WO2005024859A1 - Soft magnetic material and method for producing same - Google Patents
Soft magnetic material and method for producing same Download PDFInfo
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- WO2005024859A1 WO2005024859A1 PCT/JP2004/012846 JP2004012846W WO2005024859A1 WO 2005024859 A1 WO2005024859 A1 WO 2005024859A1 JP 2004012846 W JP2004012846 W JP 2004012846W WO 2005024859 A1 WO2005024859 A1 WO 2005024859A1
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- 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
- H01F41/0206—Manufacturing of magnetic cores by mechanical means
- H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
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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
- 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
Definitions
- the present invention relates to a soft magnetic material and a method of manufacturing the same, and more particularly, to a soft magnetic material including composite magnetic particles having metal magnetic particles and an insulating film, and a method of manufacturing the same.
- Patent Document 1 Japanese Patent Laid-Open No. 6-267723
- Patent Document 1 Japanese Patent Application Laid-Open No. 6-267723
- the soft magnetic materials disclosed in the above-mentioned documents have the problem that the electrical resistivity is too high and the magnetic flux density is small.
- the present invention has been made to solve the problems as described above, and it is an object of the present invention to provide a soft magnetic material having an optimized electrical resistivity, and a method of manufacturing the same. It is.
- the soft magnetic material according to the present invention comprises a plurality of composite magnetic particles.
- Each of the plurality of composite magnetic particles includes metal magnetic particles and at least one selected from the group consisting of aluminum oxide, zirconium oxide, and zirconium oxide surrounding the surface of the metal magnetic particles. And an insulating film.
- the electrical resistivity p of the soft magnetic material is 3000 ⁇ cm or more and 50000 / i ⁇ cm or less.
- the magnetic permeability ⁇ of the soft magnetic material is 2000 or more and 4000 or less.
- the method for producing a soft magnetic material according to the present invention is a method for producing the above-mentioned soft magnetic material, which comprises metal magnetic particles, and the surfaces of the metal magnetic particles, aluminum oxide, zinc oxide and zinc oxide oxide. Forming a molded body by pressing a plurality of composite magnetic particles having an insulating film containing at least one selected from the group consisting of A heat treatment step of 1 is provided.
- the formed body is subjected to a second heat treatment at a temperature of 400 ° C. to 900 ° C. under atmospheric pressure. It has a process. Effect of the invention
- FIG. 1 is a schematic view showing a cross section of a soft magnetic material according to an embodiment of the present invention.
- the soft magnetic material according to the present invention has a plurality of composite magnetic particles, and each of the composite magnetic particles has metal magnetic particles and an insulating film surrounding the surface of the metal magnetic particles.
- the metallic magnetic particles are generally composed of iron (Fe). While the metal magnetic particles are not limited to iron, they may be composed of other magnetic particles.
- metal magnetic particles can be iron (Fe) -silicon (Si) based alloys, iron (Fe) -nitrogen (N) based alloys, iron (Fe) -biquettes (Ni) based alloys, iron (Fe) —Carbon (C) -based alloy, iron (Fe) -boron (B) -based alloy, iron (Fe) _ cobalt (Co) -based alloy, iron (Fe) _ phosphorus (P) -based alloy, iron (Fe) _ It may be formed of a nickel (Ni) -cobalt (Co) based alloy, an iron (Fe) -aluminum (A1) -silicon (Si) based alloy or the like.
- the metal magnetic particles may be either a single metal or an alloy.
- the average particle diameter of the metal magnetic particles is preferably 5 ⁇ m or more and 200 ⁇ m or less.
- the metal is easily oxidized, which may deteriorate the magnetic properties of the soft magnetic material.
- the average particle size of the metal magnetic particles exceeds 200 ⁇ m, the compressibility of the mixed powder is reduced in the subsequent forming process. As a result, the density of the molded product obtained by the molding process may be reduced, making it difficult to handle.
- the average particle diameter means the particle diameter of particles in which the sum of mass from the smaller one reaches 50% of the total mass in the histogram of particle diameters measured by the sieve method, that is, 50% particles.
- the diameter is D.
- the insulating coating can be composed of an oxide insulator containing aluminum and Z or zirconium and / or cyne.
- the electrical resistivity p of the soft magnetic material is 3000 ⁇ cm or more and 50000 ⁇ cm or less. If the electrical resistivity p is less than 3000 ⁇ cm, the electrical resistivity decreases and the effect of suppressing the eddy current decreases.
- the electrical resistivity p exceeds 50000 ⁇ cm, the electrical resistivity becomes too large, which is not preferable.
- the increase in the electrical resistivity p means that the amount of the insulating coating is increased. If the amount of the insulating coating is too large, magnetic properties such as permeability and magnetic flux density will deteriorate.
- the electrical resistivity p of the soft magnetic material is at least 6000 ⁇ ⁇ cm 15
- the force S be less than or equal to 000 ⁇ Q cm, and further more than or equal to 8000 ⁇ ⁇ cm and less than or equal to 10000 ⁇ ⁇ cm.
- the thickness of the insulating coating is preferably ⁇ 005 ⁇ m to ⁇ 20 ⁇ m.
- the thickness of the insulating coating is preferably ⁇ 005 ⁇ m to ⁇ 20 ⁇ m.
- the magnetic permeability ⁇ of the soft magnetic material is 2000 or more and 4000 or less. More preferably, the permeability / i of the soft magnetic material is 2500 or more and 3500 or less.
- the composite magnetic particles are placed in a mold and, for example, the mixed powder is pressure-formed under conditions of a pressure of 390 MPa or more and 150 OMPa or less. Thereby, the mixed powder can be compressed to obtain a compact.
- the pressure forming atmosphere is preferably an inert gas or a reduced pressure atmosphere. In this case, oxidation of the mixed powder by oxygen in the atmosphere can be prevented.
- the warm forming method and the mold lubrication method which are known techniques in the forming process of the formed body, the formed body is densified, the space factor is improved, and the magnetic property is improved.
- the powder temperature during warm molding is preferably 100 ° C to 180 ° C.
- an organic substance may be interposed between the composite magnetic particles.
- the composite magnetic particles and the organic matter need to be mixed in advance.
- the mixing method is not particularly limited, for example, mechanical bonding, vibration ball milling, planetary ball milling, mechanofusion, coprecipitation, chemical vapor deposition (CVD), physical vapor deposition (PVD), plating, It is possible to use any of sputtering method, vapor deposition method, sol-gel method and the like.
- thermoplastic resins such as thermoplastic polyimide, thermoplastic polyamide, thermoplastic polyamide imide, polyphenylene sulfide, polyamide imide, polyether sulfone, polyether imide or polyether ether ketone can be used. .
- the organic substance functions as a lubricant among the plurality of composite magnetic particles. This can suppress breakage of the insulating coating during the molding process.
- the compact obtained by pressure formation is heat-treated at a temperature of 400 ° C. or more and 900 ° C. or less.
- a large number of strains and dislocations are generated inside the compact obtained through the pressure forming process, and the strains and dislocations cause a decrease in permeability and an increase in coercivity.
- Heat treatment is performed on the compact for the purpose of removing the strain and dislocation. Such heat treatment is required even when organic matter is interposed between composite magnetic particles.
- the soft magnetic material is compressed again to improve its density, and then the soft magnetic material is subjected to atmospheric pressure. Heat treatment at a temperature of 400 ° C to 900 ° C.
- the soft magnetic material according to the present invention can be manufactured.
- the material is configured to have a high permeability, which leads to a reduction in hysteresis loss.
- eddy current loss includes eddy current loss in each particle and eddy current loss generated between particles. It is necessary to reduce the eddy current loss across the particles, and in the present invention, it is possible to reduce the eddy current loss because the specific resistance of the soft magnetic material is increased in the range without damaging the magnetic properties.
- composition of the aluminum oxide, the zirconium oxide and the silicon oxide which constitute the insulating film in the present invention is not particularly limited.
- the composition of aluminum oxide is not limited to Al 2 O 3, and the atomic ratio of aluminum to oxygen may be changed as appropriate.
- the composition ratio of zirconium oxide may be changed as appropriate to the ratio of zirconium and oxygen.
- the composition ratio of carbon dioxide may also be appropriately changed in the ratio of carbon and oxygen.
- FIG. 1 is a schematic view showing a cross section of the soft magnetic material according to the embodiment of the present invention.
- the soft magnetic material comprises a plurality of composite magnetic particles 30.
- Each of the plurality of composite magnetic particles 30 encloses the metal magnetic particle 10 and the surface of the metal magnetic particle 10, and includes at least one selected from the group consisting of an amine oxide, zirconium oxide and an acid oxide. And an insulating film 20.
- the electrical resistivity p of the soft magnetic material is 3000 ⁇ cm or more and 50000 ⁇ cm or less.
- An organic substance 40 intervenes between the composite magnetic particles 30.
- Example 1 the soft magnetic material according to the present invention was manufactured. First, as metal magnetic particles Then, using an iron powder having an average particle size of 70 ⁇ m ⁇ , this iron powder was coated with an Al film as an insulation film using a wet method. At this time, the thickness of the insulating film was made to be lOOnm.
- This coating formed composite magnetic particles in which the surface of the iron powder was surrounded by an Al 2 O film.
- a mixed powder was formed by mixing the composite magnetic particles and particles of a polyphenol sulfide resin having an average particle diameter of 100 ⁇ m or less.
- the mixed powder was placed in a mold and subjected to pressure forming. At this time, pressure molding was performed in a nitrogen gas atmosphere, the temperature of the mold was normal temperature, and the pressure was 882 MPa. Thus, a sample of a molded body was obtained.
- the compact was heat treated. The heat treatment was performed for 3 hours at a temperature of 800 ° C. in a nitrogen gas atmosphere. Thereafter, the electrical resistivity, density, and permeability of the sample were measured. The electrical resistivity was 5670 ⁇ cm, the density was 7.5 g / cm 3 , and the permeability ⁇ was 2050.
- Somalloy 500 (trade name) was prepared as composite magnetic particles.
- Somalloy 500 is a composite magnetic particle in which a phosphate film is formed on the surface of iron powder.
- a mixed powder was formed by mixing particles of polyphenylene sulfide with the composite magnetic particles. The mixed powder was placed in a mold and pressed. At this time, pressure molding was performed in a nitrogen gas atmosphere, the temperature of the mold was normal temperature, and the pressure was 882 MPa. Thereby, a molded body was obtained.
- the compact was heat-treated.
- the heat treatment was performed for 0.5 hours at a temperature of 300 ° C. in a nitrogen gas atmosphere. Thereafter, the electrical resistivity and permeability of the molded body were measured.
- the electrical resistivity was 350 / ⁇ cm, and the permeability ⁇ was 600.
- the soft magnetic material according to the present invention can satisfy the magnetic characteristics required for the soft magnetic material.
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Abstract
Description
明 細 書 Specification
軟磁性材料およびその製造方法 Soft magnetic material and method of manufacturing the same
技術分野 Technical field
[0001] この発明は、軟磁性材料およびその製造方法に関し、より特定的には、金属磁性 粒子と絶縁被膜とを有する複合磁性粒子を備える軟磁性材料およびその製造方法 に関するものである。 The present invention relates to a soft magnetic material and a method of manufacturing the same, and more particularly, to a soft magnetic material including composite magnetic particles having metal magnetic particles and an insulating film, and a method of manufacturing the same.
^景技術 ^ Technology
[0002] 近年、電気電子部品の高密度化および小型化が図られており、モータコアゃトラン スコアなどにおいて、より精密な制御を省電力で行なえることが求められている。この ため、これらの電気電子部品に使用される軟磁性材料であって、中高周波領域にお いて優れた磁気的特性を有する軟磁性材料の開発が進められている。軟磁性材料 が中高周波領域で優れた磁気的特性を有するためには、高い飽和磁束密度、高い 透磁率および高レ、電気抵抗率を併せ持つ必要がある。 In recent years, densification and miniaturization of electric and electronic parts have been achieved, and it is required to perform more precise control with power saving in motor core, core score, and the like. For this reason, development of soft magnetic materials used for these electric and electronic components and having excellent magnetic properties in the middle high frequency region has been advanced. In order for soft magnetic materials to have excellent magnetic properties in the middle to high frequency region, it is necessary to have high saturation magnetic flux density, high permeability, high resitivity, and electrical resistivity.
[0003] このような軟磁性材料については、たとえば特開平 6— 267723号公報(特許文献 1 )に開示されている。 Such a soft magnetic material is disclosed, for example, in Japanese Patent Laid-Open No. 6-267723 (Patent Document 1).
特許文献 1:特開平 6 - 267723号公報 Patent Document 1: Japanese Patent Application Laid-Open No. 6-267723
発明の開示 Disclosure of the invention
発明が解決しょうとする課題 Problem that invention tries to solve
[0004] し力 ながら、上記の文献に開示された軟磁性材料では、電気抵抗率が高過ぎ、 かつ磁束密度が小さいという問題があった。 However, the soft magnetic materials disclosed in the above-mentioned documents have the problem that the electrical resistivity is too high and the magnetic flux density is small.
[0005] そこで、この発明は上述のような問題点を解決するためになされたものであり、この 発明の目的は、電気抵抗率が最適化された軟磁性材料およびその製造方法を提供 することである。 Therefore, the present invention has been made to solve the problems as described above, and it is an object of the present invention to provide a soft magnetic material having an optimized electrical resistivity, and a method of manufacturing the same. It is.
課題を解決するための手段 Means to solve the problem
[0006] この発明に従った軟磁性材料は、複数の複合磁性粒子を備える。複数の複合磁性 粒子の各々は、金属磁性粒子と、その金属磁性粒子の表面を取囲み、酸化アルミ二 ゥム、酸化ジルコニウムおよび酸化ケィ素からなる群より選ばれた少なくとも 1種を含 む絶縁被膜とを有する。軟磁性材料の電気抵抗率 pは 3000 μ Ω cm以上 50000 /i Ω cm以下である。 The soft magnetic material according to the present invention comprises a plurality of composite magnetic particles. Each of the plurality of composite magnetic particles includes metal magnetic particles and at least one selected from the group consisting of aluminum oxide, zirconium oxide, and zirconium oxide surrounding the surface of the metal magnetic particles. And an insulating film. The electrical resistivity p of the soft magnetic material is 3000 μΩ cm or more and 50000 / i Ω cm or less.
[0007] より好ましくは、軟磁性材料の透磁率 μは 2000以上 4000以下である。 この発明 に従った軟磁性材料の製造方法は、上述の軟磁性材料を製造するための方法であ つて金属磁性粒子と、その金属磁性粒子の表面を取囲み、酸化アルミニウム、酸化 ジノレコニゥムおよび酸化ケィ素からなる群より選ばれた少なくとも 1種を含む絶縁被膜 とを有する複数の複合磁性粒子を加圧することによって成形体を形成する工程と、成 形体に温度 400°C以上 900°C以下で第 1の熱処理をする工程を備える。 More preferably, the magnetic permeability μ of the soft magnetic material is 2000 or more and 4000 or less. The method for producing a soft magnetic material according to the present invention is a method for producing the above-mentioned soft magnetic material, which comprises metal magnetic particles, and the surfaces of the metal magnetic particles, aluminum oxide, zinc oxide and zinc oxide oxide. Forming a molded body by pressing a plurality of composite magnetic particles having an insulating film containing at least one selected from the group consisting of A heat treatment step of 1 is provided.
[0008] 好ましくは、軟磁性材料の製造方法は、第 1の熱処理後、成形体を加圧した後、大 気圧で温度 400°C以上 900°C以下で成形体に第 2の熱処理をする工程を備える。 発明の効果 Preferably, in the method of manufacturing a soft magnetic material, after pressing the formed body after the first heat treatment, the formed body is subjected to a second heat treatment at a temperature of 400 ° C. to 900 ° C. under atmospheric pressure. It has a process. Effect of the invention
[0009] この発明に従えば、所望の磁気特性を有する軟磁性材料およびその製造方法を 提供すること力 Sできる。 According to the present invention, it is possible to provide a soft magnetic material having desired magnetic properties and a method for producing the same.
図面の簡単な説明 Brief description of the drawings
[0010] [図 1]この発明の実施の形態における軟磁性材料の断面を示す模式図である。 FIG. 1 is a schematic view showing a cross section of a soft magnetic material according to an embodiment of the present invention.
符号の説明 Explanation of sign
[0011] 10 金属磁性粒子、 20 絶縁被膜、 30 複合磁性粒子。 [0011] 10 metal magnetic particles, 20 insulating coatings, 30 composite magnetic particles.
発明を実施するための最良の形態 BEST MODE FOR CARRYING OUT THE INVENTION
[0012] この発明に従った軟磁性材料は、複数の複合磁性粒子を有し、複合磁性粒子の各 々は金属磁性粒子と、その金属磁性粒子の表面を取囲む絶縁被膜とを有する。 The soft magnetic material according to the present invention has a plurality of composite magnetic particles, and each of the composite magnetic particles has metal magnetic particles and an insulating film surrounding the surface of the metal magnetic particles.
[0013] 金属磁性粒子は、一般的には鉄 (Fe)により構成されている。し力、しながら、金属磁 性粒子は鉄に限定されず、他の磁性粒子で構成されてもよい。たとえば、金属磁性 粒子は、鉄 (Fe)_シリコン (Si)系合金、鉄 (Fe)_窒素(N)系合金、鉄 (Fe)_二ッケ ノレ (Ni)系合金、鉄 (Fe)—炭素 (C)系合金、鉄 (Fe)—硼素 (B)系合金、鉄 (Fe) _コ バルト(Co)系合金、鉄(Fe) _リン (P)系合金、鉄(Fe)_ニッケル (Ni)_コバルト(Co )系合金および、鉄 (Fe)—アルミニウム (A1)—シリコン(Si)系合金などから形成されて いてもよい。金属磁性粒子は、金属単体でも合金でもいずれであってもよい。 [0014] 金属磁性粒子の平均粒径は、 5 μ m以上 200 μ m以下であることが好ましい。金属 磁性粒子の平均粒径が 5 / m未満である場合、金属が酸化されやすいため、軟磁性 材料の磁気的特性が低下する恐れがある。また、金属磁性粒子の平均粒径が 200 μ mを超える場合には、後に続く成形工程時において混合粉末の圧縮性が低下す る。これにより、成形工程によって得られた成形体の密度が低下して取扱が困難とな る恐れがある。 The metallic magnetic particles are generally composed of iron (Fe). While the metal magnetic particles are not limited to iron, they may be composed of other magnetic particles. For example, metal magnetic particles can be iron (Fe) -silicon (Si) based alloys, iron (Fe) -nitrogen (N) based alloys, iron (Fe) -biquettes (Ni) based alloys, iron (Fe) —Carbon (C) -based alloy, iron (Fe) -boron (B) -based alloy, iron (Fe) _ cobalt (Co) -based alloy, iron (Fe) _ phosphorus (P) -based alloy, iron (Fe) _ It may be formed of a nickel (Ni) -cobalt (Co) based alloy, an iron (Fe) -aluminum (A1) -silicon (Si) based alloy or the like. The metal magnetic particles may be either a single metal or an alloy. The average particle diameter of the metal magnetic particles is preferably 5 μm or more and 200 μm or less. When the average particle size of the metal magnetic particles is less than 5 / m, the metal is easily oxidized, which may deteriorate the magnetic properties of the soft magnetic material. In addition, when the average particle size of the metal magnetic particles exceeds 200 μm, the compressibility of the mixed powder is reduced in the subsequent forming process. As a result, the density of the molded product obtained by the molding process may be reduced, making it difficult to handle.
[0015] なお、平均粒径とは、ふるい法によって測定した粒径のヒストグラム中、粒径の小さ い方からの質量の和が総質量の 50%に達する粒子の粒径、つまり 50%粒径 Dをい う。 [0015] The average particle diameter means the particle diameter of particles in which the sum of mass from the smaller one reaches 50% of the total mass in the histogram of particle diameters measured by the sieve method, that is, 50% particles. The diameter is D.
[0016] 絶縁被膜は、アルミニウムおよび Zまたはジルコニウムおよび/またはケィ素を含 む酸化物絶縁体で構成することができる。金属磁性粒子の表面を絶縁被膜で覆うこ とによって、軟磁性材料の電気抵抗率 pを大きくすることができる。これにより、金属 磁性粒子間に渦電流が流れるのを抑制し、渦電流に起因する軟磁性材料の鉄損を 低減すること力 Sできる。 The insulating coating can be composed of an oxide insulator containing aluminum and Z or zirconium and / or cyne. By covering the surface of the metal magnetic particles with an insulating coating, the electrical resistivity p of the soft magnetic material can be increased. As a result, it is possible to suppress the flow of the eddy current between the metal magnetic particles, and to reduce the iron loss of the soft magnetic material caused by the eddy current.
[0017] この発明に従えば、軟磁性材料の電気抵抗率 pは 3000 μ Ω cm以上 50000 μ Ω cm以下である。電気抵抗率 pが 3000 μ Ω cm未満であれば、電気抵抗率が小さく なり、渦電流を抑制する効果が小さくなる。 According to the present invention, the electrical resistivity p of the soft magnetic material is 3000 μΩcm or more and 50000 μΩcm or less. If the electrical resistivity p is less than 3000 μΩ cm, the electrical resistivity decreases and the effect of suppressing the eddy current decreases.
[0018] これとは反対に、電気抵抗率 pが 50000 μ Ω cmを超えると電気抵抗率が大きくな り過ぎるため好ましくない。具体的には、電気抵抗率 pが大きくなることは、絶縁被膜 の量が大きくなることを意味する。絶縁被膜が多くなり過ぎると透磁率および磁束密 度などの磁気特性が悪化する。 On the other hand, when the electrical resistivity p exceeds 50000 μΩ cm, the electrical resistivity becomes too large, which is not preferable. Specifically, the increase in the electrical resistivity p means that the amount of the insulating coating is increased. If the amount of the insulating coating is too large, magnetic properties such as permeability and magnetic flux density will deteriorate.
[0019] 上記効果を高めるためには、軟磁性材料の電気抵抗率 pは 6000 μ Ω cm以上 15In order to enhance the above effect, the electrical resistivity p of the soft magnetic material is at least 6000 μ Ω cm 15
000 μ Q cm以下、さらに、 8000 μ Ω cm以上 10000 μ Ω cm以下であること力 S望ま しい。 It is desirable that the force S be less than or equal to 000 μ Q cm, and further more than or equal to 8000 μ Ω cm and less than or equal to 10000 μ Ω cm.
[0020] 絶縁被膜の厚みは 0. 005 μ m以上 20 μ m以下であることが好ましい。絶縁被膜の 厚みを 0. 005 z m以上とすることにより、渦電流によるエネルギ損失を効果的に抑制 すること力 Sできる。また、絶縁被膜の厚みを 20 z m以下とすることによって、軟磁性材 料中に占める絶縁被膜の体積比率が大きくなり過ぎることがない。これにより、所定の 飽和磁束密度を有する軟磁性材料を形成することができる。 [0020] The thickness of the insulating coating is preferably 以上 005 μm to μ20 μm. By setting the thickness of the insulating coating to not less than 0.005 g, force S can effectively suppress energy loss due to eddy current. Also, by setting the thickness of the insulating film to 20 zm or less, the volume ratio of the insulating film in the soft magnetic material does not become too large. In this way, A soft magnetic material having a saturation flux density can be formed.
[0021] より好ましくは、軟磁性材料の透磁率 μは 2000以上 4000以下である。より好ましく は、軟磁性材料の透磁率/ iは 2500以上 3500以下である。 More preferably, the magnetic permeability μ of the soft magnetic material is 2000 or more and 4000 or less. More preferably, the permeability / i of the soft magnetic material is 2500 or more and 3500 or less.
[0022] 次に、上述の軟磁性材料の製造方法にっレ、て説明する。まず、複数の複合磁性粒 子を準備する。この複合磁性粒子を金型に入れて、たとえば圧力 390MPa以上 150 OMPa以下の条件で混合粉末を加圧成形する。これにより、混合粉末が圧縮されて 成形体を得ることができる。加圧成形する雰囲気は、不活性ガスまたは減圧雰囲気 下とすることが好ましい。この場合、大気中の酸素によって混合粉末が酸化されるの を防止することができる。成形体の形成工程において、公知技術である温間成形法 や金型潤滑法を用いることにより、成形体が高密度化し、占積率が向上し、磁気特性 が向上する。温間成形時の粉末温度は、 100°Cから 180°Cが好ましい。 Next, a method of manufacturing the above-mentioned soft magnetic material will be described. First, prepare multiple composite magnetic particles. The composite magnetic particles are placed in a mold and, for example, the mixed powder is pressure-formed under conditions of a pressure of 390 MPa or more and 150 OMPa or less. Thereby, the mixed powder can be compressed to obtain a compact. The pressure forming atmosphere is preferably an inert gas or a reduced pressure atmosphere. In this case, oxidation of the mixed powder by oxygen in the atmosphere can be prevented. By using the warm forming method and the mold lubrication method which are known techniques in the forming process of the formed body, the formed body is densified, the space factor is improved, and the magnetic property is improved. The powder temperature during warm molding is preferably 100 ° C to 180 ° C.
[0023] なお、複合磁性粒子同士の結合を強めるために、複合磁性粒子の間に有機物を 介在させてもよい。この場合、複合磁性粒子と有機物とを予め混合する必要がある。 混合方法に特に制限はなぐたとえばメカニカルァロイング法、振動ボールミル、遊星 ボールミル、メカノフュージョン、共沈法、化学気相蒸着法(CVD法)、物理気相蒸着 法(PVD法)、めっき法、スパッタリング法、蒸着法またはゾルーゲル法などのいずれ を使用することも可能である。 In order to strengthen the bonds between the composite magnetic particles, an organic substance may be interposed between the composite magnetic particles. In this case, the composite magnetic particles and the organic matter need to be mixed in advance. The mixing method is not particularly limited, for example, mechanical bonding, vibration ball milling, planetary ball milling, mechanofusion, coprecipitation, chemical vapor deposition (CVD), physical vapor deposition (PVD), plating, It is possible to use any of sputtering method, vapor deposition method, sol-gel method and the like.
[0024] 有機物としては、熱可塑性ポリイミド、熱可塑性ポリアミド、熱可塑性ポリアミドイミド、 ポリフエ二レンサルファイド、ポリアミドイミド、ポリエーテルスルホン、ポリエーテルイミド またはポリエーテルエーテルケトンなどの熱可塑性樹脂を用いることができる。このよ うな有機物を設けることによって、複数の複合磁性粒子の間で有機物が潤滑剤として 機能する。これにより、成形工程時において、絶縁被膜が破壊されることを抑制でき る。 As the organic substance, thermoplastic resins such as thermoplastic polyimide, thermoplastic polyamide, thermoplastic polyamide imide, polyphenylene sulfide, polyamide imide, polyether sulfone, polyether imide or polyether ether ketone can be used. . By providing such an organic substance, the organic substance functions as a lubricant among the plurality of composite magnetic particles. This can suppress breakage of the insulating coating during the molding process.
[0025] 次に、加圧形成によって得られた成形体を温度 400°C以上 900度以下で熱処理す る。加圧成形の工程を経た成形体の内部には、歪みおよび転位が多数発生しており 、歪および転位が透磁率の低下と保磁力の増加をひきおこしている。この歪および 転位を取除くことを目的として成形体に熱処理を行なう。なお、複合磁性粒子間に有 機物を介在させる場合であってもこのような熱処理は必要とされる。 [0026] 軟磁性材料の密度を向上させ、さらに軟磁性材料内の転位および歪みを取除くた めには、再度軟磁性材料を圧縮して密度を向上させた後、軟磁性材料を大気圧で 温度 400°C以上 900°C以下で熱処理する。 Next, the compact obtained by pressure formation is heat-treated at a temperature of 400 ° C. or more and 900 ° C. or less. A large number of strains and dislocations are generated inside the compact obtained through the pressure forming process, and the strains and dislocations cause a decrease in permeability and an increase in coercivity. Heat treatment is performed on the compact for the purpose of removing the strain and dislocation. Such heat treatment is required even when organic matter is interposed between composite magnetic particles. In order to improve the density of the soft magnetic material and remove dislocations and strains in the soft magnetic material, the soft magnetic material is compressed again to improve its density, and then the soft magnetic material is subjected to atmospheric pressure. Heat treatment at a temperature of 400 ° C to 900 ° C.
[0027] このようにしてこの発明に従った軟磁性材料を製造することができる。 In this way, the soft magnetic material according to the present invention can be manufactured.
[0028] 一般的に、軟磁性材料の保磁力が小さいとヒステリシス損失が小さくなり、ヒステリシ ス損失が大きいと保磁力も大きくなり、保磁力が小さいと透磁率は大きくなる。透磁率 を向上させることによりヒステリシス損失の低減に繋がる。本発明では、透磁率が高く なるように材料を構成しているため、ヒステリシス損失の低減に繋がる。 Generally, when the coercive force of the soft magnetic material is small, the hysteresis loss is small, and when the hysteresis loss is large, the coercive force is also large, and when the coercive force is small, the permeability is large. The improvement of the permeability leads to the reduction of the hysteresis loss. In the present invention, the material is configured to have a high permeability, which leads to a reduction in hysteresis loss.
[0029] また、渦電流損失を低減するためには、複合磁性粒子間の絶縁を保つことが重要 である。軟磁性材料のバルタ体としての比抵抗を増加させることで渦電流損失の低 減に繋がる。特に、渦電流損失には、各粒子内の渦電流損失と、粒子間に亘つて発 生する渦電流損失がある。粒子間に亘る渦電流損失を低減する必要があり、本発明 では磁気特性を損なわなレ、範囲で軟磁性材料の比抵抗を高くしてレ、るため渦電流 損失の低減が可能となる。 In addition, in order to reduce eddy current loss, it is important to maintain insulation between composite magnetic particles. By increasing the resistivity of the soft magnetic material as a balta body, it leads to the reduction of the eddy current loss. In particular, eddy current loss includes eddy current loss in each particle and eddy current loss generated between particles. It is necessary to reduce the eddy current loss across the particles, and in the present invention, it is possible to reduce the eddy current loss because the specific resistance of the soft magnetic material is increased in the range without damaging the magnetic properties.
[0030] なお、本発明で絶縁被膜を構成する酸化アルミニウム、酸化ジルコニウムおよび酸 化ケィ素の組成については特に限定されるものではない。具体的には、酸化アルミ 二ゥムの組成は Al Oに限定されるものではなぐアルミニウムと酸素との原子比率は 適宜変更してもよい。また、酸化ジルコニウムの組成比も、ジルコニウムと酸素の割合 を適宜変更してもよい。また、酸化ケィ素の組成比もケィ素と酸素の割合を適宜変更 してもよい。 The composition of the aluminum oxide, the zirconium oxide and the silicon oxide which constitute the insulating film in the present invention is not particularly limited. Specifically, the composition of aluminum oxide is not limited to Al 2 O 3, and the atomic ratio of aluminum to oxygen may be changed as appropriate. In addition, the composition ratio of zirconium oxide may be changed as appropriate to the ratio of zirconium and oxygen. In addition, the composition ratio of carbon dioxide may also be appropriately changed in the ratio of carbon and oxygen.
[0031] 図 1は、この発明の実施の形態における軟磁性材料の断面を示す模式図である。 FIG. 1 is a schematic view showing a cross section of the soft magnetic material according to the embodiment of the present invention.
図 1を参照して、軟磁性材料は、複数の複合磁性粒子 30を備える。複数の複合磁性 粒子 30の各々は、金属磁性粒子 10と、金属磁性粒子 10の表面を取囲み、酸化ァ ノレミニゥム、酸化ジルコニウムおよび酸ィ匕ケィ素からなる群より選ばれた少なくとも 1種 を含む絶縁被膜 20とを有する。軟磁性材料の電気抵抗率 pが 3000 μ Ω cm以上 5 0000 μ Ω cm以下である。複合磁性粒子 30の間には、有機物 40が介在している。 (実施例 1) Referring to FIG. 1, the soft magnetic material comprises a plurality of composite magnetic particles 30. Each of the plurality of composite magnetic particles 30 encloses the metal magnetic particle 10 and the surface of the metal magnetic particle 10, and includes at least one selected from the group consisting of an amine oxide, zirconium oxide and an acid oxide. And an insulating film 20. The electrical resistivity p of the soft magnetic material is 3000 μΩ cm or more and 50000 μΩ cm or less. An organic substance 40 intervenes between the composite magnetic particles 30. (Example 1)
[0032] 実施例 1では、本発明に従った軟磁性材料を製造した。まず、金属磁性粒子として 、平均粒径が 70 μ ΐηの鉄粉を用意した、湿式法を用いて、この鉄粉に絶縁被膜とし ての Al Ο膜をコーティングした。この際、絶縁被膜の厚みを lOOnmとなるようにした[0032] In Example 1, the soft magnetic material according to the present invention was manufactured. First, as metal magnetic particles Then, using an iron powder having an average particle size of 70 μm 湿式, this iron powder was coated with an Al film as an insulation film using a wet method. At this time, the thickness of the insulating film was made to be lOOnm.
。このコーティングによって、鉄粉の表面を Al O膜で取囲んだ複合磁性粒子を形成 した。 . This coating formed composite magnetic particles in which the surface of the iron powder was surrounded by an Al 2 O film.
[0033] 複合磁性粒子と、平均粒径が 100 μ m以下のポリフエ二レンサルファイド樹脂の粒 子とを混合することによって、混合粉末を形成した。混合粉末を金型に入れて加圧成 形を行なった。このとき、窒素ガス雰囲気中で加圧成形を行ない、金型の温度を常温 とし、加圧圧力を 882MPaとした。これにより、成形体のサンプルを得た。次に、成形 体を熱処理した。熱処理は、窒素ガス雰囲気中温度 800°Cで 3時間行なった。その 後サンプルの電気抵抗率、密度、透磁率を測定したところ、電気抵抗率は 5670 μ □ cm,密度は 7. 5g/cm3、透磁率 μは 2050であった。 [0033] A mixed powder was formed by mixing the composite magnetic particles and particles of a polyphenol sulfide resin having an average particle diameter of 100 μm or less. The mixed powder was placed in a mold and subjected to pressure forming. At this time, pressure molding was performed in a nitrogen gas atmosphere, the temperature of the mold was normal temperature, and the pressure was 882 MPa. Thus, a sample of a molded body was obtained. Next, the compact was heat treated. The heat treatment was performed for 3 hours at a temperature of 800 ° C. in a nitrogen gas atmosphere. Thereafter, the electrical resistivity, density, and permeability of the sample were measured. The electrical resistivity was 5670 μ cm, the density was 7.5 g / cm 3 , and the permeability μ was 2050.
(比較例 1) (Comparative example 1)
[0034] 比較例 1では、複合磁性粒子として、ソマロイ 500 (商品名)を準備した。ソマロイ 50 0は鉄粉の表面に燐酸塩被膜が形成された複合磁性粒子である。複合磁性粒子に ポリフエ二レンサルファイドの粒子を混合することによって混合粉末を形成した。混合 粉末を金型に入れて加圧成形を行なった。この際、窒素ガス雰囲気中で加圧成形を 行ない、金型の温度を常温とし、加圧圧力を 882MPaとした。これにより、成形体を 得た。 In Comparative Example 1, Somalloy 500 (trade name) was prepared as composite magnetic particles. Somalloy 500 is a composite magnetic particle in which a phosphate film is formed on the surface of iron powder. A mixed powder was formed by mixing particles of polyphenylene sulfide with the composite magnetic particles. The mixed powder was placed in a mold and pressed. At this time, pressure molding was performed in a nitrogen gas atmosphere, the temperature of the mold was normal temperature, and the pressure was 882 MPa. Thereby, a molded body was obtained.
[0035] 次に、成形体を熱処理した。熱処理は、窒素ガス雰囲気中で温度 300°Cで 0. 5時 間行なった。その後成形体の電気抵抗率と透磁率を測定した。電気抵抗率は 350 / Ω cm、透磁率 μは 600であった。 Next, the compact was heat-treated. The heat treatment was performed for 0.5 hours at a temperature of 300 ° C. in a nitrogen gas atmosphere. Thereafter, the electrical resistivity and permeability of the molded body were measured. The electrical resistivity was 350 / Ω cm, and the permeability μ was 600.
[0036] 以上の結果から、本発明による軟磁性材料によれば、軟磁性材料に求められる磁 気的特性を満たすことができることを確認した。 From the above results, it was confirmed that the soft magnetic material according to the present invention can satisfy the magnetic characteristics required for the soft magnetic material.
[0037] 今回開示された実施の形態および実施例はすべての点で例示であって制限的な ものではないと考えられるべきである。本発明の範囲は上記した説明ではなくて特許 請求の範囲によって示され、特許請求の範囲と均等の意味および範囲内でのすべ ての変更が含まれることが意図される。 It should be understood that the embodiments and examples disclosed herein are illustrative and non-restrictive in every respect. The scope of the present invention is shown not by the above description but by the claims, and is intended to include all modifications within the meaning and scope equivalent to the claims.
Claims
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| JP4865527B2 (en) * | 2006-12-18 | 2012-02-01 | 富士電機株式会社 | Soft magnetic molded body and method for producing the same |
| JP5227756B2 (en) | 2008-01-31 | 2013-07-03 | 本田技研工業株式会社 | Method for producing soft magnetic material |
| DE102008023059B4 (en) * | 2008-05-09 | 2010-06-10 | Eto Magnetic Gmbh | Method for producing a magnetizable metallic shaped body |
| JP2009290024A (en) * | 2008-05-29 | 2009-12-10 | Denso Corp | Method for manufacturing pressed powder magnetic core |
| JP5435398B2 (en) * | 2009-08-27 | 2014-03-05 | Tdk株式会社 | Soft magnetic dust core and manufacturing method thereof |
| JP5539159B2 (en) * | 2010-11-04 | 2014-07-02 | アイダエンジニアリング株式会社 | High density molding method and high density molding apparatus for mixed powder. |
| CN107578872B (en) * | 2017-08-10 | 2019-10-22 | 深圳市铂科新材料股份有限公司 | A kind of preparation method of metal soft magnetic powder core resistant to high temperature heat treatment |
| JP2021021097A (en) * | 2019-07-25 | 2021-02-18 | Tdk株式会社 | Composite magnetic powder, powder magnetic core using the same, and manufacturing method for composite magnetic powder |
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| JPH0867941A (en) * | 1994-08-26 | 1996-03-12 | Sumitomo Special Metals Co Ltd | Production of sendust type sintered alloy |
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| JPH0867941A (en) * | 1994-08-26 | 1996-03-12 | Sumitomo Special Metals Co Ltd | Production of sendust type sintered alloy |
| JP2003037018A (en) * | 2001-07-23 | 2003-02-07 | Daido Steel Co Ltd | Manufacturing method of dust core |
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| US11495398B2 (en) * | 2017-10-18 | 2022-11-08 | Samsung Electro-Mechanics Co., Ltd. | Coil electronic component |
| US12014866B2 (en) | 2017-10-18 | 2024-06-18 | Samsung Electro-Mechanics Co., Ltd. | Coil electronic component |
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