JP2006185981A - Method of manufacturing dust core material having high strength - Google Patents
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Abstract
Description
この発明は、高強度を有する圧粉磁心材の製造方法に関するものであり、この方法で製造した圧粉磁心材はモータ、アクチュエータ、磁気センサ、リアクトルなどの各種電気または電子部品の製造に使用されるものである。 The present invention relates to a method for producing a dust core material having high strength, and the dust core material produced by this method is used in the production of various electric or electronic components such as motors, actuators, magnetic sensors, and reactors. Is.
一般に、圧粉磁心は各種電磁機器の部品として使用されており、この圧粉磁心材は、鉄粉末または鉄粉末の表面にリン酸塩を被覆した鉄粉末（以下、リン酸塩皮膜被覆鉄粉末という）を原料粉末として使用されることは知られており、その中でもリン酸皮膜被覆鉄粉末が最も多く使用されている。かかるリン酸塩性皮膜被覆鉄粉末は、その充填密度を高めるために、結合剤と共に可能な限り高圧で圧縮成形する。しかし、高圧圧縮成形して得られた圧粉磁心材は、圧縮成形時にリン酸塩性皮膜被覆鉄粉末の内部の鉄粉末に圧縮歪が生成し、軟磁性磁気特性が低下し、材料の特性を十分に発揮させることができなくなる。そのために、圧縮生成して得られた圧粉磁心材料は熱処理することにより歪みを開放し、軟磁性特性を回復させるための熱処理が施されている。 In general, a dust core is used as a part of various electromagnetic devices. This dust core material is made of iron powder or iron powder having a surface coated with phosphate (hereinafter referred to as phosphate coating-coated iron powder). Is known as a raw material powder, and among them, phosphate-coated iron powder is most frequently used. Such phosphate film-coated iron powder is compression molded with a binder at as high a pressure as possible to increase its packing density. However, the powder magnetic core material obtained by high-pressure compression molding produces compression strain in the iron powder inside the phosphate film-coated iron powder during compression molding, resulting in decreased soft magnetic properties and material properties. Cannot be fully exerted. For this purpose, the powder magnetic core material obtained by compression generation is subjected to a heat treatment to release the strain and recover the soft magnetic properties by heat treatment.
例えば、鉄粉末またはリン酸塩性皮膜被覆鉄粉末に熱可塑性ポリイミド樹脂を被覆した複合粉末を作製し、この複合粉末を加圧成形して圧粉体を作製し、この圧粉体を３００〜４５０℃に加熱することにより熱処理し、この熱処理した圧粉磁心材を１５０〜３２０℃に加熱して安定化熱処理することにより圧粉磁心材を製造する方法が記載されている（特許文献１参照）。
しかし、この従来法により得られた圧粉磁芯材は強度が十分でなく、なお一層の高強度を有する圧粉磁心材の開発が求められていた。 However, the dust core material obtained by this conventional method has insufficient strength, and there has been a demand for the development of a dust core material having even higher strength.
そこで、本発明者等は、一層の高強度を有する圧粉磁心材を製造すべく研究を行った結果、
前記リン酸塩皮膜被覆鉄粉末、鉄粉末にシリコーンレジンをコーティングした鉄粉末（以下、シリコーンレジン皮膜被覆鉄粉末という）またはリン酸塩皮膜被覆鉄粉末にシリコーンレジンをコーティングした鉄粉末（以下、シリコーンレジン−リン酸塩皮膜被覆鉄粉末という）を圧縮成形して得られた圧粉体に、温度：４５１〜６００℃で加熱する一次熱処理を施した後、温度：１５０〜３５０℃で加熱する二次熱処理を施すことにより得られた圧粉磁心材は、従来の方法で得られた圧粉磁心材に比べて機械的強度が大幅に向上する、という研究結果が得られたのである。
Therefore, the present inventors conducted research to produce a dust core material having higher strength,
Iron phosphate powder coated iron powder (hereinafter referred to as “silicone resin coated iron powder”) or phosphate powder coated iron powder coated with silicone resin (hereinafter “silicone”) The green compact obtained by compression molding (resin-phosphate film-coated iron powder) is subjected to a primary heat treatment at a temperature of 451 to 600 ° C., and then heated at a temperature of 150 to 350 ° C. The research result that the mechanical strength of the dust core material obtained by performing the next heat treatment is significantly improved as compared with the dust core material obtained by the conventional method was obtained.
この発明は、かかる研究結果に基づいてなされたものであって、
（１）リン酸塩皮膜被覆鉄粉末を圧縮成形し、熱処理を施して圧粉磁心材を製造する方法において、前記熱処理は、温度：４５１〜６００℃で加熱する一次熱処理工程およびその後温度：１５０〜３５０℃で加熱する二次熱処理工程を含む高強度を有する圧粉磁心材の製造方法、
（２）シリコーンレジン皮膜被覆鉄粉末を圧縮成形し、熱処理を施して圧粉磁心材料を製造する方法において、前記熱処理は、温度：４５１〜６００℃で加熱する一次熱処理工程およびその後温度：１５０〜３５０℃で加熱する二次熱処理工程を含む高強度を有する圧粉磁心材の製造方法、
（３）シリコーンレジン−リン酸塩皮膜被覆鉄粉末を圧縮成形し、熱処理を施して圧粉磁心材料を製造する方法において、前記熱処理は、温度：４５１〜６００℃で加熱する一次熱処理工程およびその後温度：１５０〜３５０℃で加熱する二次熱処理工程を含む高強度を有する圧粉磁心材の製造方法、に特徴を有するものである。
The present invention was made based on the results of such research,
(1) In a method for producing a powder magnetic core material by compression-molding phosphate film-coated iron powder and performing a heat treatment, the heat treatment includes a primary heat treatment step of heating at a temperature of 451 to 600 ° C. and a subsequent temperature of 150. A method for producing a powder magnetic core material having high strength including a secondary heat treatment step of heating at ~ 350 ° C,
(2) In a method for producing a powder magnetic core material by compression-molding a silicone resin film-coated iron powder and performing a heat treatment, the heat treatment is performed at a primary heat treatment step of heating at a temperature of 451 to 600 ° C., and thereafter at a temperature of 150 to A method for producing a powder magnetic core material having a high strength including a secondary heat treatment step of heating at 350 ° C.,
(3) In a method of compressing and molding a silicone resin-phosphate coating-coated iron powder and performing a heat treatment to produce a powder magnetic core material, the heat treatment includes a primary heat treatment step of heating at a temperature of 451 to 600 ° C. and thereafter Temperature: It has the characteristics in the manufacturing method of the powder magnetic core material which has the high intensity | strength including the secondary heat processing process heated at 150-350 degreeC.
前記リン酸塩皮膜被覆鉄粉末、シリコーンレジン皮膜被覆鉄粉末またはシリコーンレジン−リン酸塩皮膜被覆鉄粉末を圧縮成形して圧粉体を作製するには、前記リン酸塩皮膜被覆鉄粉末、シリコーンレジン皮膜被覆鉄粉末またはシリコーンレジン−リン酸塩皮膜被覆鉄粉末を通常の金型に充填し、この充填されたリン酸塩皮膜被覆鉄粉末、シリコーンレジン皮膜被覆鉄粉末またはシリコーンレジン−リン酸塩皮膜被覆鉄粉末を６００〜１５００ＭＰａで圧縮成形する。圧縮成形圧力が６００ＭＰａ未満では十分な密度が得られないからであり、一方、１５００ＭＰａを越えると比抵抗が低下したり、金型強度の低下により寸法精度が大幅に低下するので好ましくないからである。
このようにして作製した圧粉体を前述の温度：４５１〜６００℃に加熱する一次熱処理および温度：１５０〜３５０℃加熱する二次熱処理を行うが、この時の一次熱処理工程における加熱時間は１０〜１８０分が好ましく、前記二次熱処理工程における加熱時間は１〜１００時間が好ましい。
前記一次熱処理の前にバインダ焙焼、潤滑剤焙焼などの目的で４５１℃未満の熱処理を施しても良い。また前記一次熱処理工程と前記二次熱処理工程の間にまたは前記二次熱処理工程後に１５０℃未満の熱処理を施しても良いが、これによる材料特性の向上は見られず、不経済である。さらに前記一次熱処理工程と前記二次熱処理工程は別個に行っても良いし、連続で行っても良い。
シリコーンレジンはそれ自体樹脂であるが、３００℃から分解が始まり、分解後は無機絶縁物であるＳｉＯ２となるので、一次熱処理後の圧粉磁心材の粉末粒間にＳｉＯ２を形成するための前駆体として作用する。
In order to produce a green compact by compression-molding the phosphate film-coated iron powder, the silicone resin film-coated iron powder or the silicone resin-phosphate film-coated iron powder, the phosphate film-coated iron powder, silicone Resin film-coated iron powder or silicone resin-phosphate film-coated iron powder is filled in a normal mold, and the filled phosphate film-coated iron powder, silicone resin film-coated iron powder or silicone resin-phosphate is filled The film-coated iron powder is compression molded at 600-1500 MPa. This is because if the compression molding pressure is less than 600 MPa, a sufficient density cannot be obtained. On the other hand, if it exceeds 1500 MPa, the specific resistance is lowered or the dimensional accuracy is greatly lowered due to a decrease in mold strength, which is not preferable. .
The green compact thus produced is subjected to the primary heat treatment for heating to the aforementioned temperature: 451 to 600 ° C. and the secondary heat treatment for heating to the temperature: 150 to 350 ° C. The heating time in this primary heat treatment step is 10 The heating time in the secondary heat treatment step is preferably 1 to 100 hours.
Prior to the primary heat treatment, a heat treatment of less than 451 ° C. may be performed for the purpose of binder roasting, lubricant roasting, and the like. Further, heat treatment at a temperature of less than 150 ° C. may be performed between the primary heat treatment step and the secondary heat treatment step or after the secondary heat treatment step, but this does not improve the material properties and is uneconomical. Furthermore, the primary heat treatment step and the secondary heat treatment step may be performed separately or continuously.
Silicone resin itself is a resin, but it begins to decompose at 300 ° C. and becomes SiO 2 , which is an inorganic insulator after decomposition, so that SiO 2 is formed between the powder particles of the powder magnetic core material after the primary heat treatment. Acts as a precursor of
この発明の一次熱処理工程における加熱温度を４５１〜６００℃にしたのは、４５１℃未満では二次熱処理を経ても得られる強度が不十分であり、一方、６００℃を越えて加熱すると比抵抗が低下するようになるので好ましくないからである。またこの発明の二次熱処理工程における加熱温度を１５０〜３５０℃にしたのは、１５０℃未満で加熱しても二次熱処理による強度向上効果が不十分であるからであり、一方、３５０℃を越えて加熱すると、時間と共に比抵抗が低下するようになるので好ましくないからである。 The reason why the heating temperature in the primary heat treatment step of the present invention is set to 451 to 600 ° C. is that if it is less than 451 ° C., the strength obtained even after the secondary heat treatment is insufficient. This is because it is not preferable because it decreases. The reason why the heating temperature in the secondary heat treatment step of the present invention is set to 150 to 350 ° C. is that the effect of improving the strength by the secondary heat treatment is insufficient even when heated at less than 150 ° C. This is because heating beyond this is not preferable because the specific resistance decreases with time.
この発明により製造した圧粉磁心材は強度を一層向上させることができることから、この発明により製造した圧粉磁心材を使用したモータ、アクチュエータ、磁気センサ、リアクトルなどの各種電気または電子部品を一層薄肉化して軽量化することができ、さらに小型化することができる。 Since the powder magnetic core material manufactured according to the present invention can further improve the strength, various electric or electronic parts such as motors, actuators, magnetic sensors, reactors and the like using the powder magnetic core material manufactured according to the present invention are made thinner. Can be reduced in weight and further reduced in size.
実施例
平均粒径：１００μｍの純鉄粉末を用意し、この純鉄粉末にリン酸処理を施すことにより純鉄粉末の表面に平均厚さ：３０ｎｍのリン酸皮膜を形成したリン酸皮膜形成鉄粉末（以下、原料粉末Ａという）および純鉄粉末の表面に平均厚さ：８０ｎｍのリン酸皮膜を形成したリン酸皮膜形成鉄粉末（以下、原料粉末Ｂという）を作製した。
また、前記純鉄粉末に０．３質量％の液状シリコーン樹脂を添加し、混合することにより純鉄粉末の表面に平均厚さ：１００ｎｍのシリコーンレジン樹脂皮膜を有するシリコーンレジン皮膜被覆鉄粉末（以下、原料粉末Ｃという）を作製した。
さらに前記原料粉末Ａに０．３質量％の液状シリコーン樹脂を添加し、混合することにより純鉄粉末の表面に平均厚さ：３０ｎｍのリン酸皮膜および平均厚さ：１００ｎｍのシリコーンレジン樹脂皮膜を有するシリコーンレジン−リン酸皮膜被覆鉄粉末（以下、原料粉末Ｄいう）を作製した。
Example Pure iron powder having an average particle diameter of 100 μm was prepared, and phosphoric acid film-forming iron in which a phosphoric acid film having an average thickness of 30 nm was formed on the surface of the pure iron powder by subjecting the pure iron powder to phosphoric acid treatment. A phosphoric acid film-forming iron powder (hereinafter referred to as raw material powder B) in which a phosphoric acid film having an average thickness of 80 nm was formed on the surface of powder (hereinafter referred to as raw material powder A) and pure iron powder was produced.
Further, by adding 0.3% by mass of a liquid silicone resin to the pure iron powder and mixing it, a silicone resin film-coated iron powder having a silicone resin resin film having an average thickness of 100 nm on the surface of the pure iron powder (hereinafter referred to as “the pure iron powder”) A raw material powder C).
Furthermore, 0.3 mass% liquid silicone resin was added to the raw material powder A and mixed to form a phosphoric acid film with an average thickness of 30 nm and a silicone resin resin film with an average thickness of 100 nm on the surface of the pure iron powder. A silicone resin-phosphate film-coated iron powder (hereinafter referred to as raw material powder D) was prepared.
これら原料粉末Ａ〜Ｄを壁面に純滑剤を塗布した金型に充填し、９８０ＭＰａの成形圧力で成形することにより外径：３５mm、内径：２５mm、高さ：５mmの寸法を有するリング状成形体および長さ：６０mm、幅：１０mm、厚さ：５mmの寸法を有するバー状成形体を作製した。これらリング状成形体およびバー状成形体を表１〜２に示される条件で一次熱処理したのち二次熱処理する熱処理を施すことにより本発明法１〜１６および比較法１〜４を実施し、それによって圧粉磁芯材からなるリング状試験片およびバー状試験片を作製した。
これらリング状試験片の水中密度を測定した後、巻線を施し、Ｂ−Ｈループトレーサにより磁界１０ｋＡ／ｍにおける磁束密度Ｂ１０ｋＡ／ｍを、Ｂ−Ｈアナライザにより励磁磁束密度１．５Ｔ、周波数５０Ｈｚにおける鉄損Ｗ１．５／５０をそれぞれ測定し、その測定結果を表１〜２に示した。
また、バー状試験片において四端子法により比抵抗を、スパン４５ｍｍの三点曲げにより抗折強度をそれぞれ測定し、その測定結果を表１〜２に示した。
These raw material powders A to D are filled in a mold having a wall surface coated with a pure lubricant, and molded at a molding pressure of 980 MPa, thereby forming a ring-shaped molded body having an outer diameter of 35 mm, an inner diameter of 25 mm, and a height of 5 mm. And the bar-shaped molded object which has a dimension of length: 60mm, width: 10mm, thickness: 5mm was produced. The ring-shaped molded body and bar-shaped molded body were subjected to primary heat treatment under the conditions shown in Tables 1-2, and then subjected to secondary heat treatment to perform the present invention methods 1-16 and comparative methods 1-4, Thus, a ring-shaped test piece and a bar-shaped test piece made of a dust core material were produced.
After measuring the underwater density of these ring-shaped test pieces, winding was performed, the magnetic flux density B 10 kA / m at a magnetic field of 10 kA / m was measured by a BH loop tracer, the excitation magnetic flux density 1.5 T, frequency by a BH analyzer. The iron loss W 1.5 / 50 at 50 Hz was measured, and the measurement results are shown in Tables 1 and 2.
Further, specific resistance of the bar-shaped test piece was measured by a four-terminal method, and bending strength was measured by three-point bending with a span of 45 mm, and the measurement results are shown in Tables 1 and 2.
従来例
実施例で用意した原料粉末Ａにポリフェニレンサルファイド樹脂粉末を０．６質量％添加し混合しすることにより混合粉末を作製し、この混合粉末を常温で金型に充填し、圧力：９８０ＭＰａで圧縮成形して外径：３５mm、内径：２５mm、高さ：５mmの寸法を有するリング状成形体および長さ：６０mm、幅：１０mm、厚さ：５mmの寸法を有するバー状成形体を作製した。これらリング状成形体およびバー状成形体を表２に示される条件で一次熱処理したのち二次熱処理する熱処理を施すことにより従来法１を実施し、それにより圧粉磁芯材からなるリング状試験片およびバー状試験片を作製した。これらリング状試験片の水中密度を測定した後、巻線を施し、Ｂ−Ｈループトレーサにより磁界１０ｋＡ／ｍにおける磁束密度Ｂ１０ｋＡ／ｍをＢ−Ｈアナライザにより励磁磁束密度１．５Ｔ、周波数５０Ｈｚにおける鉄損Ｗ１．５／５０をそれぞれ測定し、その測定結果を表２に示した。
また、バー状試験片において四端子法により比抵抗を、スパン４５ｍｍの三点曲げにより抗折強度をそれぞれ測定し、その測定結果を表２に示した。
A mixed powder is prepared by adding and mixing 0.6% by mass of polyphenylene sulfide resin powder to the raw material powder A prepared in the conventional example, and filling the mixed powder into a mold at room temperature, at a pressure of 980 MPa. A ring-shaped molded body having dimensions of outer diameter: 35 mm, inner diameter: 25 mm, height: 5 mm and bar-shaped molded body having dimensions of length: 60 mm, width: 10 mm, thickness: 5 mm were produced by compression molding. . The conventional method 1 is carried out by subjecting these ring-shaped compacts and bar-shaped compacts to a primary heat treatment under the conditions shown in Table 2 followed by a secondary heat treatment, whereby a ring-shaped test comprising a dust core material. Pieces and bar-like test pieces were prepared. After measuring the underwater density of these ring-shaped test pieces, winding was performed, and the magnetic flux density B 10 kA / m at a magnetic field of 10 kA / m was applied by a B-H loop tracer, and the excitation magnetic flux density 1.5 T, frequency 50 Hz by a B-H analyzer. The iron loss W 1.5 / 50 was measured, and the measurement results are shown in Table 2.
In addition, specific resistance was measured on the bar-shaped test piece by the four probe method, and bending strength was measured by three-point bending with a span of 45 mm, and the measurement results are shown in Table 2.
表１〜２に示される結果から、本発明法１〜１７で作製した試験片は、従来法１で作製した試験片に比べて比抵抗はほぼ同じであるが、特に抗折強度が優れていることが分かる。また、この発明の条件から外れた比較法１〜４で作製した試験片は一部好ましくない特性が現れることがわかる。 From the results shown in Tables 1 and 2, the test pieces produced by the present invention methods 1 to 17 have substantially the same specific resistance as the test pieces produced by the conventional method 1, but the bending strength is particularly excellent. I understand that In addition, it can be seen that some of the specimens produced by Comparative Methods 1 to 4 deviating from the conditions of the present invention exhibit undesirable characteristics.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009060895A1 (en) * | 2007-11-07 | 2009-05-14 | Mitsubishi Materials Pmg Corporation | High-strength soft-magnetic composite material obtained by compaction/burning and process for producing the same |
| JP2010225673A (en) * | 2009-03-19 | 2010-10-07 | Kobe Steel Ltd | Mixed powder for dust core, and method of manufacturing dust core using mixed the powder |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009060895A1 (en) * | 2007-11-07 | 2009-05-14 | Mitsubishi Materials Pmg Corporation | High-strength soft-magnetic composite material obtained by compaction/burning and process for producing the same |
| JP2010225673A (en) * | 2009-03-19 | 2010-10-07 | Kobe Steel Ltd | Mixed powder for dust core, and method of manufacturing dust core using mixed the powder |
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