JP2011171346A - Iron-based soft magnetic powder for dust core, method of manufacturing the same, and dust core - Google Patents
Iron-based soft magnetic powder for dust core, method of manufacturing the same, and dust core Download PDFInfo
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- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 4
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
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- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
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- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 description 1
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- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
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- Powder Metallurgy (AREA)
- Soft Magnetic Materials (AREA)
Abstract
Description
本発明は、鉄粉や鉄基合金粉末等の鉄基軟磁性粉末の表面に耐熱性の高い絶縁被膜を形成した圧粉磁心用鉄基軟磁性粉末と、その圧粉磁心用鉄基軟磁性粉末の製造方法、並びにその圧粉磁心用鉄基軟磁性粉末を用いて作製された圧粉磁心に関するものである。 The present invention relates to an iron-based soft magnetic powder for a dust core in which an insulating coating having high heat resistance is formed on the surface of an iron-based soft magnetic powder such as iron powder or iron-based alloy powder, and an iron-based soft magnetic powder for the dust core. The present invention relates to a powder manufacturing method, and a dust core produced using the iron-based soft magnetic powder for the dust core.
従来から交流で使用されるモータ、トランスなどの電磁気部品の磁心には、電磁鋼板や電気鉄板を積層した磁心が用いられていたが、近年は、これら電磁鋼板や電気鉄板を積層した磁心に比べ、より磁気特性に優れ、三次元形状の自由度も高いことから、表面に絶縁処理した純鉄粉や軟磁性鉄基合金粉末等の圧粉磁心用鉄基軟磁性粉末（以下、純鉄粉と軟磁性鉄基合金粉末等をまとめて圧粉磁心用鉄基軟磁性粉末ともいう）を、圧縮成形した圧粉磁心が用いられるようになってきた。 Conventionally, the magnetic cores of electromagnetic parts such as motors and transformers used in AC have been laminated with magnetic steel plates and electric iron plates. However, in recent years, compared with magnetic cores laminated with these magnetic steel plates and electric iron plates. Because of its superior magnetic properties and high degree of freedom in three-dimensional shape, iron-based soft magnetic powders for dust cores such as pure iron powder and soft magnetic iron-based alloy powder with insulation treatment on the surface (hereinafter referred to as pure iron powder) And a soft magnetic iron-base alloy powder are also referred to as iron-based soft magnetic powders for dust cores), and a dust core obtained by compression molding has been used.
表面に絶縁処理した純鉄粉や軟磁性鉄基合金粉末等の圧粉磁心用鉄基軟磁性粉末、或いは、その圧粉磁心用鉄基軟磁性粉末を圧縮成形して作製した圧粉磁心としては、鉄基軟磁性粉末の表面をリン酸等から得られるガラス状絶縁層で被覆した提案が特許文献１としてあり、古くから知られている。また、その鉄基軟磁性粉末とガラス状絶縁層の密着性を向上させるために、鉄基軟磁性粉末の表面を大気中で酸化してその表面に酸化被膜を形成した技術が特許文献２として提案されている。しかしながら、これらガラス状絶縁層等の無機系絶縁被膜は、熱的安定性に優れているはずであるが、高温での熱処理（焼鈍）を行うと絶縁性が低下してしまうという問題があった。 As an iron-based soft magnetic powder for powder magnetic cores, such as pure iron powder and soft magnetic iron-based alloy powder with insulation treatment on the surface, or a powder magnetic core produced by compression molding the iron-based soft magnetic powder for dust cores Has been proposed for a long time as a patent document 1 in which the surface of an iron-based soft magnetic powder is covered with a glassy insulating layer obtained from phosphoric acid or the like. Patent Document 2 discloses a technique in which the surface of an iron-based soft magnetic powder is oxidized in the atmosphere to form an oxide film on the surface in order to improve the adhesion between the iron-based soft magnetic powder and the glassy insulating layer. Proposed. However, these inorganic insulating coatings such as glass-like insulating layers should be excellent in thermal stability, but there is a problem that the insulating properties deteriorate when heat treatment (annealing) at high temperature is performed. .
このような観点から、耐熱性の高いシリコーン樹脂を絶縁被膜として採用する技術が開発されている。特許文献３記載の技術では、特定のメチル−フェニルシリコーン樹脂を絶縁材料として用いている。しかし、この技術では、熱的安定性を確保するために、鉄粉に対して１質量％以上の樹脂を用いており、高密度成形という観点からはまだ改善の余地がある技術である。また、特許文献４や特許文献５として、耐熱性を確保するために、シリコーン樹脂にガラス粉末や顔料を加える提案もなされている。しかし、これらの技術は、ガラス粉末や顔料を添加することで高密度化が阻害されてしまう点で問題があった。 From such a point of view, a technology that employs a silicone resin having high heat resistance as an insulating coating has been developed. In the technique described in Patent Document 3, a specific methyl-phenyl silicone resin is used as an insulating material. However, in this technique, in order to ensure thermal stability, 1 mass% or more of resin is used with respect to iron powder, and there is still room for improvement from the viewpoint of high density molding. Moreover, as patent document 4 and patent document 5, in order to ensure heat resistance, the proposal which adds glass powder and a pigment to silicone resin is also made | formed. However, these techniques have a problem in that densification is inhibited by adding glass powder or pigment.
そこで、本発明者らが提案したのが、特許文献６に記載の技術である。この技術は、鉄基軟磁性粉末の表面に、内側から順に、リン酸系化成被膜、シリコーン樹脂被膜を形成し、そのリン酸系化成被膜に、Ｃｏ、Ｎａ、Ｓ、ＳｉおよびＷよりなる群から選択される１種以上の元素を含ませた圧粉磁心用鉄基軟磁性粉末等に関する技術であり、この成分組成のリン酸系化成被膜と、シリコーン樹脂被膜を複合させることで、より高度な耐熱性を有する電気絶縁膜を形成することに成功した。しかしながら、リン酸系化成被膜に含有させる元素のうち、ＣｏやＷなどは入手困難な希少金属であって、コストが高いことが問題点であり、原料を容易に入手でき、また、コストの上昇なしにこの技術と同等の効果が得られる汎用技術が開発されることが待ち望まれていた。 Therefore, the technique described in Patent Document 6 has been proposed by the present inventors. In this technique, a phosphoric acid-based chemical conversion film and a silicone resin film are formed on the surface of an iron-based soft magnetic powder in order from the inside, and the phosphoric acid-based chemical conversion film is formed of a group consisting of Co, Na, S, Si and W. Is a technology related to iron-based soft magnetic powders for dust cores containing at least one element selected from the group consisting of phosphoric acid-based chemical conversion coatings and silicone resin coatings. Succeeded in forming an electrical insulating film having excellent heat resistance. However, among the elements contained in the phosphoric acid-based chemical conversion coating, Co, W, etc. are rare metals that are difficult to obtain, and the problem is that the cost is high, the raw materials can be easily obtained, and the cost increases. There is a long-awaited development of a general-purpose technology that can achieve the same effect as this technology.
本発明は、上記従来の問題を解決せんとしてなされたもので、入手困難で、且つ高価なＣｏやＷなどの希少金属を用いることがなくても、且つ、高密度に成形するために絶縁材料の量を低減しても、鉄粉粒子間を効果的に絶縁することができ、機械的強度にも優れ、更に、高温での熱処理を行っても電気絶縁性を維持できるような熱的安定性に優れた圧粉磁心用鉄基軟磁性粉末、およびその圧粉磁心用鉄基軟磁性粉末の製造方法、並びにその圧粉磁心用鉄基軟磁性粉末を用いて作製した圧粉磁心を提供することを課題とするものである。 The present invention has been made as a solution to the above-described conventional problems, and it is difficult to obtain and does not use expensive rare metals such as Co and W, and it is an insulating material for molding at a high density. Even if the amount of iron is reduced, it is possible to effectively insulate between iron powder particles, excellent mechanical strength, and thermal stability that can maintain electrical insulation even after heat treatment at high temperature Provided with an iron-based soft magnetic powder for dust cores excellent in performance, a method for producing the iron-based soft magnetic powder for dust cores, and a dust core produced using the iron-based soft magnetic powder for dust cores It is an object to do.
請求項１記載の発明は、鉄基軟磁性粉末の表面に、内側から順に、リン酸系化成被膜、シリコーン樹脂被膜が形成されており、前記リン酸系化成被膜には、Ｐ、Ｂ、ＭｇおよびＡｌが含有されていることを特徴とする圧粉磁心用鉄基軟磁性粉末である。 In the invention according to claim 1, a phosphoric acid-based chemical conversion film and a silicone resin film are formed in order from the inside on the surface of the iron-based soft magnetic powder, and the phosphoric acid-based chemical conversion film includes P, B, Mg And an iron-based soft magnetic powder for a dust core, characterized by containing Al.
請求項２記載の発明は、前記リン酸系化成被膜に含有される各元素は、前記リン酸系化成被膜が表面に形成された鉄基軟磁性粉末１００質量部に対して、Ｐ：０．０１０〜０．１００質量部、Ｂ：０．００１〜０．０１０質量部、Ｍｇ：０．００１〜０．０２０質量部、Ａｌ：０．００５〜０．０５０質量部が夫々含有されていることを特徴とする請求項１記載の圧粉磁心用鉄基軟磁性粉末である。 According to a second aspect of the present invention, each element contained in the phosphoric acid-based chemical conversion film is formed by adding P = 0.0.0 to 100 parts by mass of the iron-based soft magnetic powder having the phosphoric acid-based chemical conversion film formed on the surface thereof. 0.10 to 0.100 parts by mass, B: 0.001 to 0.010 parts by mass, Mg: 0.001 to 0.020 parts by mass, Al: 0.005 to 0.050 parts by mass, respectively. The iron-based soft magnetic powder for dust core according to claim 1.
請求項３記載の発明は、請求項１または２記載の圧粉磁心用鉄基軟磁性粉末の製造方法であって、Ｂ、ＭｇおよびＡｌを含有するリン酸系化成処理溶液と鉄基軟磁性粉末とを混合した後、水および／または有機溶媒を蒸発させてリン酸系化成被膜を前記鉄基軟磁性粉末の表面に形成する工程と、シリコーン樹脂を有機溶媒に溶解し、このシリコーン樹脂溶液と、前記リン酸系化成被膜が表面に形成された鉄基軟磁性粉末とを混合した後、溶媒を蒸発させてシリコーン樹脂被膜を前記リン酸系化成被膜の上に形成する工程とを含むことを特徴とする圧粉磁心用鉄基軟磁性粉末の製造方法である。 Invention of Claim 3 is a manufacturing method of the iron-base soft magnetic powder for dust cores of Claim 1 or 2, Comprising: The phosphoric acid type | system | group chemical conversion treatment solution containing B, Mg, and Al, and iron-base soft magnetism After mixing the powder, water and / or an organic solvent is evaporated to form a phosphoric acid-based chemical conversion coating on the surface of the iron-based soft magnetic powder, and the silicone resin is dissolved in the organic solvent. And a step of mixing the iron-based soft magnetic powder having the phosphoric acid-based chemical conversion film formed on the surface thereof and then evaporating the solvent to form a silicone resin film on the phosphoric acid-based chemical conversion film. This is a method for producing an iron-based soft magnetic powder for a dust core.
請求項４記載の発明は、請求項１または２に記載の圧粉磁心用鉄基軟磁性粉末を圧縮成形して作製されたことを特徴とする圧粉磁心である。 The invention described in claim 4 is a dust core produced by compression-molding the iron-based soft magnetic powder for dust core according to claim 1 or 2.
本発明によると、入手困難で、且つ高価な希少金属を用いることなくても、Ｂ、ＭｇおよびＡｌというごく一般的な元素を添加するだけで、リン酸系化成被膜の耐熱性を改善することができ、また、そのリン酸系化成被膜とシリコーン樹脂被膜とを複合させることで、より高度な耐熱性を有する電気絶縁層を形成することができる。 According to the present invention, it is possible to improve the heat resistance of a phosphoric acid-based chemical conversion film by adding only common elements such as B, Mg and Al without using rare metals which are difficult to obtain and expensive. In addition, an electrical insulating layer having higher heat resistance can be formed by combining the phosphoric acid-based chemical conversion coating and the silicone resin coating.
また、Ｐ、Ｂ、ＭｇおよびＡｌを含有するリン酸系化成被膜を鉄基軟磁性粉末素材の表面に形成することにより、高い耐熱性、電気絶縁性を確保するこができ、更には、圧粉磁心用鉄基軟磁性粉末を用いて作製される圧粉磁心の高密度化を図ることもできる。 Moreover, by forming a phosphoric acid-based chemical conversion coating containing P, B, Mg and Al on the surface of the iron-based soft magnetic powder material, high heat resistance and electrical insulation can be ensured. It is also possible to increase the density of the powder magnetic core produced using the iron-based soft magnetic powder for powder magnetic core.
よって、本発明の圧粉磁心用鉄基軟磁性粉末を用いて製造した圧粉磁心は、高磁束密度、低鉄損、高機械的強度という交流で使用されるモータ、トランスなどの電磁気部品の磁心としての要求特性を全て満足する高性能なものとなる。 Therefore, the dust core manufactured using the iron-based soft magnetic powder for dust cores of the present invention is used for electromagnetic parts such as motors and transformers used in alternating current with high magnetic flux density, low iron loss, and high mechanical strength. High performance that satisfies all the required characteristics of the magnetic core.
本発明者らは、リン酸のみからなる被膜や、特許文献１記載のリン酸等から得られるガラス状絶縁層でなる被膜を、鉄基軟磁性粉末基材の表面に形成した後、その鉄基軟磁性粉末を圧粉成形により圧粉成形体（圧粉磁心）とし、温度を変化させてその圧粉成形体の比抵抗（μΩ・ｍ）を測定した。その結果、いずれの例も、４５０℃（窒素雰囲気下で１時間）での処理により、その比抵抗は、１０μΩ・ｍ程度にまで低下してしまことが確認された。 The present inventors formed a film made only of phosphoric acid or a film made of a glass-like insulating layer obtained from phosphoric acid described in Patent Document 1 on the surface of the iron-based soft magnetic powder substrate, and then the iron The base soft magnetic powder was compacted into a compact (compact core), and the specific resistance (μΩ · m) of the compact was measured while changing the temperature. As a result, it was confirmed that the specific resistance of each example decreased to about 10 μΩ · m by treatment at 450 ° C. (1 hour in a nitrogen atmosphere).
本発明者らが、この比抵抗の低下原因を検討したところ、リン酸系の被膜中に含有されるリン酸由来の酸素原子が、高温での熱処理中に拡散してＦｅと結合し、半導体として機能するようなＦｅの酸化物を形成するため、比抵抗を低下させていることが推測された。その理由から、このような半導体的酸化物の形成を何らかの方法で阻害することが、リン酸系被膜の熱的安定性の改善につながると考え、検討した結果、発明に至ったのが特許文献６に記載の発明である。 The present inventors examined the cause of the decrease in specific resistance. As a result, phosphoric acid-derived oxygen atoms contained in the phosphoric acid-based coating diffused during the heat treatment at high temperature and bonded to Fe, thereby forming a semiconductor. It was speculated that the specific resistance was lowered in order to form an oxide of Fe that functions as: For that reason, it was considered that inhibiting the formation of such semiconducting oxides in some way would lead to improvement in the thermal stability of the phosphoric acid-based coating, and as a result of investigation, the patent document was the result of the invention. 6. The invention described in item 6.
しかしながら、この特許文献６に記載の発明では、リン酸系化成被膜に含有させる元素のうち、ＣｏやＷなどは入手困難な希少金属であって、また、コストが高くなることが問題であり、これら希少金属に代えて、一般的な元素を添加しても、同等の効果を得ることができないかと考え、更に、鋭意、検討を進めた。その結果、リン酸系化成被膜に、これら希少金属に代えて、Ｐ、Ｂ、ＭｇおよびＡｌを含有することでも、同等の効果を得られることを見出し、本発明の完成に至った。 However, in the invention described in Patent Document 6, among the elements to be contained in the phosphoric acid-based chemical conversion coating, Co and W are rare metals that are difficult to obtain, and the problem is that the cost is high. Instead of these rare metals, we thought that it would be possible to obtain the same effect by adding a general element, and further diligently studied. As a result, it has been found that the same effect can be obtained even if P, B, Mg and Al are contained in the phosphoric acid-based chemical conversion coating instead of these rare metals, and the present invention has been completed.
以下、本発明を実施形態に基づいて更に詳細に説明する。 Hereinafter, the present invention will be described in more detail based on embodiments.
本発明の圧粉磁心用鉄基軟磁性粉末は、鉄基軟磁性粉末の表面に、内側から順に、リン酸系化成被膜、シリコーン樹脂被膜が、絶縁被膜として形成されてなるものである。これら絶縁被膜のうち、内側のリン酸系化成被膜は、電気絶縁性を確保するために、また、最表面のシリコーン樹脂被膜は、電気絶縁性の熱的安定性を向上させるためと機械的強度発現のために形成する。この圧粉磁心用鉄基軟磁性粉末は、必要に応じて圧縮成形時の摩擦を低減するための潤滑剤が配合されて圧縮成形され、主に交流で使用されるモータ、トランスなどの電磁気部品の磁心等として使用される。 The iron-based soft magnetic powder for dust core of the present invention is formed by forming a phosphoric acid-based chemical coating and a silicone resin coating as an insulating coating on the surface of the iron-based soft magnetic powder in order from the inside. Among these insulating coatings, the inner phosphoric acid-based chemical conversion coating is used to ensure electrical insulation, and the outermost silicone resin coating is used to improve the thermal stability of electrical insulation and mechanical strength. Form for expression. This iron-based soft magnetic powder for powder magnetic cores is compression-molded with a lubricant to reduce friction during compression molding as necessary, and is mainly used for AC components such as motors and transformers. Used as a magnetic core.
鉄基軟磁性粉末は、強磁性体の金属粉末であり、具体例としては、純鉄粉、鉄基合金粉末（Ｆｅ−Ａｌ合金、Ｆｅ−Ｓｉ合金、センダスト、パーマロイ等）、アモルファス粉末等を挙げることができる。このような鉄基軟磁性粉末は、例えば、アトマイズ法によって、微粒子とした後に還元し、その後、粉砕すること等によって製造することができる。このような製造法では、ふるい分け法で評価される粒度分布で、累積粒度分布が５０％になる粒径が２０〜２５０μｍ程度の鉄基軟磁性粉末が得られるが、本発明においては、平均粒径が５０〜１５０μｍ程度の鉄基軟磁性粉末を用いることが好ましい。 The iron-based soft magnetic powder is a ferromagnetic metal powder. Specific examples include pure iron powder, iron-based alloy powder (Fe-Al alloy, Fe-Si alloy, Sendust, Permalloy, etc.), amorphous powder, and the like. Can be mentioned. Such an iron-based soft magnetic powder can be produced by, for example, reducing the fine particles by the atomizing method, then reducing the fine particles, and then pulverizing. In such a production method, an iron-based soft magnetic powder having a particle size distribution evaluated by the sieving method and having a cumulative particle size distribution of 50% and a particle size of about 20 to 250 μm is obtained. It is preferable to use an iron-based soft magnetic powder having a diameter of about 50 to 150 μm.
本発明においては、圧粉磁心用鉄基軟磁性粉末の製造にあたり、まず、鉄基軟磁性粉末の表面にリン酸系化成被膜を形成する。このリン酸系化成被膜は、オルトリン酸：Ｈ３ＰＯ４（単にリン酸ともいう）などの化成処理によって生成するガラス状の被膜である。但し、本発明では、このリン酸系化成被膜が、Ｐ、Ｂ、ＭｇおよびＡｌを含有するものでなくてはならない。リン酸系化成被膜中の酸素原子が高温での熱処理中にＦｅと半導体を形成するのを阻害して、熱処理中の比抵抗の低下を抑制するために、これらの元素を併せて含有させることが特に有効であることが見出されたからである。 In the present invention, in producing the iron-based soft magnetic powder for a dust core, first, a phosphoric acid-based chemical conversion film is formed on the surface of the iron-based soft magnetic powder. This phosphoric acid-based chemical conversion film is a glassy film generated by chemical conversion treatment of orthophosphoric acid: H 3 PO 4 (also simply referred to as phosphoric acid). However, in this invention, this phosphoric acid type | system | group chemical conversion film must contain P, B, Mg, and Al. In order to prevent oxygen atoms in the phosphoric acid-based chemical conversion film from forming Fe and semiconductors during heat treatment at high temperatures, and to suppress a decrease in specific resistance during heat treatment, these elements should be included together. Is found to be particularly effective.
これらの元素の添加によって、高温熱処理中の比抵抗の低下を抑制するためには、リン酸系化成被膜が表面に形成された鉄基軟磁性粉末１００質量部に対して、Ｐ：０．０１０〜０．１００質量部、Ｂ：０．００１〜０．０１０質量部、Ｍｇ：０．００１〜０．０２０質量部、Ａｌ：０．００５〜０．０５０質量部が夫々含有されていることが好ましい。 In order to suppress the decrease in specific resistance during the high-temperature heat treatment by adding these elements, P: 0.010 with respect to 100 parts by mass of the iron-based soft magnetic powder having the phosphoric acid-based chemical conversion film formed on the surface. ~ 0.100 parts by mass, B: 0.001 to 0.010 parts by mass, Mg: 0.001 to 0.020 parts by mass, Al: 0.005 to 0.050 parts by mass, respectively. preferable.
これらの元素のうち、Ｐは酸素を介して鉄基軟磁性粉末の表面と化学結合を形成する。従って、Ｐの含有量が少なすぎると、化学結合量が不十分となり強固な被膜を形成できなくなるおそれがあり好ましくない。一方、Ｐの含有量が多すぎると、化学結合に関与しないＰが未反応のまま被膜に残留し、却って結合強度を低下させるおそれがあり好ましくない。従って、Ｐの含有量を、強固な被膜を形成する上で問題のない、０．０１０〜０．１００質量部とした。 Among these elements, P forms a chemical bond with the surface of the iron-based soft magnetic powder through oxygen. Therefore, if the P content is too small, the amount of chemical bonding is insufficient, and a strong film may not be formed. On the other hand, if the content of P is too large, P which does not participate in chemical bonding remains unreacted in the film, which may undesirably decrease the bonding strength. Therefore, the content of P is set to 0.010 to 0.100 parts by mass which causes no problem in forming a strong film.
また、Ｂ、ＭｇおよびＡｌは、高温熱処理中（高温焼鈍中）にＦｅと酸素が半導体を形成するのを阻害して、比抵抗が低下するのを抑制する作用を有する。特にこれらの元素は、複合添加することによってその作用が顕著に現れるため、Ｐと併せて必ず複合添加する必要がある。これらの元素の含有量が少なすぎると、比抵抗の低下を抑制する作用を発揮できなくなる。一方、これらの元素の含有量が多すぎると、複合添加時に相対的なバランスを維持できなくなり、また、酸素を介したＰと鉄基軟磁性粉末の表面との化学結合を阻害するおそれを生じる。従って、Ｂの含有量は０．００１〜０．０１０質量部、Ｍｇの含有量は０．００１〜０．０２０質量部、Ａｌの含有量は０．００５〜０．０５０質量部とした。 Further, B, Mg, and Al have an effect of inhibiting Fe and oxygen from forming a semiconductor during high-temperature heat treatment (during high-temperature annealing) and suppressing a decrease in specific resistance. In particular, these elements have a remarkable effect when they are added in combination. Therefore, it is necessary to always add them together with P. If the content of these elements is too small, the effect of suppressing the decrease in specific resistance cannot be exhibited. On the other hand, if the content of these elements is too large, the relative balance cannot be maintained at the time of composite addition, and the chemical bond between oxygen and the surface of the iron-based soft magnetic powder via oxygen may be hindered. . Therefore, the B content was 0.001 to 0.010 parts by mass, the Mg content was 0.001 to 0.020 parts by mass, and the Al content was 0.005 to 0.050 parts by mass.
このリン酸系化成被膜の膜厚は１〜２５０ｎｍが好ましい。膜厚が１ｎｍより薄いと絶縁効果が発現し難く、２５０ｎｍを超えると絶縁効果が飽和する上、成形される圧粉磁心の高密度化を阻害するためである。また、その付着量は、０．０１〜０．８質量部程度が好ましい。 The thickness of the phosphoric acid-based chemical conversion film is preferably 1 to 250 nm. This is because if the film thickness is less than 1 nm, the insulating effect is hardly exhibited, and if it exceeds 250 nm, the insulating effect is saturated, and the density of the molded dust core is hindered. Moreover, the adhesion amount is preferably about 0.01 to 0.8 part by mass.
リン酸系化成被膜は、水性溶媒に、Ｐ、Ｂ、ＭｇおよびＡｌを含有する化合物（元素単体でも可）等を溶解させて得たリン酸系化成処理溶液（処理液）を鉄基軟磁性粉末と混合し、乾燥させることで形成できる。具体的には、水性溶媒にオルトリン酸（Ｈ３ＰＯ４）などを溶解して、固形分０．１〜１０質量部程度の処理液とし、鉄基軟磁性粉末：１００質量部に対して、その処理液を１〜１０質量部添加して、ミキサー、ボールミル、ニーダー、Ｖ型混合機、造粒機等で混合し、大気中、減圧下、或いは真空下で、１５０〜２５０℃で乾燥すれば形成できる。 Phosphoric acid-based chemical conversion coating is a phosphate-based chemical conversion treatment solution (treatment solution) obtained by dissolving a compound containing P, B, Mg, and Al (elemental elements) in an aqueous solvent. It can be formed by mixing with powder and drying. Specifically, orthophosphoric acid (H 3 PO 4 ) or the like is dissolved in an aqueous solvent to obtain a treatment liquid having a solid content of about 0.1 to 10 parts by mass, and iron-based soft magnetic powder: 100 parts by mass, Add 1-10 parts by mass of the treatment liquid, mix with a mixer, ball mill, kneader, V-type mixer, granulator, etc., and dry at 150-250 ° C. in air, under reduced pressure, or under vacuum. Can be formed.
Ｐ、Ｂ、ＭｇおよびＡｌを含有する化合物としては、オルトリン酸（Ｈ３ＰＯ４）：Ｐ源、ホウ酸（Ｈ３ＢＯ３）：Ｂ源、酸化マグネシウム（ＭｇＯ）：Ｍｇ源、Ａｌ（Ｈ２ＰＯ４）３：ＰおよびＡｌ源、等を挙げることができる。尚、Ｂ、ＭｇおよびＡｌは、化合物とせずそのまま添加しても良い。また、水性溶媒としては、水、アルコールやケトン等の親水性有機溶媒、或いはこれらの混合物等を挙げることができる。また、この水性溶媒中には界面活性剤を添加しても良い。 As the compound containing P, B, Mg and Al, orthophosphoric acid (H 3 PO 4 ): P source, boric acid (H 3 BO 3 ): B source, magnesium oxide (MgO): Mg source, Al (H 2 PO 4 ) 3 : P and Al sources, and the like. Note that B, Mg, and Al may be added as they are without being compounded. Examples of the aqueous solvent include water, hydrophilic organic solvents such as alcohol and ketone, and mixtures thereof. Further, a surfactant may be added to this aqueous solvent.
次に、リン酸系化成被膜の上にシリコーン樹脂被膜を形成する。このシリコーン樹脂被膜を構成するシリコーン樹脂は、その架橋・硬化反応終了時（圧粉磁心の成形時）に、粉末同士が強固に結合するので、成形される圧粉磁心の機械的強度が増大する。また、耐熱性に優れたＳｉ−Ｏ結合を形成して熱的安定性に優れた絶縁被膜となる。 Next, a silicone resin film is formed on the phosphoric acid-based chemical conversion film. Since the silicone resin constituting the silicone resin coating is firmly bonded to each other at the end of the crosslinking / curing reaction (when the dust core is molded), the mechanical strength of the molded dust core is increased. . In addition, an Si—O bond having excellent heat resistance is formed to provide an insulating film having excellent thermal stability.
このシリコーン樹脂としては、硬化が遅くなると粉末がべとついて被膜形成後のハンドリング性が悪くなる二官能性のＤ単位（Ｒ２ＳｉＸ２：Ｘは加水分解性基）よりは、三官能性のＴ単位（ＲＳｉＸ３：Ｘは加水分解性基）を多く含有する方が好ましい。また、四官能性のＱ単位（ＳｉＸ４：Ｘは加水分解性基）が多く含まれていると、後述する予備硬化の際に粉末同士が強固に結着してしまい、後の成形が行えなくなることがあるので好ましくない。よって、Ｔ単位が６０モル％以上、好ましくは８０モル％以上、最も好ましくは全てがＴ単位のシリコーン樹脂被膜が形成されていることが推奨される。 This silicone resin is more trifunctional than the bifunctional D unit (R 2 SiX 2 : X is a hydrolyzable group) that the powder becomes sticky when curing is delayed and the handling properties after film formation are poor. It is preferable to contain a lot of T units (RSiX 3 : X is a hydrolyzable group). Moreover, when many tetrafunctional Q units (SiX 4 : X is a hydrolyzable group) are contained, the powders are firmly bound during pre-curing described later, and subsequent molding can be performed. Since it may disappear, it is not preferable. Therefore, it is recommended that a silicone resin film having a T unit of 60 mol% or more, preferably 80 mol% or more, and most preferably all of T units is formed.
よって、本発明では、シリコーン樹脂としては、メチル基が５０モル％以上のメチルフェニルシリコーン樹脂を用いることが好ましく、また、メチル基が７０モル％以上のメチルフェニルシリコーン樹脂を用いることがより好ましく、フェニル基が全く存在しないメチルフェニルシリコーン樹脂を用いることが最も好ましい。メチル基が５０モル％以上のメチルフェニルシリコーン樹脂としては、信越化学工業製のＫＲ２５５、ＫＲ３１１を、メチル基が７０モル％以上のメチルフェニルシリコーン樹脂としては、信越化学工業製のＫＲ３００を、フェニル基が全く存在しないメチルフェニルシリコーン樹脂としては、信越化学工業製のＫＲ２５１、ＫＲ４００、ＫＲ２２０Ｌ、ＫＲ２４２Ａ、ＫＲ２４０、ＫＲ５００、ＫＣ８９、また、東レダウコーニング社製のＳＲ２４００を、夫々例示することができる。尚、シリコーン樹脂のメチル基とフェニル基の比率や官能性については、ＦＴ−ＩＲ等で分析することができる。 Therefore, in the present invention, as the silicone resin, it is preferable to use a methylphenyl silicone resin having a methyl group of 50 mol% or more, and more preferable to use a methylphenylsilicone resin having a methyl group of 70 mol% or more. Most preferably, a methylphenyl silicone resin having no phenyl groups is used. As methylphenyl silicone resins having a methyl group of 50 mol% or more, KR255 and KR311 manufactured by Shin-Etsu Chemical Co., Ltd., and as methylphenyl silicone resins having a methyl group of 70 mol% or more, KR300 manufactured by Shin-Etsu Chemical Co., Ltd. Examples of the methylphenyl silicone resin in which no is present include KR251, KR400, KR220L, KR242A, KR240, KR500, KC89 manufactured by Shin-Etsu Chemical Co., Ltd., and SR2400 manufactured by Toray Dow Corning Co., Ltd. The ratio and functionality of the methyl group and phenyl group of the silicone resin can be analyzed by FT-IR or the like.
このシリコーン樹脂被膜の膜厚は１〜３００ｎｍが好ましい。より好ましい膜厚は１０〜２００ｎｍである。また、その付着量は、リン酸系化成被膜が表面に形成された鉄基軟磁性粉末と、シリコーン樹脂被膜の合計を１００質量部としたとき、０．０１〜０．５質量部であることが好ましい。０．０１質量部より少ないと、絶縁性に劣り、電気抵抗が低くなる。また、０．５質量部より多いと、圧粉磁心の高密度化ができにくくなる。 The thickness of the silicone resin film is preferably 1 to 300 nm. A more preferable film thickness is 10 to 200 nm. Moreover, the adhesion amount is 0.01-0.5 mass part, when the total of the iron-based soft magnetic powder having the phosphoric acid-based chemical conversion film formed on the surface and the silicone resin film is 100 mass parts. Is preferred. When the amount is less than 0.01 parts by mass, the insulating property is inferior and the electrical resistance is lowered. On the other hand, when the amount is more than 0.5 parts by mass, it is difficult to increase the density of the dust core.
また、シリコーン樹脂被膜とリン酸系化成被膜を合わせた厚みは５００ｎｍ以下であることが好ましい。合計膜厚が５００ｎｍを超えると磁束密度の低下が大きくなることがある。 Further, the total thickness of the silicone resin film and the phosphoric acid-based chemical film is preferably 500 nm or less. When the total film thickness exceeds 500 nm, the decrease in magnetic flux density may increase.
リン酸系化成被膜の表面に、シリコーン樹脂被膜を形成するには、アルコール類やトルエン、キシレン等の石油系有機溶剤などにシリコーン樹脂を溶解させて、そのシリコーン樹脂と鉄基軟磁性粉末とを混合した後、有機溶媒を揮発させれば良い。このシリコーン樹脂被膜の形成条件は特に限定されるわけではないが、固形分が２〜１０質量部になるように調製したシリコーン樹脂溶液を、リン酸系化成被膜が表面に形成された鉄基軟磁性粉末：１００質量部に対して、０．５〜１０質量部添加し、混合して乾燥することが好ましい。シリコーン樹脂溶液の添加量が０．５質量部より少ないと、混合に時間がかかりすぎたり、形成される被膜が不均一になったりするおそれがある。一方、シリコーン樹脂溶液の添加量が１０質量部を超えると、乾燥に時間がかかりすぎたり、乾燥が不十分になったりするおそれがある。尚、シリコーン樹脂溶液は適宜加熱しておいても構わない。また、これらの混合には、ミキサー、ボールミル、ニーダー、Ｖ型混合機、造粒機等を用いることができる。 In order to form a silicone resin coating on the surface of the phosphoric acid-based chemical conversion coating, the silicone resin is dissolved in a petroleum-based organic solvent such as alcohol, toluene, xylene, etc., and the silicone resin and the iron-based soft magnetic powder are mixed. After mixing, the organic solvent may be volatilized. The conditions for forming this silicone resin coating are not particularly limited, but a silicone resin solution prepared so that the solid content is 2 to 10 parts by mass is obtained from an iron-based soft coating with a phosphate-based chemical conversion coating formed on the surface. Magnetic powder: It is preferable to add 0.5 to 10 parts by mass with respect to 100 parts by mass, mix and dry. When the addition amount of the silicone resin solution is less than 0.5 parts by mass, it may take too much time for mixing, or the formed film may be nonuniform. On the other hand, when the addition amount of the silicone resin solution exceeds 10 parts by mass, drying may take too much time or drying may be insufficient. The silicone resin solution may be appropriately heated. Moreover, a mixer, a ball mill, a kneader, a V-type mixer, a granulator, etc. can be used for these mixing.
このシリコーン樹脂被膜形成における最後の乾燥工程においては、シリコーン樹脂被膜の形成に用いた有機溶剤が揮発する温度で、且つ、シリコーン樹脂の硬化温度未満の温度に加熱して、有機溶剤を十分に蒸発揮散させることが好ましい。具体的な乾燥温度としては、有機溶剤がアルコール類や石油系有機溶剤である場合は、６０〜８０℃程度が好適な温度である。また、その乾燥後には、凝集ダマを除くために、シリコーン樹脂被膜が最表面に形成された鉄基軟磁性粉末（圧粉磁心用鉄基軟磁性粉末）を、目開き３００〜５００μｍ程度の篩に通過させておくことが好ましい。 In the final drying step in this silicone resin film formation, the organic solvent used to form the silicone resin film is heated to a temperature at which the organic solvent volatilizes and is lower than the curing temperature of the silicone resin to sufficiently evaporate the organic solvent. It is preferable to volatilize. As a specific drying temperature, when the organic solvent is an alcohol or a petroleum organic solvent, about 60 to 80 ° C. is a suitable temperature. Further, after the drying, in order to remove agglomeration, an iron-based soft magnetic powder (iron-based soft magnetic powder for a dust core) having a silicone resin coating formed on the outermost surface is sieved with a sieve having an opening of about 300 to 500 μm. It is preferable to let it pass through.
乾燥後には、シリコーン樹脂被膜を予備硬化させることが推奨される。予備硬化とは、シリコーン樹脂被膜の硬化時における軟化過程を圧粉磁心用鉄基軟磁性粉末が粉末状態のまま終了させる処理のことをいう。この予備硬化処理によって、１００〜２５０℃程度での温間成形時に圧粉磁心用鉄基軟磁性粉末の流れ性を確保することができる。具体的な手法としては、圧粉磁心用鉄基軟磁性粉末を、そのシリコーン樹脂の硬化温度近傍で短時間加熱する方法が簡便であるが、硬化剤を用いる手法も採用することができる。尚、予備硬化処理と硬化（完全硬化）処理の違いは、予備硬化処理では、圧粉磁心用鉄基軟磁性粉末同士が完全に接着固化することなく、容易に解砕することが可能であるのに対し、圧粉磁心用鉄基軟磁性粉末の成形後に行う高温加熱硬化処理（完全硬化処理）では、シリコーン樹脂が硬化して圧粉磁心用鉄基軟磁性粉末同士が接着固化する点である。この完全硬化処理によって、圧粉磁心の成形体強度が向上する。 It is recommended to pre-cure the silicone resin coating after drying. Pre-curing refers to a process in which the softening process at the time of curing the silicone resin coating is completed while the iron-based soft magnetic powder for dust core is in a powder state. By this pre-curing treatment, the flowability of the iron-based soft magnetic powder for dust core can be ensured during warm forming at about 100 to 250 ° C. As a specific method, a method of heating the iron-based soft magnetic powder for dust core in the vicinity of the curing temperature of the silicone resin for a short time is simple, but a method using a curing agent can also be employed. The difference between the pre-curing process and the curing (complete curing) process is that the pre-curing process can be easily crushed without causing the iron-based soft magnetic powders for dust cores to be completely bonded and solidified. On the other hand, in the high-temperature heat-curing process (complete curing process) performed after molding of the iron-based soft magnetic powder for dust core, the silicone resin is cured and the iron-based soft magnetic powder for dust core is bonded and solidified. is there. By this complete curing treatment, the strength of the compact of the dust core is improved.
以上のように、シリコーン樹脂被膜を予備硬化させた後、解砕することで、流動性に優れた圧粉磁心用鉄基軟磁性粉末を得ることができ、続く工程の圧縮成形の際に、成形型へ砂のような状態で圧粉磁心用鉄基軟磁性粉末をスムーズに投入することができるようになる。予備硬化させない場合は、温間成形時等に圧粉磁心用鉄基軟磁性粉末が付着してスムーズに成形型へ投入することができなくなることがある。また、予備硬化させることで、最終的に得られる圧粉磁心の比抵抗が非常に向上する。その理由は明確ではないが、硬化の際に圧粉磁心用鉄基軟磁性粉末との密着性が上がるためではないかと考えられる。 As described above, after pre-curing the silicone resin coating, it can be crushed to obtain an iron-based soft magnetic powder for a dust core excellent in fluidity, and at the time of compression molding in the subsequent process, The iron-based soft magnetic powder for dust core can be smoothly put into the mold in a sandy state. If it is not pre-cured, the iron-based soft magnetic powder for the dust core may adhere to the molding die during warm molding or the like and may not be smoothly put into the mold. Moreover, the specific resistance of the finally obtained dust core is greatly improved by pre-curing. The reason for this is not clear, but it is thought to be because the adhesion with the iron-based soft magnetic powder for dust cores is increased during curing.
短時間加熱法によって、予備硬化を行う場合、１００〜２００℃で５〜１００分の加熱処理を行うと良い。また、１３０〜１７０℃で１０〜３０分の加熱処理を行うことがより好ましい。予備硬化後の圧粉磁心用鉄基軟磁性粉末も、目開き３００〜５００μｍ程度の篩を通過させておくことが好ましい。 When pre-curing is performed by a short-time heating method, heat treatment at 100 to 200 ° C. for 5 to 100 minutes is preferable. Moreover, it is more preferable to perform the heat processing for 10 to 30 minutes at 130-170 degreeC. The pre-cured iron-based soft magnetic powder for a dust core is preferably passed through a sieve having an opening of about 300 to 500 μm.
本発明の圧粉磁心用鉄基軟磁性粉末には、更に潤滑剤が含有されていても良い。この潤滑剤の作用により、圧粉磁心用鉄基軟磁性粉末を圧縮成形する際の圧粉磁心用鉄基軟磁性粉末間、或いは、圧粉磁心用鉄基軟磁性粉末と成形型の内壁間の摩擦抵抗を低減することができ、成形体の型かじりの発生や成形時の発熱を抑制することができる。このような効果を有効に発揮させるためには、圧粉磁心用鉄基軟磁性粉末全量中、潤滑剤が０．２質量部以上含有されていることが好ましい。しかし、潤滑剤の含有量が多くなりすぎると、圧粉磁心の高密度化に影響を及ぼすため、その含有量は多くとも０．８質量部にとどめておくことが好ましい。尚、圧縮成形する際に、成形型の内壁面に潤滑剤を塗布した後に成形する型潤滑成形を実施する場合は、潤滑剤の含有量は０．２質量部未満であっても構わない。 The iron-based soft magnetic powder for dust core of the present invention may further contain a lubricant. Due to the action of this lubricant, between the iron-based soft magnetic powder for dust core when compressing the iron-based soft magnetic powder for dust core, or between the iron-based soft magnetic powder for dust core and the inner wall of the mold The frictional resistance of the molded body can be reduced, and the occurrence of mold galling and the heat generation during molding can be suppressed. In order to effectively exhibit such an effect, it is preferable that 0.2 parts by mass or more of the lubricant is contained in the total amount of the iron-based soft magnetic powder for dust core. However, if the content of the lubricant is excessively large, the density of the dust core is affected. Therefore, the content is preferably kept at 0.8 parts by mass at the most. In addition, when carrying out the mold | die lubrication molding which shape | molds after apply | coating a lubricant to the inner wall surface of a shaping | molding die at the time of compression molding, content of a lubricant may be less than 0.2 mass part.
尚、この潤滑剤としては、ステアリン酸亜鉛、ステアリン酸カルシウムなどのステアリン酸の金属塩粉末、パラフィン、ワックス、天然樹脂誘導体、合成樹脂誘導体等を挙げることができる。 Examples of the lubricant include metal salt powders of stearic acid such as zinc stearate and calcium stearate, paraffin, wax, natural resin derivatives, and synthetic resin derivatives.
この圧粉磁心用鉄基軟磁性粉末を用いて圧粉磁心を作製するにあたっては、先に説明したように、まず、圧粉磁心用鉄基軟磁性粉末を成形型に投入して圧縮成形する。この圧縮成形法は特に限定されないが、従来から公知の圧縮成形法を採用することが可能である。次に、その圧縮成形法の一例を説明する。 In producing a dust core using the iron-based soft magnetic powder for dust core, as described above, first, the iron-based soft magnetic powder for dust core is put into a mold and compression-molded. . Although this compression molding method is not particularly limited, a conventionally known compression molding method can be employed. Next, an example of the compression molding method will be described.
圧縮成形の好適な条件は、面圧で、４９０〜１９６０ＭＰａ、より好ましくは７９０〜１１８０ＭＰａである。その中でも、特に９８０ＭＰａ以上の条件で圧縮成形を行うと、密度が７．５０ｇ／ｃｍ３の圧縮磁心を得やすくなり、高密度で磁気特性（磁束密度）に優れた圧縮磁心を得ることが可能になるため好ましい。また、成形温度は、室温成形、温間成形（１００〜２５０℃）のいずれであっても構わないが、型潤滑成形で温間成形を行う方が、より高強度の圧縮磁心を得ることができるため好ましい。 A suitable condition for the compression molding is a surface pressure of 490 to 1960 MPa, more preferably 790 to 1180 MPa. Among them, especially when compression molding is performed under a condition of 980 MPa or more, it becomes easy to obtain a compression core having a density of 7.50 g / cm 3, and a compression core having high density and excellent magnetic properties (magnetic flux density) can be obtained. Therefore, it is preferable. The molding temperature may be either room temperature molding or warm molding (100 to 250 ° C.), but a higher strength compression magnetic core can be obtained by performing warm molding with mold lubrication molding. This is preferable because it is possible.
圧縮成形後は、圧縮磁心のヒステリシス損を低減するため、高温で熱処理（焼鈍）を行う。このときの熱処理温度は４００℃以上の高温であることが好ましく、比抵抗の劣化がなければ、更に高温で熱処理することが好ましい。熱処理雰囲気は、酸素を含まなければ特に限定されないが、窒素等の不活性雰囲気下が好ましい。また、熱処理時間は、比抵抗の劣化がなければ特に限定されないが、２０分以上が好ましく、３０分以上がより好ましく、１時間以上が更に好ましい。 After compression molding, heat treatment (annealing) is performed at a high temperature in order to reduce the hysteresis loss of the compression core. The heat treatment temperature at this time is preferably a high temperature of 400 ° C. or higher, and if the specific resistance is not deteriorated, the heat treatment is preferably performed at a higher temperature. The heat treatment atmosphere is not particularly limited as long as it does not contain oxygen, but is preferably an inert atmosphere such as nitrogen. Further, the heat treatment time is not particularly limited as long as the specific resistance is not deteriorated, but is preferably 20 minutes or more, more preferably 30 minutes or more, and further preferably 1 hour or more.
以下、実施例を挙げて本発明をより具体的に説明するが、本発明はもとより下記実施例によって制限を受けるものではなく、本発明の趣旨に適合し得る範囲で適宜変更を加えて実施することも可能であり、それらは何れも本発明の技術的範囲に含まれる。 EXAMPLES Hereinafter, the present invention will be described more specifically with reference to examples. However, the present invention is not limited by the following examples, and the present invention is implemented with appropriate modifications within a range that can meet the gist of the present invention. These are all included in the technical scope of the present invention.
鉄基軟磁性粉末としては、純鉄粉（神戸製鋼所製、アトメル３００ＮＨ、平均粒径８０〜１００μｍ）を用いた。比較例１では、水：１０００質量部、Ｈ３ＰＯ４：１９３質量部を、比較例２では、水：１０００質量部、Ｈ３ＰＯ４：１９３質量部、ＭｇＯ：３１質量部、Ｈ３ＢＯ３：３０質量部を、比較例３および比較例４では、水：１０００質量部、ＮａＨＰＯ４：８８．５質量部、Ｈ３ＰＯ４：１８１質量部、Ｈ２ＳＯ４：６１質量部、Ｃｏ３（ＰＯ４）２：３０質量部を、発明例５および発明例６では、水：１０００質量部、Ｈ３ＰＯ４：１９３質量部、ＭｇＯ：３１質量部、Ｈ３ＢＯ３：３０質量部、Ａｌ（Ｈ２ＰＯ４）３：３２３質量部を、夫々原液とし、１０倍に希釈した処理液を、前記純鉄粉１００質量部に対して５質量部添加し、Ｖ型混合機を用いて３０分以上混合した後、２００℃の大気中で３０分乾燥し、目開き３００μｍのふるいに通した。 As the iron-based soft magnetic powder, pure iron powder (manufactured by Kobe Steel, Atmel 300NH, average particle size of 80 to 100 μm) was used. In Comparative Example 1, water: 1000 parts by mass, H 3 PO 4 : 193 parts by mass, and in Comparative Example 2, water: 1000 parts by mass, H 3 PO 4 : 193 parts by mass, MgO: 31 parts by mass, H 3 BO. 3 : 30 parts by mass, in Comparative Example 3 and Comparative Example 4, water: 1000 parts by mass, NaHPO 4 : 88.5 parts by mass, H 3 PO 4 : 181 parts by mass, H 2 SO 4 : 61 parts by mass, Co 3 (PO 4 ) 2 : 30 parts by mass, in Invention Example 5 and Invention Example 6, water: 1000 parts by mass, H 3 PO 4 : 193 parts by mass, MgO: 31 parts by mass, H 3 BO 3 : 30 parts by mass , Al (H 2 PO 4 ) 3 : 323 parts by mass, respectively, 5 parts by mass of a 10-fold diluted treatment liquid was added to 100 parts by mass of the pure iron powder, and a V-type mixer was used. For 30 minutes or more, then dry in the atmosphere at 200 ° C for 30 minutes. And it was passed through a sieve having a mesh opening 300μm.
次に、フェニル基が存在しないメチルフェニルシリコーン樹脂をトルエンに溶解させて、固形分濃度が５％（比較例１〜３、発明例５）或いは１０％（比較例４、発明例６）の樹脂溶液を作製し、それら樹脂溶液を純鉄粉に対して樹脂固形分が、０．１％（比較例１〜３、発明例５）或いは０．２％（比較例４、発明例６）となるように添加混合し、２００℃の大気中で３０分乾燥した後、１５０℃で３０分の予備硬化処理を行った。 Next, a methylphenyl silicone resin having no phenyl group is dissolved in toluene, and the solid content concentration is 5% (Comparative Examples 1 to 3, Invention Example 5) or 10% (Comparative Example 4 and Invention Example 6). Solutions are prepared, and the resin solid content of these resin solutions is 0.1% (Comparative Examples 1-3, Invention Example 5) or 0.2% (Comparative Example 4, Invention Example 6) with respect to pure iron powder. The mixture was added and mixed so that it was dried in air at 200 ° C. for 30 minutes, and then pre-cured at 150 ° C. for 30 minutes.
作製した粉末を１３０℃に加熱した後、同じく１３０℃に加熱した金型を用い、その金型の表面にステアリン酸亜鉛をアルコールに分散させて塗布し、面圧１１７６ＭＰａで圧粉成形を行った。成形体の寸法は、３１．７５ｍｍ×１２．７ｍｍ×約５ｍｍである。その後、窒素雰囲気下で、全ての比較例、発明例共に、５５０℃と６００℃の２種類の条件で、３０分の加熱を行った。 The prepared powder was heated to 130 ° C., and then a mold heated to 130 ° C. was used, and zinc stearate was dispersed and applied to the surface of the mold and compacted at a surface pressure of 1176 MPa. . The size of the molded body is 31.75 mm × 12.7 mm × about 5 mm. Thereafter, heating was performed for 30 minutes in a nitrogen atmosphere under the two conditions of 550 ° C. and 600 ° C. for all of the comparative examples and the inventive examples.
得られた成形体の密度、抗折強度（３点曲げ試験：日本粉末冶金工業会のＪＰＭＡ Ｍ ０９−１９９２に準拠）、並びに比抵抗を測定した。その測定結果を、前記成形体の製造条件の詳細と共に、表１に示す。 The density, bending strength (three-point bending test: based on JPMA M 09-1992 of Japan Powder Metallurgy Industry Association), and specific resistance of the obtained molded body were measured. The measurement results are shown in Table 1 together with details of the manufacturing conditions of the molded body.
比較例１は、鉄基軟磁性粉末の表面にＰを含有するリン酸系化成被膜を形成したもの、比較例２は、鉄基軟磁性粉末の表面にＰ、Ｂ、Ｍｇを含有するリン酸系化成被膜を形成したものである。また、比較例３および比較例４は、鉄基軟磁性粉末の表面にＰ、Ｎａ、Ｓ、Ｃｏを含有するリン酸系化成被膜を形成したものであり、成形体密度、抗折強度、比抵抗が優れているという結果が既に得られているが、入手困難な希少金属であるＣｏを添加元素として用いる必要があるものである。一方、発明例５および６は、添加元素は容易に入手できる一般的な元素のみであり、鉄基軟磁性粉末の表面にＰ、Ｂ、Ｍｇ、Ａｌを含有するリン酸系化成被膜を形成したものである。 Comparative Example 1 is one in which a phosphoric acid-based chemical conversion film containing P is formed on the surface of an iron-based soft magnetic powder, and Comparative Example 2 is phosphoric acid containing P, B, and Mg on the surface of an iron-based soft magnetic powder. A system conversion coating is formed. Comparative Example 3 and Comparative Example 4 are obtained by forming a phosphoric acid-based chemical conversion film containing P, Na, S, Co on the surface of the iron-based soft magnetic powder, and the compact density, bending strength, ratio Although the result that resistance is excellent has already been obtained, it is necessary to use Co which is a rare metal which is difficult to obtain as an additional element. On the other hand, in Invention Examples 5 and 6, the additive element is only a general element that can be easily obtained, and a phosphate-based chemical conversion film containing P, B, Mg, and Al is formed on the surface of the iron-based soft magnetic powder. Is.
表１によると、鉄基軟磁性粉末の表面にＰ、Ｂ、Ｍｇ、Ａｌを含有するリン酸系化成被膜を形成した発明例５および発明例６は、鉄基軟磁性粉末の表面にＰ、Ｎａ、Ｓ、Ｃｏを含有するリン酸系化成被膜を形成した比較例３および比較例４と比べて、成形体密度、抗折強度、比抵抗には何ら遜色がなく、成形体密度、抗折強度、比抵抗のバランスに優れていることが分かる。また、発明例５および発明例６は、熱処理温度を５５０℃とした場合は、むしろ、比較例３および比較例４よりも比抵抗が優れており、熱処理温度を６００℃とした場合は、むしろ、比較例３および比較例４よりも抗折強度が優れているという測定結果を得ることができた。 According to Table 1, Invention Example 5 and Invention Example 6 in which a phosphoric acid-based chemical conversion film containing P, B, Mg, Al is formed on the surface of the iron-based soft magnetic powder have P, Compared with Comparative Example 3 and Comparative Example 4 in which a phosphoric acid-based chemical conversion film containing Na, S, and Co was formed, the molded body density, the bending strength, and the specific resistance were not inferior, and the molded body density and the bending strength were the same. It can be seen that the balance of strength and specific resistance is excellent. Inventive Example 5 and Inventive Example 6 are more excellent in specific resistance than Comparative Example 3 and Comparative Example 4 when the heat treatment temperature is 550 ° C., and rather when the heat treatment temperature is 600 ° C. The measurement result that the bending strength was superior to Comparative Example 3 and Comparative Example 4 could be obtained.
尚、鉄基軟磁性粉末の表面にＰ、Ｂ、Ｍｇを含有するリン酸系化成被膜を形成した場合、すなわちＡｌを添加元素として用いなかった比較例２では、比較例１と比べても優れた測定結果を得ることができなかった。 In addition, when the phosphoric acid-based chemical conversion film containing P, B, and Mg is formed on the surface of the iron-based soft magnetic powder, that is, Comparative Example 2 in which Al is not used as an additive element, it is superior to Comparative Example 1. Measurement results could not be obtained.
Claims (4)
前記リン酸系化成被膜には、Ｐ、Ｂ、ＭｇおよびＡｌが含有されていることを特徴とする圧粉磁心用鉄基軟磁性粉末。 On the surface of the iron-based soft magnetic powder, a phosphoric acid-based chemical conversion coating and a silicone resin coating are formed in order from the inside.
An iron-based soft magnetic powder for a dust core, wherein the phosphoric acid-based chemical conversion film contains P, B, Mg and Al.
Ｂ、ＭｇおよびＡｌを含有するリン酸系化成処理溶液と鉄基軟磁性粉末とを混合した後、水および／または有機溶媒を蒸発させてリン酸系化成被膜を前記鉄基軟磁性粉末の表面に形成する工程と、
シリコーン樹脂を有機溶媒に溶解し、このシリコーン樹脂溶液と、前記リン酸系化成被膜が表面に形成された鉄基軟磁性粉末とを混合した後、溶媒を蒸発させてシリコーン樹脂被膜を前記リン酸系化成被膜の上に形成する工程とを含むことを特徴とする圧粉磁心用鉄基軟磁性粉末の製造方法。 A method for producing an iron-based soft magnetic powder for a dust core according to claim 1 or 2,
After mixing the phosphoric acid-based chemical conversion treatment solution containing B, Mg and Al and the iron-based soft magnetic powder, water and / or an organic solvent is evaporated to form a phosphate-based chemical conversion coating on the surface of the iron-based soft magnetic powder. Forming the step,
A silicone resin is dissolved in an organic solvent, and the silicone resin solution is mixed with the iron-based soft magnetic powder having the phosphoric acid-based chemical conversion film formed on the surface, and then the solvent is evaporated to form the silicone resin film with the phosphoric acid. A method for producing an iron-based soft magnetic powder for a dust core, comprising the step of forming on a chemical conversion coating.
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| JP2014135491A (en) * | 2013-01-10 | 2014-07-24 | Robert Bosch Gmbh | Soft magnetic composite material and method for producing said material |
| CN104028748A (en) * | 2014-05-28 | 2014-09-10 | 浙江大学 | Surface boronizing insulation coating method of soft magnet compound materials |
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| CN104505209B (en) * | 2014-12-22 | 2017-09-29 | 合肥工业大学 | A kind of soft magnetic metal composite core and preparation method thereof |
| CN115428103A (en) * | 2020-04-02 | 2022-12-02 | 杰富意钢铁株式会社 | Iron-based soft magnetic powder for dust core, and method for producing same |
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