JP4480627B2 - Composite soft magnetic powder and method for producing the same - Google Patents
Composite soft magnetic powder and method for producing the same Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims description 62
- 239000006247 magnetic powder Substances 0.000 title claims description 26
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 162
- 239000011777 magnesium Substances 0.000 claims description 103
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 87
- 229910052742 iron Inorganic materials 0.000 claims description 53
- 229910052749 magnesium Inorganic materials 0.000 claims description 43
- 229910017135 Fe—O Inorganic materials 0.000 claims description 41
- 239000000696 magnetic material Substances 0.000 claims description 26
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 25
- 229910052717 sulfur Inorganic materials 0.000 claims description 25
- 239000011593 sulfur Substances 0.000 claims description 25
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 22
- 239000000243 solution Substances 0.000 claims description 15
- 239000013078 crystal Substances 0.000 claims description 14
- 239000006104 solid solution Substances 0.000 claims description 7
- 238000010304 firing Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 6
- 238000000151 deposition Methods 0.000 claims description 5
- -1 magnesium alkoxide Chemical class 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 239000000843 powder Substances 0.000 description 22
- 239000012298 atmosphere Substances 0.000 description 15
- 229910000859 α-Fe Inorganic materials 0.000 description 13
- 230000004907 flux Effects 0.000 description 11
- 239000011812 mixed powder Substances 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 8
- 230000001590 oxidative effect Effects 0.000 description 8
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- 230000008021 deposition Effects 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 238000005452 bending Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 239000000700 radioactive tracer Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000000682 scanning probe acoustic microscopy Methods 0.000 description 2
- 229920002050 silicone resin Polymers 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Description
この発明は、少なくとも（Ｍｇ，Ｆｅ）Ｏを含むＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜が鉄粉末の表面に被覆されてなるＭｇ含有酸化鉄膜被覆鉄粉末の表面にさらにＭｇＯ−ＳｉＯ２系複合酸化物膜（好ましくはモル比でＭｇＯ／ＳｉＯ２の値が２のフォレストライト）を被覆してなる複合軟磁性粉末に関するものであり、この複合軟磁性粉末を使用して作製した高強度、高磁束密度および高抵抗を有する鉄損の少ない複合軟磁性材に関するものであり、そして、この高強度、高磁束密度および高抵抗を有する鉄損の少ない複合軟磁性材は、低鉄損を必要とする各種電磁気回路部品、例えば、モータ、アクチュエータ、ヨーク、ローター、コア、リアクトルなどの各種電磁気部品の素材として使用することができるものである。 According to the present invention, the Mg-Fe-O ternary oxide deposit film containing at least (Mg, Fe) O is coated on the surface of the iron powder, and the Mg-containing iron oxide film-coated iron powder is further coated with MgO-SiO The present invention relates to a composite soft magnetic powder formed by coating a two- system composite oxide film (preferably a forestlite having a molar ratio of MgO / SiO 2 of 2). The present invention relates to a composite soft magnetic material with low iron loss having strength, high magnetic flux density and high resistance, and this low strength iron composite material having high strength, high magnetic flux density and high resistance has low iron loss. It can be used as a material for various electromagnetic circuit components that require a large amount of electromagnetic components such as motors, actuators, yokes, rotors, cores, reactors, and the like.
一般に、各種電磁気回路部品に使用される軟磁性材は、鉄損が小さいことが要求されるため、電気抵抗を高くして渦電流損を低減させ、保磁力を小さくしてヒステリシス損を低減させることは一般に知られている。さらに、近年、電磁気回路の小型化、高応答化が求められているところから、磁束密度がより高いことも重要視されている。 In general, soft magnetic materials used in various electromagnetic circuit components are required to have low iron loss. Therefore, electrical resistance is increased to reduce eddy current loss, and coercive force is reduced to reduce hysteresis loss. It is generally known. Further, in recent years, since the miniaturization and high response of the electromagnetic circuit are demanded, it is important to have a higher magnetic flux density.
かかる高比抵抗を有する軟磁性材料を製造するための原料粉末の一例として鉄粉末の表面に化学的な方法によりＭｇ含有フェライト膜を被覆したＭｇ含有酸化鉄膜被覆鉄粉末が知られており（特許文献１参照）、この化学的な方法によりＭｇ含有フェライト膜を被覆したＭｇ含有酸化鉄膜被覆鉄粉末を低融点ガラス粉末と共に混合して混合粉末を作製し、この混合粉末を圧縮成形し熱処理して圧粉磁性材料などを製造する方法も知られている（特許文献２または３参照）。
しかし、従来のＭｇ含有フェライト膜を被覆したＭｇ含有酸化鉄膜被覆鉄粉末は、鉄粉末の表面にＭｇ含有フェライト膜を化学的方法により被覆するために、プレス成形した圧粉体に高温歪取り焼成を行って得られた複合軟磁性材は、フェライト膜が不安定となり変化して絶縁性が低下すると共に、鉄粉末の表面に対するＭｇ含有フェライト膜の密着性が十分でなく、従来のＭｇ含有フェライト膜を被覆したＭｇ含有酸化鉄膜被覆鉄粉末をプレス成形したのち焼成しても十分な強度の複合軟磁性材を作製することができず、また従来の複合粉末を使用して作製した複合軟磁性材はプレス成形中にＭｇ含有フェライト膜が剥離したり破れるなどして十分な絶縁効果が発揮できず、したがって、十分な高比抵抗が得られないという問題点があった。 However, the conventional iron powder coated with Mg-containing iron oxide film coated with Mg-containing ferrite film has a high-temperature strain-relief effect on press-molded green compacts to coat the Mg-containing ferrite film on the surface of the iron powder by a chemical method. In the composite soft magnetic material obtained by firing, the ferrite film becomes unstable and changes, resulting in a decrease in insulation, and the adhesion of the Mg-containing ferrite film to the surface of the iron powder is not sufficient. A composite soft magnetic material with sufficient strength cannot be produced even if it is fired after press-molding iron powder coated with Mg-containing iron oxide film coated with ferrite film, and composite produced using conventional composite powder The soft magnetic material has a problem that the Mg-containing ferrite film is peeled off or torn during press molding so that a sufficient insulation effect cannot be exhibited, and therefore a sufficiently high specific resistance cannot be obtained.
本発明者らは、かかる問題点を解決するために、先に、
（ａ）少なくとも（Ｍｇ，Ｆｅ）Ｏを含むＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜が鉄粉末の表面に被覆されているＭｇ含有酸化鉄膜被覆鉄粉末、
（ｂ）少なくとも（Ｍｇ，Ｆｅ）Ｏを含むＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜が鉄粉末の表面に被覆されているＭｇ含有酸化鉄膜被覆鉄粉末であって、前記鉄粉末と前記少なくとも（Ｍｇ，Ｆｅ）Ｏを含むＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜との界面領域に、鉄粉末の中心部に含まれる硫黄よりも高濃度の硫黄を含む硫黄濃化層を有するＭｇ含有酸化鉄膜被覆鉄粉末、
（ｃ）前記Ｍｇ含有酸化膜被覆鉄粉末のＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜に含まれる（Ｍｇ，Ｆｅ）Ｏは、結晶質のＭｇＯ固溶ウスタイト相である前記（ａ）または（ｂ）記載のＭｇ含有酸化膜被覆鉄粉末、
（ｄ）前記少なくとも（Ｍｇ，Ｆｅ）Ｏを含むＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜は、結晶粒径：２００ｎｍ以下の微細結晶組織を有する前記（ａ）、（ｂ）または（ｃ）記載のＭｇ含有酸化鉄膜被覆鉄粉末、
（ｅ）前記少なくとも（Ｍｇ，Ｆｅ）Ｏを含むＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜は、その最表面が実質的にＭｇＯで構成されている前記（ａ）、（ｂ）、（ｃ）または（ｄ）記載のＭｇ含有酸化鉄膜被覆鉄粉末、などを発明した。
In order to solve such problems, the present inventors firstly
(A) a Mg-containing iron oxide film-coated iron powder in which an Mg-Fe-O ternary oxide deposited film containing at least (Mg, Fe) O is coated on the surface of the iron powder;
(B) a Mg-containing iron oxide film-coated iron powder in which an Mg-Fe-O ternary oxide deposition film containing at least (Mg, Fe) O is coated on the surface of the iron powder, In the interface region with the Mg—Fe—O ternary oxide deposited film containing at least (Mg, Fe) O, a sulfur enriched layer containing sulfur at a higher concentration than sulfur contained in the central portion of the iron powder. Mg-containing iron oxide film-coated iron powder having,
(C) (Mg, Fe) O contained in the Mg—Fe—O ternary oxide deposited film of the Mg-containing oxide film-coated iron powder is the crystalline MgO solid solution wustite phase (a) or (B) the Mg-containing oxide film-coated iron powder according to the description,
(D) The Mg—Fe—O ternary oxide deposited film containing at least (Mg, Fe) O has the fine crystal structure of crystal grain size: 200 nm or less (a), (b) or (c ) Mg-containing iron oxide film-coated iron powder according to
(E) The Mg—Fe—O ternary oxide deposited film containing at least (Mg, Fe) O has the outermost surface substantially composed of MgO (a), (b), ( Invented the iron powder coated with Mg-containing iron oxide film described in c) or (d).
この先に発明した前記（ａ）、（ｂ）、（ｃ）、（ｄ）または（ｅ）記載のＭｇ含有酸化鉄膜被覆鉄粉末は、鉄粉末を予め酸化雰囲気中で加熱するなどして酸化処理を施すことにより鉄粉末の表面に酸化鉄膜を形成した鉄粉末（以下、酸化処理鉄粉末という）を作製し、この酸化処理鉄粉末にＭｇ粉末を添加し混合して得られた混合粉末を不活性ガス雰囲気または真空雰囲気中で加熱するなどした後さらに酸化性雰囲気中で加熱する酸化処理を施すことにより得られたものであり、これら先に発明したＭｇ含有酸化鉄膜被覆鉄粉末は、
（イ）一般に知られているＭｇＯ−ＦｅＯ−Ｆｅ２Ｏ３系の中でで代表される（Ｍｇ，Ｆｅ）Ｏ、（Ｍｇ，Ｆｅ）３Ｏ４などのＭｇ−Ｆｅ−Ｏ三元系各種酸化物のうちで、少なくとも（Ｍｇ，Ｆｅ）Ｏを含むＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜が鉄粉末の表面に形成され、この少なくとも（Ｍｇ，Ｆｅ）Ｏを含むＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜が鉄粉末の表面に被覆されたＭｇ含有酸化膜被覆鉄粉末は、従来の鉄粉末の表面にＭｇ含有フェライト膜を形成したＭｇ含有酸化膜被覆鉄粉末に比べて酸化膜の鉄粉末に対する密着性が格段に優れることから、プレス成形中に絶縁皮膜である酸化膜が破壊されて鉄粉末同士が接触することが少なく、プレス成形後に高温歪取り焼成を行っても酸化膜の絶縁性が低下することなく高抵抗を維持することができるので渦電流損失が低くなり、さらに歪取り焼成を行った場合に、より保磁力が低減できることからヒステリシス損失を低く抑えることができ、したがって、低鉄損を有する複合軟磁性材料が得られること、
（ロ）前記Ｍｇ含有酸化膜被覆鉄粉末のＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜に含まれる（Ｍｇ，Ｆｅ）Ｏは、結晶質のＭｇＯ固溶ウスタイト（ＭｇＯがウスタイト（ＦｅＯ）に固溶している物質）であることが一層好ましいこと、
（ハ）前記鉄粉末と少なくとも（Ｍｇ，Ｆｅ）Ｏを含むＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜との界面領域には、鉄粉末の中心部に不可避不純物として含まれている硫黄よりも高濃度の硫黄を含む硫黄濃化層が形成されること、
（ニ）前記少なくとも（Ｍｇ，Ｆｅ）Ｏを含むＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜は結晶粒径：２００ｎｍ以下の微細結晶組織を有すること、
（ホ）前記鉄粉末の表面に形成されている少なくとも（Ｍｇ，Ｆｅ）Ｏを含むＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜は、その最表面に含まれるＭｇＯの量が多いほど好ましく、その最表面は実質的にＭｇＯで構成されていることが最も好ましいこと、などの知見に基づいて成されたものである。
The Mg-containing iron oxide film-coated iron powder described in (a), (b), (c), (d) or (e) previously invented is oxidized by heating the iron powder in an oxidizing atmosphere in advance. A mixed powder obtained by preparing an iron powder having an iron oxide film formed on the surface of the iron powder (hereinafter referred to as an oxidized iron powder) by adding a Mg powder and mixing the oxidized iron powder. Is heated in an inert gas atmosphere or a vacuum atmosphere, and then is further subjected to an oxidation treatment in an oxidizing atmosphere. These previously invented Mg-containing iron oxide film-coated iron powders are: ,
(B) Various Mg-Fe-O ternary systems such as (Mg, Fe) O, (Mg, Fe) 3 O 4 and the like represented by the generally known MgO-FeO-Fe 2 O 3 systems Among the oxides, an Mg—Fe—O ternary oxide deposition film containing at least (Mg, Fe) O is formed on the surface of the iron powder, and this Mg—Fe— containing at least (Mg, Fe) O is formed. The Mg-containing oxide film-coated iron powder in which the O ternary oxide deposited film is coated on the surface of the iron powder is compared with the Mg-containing oxide film-coated iron powder in which the Mg-containing ferrite film is formed on the surface of the conventional iron powder. Since the adhesion of the oxide film to the iron powder is remarkably excellent, the oxide film, which is an insulating film, is hardly broken during press molding, and the iron powder is less likely to come into contact with each other. Maintains high resistance without degrading oxide insulation Therefore, the eddy current loss is reduced, and when the strain relief firing is performed, the coercive force can be further reduced, so that the hysteresis loss can be suppressed low. Therefore, a composite soft magnetic material having a low iron loss can be obtained. To obtain,
(B) (Mg, Fe) O contained in the Mg—Fe—O ternary oxide deposited film of the Mg-containing oxide film-coated iron powder is crystalline MgO solid solution wustite (MgO becomes wustite (FeO)). It is more preferable that the substance is a solid solution)
(C) In the interface region between the iron powder and the Mg—Fe—O ternary oxide deposited film containing at least (Mg, Fe) O, sulfur contained as an inevitable impurity in the center of the iron powder A sulfur-enriched layer containing a high concentration of sulfur is formed,
(D) the Mg—Fe—O ternary oxide deposited film containing at least (Mg, Fe) O has a fine crystal structure with a crystal grain size of 200 nm or less;
(E) The Mg-Fe-O ternary oxide deposited film containing at least (Mg, Fe) O formed on the surface of the iron powder is preferably as the amount of MgO contained in the outermost surface is larger, The outermost surface is made based on the knowledge that it is most preferable that the outermost surface is substantially composed of MgO.
これら先に発明した前記（ａ）〜（ｄ）のＭｇ含有酸化鉄膜被覆鉄粉末を製造するには、まず、鉄粉末を予め酸化雰囲気中、温度：５０〜５００℃に加熱して酸化処理することにより鉄粉末の表面に酸化鉄膜を形成した酸化処理鉄粉末を作製し、これらの粉末にＭｇ粉末を添加し混合して得られた混合粉末を温度：１５０〜１１００℃、圧力：１×１０−１２〜１×１０−１ＭＰａの不活性ガス雰囲気または真空雰囲気中で加熱した後、必要によりさらに酸化性雰囲気中、温度：５０〜３５０℃で加熱したのち酸化処理を施すことにより作製する。 In order to produce the Mg-containing iron oxide film-coated iron powders of the above-described inventions (a) to (d), first, the iron powder is preliminarily heated in an oxidizing atmosphere at a temperature of 50 to 500 ° C. to be oxidized. Thus, an oxidized iron powder having an iron oxide film formed on the surface of the iron powder is produced, and the mixed powder obtained by adding and mixing the Mg powder to these powders is temperature: 150 to 1100 ° C., pressure: 1 Prepared by heating in an inert gas atmosphere or vacuum atmosphere of × 10 −12 to 1 × 10 −1 MPa, and further heating in an oxidizing atmosphere, if necessary, at a temperature of 50 to 350 ° C., followed by oxidation treatment. To do.
また、先に発明した前記（ｅ）記載の少なくとも（Ｍｇ，Ｆｅ）Ｏを含むＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜の最表面が実質的にＭｇＯで構成されているＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜は、鉄粉末を予め酸化雰囲気中、温度：５０〜５００℃に加熱して酸化処理することにより鉄粉末の表面に酸化鉄膜を形成した酸化処理鉄粉末を作製し、これらの粉末にＭｇ粉末を一層多く添加し混合して得られた混合粉末を温度：１５０〜１１００℃、圧力：１×１０−１２〜１×１０−１ＭＰａの不活性ガス雰囲気または真空雰囲気中で加熱した後、さらに酸化性雰囲気中で一層長時間加熱したのち酸化処理を施すことにより得られる。 Further, the Mg—Fe— in which the outermost surface of the Mg—Fe—O ternary oxide deposited film containing at least (Mg, Fe) O described in the above (e) is substantially composed of MgO. O ternary oxide deposited film is prepared by oxidizing iron powder by heating it in an oxidizing atmosphere at a temperature of 50-500 ° C in advance to form an iron oxide film on the surface of the iron powder. Then, the mixed powder obtained by adding and mixing more Mg powder to these powders is an inert gas atmosphere or vacuum at a temperature of 150 to 1100 ° C. and a pressure of 1 × 10 −12 to 1 × 10 −1 MPa. After heating in an atmosphere, it is obtained by further heating in an oxidizing atmosphere for a longer time and then performing an oxidation treatment.
前述の先に発明した前記（ａ）〜（ｅ）のＭｇ含有酸化鉄膜被覆鉄粉末の表面に形成されているＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜に含まれるＭｇウスタイトは（Ｍｇ，Ｆｅ）：Ｏ＝１：１のものだけではなくＯが固溶幅を有していても良い。
「堆積膜」という用語は、通常、真空蒸発やスパッタされた皮膜構成原子が例えば基板上に堆積した皮膜を示すが、前記鉄粉末の表面に形成されている少なくとも（Ｍｇ，Ｆｅ）Ｏを含むＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜は、酸化鉄膜を有する鉄粉末表面の酸化鉄（Ｆｅ−Ｏ）とＭｇが反応を伴って当該鉄粉末表面に堆積した皮膜を示す。そして、この鉄粉末の表面に形成されている少なくとも（Ｍｇ，Ｆｅ）Ｏを含むＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜の膜厚は、圧粉成形した複合軟磁性材の高磁束密度と高比抵抗を得るために、５ｎｍ〜５００ｎｍの範囲内にあることが好ましい。膜厚が５ｎｍより薄いと圧粉成形した複合軟磁性材の比抵抗が充分でなく渦電流損が増加するので好ましくなく、一方、膜厚が５００ｎｍより厚いと圧粉成形した複合軟磁性材の磁束密度が低下して好ましくないからである。さらに好ましい膜厚は５ｎｍ〜２００ｎｍの範囲内である。
Mg wustite contained in the Mg-Fe-O ternary oxide deposited film formed on the surface of the Mg-containing iron oxide film-coated iron powder of the above-described inventions (a) to (e) is (Mg , Fe): O = 1: 1: 1 as well as O may have a solid solution width.
The term “deposited film” usually refers to a film in which atoms constituting the film formed by vacuum evaporation or sputtering are deposited on a substrate, for example, and includes at least (Mg, Fe) O formed on the surface of the iron powder. The Mg—Fe—O ternary oxide deposition film indicates a film in which iron oxide (Fe—O) and Mg on the iron powder surface having an iron oxide film are deposited on the iron powder surface with a reaction. The film thickness of the Mg—Fe—O ternary oxide deposited film containing at least (Mg, Fe) O formed on the surface of the iron powder is equal to the high magnetic flux density of the compacted composite soft magnetic material. In order to obtain a high specific resistance, it is preferably in the range of 5 nm to 500 nm. If the film thickness is less than 5 nm, the specific resistance of the powder-molded composite soft magnetic material is not sufficient and the eddy current loss increases. On the other hand, if the film thickness is thicker than 500 nm, it is not preferable. This is because the magnetic flux density is lowered, which is not preferable. A more preferable film thickness is in the range of 5 nm to 200 nm.
また、先に発明した前記（ａ）〜（ｅ）のＭｇ含有酸化鉄膜被覆鉄粉末の表面に形成されている少なくとも（Ｍｇ，Ｆｅ）Ｏを含むＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜は、前記少なくとも（Ｍｇ，Ｆｅ）Ｏを含むＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜と鉄粉末との界面領域に、鉄粉末の中心部に含まれる硫黄よりも高濃度の硫黄を含む硫黄濃化層を有する。この硫黄濃化層を有することはオージェ電子分光法により硫黄濃度を測定し、これをグラフに表すと、硫黄濃度ピークを示すことから確認することができる。界面領域にこの様な硫黄濃化層を有することにより少なくとも（Ｍｇ，Ｆｅ）Ｏを含むＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜の鉄粉末表面に対する密着性がより一層優れるようになり、圧粉成形時の粉末の変形に堆積膜が追従して被覆の破れを防止することができ、焼成時にも鉄粉末同士の接触結合を防止することができて高抵抗を維持することができ、したがって渦電流損失が低くなる。硫黄濃化層の硫黄は、鉄粉末には不可避不純物として硫黄が含まれており、大部分はこの鉄粉末の表面部分に含まれる硫黄から供給されると考えられている。
前記（ａ）〜（ｅ）のＭｇ含有酸化鉄膜被覆鉄粉末の表面に形成されている少なくとも（Ｍｇ，Ｆｅ）Ｏを含むＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜は、その結晶粒が微細であるほど好ましく、結晶粒径が２００ｎｍ以下の微細結晶組織を有する事が好ましい。この様な微細結晶組織を有することにより、圧粉成形時の粉末の変形に微結晶Ｍｇ−Ｆｅ−Ｏ三元系酸化物堆積膜が追従して被覆の破れを防止することができ、焼成時にも鉄粉末同士の接触結合を防止することができ、また、高温歪取り焼成を行っても酸化物が安定で絶縁性低下が防止でき高抵抗で渦電流損失が低くなる。結晶粒径が２００ｎｍより大きいとＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜の膜厚が５００ｎｍよりも厚くなり圧粉成形した複合軟磁性材の磁束密度が低下するようになるので好ましくない。
また、前記（ｅ）のＭｇ含有酸化鉄膜被覆鉄粉末の表面に形成されている少なくとも（Ｍｇ，Ｆｅ）Ｏを含むＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜は、その最表面におけるＭｇＯの含有量が多くなるほど好ましく、実質的にＭｇＯで構成されていることが最も好ましい。最表面が実質的にＭｇＯであると、プレス成形した圧粉体の焼成時にもＦｅの拡散が防止され鉄粉末同士の接触結合を防止することができ絶縁性低下が防止でき高抵抗で渦電流損失が低くなるからである。
Further, Mg-Fe-O ternary oxide deposition containing at least (Mg, Fe) O formed on the surface of the Mg-containing iron oxide film-coated iron powder of the above-described inventions (a) to (e). The film has a higher concentration of sulfur than the sulfur contained in the center of the iron powder in the interface region between the Mg-Fe-O ternary oxide deposited film containing at least (Mg, Fe) O and the iron powder. It has a sulfur enriched layer. Having this sulfur-concentrated layer can be confirmed from the fact that the sulfur concentration is measured by Auger electron spectroscopy, and this is shown in a graph, showing a sulfur concentration peak. By having such a sulfur-concentrated layer in the interface region, the adhesion of the Mg-Fe-O ternary oxide deposited film containing at least (Mg, Fe) O to the iron powder surface becomes even better. The deposited film can follow the deformation of the powder at the time of compacting to prevent the coating from being torn, the contact bonding between the iron powders can be prevented even during firing, and high resistance can be maintained, Therefore, eddy current loss is reduced. The sulfur in the sulfur-concentrated layer is considered to be supplied from sulfur contained in the surface portion of the iron powder because the iron powder contains sulfur as an inevitable impurity.
The Mg—Fe—O ternary oxide deposited film containing at least (Mg, Fe) O formed on the surface of the Mg-containing iron oxide film-coated iron powders (a) to (e) has crystal grains. Is preferably as fine as possible, and preferably has a fine crystal structure with a crystal grain size of 200 nm or less. By having such a fine crystal structure, the microcrystalline Mg—Fe—O ternary oxide deposited film can follow the deformation of the powder during compacting and prevent the coating from being broken. In addition, contact bonding between iron powders can be prevented, and even when high-temperature strain relief firing is performed, the oxide is stable and insulation deterioration can be prevented, and eddy current loss is reduced with high resistance. If the crystal grain size is larger than 200 nm, the Mg—Fe—O ternary oxide deposited film becomes thicker than 500 nm, and the magnetic flux density of the compacted composite soft magnetic material is lowered.
In addition, the Mg—Fe—O ternary oxide deposited film containing at least (Mg, Fe) O formed on the surface of the Mg-containing iron oxide film-coated iron powder of (e) is MgO on the outermost surface. The content of is preferably as high as possible, and is most preferably substantially composed of MgO. When the outermost surface is substantially MgO, the diffusion of Fe is prevented even during firing of the green compact that has been press-molded, and contact bonding between iron powders can be prevented. This is because loss is reduced.
以上、先に発明した（ａ）〜（ｅ）記載のＭｇ含有酸化鉄膜被覆鉄粉末について詳述したが、この発明は、前記の先に発明した（ａ）〜（ｅ）記載のＭｇ含有酸化鉄膜被覆鉄粉末の表面に、さらにモル比でＭｇＯ／ＳｉＯ２の値が１．０〜３．０の範囲内にあるＭｇＯ−ＳｉＯ２系複合酸化物膜を被覆することにより一層圧縮成形性および焼結性を向上させた複合軟磁性粉末およびその製造方法を提供することを目的とするものである。
すなわち、一般に、ＭｇＯ−ＳｉＯ２系複合酸化物膜は、電気的絶縁性が高く、さらに比較的軟らかい硬さ（モース硬さ１〜４）を有するとともに、さらに減摩作用や潤滑作用に富むために成形時には潤滑材としても働く作用を有することから、先に発明した（ａ）〜（ｅ）記載のＭｇ含有酸化鉄膜被覆鉄粉末の表面にさらにＭｇＯ−ＳｉＯ２系複合酸化物膜を被覆した複合軟磁性粉末は圧縮成形性が一層向上し、さらにＭｇＯ−ＳｉＯ２系複合酸化物膜はＭｇＯよりも融点が低いために、ＭｇＯ−ＳｉＯ２系複合酸化物膜を前記（ａ）〜（ｅ）記載のＭｇ含有酸化鉄膜被覆鉄粉末に被覆したこの発明の複合軟磁性粉末は焼結性が一層向上する。
As described above, the Mg-containing iron oxide film-coated iron powder described in (a) to (e) described above has been described in detail. This invention includes the Mg-containing composition described in (a) to (e) described above. Further compression molding is performed by coating the surface of the iron powder coated iron powder with a MgO-SiO 2 composite oxide film having a molar ratio of MgO / SiO 2 in the range of 1.0 to 3.0. It is an object of the present invention to provide a composite soft magnetic powder having improved properties and sinterability and a method for producing the same.
That is, in general, the MgO—SiO 2 -based composite oxide film has high electrical insulation, has a relatively soft hardness (Mohs hardness 1 to 4), and is further rich in antifriction and lubrication. Since it acts as a lubricant during molding, the surface of the Mg-containing iron oxide film-coated iron powder described in (a) to (e) above was further coated with a MgO—SiO 2 composite oxide film. The composite soft magnetic powder has further improved compression moldability, and the MgO—SiO 2 composite oxide film has a lower melting point than MgO. Therefore, the MgO—SiO 2 composite oxide film is changed from the above (a) to (e). The composite soft magnetic powder according to the present invention coated with the Mg-containing iron oxide film-coated iron powder described in (1) further improves the sinterability.
しかがって、この発明は、（１）少なくとも（Ｍｇ，Ｆｅ）Ｏを含むＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜が鉄粉末の表面に被覆されているＭｇ含有酸化鉄膜被覆鉄粉末の表面に、さらにモル比でＭｇＯ／ＳｉＯ２の値が１．０〜３．０の範囲内にあるＭｇＯ−ＳｉＯ２系複合酸化物膜を被覆してなる複合軟磁性粉末、
（２）少なくとも（Ｍｇ，Ｆｅ）Ｏを含むＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜が鉄粉末の表面に被覆されておりかつ前記少なくとも（Ｍｇ，Ｆｅ）Ｏを含むＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜と鉄粉末との界面領域に鉄粉末の中心部に含まれる硫黄よりも高濃度の硫黄を含む硫黄濃化層を有するＭｇ含有酸化鉄膜被覆鉄粉末の表面に、さらにモル比でＭｇＯ／ＳｉＯ２の値が１．０〜３．０の範囲内にあるＭｇＯ−ＳｉＯ２系複合酸化物膜を被覆してなる複合軟磁性粉末、
（３）前記Ｍｇ含有酸化膜被覆鉄粉末のＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜に含まれる（Ｍｇ，Ｆｅ）Ｏは、結晶質のＭｇＯ固溶ウスタイト相である前記（１）または（２）記載の複合軟磁性粉末、
（４）前記少なくとも（Ｍｇ，Ｆｅ）Ｏを含むＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜は、結晶粒径：２００ｎｍ以下の微細結晶組織を有する前記（１）、（２）または（３）記載の複合軟磁性粉末、
（５）前記少なくとも（Ｍｇ，Ｆｅ）Ｏを含むＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜は、その最表面が実質的にＭｇＯで構成されている前記（１）、（２）、（３）または（４）記載の複合軟磁性粉末、に特徴を有するものである。
Therefore, the present invention provides (1) a Mg-containing iron oxide film-coated iron in which a surface of an iron powder is coated with a Mg—Fe—O ternary oxide deposited film containing at least (Mg, Fe) O. A composite soft magnetic powder obtained by coating the surface of the powder with a MgO—SiO 2 composite oxide film having a molar ratio of MgO / SiO 2 in the range of 1.0 to 3.0,
(2) A Mg—Fe—O ternary oxide deposited film containing at least (Mg, Fe) O is coated on the surface of the iron powder, and the Mg—Fe—O containing at least (Mg, Fe) O. On the surface of the Mg-containing iron oxide film-coated iron powder having a sulfur concentrated layer containing sulfur at a higher concentration than sulfur contained in the center of the iron powder in the interface region between the ternary oxide deposited film and the iron powder, Furthermore, a composite soft magnetic powder formed by coating a MgO—SiO 2 composite oxide film having a molar ratio of MgO / SiO 2 in the range of 1.0 to 3.0,
(3) The (Mg, Fe) O contained in the Mg—Fe—O ternary oxide deposited film of the Mg-containing oxide film-coated iron powder is a crystalline MgO solid solution wustite phase (1) or (2) the composite soft magnetic powder as described above,
(4) The Mg—Fe—O ternary oxide deposited film containing at least (Mg, Fe) O has a fine crystal structure with a crystal grain size of 200 nm or less (1), (2) or (3 ) Composite soft magnetic powder according to
(5) The Mg—Fe—O ternary oxide deposited film containing at least (Mg, Fe) O has the outermost surface substantially composed of MgO (1), (2), ( 3) or the composite soft magnetic powder described in (4).
この発明の前記（１）、（２）、（３）、（４）または（５９記載の複合軟磁性粉末は、前記（ａ）、（ｂ）、（ｃ）、（ｄ）または（ｅ）記載のＭｇ含有酸化鉄膜被覆鉄粉末の表面に容量比でアルコキシシラン溶液：１に対してマグネシウムアルコキシド溶液：１〜３の範囲内の比率で混合して得られたＭｇＯとＳｉＯ２の混合酸化物ゾル溶液を付着させたのち加熱乾燥することにより製造することができる。
したがって、この発明は、
（６）容量比でアルコキシシラン溶液：１に対してマグネシウムアルコキシド溶液：１〜３の範囲内の比率で混合して得られたＭｇＯとＳｉＯ２の混合酸化物ゾル溶液をＭｇ含有酸化鉄膜被覆鉄粉末の表面に付着させたのち加熱乾燥することを特徴とする複合軟磁性粉末の製造方法、に特徴を有するものである。
The composite soft magnetic powder according to (1), (2), (3), (4) or (59) of the present invention is the above (a), (b), (c), (d) or (e) Mixed oxidation of MgO and SiO 2 obtained by mixing the Mg-containing iron oxide film-coated iron powder described above at a volume ratio of alkoxysilane solution: 1 to magnesium alkoxide solution: ratio within the range of 1 to 3 The product sol solution can be attached and then dried by heating.
Therefore, the present invention
(6) volume ratio in the alkoxysilane solution: 1 Magnesium respect alkoxide solution: mixing a mixed oxide sol solution of MgO and SiO 2 obtained Mg-containing iron oxide film coating at a ratio in the 1-3 range It is characterized by a method for producing a composite soft magnetic powder, characterized in that it is dried by heating after adhering to the surface of iron powder.
前記（１）、（２）、（３）、（４）または（５）記載の複合軟磁性粉末を圧縮成形したのち５００〜１２００℃で焼結することにより高強度、高磁束密度および高抵抗を有する鉄損の少ない複合軟磁性材を製造することができる。したがって、この発明は、
（７）前記（１）、（２）、（３）、（４）または（５）記載の複合軟磁性粉末を圧縮成形したのち５００〜１２００℃で焼成する複合軟磁性材の製造方法、
（８）前記（７）記載の方法で製造した複合軟磁性材、に特徴を有するものである。
The composite soft magnetic powder described in (1), (2), (3), (4) or (5) is compression-molded and then sintered at 500 to 1200 ° C. to obtain high strength, high magnetic flux density and high resistance. It is possible to produce a composite soft magnetic material having a low iron loss. Therefore, the present invention
(7) A method for producing a composite soft magnetic material, wherein the composite soft magnetic powder according to (1), (2), (3), (4) or (5) is compression-molded and then fired at 500 to 1200 ° C.
(8) The composite soft magnetic material manufactured by the method described in (7) above is characterized.
この発明によると、高強度および高抵抗を有し、さらに高磁束密度の複合軟磁性材を提供することができ、電気および電子産業において優れた効果をもたらすものである。 According to the present invention, it is possible to provide a composite soft magnetic material having high strength and high resistance, and having a high magnetic flux density, which provides excellent effects in the electrical and electronic industries.
実施例１
原料粉末として、平均粒径：７０μｍを有し不可避不純物として硫黄を極微量含む純鉄粉末を用意し、さらに、平均粒径：５０μｍのＭｇ粉末を用意した。
まず、前記純鉄粉末を大気中、温度：２２０℃、２時間保持の条件で酸化処理することにより表面に酸化鉄膜を有する酸化処理鉄粉末を作製し、この酸化処理鉄粉末に対し先に用意したＭｇ粉末を、酸化処理鉄粉末：Ｍｇ粉末＝９９．８質量％：０．３質量％の割合で添加し混合して混合粉末を作製し、得られた混合粉末を温度：６５０℃、圧力：２．７×１０−４ＭＰａ、１時間保持したのち、さらに大気中、温度：２００℃、１時間保持することにより鉄粉末の表面に堆積膜が被覆されているＭｇ含有酸化鉄膜被覆鉄粉末を作製した。このＭｇ含有酸化鉄膜被覆鉄粉末に形成された堆積膜をＸ線光電子分光装置により分析を行い、結合エネルギーを解析したところ、少なくとも（Ｍｇ，Ｆｅ）Ｏが含まれているＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜であることが解った。
このＭｇ含有酸化鉄膜被覆鉄粉末における鉄粉末とＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜との界面領域をオージェ電子分光装置を用いた方法により調べた結果、前記少なくとも（Ｍｇ，Ｆｅ）Ｏが含まれているＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜と鉄粉末との界面領域に、鉄粉末の中心部に含まれる不純物硫黄（バックグラウンド）よりも明らかにオージェ電子分光法でピークをもって硫黄が検出されていることから鉄粉末の中心部に含まれる硫黄よりも高濃度の硫黄を含む硫黄濃化層を有することが解った。さらに、Ｍｇ含有酸化鉄膜被覆鉄粉末における少なくとも（Ｍｇ，Ｆｅ）Ｏが含まれているＭｇ−Ｆｅ−Ｏ三元系酸化物堆積膜の組織を電子顕微鏡で観察した結果、その堆積膜の平均厚さは６０ｎｍ、最大結晶粒径は４０ｎｍであることがわかった。
Example 1
A pure iron powder having an average particle size of 70 μm and containing an extremely small amount of sulfur as an inevitable impurity was prepared as a raw material powder, and an Mg powder having an average particle size of 50 μm was prepared.
First, an oxidized iron powder having an iron oxide film on its surface is produced by oxidizing the pure iron powder in the atmosphere at a temperature of 220 ° C. for 2 hours. The prepared Mg powder was added and mixed at a ratio of oxidized iron powder: Mg powder = 99.8% by mass: 0.3% by mass to prepare a mixed powder, and the obtained mixed powder was heated to 650 ° C. Pressure: 2.7 × 10 −4 MPa After holding for 1 hour, further in the atmosphere, temperature: 200 ° C., and holding for 1 hour, the Mg-containing iron oxide film coated with the deposited film on the surface of the iron powder Iron powder was produced. The deposited film formed on the Mg-containing iron oxide film-coated iron powder was analyzed by an X-ray photoelectron spectrometer and the binding energy was analyzed. As a result, Mg—Fe—O containing at least (Mg, Fe) O was found. It was found to be a ternary oxide deposited film.
As a result of investigating the interface region between the iron powder and the Mg—Fe—O ternary oxide deposited film in the Mg-containing iron oxide film-coated iron powder by a method using an Auger electron spectrometer, at least (Mg, Fe) In the interface region between the Mg-Fe-O ternary oxide deposited film containing O and the iron powder, the Auger electron spectroscopy clearly shows the impurity sulfur (background) contained in the center of the iron powder. Since sulfur was detected with a peak, it was found that a sulfur concentrated layer containing sulfur at a higher concentration than sulfur contained in the center of the iron powder was obtained. Furthermore, as a result of observing the structure of the Mg—Fe—O ternary oxide deposited film containing at least (Mg, Fe) O in the Mg-containing iron oxide film coated iron powder with an electron microscope, the average of the deposited film It was found that the thickness was 60 nm and the maximum crystal grain size was 40 nm.
さらに、水と塩酸を添加した前加水分解アルコキシシラン溶液およびマグネシウムアルコキシド溶液を用意し、前加水分解アルコキシシラン溶液：１に対してマグネシウムアルコキシド溶液：２の容量比で混合してＭｇＯとＳｉＯ２の混合酸化物ゾル溶液を作製し、このＭｇＯとＳｉＯ２の混合酸化物ゾル溶液を先に作製したＭｇ含有酸化鉄膜被覆鉄粉末に対してＭｇＯとＳｉＯ２の混合酸化物換算で０．２質量％添加し混合し、得られた混合粉末を温度：１５０℃で加熱乾燥することによりＭｇ含有酸化鉄膜被覆鉄粉末の表面に２ＭｇＯ・ＳｉＯ２からなるＭｇＯ−ＳｉＯ２系複合酸化物膜を被覆した本発明複合軟磁性粉末を作製した。 Further, a pre-hydrolyzed alkoxysilane solution and a magnesium alkoxide solution to which water and hydrochloric acid were added were prepared, and the pre-hydrolyzed alkoxysilane solution: 1 was mixed at a volume ratio of magnesium alkoxide solution: 2: MgO and SiO 2 . mixed oxide sol solution was prepared, 0.2 weight a mixed oxide in terms of MgO and SiO 2 with respect to Mg-containing iron oxide film-coated iron powder to prepare a mixed oxide sol solution of MgO and SiO 2 above The resulting mixed powder is heated and dried at a temperature of 150 ° C. to coat the Mg-containing iron oxide film-coated iron powder with a MgO—SiO 2 composite oxide film composed of 2MgO · SiO 2. The composite soft magnetic powder of the present invention was produced.
この本発明複合軟磁性粉末を金型に入れ、プレス成形して縦：５５ｍｍ、横：１０ｍｍ、厚さ：５ｍｍの寸法を有する板状圧粉体および外径：３５ｍｍ、内径：２５ｍｍ、高さ：５ｍｍの寸法を有するリング形状圧粉体を成形し、得られた板状圧粉体およびリング状圧粉体を窒素雰囲気中、温度：５００℃、３０分保持の条件で焼結することにより板状およびリング状焼結体からなる複合軟磁性材を作製し、得られた板状焼結体からなる複合軟磁性材の相対密度、比抵抗および抗折力を測定してその結果を表１に示し、さらにリング状焼結体からなる複合軟磁性材に巻き線を施し、ＢＨトレーサで磁束密度を測定し、それらの結果を表１に示した。 The composite soft magnetic powder of the present invention is placed in a mold and press-molded to form a plate-shaped green compact having dimensions of length: 55 mm, width: 10 mm, thickness: 5 mm, outer diameter: 35 mm, inner diameter: 25 mm, height By molding a ring-shaped green compact having a dimension of 5 mm, and sintering the obtained plate-shaped green compact and the ring-shaped green compact in a nitrogen atmosphere at a temperature of 500 ° C. for 30 minutes. A composite soft magnetic material composed of a plate-shaped and ring-shaped sintered body was prepared, and the relative density, specific resistance, and bending strength of the obtained composite soft magnetic material composed of a plate-shaped sintered body were measured, and the results were displayed. 1 and further, the composite soft magnetic material made of a ring-shaped sintered body was wound, and the magnetic flux density was measured with a BH tracer. The results are shown in Table 1.
従来例１
純鉄粉末の表面にＭｇ含有フェライト層を化学的方法で形成したＭｇ含有フェライト被覆鉄粉末を用意し、このＭｇ含有フェライト被覆鉄粉末にシリコーン樹脂およびＭｇＯ粉末をシリコーン樹脂：０．１４、ＭｇＯ：０．０６、残部：Ｍｇ含有フェライト被覆鉄粉末の割合となるように混合して従来混合粉末を作製し、得られた従来混合粉末を金型に入れ、プレス成形して縦：５５ｍｍ、横：１０ｍｍ、厚さ：５ｍｍの寸法を有する板状圧粉体および外径：３５ｍｍ、内径：２５ｍｍ、高さ：５ｍｍの寸法を有するリング形状圧粉体を成形し、得られた圧粉体を窒素雰囲気中、温度：５００℃、３０分保持の条件で焼結することにより板状およびリング状焼結体からなる複合軟磁性粉末を作製した。得られた板状焼結体からなる複合軟磁性材の相対密度、比抵抗および抗折力を測定してその結果を表１に示し、さらにリング状焼結体からなる複合軟磁性材に巻き線を施し、ＢＨトレーサで磁束密度を測定し、それらの結果を表１に示した。
Conventional Example 1
An Mg-containing ferrite-coated iron powder in which a Mg-containing ferrite layer is formed on the surface of pure iron powder by a chemical method is prepared, and a silicone resin and MgO powder are added to the Mg-containing ferrite-coated iron powder as a silicone resin: 0.14, MgO: 0.06, balance: Mg-containing ferrite-coated iron powder is mixed to obtain a conventional mixed powder, and the obtained conventional mixed powder is placed in a mold and press-molded to obtain a length of 55 mm and a width: A plate-shaped green compact having dimensions of 10 mm, thickness: 5 mm, and a ring-shaped green compact having dimensions of outer diameter: 35 mm, inner diameter: 25 mm, height: 5 mm, and forming the green compact into nitrogen A composite soft magnetic powder composed of a plate-shaped and ring-shaped sintered body was produced by sintering under conditions of temperature: 500 ° C. and holding for 30 minutes in an atmosphere. The composite soft magnetic material made of the plate-like sintered body was measured for the relative density, specific resistance and bending strength, and the results are shown in Table 1, and further wound on the composite soft magnetic material made of the ring-like sintered body. The magnetic flux density was measured with a BH tracer, and the results are shown in Table 1.
表１に示される結果から、本発明複合軟磁性粉末で作製した複合軟磁性材は従来複合軟磁性粉末で作製した複合軟磁性材と比べて、抗折強度、磁束密度および比抵抗が共に優れていることが分かる。 From the results shown in Table 1, the composite soft magnetic material produced with the composite soft magnetic powder of the present invention is superior in both bending strength, magnetic flux density and specific resistance compared to the composite soft magnetic material produced with the conventional composite soft magnetic powder. I understand that
Claims (12)
An electric device incorporating the electromagnetic circuit component according to claim 10 or 11.
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| JP2005161479A JP4480627B2 (en) | 2005-06-01 | 2005-06-01 | Composite soft magnetic powder and method for producing the same |
| US11/814,603 US9269481B2 (en) | 2005-01-25 | 2005-11-02 | Iron powder coated with Mg-containing oxide film |
| EP05805498A EP1852199B1 (en) | 2005-01-25 | 2005-11-02 | Mg-CONTAINING OXIDE COATED IRON POWDER |
| CA002598842A CA2598842A1 (en) | 2005-01-25 | 2005-11-02 | Iron powder coated with mg-containing oxide film |
| PCT/JP2005/020204 WO2006080121A1 (en) | 2005-01-25 | 2005-11-02 | Mg-CONTAINING OXIDE COATED IRON POWDER |
| EP10172637.0A EP2248617B1 (en) | 2005-01-25 | 2005-11-02 | Iron powder coated with Mg-containing oxide film |
| EP12172935.4A EP2502689B8 (en) | 2005-01-25 | 2005-11-02 | Iron powder coated with Mg-containing oxide film |
| US13/228,139 US8481178B2 (en) | 2005-01-25 | 2011-09-08 | Iron powder coated with Mg-containing oxide film |
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