft magnetic powder according to one embodiment of the present invention includes particles having a plurality of crystallites and an amorphous phase existing around the crystallites.
- FIG. 1 shows a schematic diagram of crystallites and an amorphous phase contained in soft magnetic powder.
- the average particle size of the crystallites contained in the soft magnetic powder according to the present embodiment is 30 nm or less.
- the average grain size of the crystallites may be 2 nm or more.
- the average thickness of the amorphous phase contained in the soft magnetic powder according to this embodiment is 30 nm or less.
- the average thickness of the amorphous phase may be 1 nm or more.
- the “amorphous phase thickness” means the thickness of the amorphous phase existing between adjacent crystallites.
- the average thickness of the amorphous phase can be determined from a TEM photograph. Specifically, in the TEM photograph of the soft magnetic powder, r is the minor axis of the cross section of the particle contained in the soft magnetic powder, and the depth from the surface of the particle is arbitrarily in the region of 0.2r to 0.4r.
- the boundary between the crystal phase of one crystallite and the surrounding amorphous phase, the crystal phase of the crystallite adjacent to the one crystallite, and the surrounding amorphous phase Measure the length of the line connecting the boundary of Let the average value of the length of this line segment be the average thickness of an amorphous phase.
- the soft magnetic powder according to the present embodiment Since the average particle size of the crystallites contained in the soft magnetic powder and the average thickness of the amorphous phase are within the above ranges, the soft magnetic powder according to the present embodiment has nano-sized crystallites present at a high density. Therefore, it has high soft magnetic properties. Therefore, when the soft magnetic powder according to the present embodiment is used as a magnetic core material, a coil component having high magnetic characteristics can be obtained. Specifically, core loss can be reduced, and high magnetic permeability and high saturation magnetic flux density can be achieved.
- the average Fe concentration in the amorphous phase and the crystallite can be obtained by combining TEM measurement and energy dispersive X-ray analysis (EDS). Specifically, in the TEM photograph of the soft magnetic powder, r is the minor axis of the cross section of the particle contained in the soft magnetic powder, and the depth from the surface of the particle is arbitrarily in the region of 0.2r to 0.4r.
- the Fe concentration at the center of the crystallite is obtained by EDS measurement, and the average value is taken as the average Fe concentration in the crystallite.
- the Fe at the midpoint of the line segment connecting the boundary between the crystal phase of the crystallite and the surrounding amorphous phase and the boundary between the crystal phase of the crystallite adjacent to the crystallite and the surrounding amorphous phase at the shortest is determined by EDS measurement, and the average value is defined as the average Fe concentration in the amorphous phase.
- the ratio of the average Fe concentration in the amorphous phase to the average Fe concentration in the crystallite is 0.90 or less. It is preferable. When the ratio of the average Fe concentration is 0.90 or less, the Fe concentration in the crystallite increases, and as a result, the saturation magnetic flux density increases.
- the degree of crystallinity of the soft magnetic powder is preferably greater than 20%, more preferably 30% or more. When the crystallinity of the soft magnetic powder is 30% or more, the soft magnetic characteristics can be further improved.
- the crystallinity of the soft magnetic powder can be measured by a method described below by a powder X-ray diffraction method.
- FIG. 2 is a schematic diagram for explaining an X-ray diffraction pattern analysis method.
- a crystal peak indicating a body-centered cubic structure is indicated by P
- a crystal peak indicating a low symmetry crystal structure is indicated by P2
- a halo region indicating amorphous property is indicated by H. It is.
- the crystallinity can be calculated by using the following formula (3) based on the X-ray diffraction spectrum of the soft magnetic powder.
- X ⁇ Ic / (Ic + Ic ′ + Ia) ⁇ ⁇ 100 (3)
- Ic area of crystal peak region showing body-centered cubic structure
- Ic ′ area of crystal peak region showing low symmetry crystal structure
- Ia showing amorphous property Hello area
- the crystal peak P showing a body-centered cubic structure is a peak in which the diffraction angle 2 ⁇ from the 110 plane of Fe is in the range of 44.5 ° to 45.5 °.
- the soft magnetic powder preferably contains a crystal phase mainly having a body-centered cubic structure.
- the crystal phase mainly has a body-centered cubic structure
- the soft magnetic characteristics are further improved.
- Whether or not the crystal phase mainly has a body-centered cubic structure can be evaluated by a powder X-ray diffraction method.
- the peak area ratio Y of the crystal peak showing a crystal structure with low symmetry can be expressed by the following formula (4).
- Y ⁇ Ic ′ / (Ic + Ic ′ + Ia) ⁇ ⁇ 100 (4)
- the value of Y is 1 or less, it can be considered that the crystal phase mainly has a body-centered cubic structure.
- the particles contained in the soft magnetic powder preferably contain an alloy composition represented by the general formula Fe a Si b B c P d Cu e M f C g Cr h .
- a part of Fe is substituted with at least one element of Ni and Co (that is, 0 ⁇ f ⁇ 12 in the above general formula).
- the magnetic properties can be further improved.
- a part of Fe is substituted with C (that is, 0 ⁇ g ⁇ 8 in the above general formula).
- C that is, 0 ⁇ g ⁇ 8 in the above general formula.
- a part of Fe is replaced with Cr (that is, 0 ⁇ h ⁇ 10 in the above general formula). Cr tends to be oxidized more easily than Fe. Therefore, when a part of Fe is replaced with Cr, Cr is preferentially oxidized, so that oxidation of Fe can be suppressed, and thereby deterioration of magnetic properties can be suppressed.
- the particles contained in the soft magnetic powder preferably include an alloy composition represented by the general formula Fe a ′ Si b ′ B c ′ P d ′ Cu e ′ M ′ f ′ .
- a ′, b ′, c ′, d ′, e ′ and f ′ are respectively 81 ⁇ (a ′ + f ′) ⁇ 86, 2 ⁇ b ′ ⁇ 8, 6 ⁇ c ′ ⁇ 10, 2 ⁇ d ′ ⁇ 5, 0.4 ⁇ e ′ ⁇ 1.4, 0.08 ⁇ e ′ / d ′ ⁇ 0.8, and 0 ⁇ f ′ ⁇ 3, and M ′ is Ti, Zr, Hf, Nb , Ta, Mo, W, Cr, Co, Ni, Al, Mn, Ag, Zn, Sn, As, Sb, Bi, Y, N, O and at least one element of rare earth elements.
- the method for producing a soft magnetic powder according to the present embodiment includes a step of cooling a molten metal of a mother alloy to obtain an alloy powder mainly composed of an amorphous phase, a step of subjecting the alloy powder to a first heat treatment, Subjecting the alloy powder subjected to the heat treatment to a second heat treatment to obtain a soft magnetic powder.
- a step of cooling a molten metal of a mother alloy to obtain an alloy powder mainly composed of an amorphous phase
- Subjecting the alloy powder subjected to the heat treatment to a second heat treatment to obtain a soft magnetic powder.
- the molten metal of the mother alloy is cooled to obtain an alloy powder mainly composed of an amorphous phase.
- the mother alloy is prepared by weighing raw materials such as Fe, Si, Fe—B alloy, Fe—P alloy, Cu, Ni, Co, C, Cr, etc. so as to have a predetermined alloy composition, and heating and melting above the melting point, The lysate can then be prepared by cooling.
- the master alloy preferably has a composition represented by the general formula Fe a Si b B c P d Cu e M f C g Cr h .
- the mother alloy has the above composition
- an amorphous phase can be stably formed, and a soft magnetic powder with higher soft magnetic properties can be obtained.
- the mother alloy having the above-described composition is suitable for pulverizing the molten mother alloy with a high-pressure gas flow in the production of the alloy powder described later.
- the master alloy preferably has a composition represented by the general formula Fe a ′ Si b ′ B c ′ P d ′ Cu e ′ M ′ f ′ .
- a ′, b ′, c ′, d ′, e ′ and f ′ are respectively 81 ⁇ (a ′ + f ′) ⁇ 86, 2 ⁇ b ′ ⁇ 8, 6 ⁇ c ′ ⁇ 10, 2 ⁇ d ′ ⁇ 5, 0.4 ⁇ e ′ ⁇ 1.4, 0.08 ⁇ e ′ / d ′ ⁇ 0.8, and 0 ⁇ f ′ ⁇ 3, and M ′ is Ti, Zr, Hf, Nb , Ta, Mo, W, Cr, Co, Ni, Al, Mn, Ag, Zn, Sn, As, Sb, Bi, Y, N, O and at least one element of rare earth elements.
- the mother alloy having the above composition is suitable for the case of pulverizing the molten metal of the mother alloy with a high-pressure water flow in the production of the alloy powder to be described later, or when pulverizing the molten metal of the mother alloy with a high-pressure gas flow and cooling with water. ing.
- the alloy powder mainly composed of an amorphous phase is obtained by cooling the molten metal of the mother alloy.
- the alloy powder can be produced, for example, by pulverizing a molten metal of the mother alloy with a high-pressure water flow or a high-pressure gas flow and cooling. That is, the alloy powder can be formed by spraying high-pressure water or high-pressure gas on the molten metal.
- the high pressure gas is a gas having a pressure of 1 MPa or more and 10 MPa.
- the mother alloy is crushed to a size of about 3 cm so as to be easily melted, it is put into a crucible of an atomizing device such as a gas atomizing device, and high frequency induction heating is performed to melt the mother alloy to obtain a molten metal.
- the inside of the atomizer is preferably set to an inert atmosphere such as an argon atmosphere.
- the molten alloy is pulverized by jetting a jet fluid (that is, a high-pressure water stream or a high-pressure gas stream) onto the molten metal, and cooled (rapidly cooled) to obtain an alloy powder mainly composed of an amorphous phase.
- argon gas, nitrogen gas, or the like can be used as the jet fluid. Cooling can be performed using a cooling medium such as water or gas.
- a gas for example, an inert gas such as argon gas or nitrogen gas is preferably used as the cooling medium.
- the alloy powder is subjected to a first heat treatment.
- the first heat treatment can be performed using a heating device such as an infrared heating device.
- the atmosphere in the heating device is preferably an inert gas atmosphere such as helium gas.
- the atmosphere in the heating device may be a mixed gas atmosphere in which hydrogen gas is added to helium gas. By adding hydrogen gas, oxidation of the metal element during heat treatment can be suppressed. Hydrogen gas may be added at about 3% in terms of partial pressure.
- the present inventors set the maximum temperature T1 in the first heat treatment to a temperature at which the Avrami constant is 1.7 or more, and set the maximum temperature T2 in the second heat treatment described later to a temperature lower than T1.
- the inventors have found that nano-sized fine crystallites can be formed with high density.
- the Avrami constant is a parameter indicating the mode of crystallization. The smaller the Avrami constant, the more difficult the crystallization proceeds, and the larger the Avrami constant, the easier the crystallization proceeds. When the degree of crystallinity is the same value, the larger the Avrami constant, the smaller the size of crystallites can be formed.
- the Avrami constant of the alloy powder can be determined by the procedure described below by differential scanning calorimetry (DSC).
- DSC differential scanning calorimetry
- the isothermal DSC measurement of the alloy powder (temperature increase rate 400 ° C./min, isothermal holding measurement time 60 minutes) is performed twice in an argon atmosphere. Since the alloy powder is completely crystallized by the first measurement, no exothermic reaction due to self-heating occurs in the second measurement.
- the calorific value of the alloy powder sample is calculated from the difference between the DSC curve obtained by the first measurement and the DSC curve obtained by the second measurement.
- the cumulative calorific value from the start of isothermal measurement is obtained as a function of time t.
- t isothermal holding time (seconds)
- the maximum value of the Avrami constant obtained in this way is set as the Avrami constant at each temperature.
- the maximum temperature T1 in the first heat treatment is set to a temperature at which the Avrami constant is 1.7 or more.
- the crystallinity of the alloy powder after the first heat treatment measured by powder X-ray diffraction, is 20% or less.
- the crystallinity after the first heat treatment is a relatively low value of 20% or less, the self-heating of the alloy powder in the first heat treatment can be suppressed.
- the crystallinity can be calculated by the above-mentioned formula (3) by powder X-ray diffraction method.
- the first heat treatment for a period of time not less than 0.01 when the crystallization reaction ratio is 0.01 or more and not more than a time when the crystallization reaction ratio is 0.4 or less.
- the time of the first heat treatment is within the above range, it is easy to set the crystallinity of the alloy powder after the first heat treatment to an appropriate value.
- the alloy powder subjected to the first heat treatment is subjected to the second heat treatment to obtain a soft magnetic powder.
- the second heat treatment can be performed using a heating device such as an infrared heating device. Note that the first heat treatment and the second heat treatment may be performed continuously in the same heating apparatus, or may be performed using different heating apparatuses.
- the atmosphere in the heating device is preferably an inert gas atmosphere such as argon gas.
- the maximum temperature T2 in the second heat treatment is set to a temperature lower than T1.
- the second heat treatment is preferably performed for 1 minute to 120 minutes, more preferably 5 minutes to 60 minutes.
- time of the second heat treatment is within the above range, a soft magnetic powder in which nano-sized fine crystallites are formed at a high density can be obtained, and the soft magnetic characteristics are further improved.
- the crystallinity of the soft magnetic powder after the second heat treatment is greater than 20%.
- a soft magnetic powder having excellent soft magnetic properties can be obtained.
- the magnetic core according to the present embodiment is formed of a composite material containing the soft magnetic powder according to the present invention and a resin.
- a resin for example, an epoxy resin, a phenol resin, a silicone resin, or the like can be used.
- the content of the soft magnetic powder in the composite material is preferably 60 vol% or more and 90 vol% or less. When the content of the soft magnetic powder is within the above range, a magnetic core having excellent magnetic properties can be obtained.
- the dimension and shape of the magnetic core are not particularly limited, and can be appropriately set according to the intended use.
- the magnetic core may be, for example, a toroidal core having an outer diameter of 13 mm, an inner diameter of 8 mm, and a thickness of 2.5 mm.
- the method of manufacturing a magnetic core according to the present embodiment includes a step of mixing the soft magnetic powder according to the present invention and a resin such as an epoxy resin, a phenol resin, and a silicone resin, and molding the resulting mixture to obtain a molded body, Heating the molded body.
- the molded body can be obtained, for example, by press molding a mixture containing soft magnetic powder and resin at a pressure of about 100 MPa.
- the size and shape of the molded body are not particularly limited, and can be appropriately set according to the desired size and shape of the magnetic core.
- the heating temperature of a molded object can be suitably set according to the kind etc. of resin to be used.
- the coil component according to this embodiment includes a magnetic core according to the present invention and a coil conductor wound around the magnetic core.
- the coil conductor can be formed by winding a metal wire such as a copper wire covered with enamel around a magnetic core. Since the coil component according to the present embodiment uses the soft magnetic powder according to the present invention as a magnetic core material, the coil component has excellent magnetic characteristics.
- the coil component according to the present embodiment is embedded in a magnetic body portion including as a main component a composite material containing the soft magnetic powder according to the present invention and a resin such as an epoxy resin, a phenol resin, or a silicone resin. Coil conductors. Since the coil component according to the present embodiment uses the soft magnetic powder according to the present invention as a magnetic core material, the coil component has excellent magnetic characteristics.
- the content of the soft magnetic powder in the composite material is preferably 60 vol% or more and 90 vol% or less. When the content of the soft magnetic powder is within the above range, the magnetic characteristics of the coil component can be further improved.
- the coil component according to the present embodiment can be manufactured, for example, according to the procedure described below.
- a plurality of composite material sheets are formed. And a coil conductor is arrange
- a coil component can be obtained by thermocompression bonding of the sheet with the coil conductor disposed between the sheets.
- the stator core of a motor can be formed using the soft magnetic powder of the present invention.
- a coil component in which a coil conductor is wound around an armature tooth, a rotor rotatably disposed inside the coil component, and a plurality of armature teeth are provided at equal intervals on the same circumference.
- a stator core Since the soft magnetic powder of the present invention has a high saturation magnetic flux density and low magnetic loss, it is possible to obtain a high-quality motor with low power loss by forming a stator core with the soft magnetic powder of the present invention. Become.
- the soft magnetic powders of Examples 1 to 37 were prepared according to the procedure described below.
- This mother alloy was crushed to a size of about 3 cm, put into a crucible of a gas atomizer, and melted by high frequency induction heating to obtain a molten metal.
- the atmosphere inside the gas atomizer was set to an argon atmosphere.
- an argon gas jet fluid was jetted into the molten metal, pulverized, and quenched with cooling water to obtain alloy powders of Examples 1 to 37.
- the alloy powders of Examples 1 to 16 and 18 to 37 were subjected to the first heat treatment using an infrared heating device.
- the maximum temperature in the first heat treatment was set to the temperatures shown in Tables 1, 4, 7, and 10.
- the atmosphere in the heating apparatus was set to a mixed gas atmosphere in which 3% hydrogen gas in terms of partial pressure was added to helium gas.
- the first heat treatment was performed for 10 seconds.
- the alloy powder of Example 17 was not subjected to the first heat treatment.
- crystal structure means the crystal structure of soft magnetic powder
- bcc means that the soft magnetic powder mainly has a body-centered cubic structure
- Bcc + lsp means that the soft magnetic powder has a low symmetric phase in addition to the body-centered cubic structure.
- TEM Transmission electron microscope
- n selected arbitrarily in the region where the depth from the surface of the particle is 0.2r to 0.4r, where r is the minor axis of the cross section of the particle contained in the soft magnetic powder.
- the average Fe concentration in the amorphous phase and crystallites was determined by TEM-EDS.
- n is selected arbitrarily in the region where the depth from the surface of the particle is 0.2r to 0.4r, where r is the minor axis of the cross section of the particle contained in the soft magnetic powder (n For the crystallites of ⁇ 5), the Fe concentration at the center of the crystallite was determined by EDS measurement, and the average value was taken as the average Fe concentration in the crystallite.
- the concentration was determined by EDS measurement, and the average value was taken as the average Fe concentration in the amorphous phase.
- the ratio of the average Fe concentration in the amorphous phase to the average Fe concentration in the crystallite shown as “Fe concentration ratio” in the table) was determined. The results are shown in Tables 2, 5, 8 and 11. In the soft magnetic powder of Example 17, no crystalline phase was detected, so the average Fe concentration in the crystallites could not be measured.
- coil parts were produced according to the procedure described below. First, 3 parts by weight of epoxy resin is added to 100 parts by weight of each sample (ratio of epoxy resin: 15 vol%), press-molded with a pressure of 100 MPa, an outer diameter of 13 mm, an inner diameter of 8 mm, and a thickness of 2.5 mm. A toroidal core was produced. Next, a copper wire with a wire diameter of 0.3 mm covered with enamel is placed on the outer periphery of the toroidal core so that the number of turns of the primary winding for excitation and the secondary winding for voltage detection are both 16. The coil parts of Examples 1 to 37 were manufactured by winding twice.
- the core loss (magnetic loss) of the coil component was measured at an applied magnetic field of 30 mT and a measurement frequency of 1 MHz, using a BH analyzer SY-8217 manufactured by Iwatsu Measurement Co., Ltd. The results are shown in Tables 2, 5, 8 and 11. In Tables 1 to 11, those marked with “*” are comparative examples.
- the coil component using the soft magnetic powder of Example 1 in which the maximum temperature T1 in the first heat treatment is set to a temperature where the Avrami constant is less than 1.7 is greater than 2000 kW / m 3 Has core loss. This is considered due to the fact that the average particle size of the crystallites present in the soft magnetic powder was larger than 30 nm.
- the coil parts using the soft magnetic powders of Examples 1, 2 and 16 whose crystallinity after the first heat treatment was greater than 20% had a core loss greater than 2000 kW / m 3 . This is considered due to the fact that the average particle size of the crystallites present in the soft magnetic powder was larger than 30 nm.
- the coil parts using the soft magnetic powders of Examples 8 to 10 in which the maximum temperature T2 in the second heat treatment was higher than the maximum temperature T1 in the first heat treatment had a core loss greater than 2000 kW / m 3 . This is considered due to the fact that the average particle size of the crystallites present in the soft magnetic powder was larger than 30 nm.
- Coil parts using the soft magnetic powders of Examples 14 and 15 whose crystallinity after the second heat treatment was less than 20% had a core loss greater than 2000 kW / m 3 . This is presumably because the average thickness of the amorphous phase present in the soft magnetic powder was larger than 30 nm.
- the coil component using the soft magnetic powder of Example 17 that was not subjected to the first and second heat treatments had a core loss greater than 2000 kW / m 3 . This is considered due to the fact that fine crystallites were not formed in the soft magnetic powder of Example 17.
- the coil components using the soft magnetic powders of Examples 3 to 7 and 11 to 13 had a core loss of 2000 kW / m 3 or less. This shows that the core loss was able to be reduced by using the soft magnetic powder according to the present invention.
- the coil component using the soft magnetic powder of Example 27 whose crystallinity after the first heat treatment was greater than 20% had a core loss greater than 2000 kW / m 3 . This is considered due to the fact that the average particle size of the crystallites present in the soft magnetic powder was larger than 30 nm.
- the coil parts using the soft magnetic powders of Examples 18 to 26 had a core loss of 2000 kW / m 3 or less. This shows that the core loss was able to be reduced by using the soft magnetic powder according to the present invention.
- the coil component using the soft magnetic powder of Example 32 in which the maximum temperature T1 in the first heat treatment was set to a temperature where the Avrami constant was smaller than 1.7 was larger than 2000 kW / m 3
- the coil parts using the soft magnetic powders of Examples 28 to 31 had a core loss of 2000 kW / m 3 or less. This shows that the core loss was able to be reduced by using the soft magnetic powder according to the present invention.
- the coil component using the soft magnetic powder of Example 37 whose crystallinity after the first heat treatment was greater than 20% had a core loss greater than 2000 kW / m 3 . This is presumably because the average particle size of the crystallites present in the soft magnetic powder was larger than 30 nm and the average thickness of the amorphous phase was larger than 30 nm.
- the coil parts using the soft magnetic powders of Examples 33 to 36 had a core loss of 2000 kW / m 3 or less. This shows that the core loss was able to be reduced by using the soft magnetic powder according to the present invention.
- the soft magnetic powder according to the present invention as a magnetic core material, a coil component having excellent magnetic properties can be obtained, and it can be used for an electronic device that requires high performance.
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Abstract
Description
結晶子の平均粒径が30nm以下であり、アモルファス相の平均厚さが30nm以下であり、
粒子の断面の短径をrとしたとき、粒子の表面からの深さが0.2r以上0.4r以下である領域において、アモルファス相における平均Fe濃度が前記結晶子における平均Fe濃度よりも低い、軟磁性粉末が提供される。
合金粉末を第1の熱処理に付す工程と、
第1の熱処理に付した合金粉末を第2の熱処理に付して、軟磁性粉末を得る工程と
を含む、軟磁性粉末の製造方法であって、
第1の熱処理における最高温度T1は、Avrami定数が1.7以上となる温度であり、第2の熱処理における最高温度T2はT1より低い温度であり、
粉末X線回折法により測定される結晶化度が、第1の熱処理後の合金粉末において20%以下であり、第2の熱処理後の軟磁性粉末において20%より大きい、方法が提供される。
成形体を加熱する工程と
を含む、磁心の製造方法が提供される。
D=Σ(DL+DS)/2n (2)
(D:結晶子の平均粒径)
X={Ic/(Ic+Ic’+Ia)}×100 (3)
(X:結晶化度、Ic:体心立方構造を示す結晶ピーク領域の面積、Ic’:対称性の低い(lowly symmetry)結晶構造を示す結晶ピーク領域の面積、Ia:非晶質性を示すハロー領域の面積)
なお、体心立方構造を示す結晶ピークPは、Feの110面からの回折角2θが44.5°以上45.5°以下の範囲にあるピークである。
Y={Ic’/(Ic+Ic’+Ia)}×100 (4)
Yの値が1以下である場合、結晶相が主に体心立方構造を有するとみなすことができる。
N=d{ln(-ln(1-x))}/d{ln(t-τ)} (5)
(x:結晶化反応比率(=累計発熱量/全発熱量)、t:等温保持時間(秒)、τ:インキュベーションタイム(秒)(x=0.01となる時間))
このようにして求めたAvrami定数の最大値を、各温度におけるAvrami定数とする。
母合金の原料として、Fe、Si、Fe-B合金、Fe-P合金、Cu、Ni、Co、CおよびCrを用いた。これらの原料を、所定の合金組成になるように秤量した。例1~17については、合金組成がFe80.3Si4B7P8Cu0.7となるように原料を秤量し、例18~27については表3、例28~32については表6、例33~37については表9に記載の組成となるように原料を秤量した。秤量した原料を、高周波誘導加熱炉で融点以上に加熱し溶解させ、次いでこの溶解物を銅製の鋳込み型に流し込んで冷却して、母合金を作製した。この母合金を3cm程度の大きさに破砕し、ガスアトマイズ装置の坩堝に投入し、高周波誘導加熱により母合金を溶解させて、溶湯を得た。ガスアトマイズ装置の内部の雰囲気はアルゴン雰囲気に設定した。次いで、アルゴンガスのジェット流体を溶湯に噴射して粉砕し、冷却水で急冷して、例1~37の合金粉末を得た。
例1~16および18~37の各合金粉末について、示差走査型熱量分析計(PerkinElmer社製DSC8500)を用いて、アルゴン雰囲気中で等温DSC測定(昇温速度400℃/分、等温保持測定時間60分)を2回行った。2回目の測定により得られたDSCカーブをバックグラウンドとして、1回目の測定により得られたDSCカーブと2回目の測定により得られたDSCカーブの差より合金粉末試料の発熱量を算出した。等温測定開始からの累計発熱量を時間tの関数として求めた。t=60分における累計発熱量を全発熱量と定義した。上述の式(5)に基づいて、各温度における最大のAvrami定数を算出した。結果を表1、4、7および10に示す。なお、例17の合金粉末は、後述するように第1の熱処理を行わなかったので、DSC測定およびAvrami定数の算出は行わなかった。
赤外線加熱装置を用いて、例1~16および18~37の合金粉末を第1の熱処理に付した。第1の熱処理における最高温度は、表1、4、7および10に示す温度に設定した。加熱装置内の雰囲気は、分圧換算で3%の水素ガスをヘリウムガスに添加した混合ガス雰囲気に設定した。第1の熱処理は10秒間行った。なお、例17の合金粉末については、第1の熱処理を行わなかった。
第1の熱処理後の合金粉末について、粉末X線回折装置(リガク社製RINT2200)を使用して、回折角2θが30°以上65°以下の範囲で、ステップ幅0.02°、ステップ時間2秒の測定条件でX線回折スペクトルを測定した。得られたX線回折スペクトルから各試料の粉末構造相を同定した。また、このX線回折スペクトルに基づいて、上述の式(3)を用いて第1の熱処理後の合金粉末の結晶化度Xを算出した。結果を表1、4、7および10に示す。
赤外線加熱装置を用いて、第1の熱処理後の合金粉末を第2の熱処理に付して、例1~37の軟磁性粉末を得た。第2の熱処理における最高温度は、表1、4、7および10に示す温度に設定した。加熱装置内の雰囲気はアルゴン雰囲気に設定した。第1の熱処理は10分間行った。なお、例17の合金粉末については、第2の熱処理を行わなかった。
第2の熱処理により得られた例1~37の軟磁性粉末について、粉末X線回折装置(リガク社製RINT2200)を使用して、回折角2θが30°以上65°以下の範囲で、ステップ幅0.01°、ステップ時間2秒の測定条件でX線回折スペクトルを測定した。得られたX線回折スペクトルに基づいて、上述の式(3)を用いて軟磁性粉末の結晶化度Xを算出した。結果を表1、4、7および10に示す。
例1~37の軟磁性粉末について、透過型電子顕微鏡(TEM)写真を撮影した。TEM写真を用いて、結晶子の平均粒径およびアモルファス相の平均厚さを求めた。結晶子の平均粒径は、各試料のTEM写真において、軟磁性粉末に含まれる粒子の断面の短径をrとして、粒子の表面からの深さが0.2r以上0.4r以下の領域において任意に選択したn個(n≧5)の結晶子の長径DLおよび短径DSを測定し、上述の式(2)を用いて算出した。更に、各試料のTEM写真において、軟磁性粉末に含まれる粒子の断面の短径をrとして、粒子の表面からの深さが0.2r以上0.4r以下の領域において任意に選択したn個(n≧5)の結晶子について、一の結晶子の結晶相と周辺のアモルファス相との境界と、その一の結晶子に隣接する結晶子の結晶相と周辺のアモルファス相との境界とを最短で結ぶ線分の長さを測定した。この線分の長さの平均値を、アモルファス相の平均厚さとした。結果を表2、5、8および11に示す。なお、例17の軟磁性粉末においては結晶子が検出されなかったので、結晶子の平均粒径およびアモルファス相の平均厚さを測定することはできなかった。
例1~37の軟磁性粉末について、TEM-EDSによりアモルファス相および結晶子における平均Fe濃度を求めた。各試料のTEM写真において、軟磁性粉末に含まれる粒子の断面の短径をrとして、粒子の表面からの深さが0.2r以上0.4r以下の領域において任意に選択したn個(n≧5)の結晶子について、結晶子の中心におけるFe濃度をEDS測定により求め、その平均値を結晶子における平均Fe濃度とした。また、上述の結晶子の結晶相と周辺のアモルファス相との境界と、その結晶子に隣接する結晶子の結晶相と周辺のアモルファス相との境界とを最短で結ぶ線分の中点におけるFe濃度をEDS測定により求め、その平均値をアモルファス相における平均Fe濃度とした。更に、結晶子における平均Fe濃度に対するアモルファス相における平均Fe濃度の比(表において「Fe濃度比率」で示す)を求めた。結果を表2、5、8および11に示す。なお、例17の軟磁性粉末においては結晶相が検出されなかったので、結晶子における平均Fe濃度を測定することはできなかった。
例1~37の軟磁性粉末を用いて、以下に説明する手順でコイル部品を作製した。まず、各試料100重量部に対し3重量部のエポキシ樹脂を添加し(エポキシ樹脂の割合:15vol%)、100MPaの圧力でプレス成形して、外径13mm、内径8mm、厚さ2.5mmのトロイダルコアを作製した。次いで、励磁用の一次側巻線および電圧検出用の二次側巻線の各巻数がいずれも16となるように、エナメルで被覆された線径0.3mmの銅線をトロイダルコアの外周に二重に巻き付けて、例1~37のコイル部品を作製した。
岩通計測株式会社製のB-HアナライザSY-8217を用いて、印加磁界30mT、測定周波数1MHzにおけるコイル部品のコアロス(磁気損失)を測定した。結果を表2、5、8および11に示す。なお、表1~11において「*」を付したものは比較例である。
Claims (21)
- 複数の結晶子と、前記結晶子の周りに存在するアモルファス相とを有する粒子を含む軟磁性粉末であって、
前記結晶子の平均粒径が30nm以下であり、前記アモルファス相の平均厚さが30nm以下であり、
前記粒子の断面の短径をrとしたとき、前記粒子の表面からの深さが0.2r以上0.4r以下である領域において、前記アモルファス相における平均Fe濃度が前記結晶子における平均Fe濃度よりも低い、軟磁性粉末。 - 前記粒子の表面からの深さが0.2r以上0.4r以下である領域において、前記結晶子における平均Fe濃度に対する前記アモルファス相における平均Fe濃度の比が0.90以下である、請求項1に記載の軟磁性粉末。
- 粉末X線回折法により測定される結晶化度が30%以上である、請求項1または2に記載の軟磁性粉末。
- 前記軟磁性粉末が、主に体心立方構造を有する結晶相を含む、請求項3に記載の軟磁性粉末。
- 前記粒子が一般式FeaSibBcPdCueMfCgCrhで表される合金組成物を含み、式中、a、b、c、d、e、f、gおよびhはそれぞれ、71.0≦(a+f+g+h)≦81.0、0.14≦b/c≦5、0≦d≦14、0<e≦1.4、d≦0.8(a+f+g+h)-50、e<-0.1(a+d+f+g+h)+10、0≦f≦12、0≦g≦8、0≦h≦10、およびa+b+c+d+e+f+g+h=100を満たし、MはNiおよびCoの少なくとも1種の元素である、請求項1~4のいずれか1項に記載の軟磁性粉末。
- 前記一般式中、0<f≦12を満たす、請求項5に記載の軟磁性粉末。
- 前記一般式中、0<g≦8を満たす、請求項5または6に記載の軟磁性粉末。
- 前記一般式中、0<h≦10を満たす、請求項5~7のいずれか1項に記載の軟磁性粉末。
- 前記粒子が一般式Fea’Sib’Bc’Pd’Cue’M’f’で表される合金組成物を含み、式中、a’、b’、c’、d’、e’およびf’はそれぞれ、81≦(a’+f’)≦86、2≦b’≦8、6≦c’≦10、2≦d’≦5、0.4≦e’≦1.4、0.08≦e’/d’≦0.8、および0≦f’≦3を満たし、M’はTi、Zr、Hf、Nb、Ta、Mo、W、Cr、Co、Ni、Al、Mn、Ag、Zn、Sn、As、Sb、Bi、Y、N、Oおよび希土類元素の少なくとも1種の元素である、請求項1~4のいずれか1項に記載の軟磁性粉末。
- 母合金の溶湯を冷却して、主にアモルファス相からなる合金粉末を得る工程と、
前記合金粉末を第1の熱処理に付す工程と、
前記第1の熱処理に付した合金粉末を第2の熱処理に付して、軟磁性粉末を得る工程と
を含む、軟磁性粉末の製造方法であって、
前記第1の熱処理における最高温度T1は、Avrami定数が1.7以上となる温度であり、前記第2の熱処理における最高温度T2はT1より低い温度であり、
粉末X線回折法により測定される結晶化度が、前記第1の熱処理後の合金粉末において20%以下であり、前記第2の熱処理後の軟磁性粉末において20%より大きい、方法。 - 前記母合金の溶湯を高圧ガス流で粉砕して冷却することにより、主にアモルファス相からなる合金粉末を得る、請求項10に記載の方法。
- 前記母合金の組成が、一般式FeaSibBcPdCueMfCgCrhで表され、式中、a、b、c、d、e、f、gおよびhはそれぞれ、71.0≦(a+f+g+h)≦81.0、0.14≦b/c≦5、0≦d≦14、0<e≦1.4、d≦0.8(a+f+g+h)-50、e<-0.1(a+d+f+g+h)+10、0≦f≦12、0≦g≦8、0≦h≦10、およびa+b+c+d+e+f+g+h=100を満たし、MはNiおよびCoの少なくとも1種の元素である、請求項10または11に記載の方法。
- 冷却媒としてガスを用いて前記冷却を行う、請求項12に記載の方法。
- 前記母合金の組成が、一般式Fea’Sib’Bc’Pd’Cue’M’f’で表され、式中、a’、b’、c’、d’、e’およびf’はそれぞれ、81≦(a’+f’)≦86、2≦b’≦8、6≦c’≦10、2≦d’≦5、0.4≦e’≦1.4、0.08≦e’/d’≦0.8、および0≦f’≦3を満たし、M’はTi、Zr、Hf、Nb、Ta、Mo、W、Cr、Co、Ni、Al、Mn、Ag、Zn、Sn、As、Sb、Bi、Y、N、Oおよび希土類元素の少なくとも1種の元素である、請求項10または11に記載の方法。
- 冷却媒としてガスを用いて前記冷却を行う、請求項14に記載の方法。
- 請求項1~9のいずれか1項に記載の軟磁性粉末と、樹脂とを含有する複合材料で形成された磁心。
- 前記複合材料中の前記軟磁性粉末の含有量が60vol%以上90vol%以下である、請求項16に記載の磁心。
- 請求項1~9のいずれか1項に記載の軟磁性粉末と、樹脂とを混合し、得られる混合物を成形して成形体を得る工程と、
前記成形体を加熱する工程と
を含む、磁心の製造方法。 - 請求項16または17に記載の磁心と、該磁心に巻回されたコイル導体とを含む、コイル部品。
- 請求項1~9のいずれか1項に記載の軟磁性粉末と樹脂とを含有する複合材料を主成分として含む磁性体部と、該磁性体部に埋設されたコイル導体とを含む、コイル部品。
- 前記複合材料中の前記軟磁性粉末の含有量が60vol%以上90vol%以下である、請求項20に記載のコイル部品。
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Also Published As
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JP6427677B2 (ja) | 2018-11-21 |
CN111446057B (zh) | 2021-06-22 |
US20180154434A1 (en) | 2018-06-07 |
JP6482718B1 (ja) | 2019-03-13 |
US11851738B2 (en) | 2023-12-26 |
JPWO2017022594A1 (ja) | 2018-06-28 |
CN107949889B (zh) | 2020-04-24 |
CN107949889A (zh) | 2018-04-20 |
CN111446057A (zh) | 2020-07-24 |
JP2019060020A (ja) | 2019-04-18 |
DE112016003044T5 (de) | 2018-06-14 |
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