JP6103191B2 - A method for producing granulated powder using magnetic powder as a raw material. - Google Patents
A method for producing granulated powder using magnetic powder as a raw material. Download PDFInfo
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- 239000006247 magnetic powder Substances 0.000 title claims description 45
- 239000000843 powder Substances 0.000 title description 134
- 239000002994 raw material Substances 0.000 title description 2
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- 239000000203 mixture Substances 0.000 claims description 26
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 25
- 239000002002 slurry Substances 0.000 claims description 23
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- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 11
- 229910052710 silicon Inorganic materials 0.000 claims description 11
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- 229910000976 Electrical steel Inorganic materials 0.000 claims description 6
- DKPFZGUDAPQIHT-UHFFFAOYSA-N butyl acetate Chemical compound CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000006249 magnetic particle Substances 0.000 claims description 5
- 229910000889 permalloy Inorganic materials 0.000 claims description 5
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
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- 239000000463 material Substances 0.000 description 5
- QPCHRHAEECSKLT-UHFFFAOYSA-N 1-(2-butan-2-yloxyethoxy)ethanol Chemical compound CCC(C)OCCOC(C)O QPCHRHAEECSKLT-UHFFFAOYSA-N 0.000 description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 3
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- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000000428 dust Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
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- 229910008458 Si—Cr Inorganic materials 0.000 description 2
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 description 2
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- FDPIMTJIUBPUKL-UHFFFAOYSA-N pentan-3-one Chemical compound CCC(=O)CC FDPIMTJIUBPUKL-UHFFFAOYSA-N 0.000 description 2
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 2
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- LIPRQQHINVWJCH-UHFFFAOYSA-N 1-ethoxypropan-2-yl acetate Chemical compound CCOCC(C)OC(C)=O LIPRQQHINVWJCH-UHFFFAOYSA-N 0.000 description 1
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 1
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- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
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- 229910052738 indium Inorganic materials 0.000 description 1
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- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 229910001004 magnetic alloy Inorganic materials 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
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Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/153—Amorphous metallic alloys, e.g. glassy metals
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- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Soft Magnetic Materials (AREA)
Description
本発明は、圧粉磁芯の材料となる金属磁性粒子の製造方法に関する。より詳細には、主としてインダクタリアクトル等の電子機器の製造に使用する金属磁性粒子の製造方法に関する。 The present invention relates to a method for producing metal magnetic particles as a material for a dust core. More specifically, the present invention relates to a method for producing metal magnetic particles mainly used for producing an electronic device such as an inductor reactor.
近年、家電及び電子機器の省エネルギー化と小型化に伴って、これらに使用される磁芯に対しても、高出力かつ電力変換効率の高い、小型のものが求められている。サイズが小さいにもかかわらず、高出力、かつ電力変換効率の高い磁芯とするためには、動作周波数を高くすることが有効であることが知られており、高周波領域においても、磁束密度と透磁率とが高く、鉄損が低い材料粉末が求められている。 In recent years, along with the energy saving and miniaturization of home appliances and electronic devices, small cores with high output and high power conversion efficiency are also demanded for the magnetic cores used therein. In order to make a magnetic core with high output and high power conversion efficiency despite its small size, it is known that it is effective to increase the operating frequency. There is a demand for a material powder having high permeability and low iron loss.
従来、このような磁芯としては、鉄とケイ素との混合物である軟磁性粉末が使用されてきた。
一般的に、圧粉磁芯は、シリコン系樹脂被膜を有する軟磁性粉末を加圧成形し、得られた圧粉体を高温で熱処理し、前記シリコン系樹脂被膜をＳｉＯx系絶縁体に変性させることによって製造されている。このようにして得られた圧粉磁芯の磁気特性や機械的特性は、通常、出発材料として使用した軟磁性粉末の組成・形状、成形条件、熱処理条件等に依存する。このため、圧粉磁芯に用いられる材料やその製造方法に関して、特開２００７−１２７４４号公報（以下、「従来技術１」という。）に記載された発明のように、従来から、種々の提案がなされている。
Conventionally, soft magnetic powder that is a mixture of iron and silicon has been used as such a magnetic core.
Generally, a powder magnetic core is formed by press-molding a soft magnetic powder having a silicon-based resin coating, heat-treating the obtained green compact at a high temperature, and modifying the silicon-based resin coating into a SiO x insulating material. It is manufactured by letting The magnetic properties and mechanical properties of the dust core thus obtained usually depend on the composition and shape of the soft magnetic powder used as the starting material, molding conditions, heat treatment conditions, and the like. For this reason, various proposals regarding materials used for the dust core and the manufacturing method thereof have been proposed in the past, as in the invention described in Japanese Patent Application Laid-Open No. 2007-12744 (hereinafter referred to as “Prior Art 1”). Has been made.
また、粒子径が３〜５μｍと非常に小さい磁性粉を使用した造粒物は、（１）磁性粉と樹脂とを混合するスラリー製造工程と、（２）加熱によって有機溶剤を揮発させる乾燥工程と、（３）磁性粉と樹脂との混合物を、メッシュを通して解砕し、整粒する整粒工程と、を備える方法によって、磁性粉が製造されていた。 In addition, the granulated product using magnetic powder having a particle size of 3 to 5 μm is as follows: (1) a slurry manufacturing process in which magnetic powder and resin are mixed; and (2) a drying process in which the organic solvent is volatilized by heating. And (3) a particle size adjusting step of crushing a mixture of magnetic powder and resin through a mesh and adjusting the size, magnetic powder has been produced.
一方、積層セラミックコンデンサ等の積層型セラミック電子部品を使用する際には、セラミックスラリー、導電性ペースト、セラミックペーストが使用されることが、特許第４７１４９９６号公報（以下、「従来技術２」という。）に開示されている。ここで、上記セラミックスラリーは、セラミックグリーンシートの形成に使用される。また、導電性ペーストは、上記セラミックグリーンシートの主面上部分的に付与され、内部導体回路要素膜を形成する。そして、セラミックペーストは、上記導電性ペーストを付与したことによって生じた、セラミックグリーンシートの主面と内部導体回路要素膜との段差を埋めるために使用される。 On the other hand, when a multilayer ceramic electronic component such as a multilayer ceramic capacitor is used, ceramic slurry, conductive paste, and ceramic paste are used in Japanese Patent No. 4714996 (hereinafter referred to as “Prior Art 2”). ). Here, the ceramic slurry is used for forming a ceramic green sheet. Further, the conductive paste is partially applied on the main surface of the ceramic green sheet to form an internal conductor circuit element film. The ceramic paste is used to fill a step between the main surface of the ceramic green sheet and the internal conductor circuit element film, which is generated by applying the conductive paste.
そして、セラミックペーストは、第２のセラミック粉末と第２の樹脂成分とを含み、第１次分散工程と第２次分散工程とを行うことによって製造される。第１次分散工程では、低沸点の有機溶剤と第２のセラミック粉末とからなる１次混合物が分散処理される。次に、第２次分散工程では、第１次工程で分散された混合物に第２の有機バインダーを加えて分散処理が行われる。ここで使用されるセラミック粉末は磁性セラミック粉末である。 The ceramic paste contains the second ceramic powder and the second resin component, and is manufactured by performing a primary dispersion step and a secondary dispersion step. In the first dispersion step, a primary mixture composed of a low-boiling organic solvent and the second ceramic powder is subjected to a dispersion treatment. Next, in the second dispersion step, a dispersion treatment is performed by adding a second organic binder to the mixture dispersed in the first step. The ceramic powder used here is a magnetic ceramic powder.
上述したように、磁性粉末が使用される電子部品の小型化に伴って、使用される磁性粉末の粒子径も小さくなるが、磁性粉末は、粒子径が小さくなると個々の粒子の凝集力が強まることが知られている。
上述した製造方法を採用すると、磁性体と樹脂との混合物が乾燥工程の後に強固に凝集する。このため、得られた乾燥物をメッシュに通しても、粒径が不揃いになってしまい、均一な粒径を有する造粒物（以下、「造粒粉」ということがある。）を得ることができないという問題点があった。
As described above, the particle size of the magnetic powder to be used becomes smaller as the electronic component using the magnetic powder becomes smaller. However, when the particle size of the magnetic powder becomes smaller, the cohesive force of individual particles becomes stronger. It is known.
If the manufacturing method mentioned above is employ | adopted, the mixture of a magnetic body and resin will aggregate firmly after a drying process. For this reason, even if the obtained dried product is passed through a mesh, the particle size becomes uneven, and a granulated product having a uniform particle size (hereinafter sometimes referred to as “granulated powder”) is obtained. There was a problem that could not.
上述した従来例１は、第１次分散工程では、有機バインダーを添加していないことから、低粘度下での分散処理が可能となり、セラミックペーストに含まれるセラミック粉末の分散性を高めることができること、及びセラミック粉末の凝集状態を十分に解砕できるという点では優れた技術である。しかし、粒径分布に関しては考慮されていない。
一方で、金型に巻線を配置し、上記のような粒径が不均一な造粒粉を入れてプレス形成を行って磁性素子を製造すると、造粒粉の流れが悪くなり、成形不良を起こす。さらに、粒径の小さい造粒粉が金型のパンチとダイとの隙間に入ると、金型が摩損することがある。このため、粒径が不均一な造粒粉を使用すると、生産効率が悪くなるという問題点があった。
したがって、均一な粒径を有する造粒粉を、効率良く製造することができる方法に対する強い社会的要請があった。
In the above-mentioned conventional example 1, since the organic binder is not added in the first dispersion step, the dispersion treatment can be performed under a low viscosity, and the dispersibility of the ceramic powder contained in the ceramic paste can be improved. And it is an excellent technique in that the agglomerated state of the ceramic powder can be sufficiently crushed. However, no consideration is given to the particle size distribution.
On the other hand, when a magnetic element is manufactured by placing a winding in a mold and putting a granulated powder with a non-uniform particle size as described above into a press to produce a magnetic element, the flow of the granulated powder becomes worse and the molding is poor. Wake up. Furthermore, when granulated powder having a small particle size enters the gap between the punch and die of the mold, the mold may be worn. For this reason, when granulated powder with non-uniform particle size is used, there is a problem that production efficiency is deteriorated.
Therefore, there has been a strong social demand for a method capable of efficiently producing granulated powder having a uniform particle size.
本発明の発明者は、上記のような状況の下で鋭意研究を進め、本発明を完成したものである。
すなわち、本発明の第１の態様は、磁性粉末と、樹脂と、低沸点溶剤、高沸点溶剤とを混合し、スラリー状混合物を製造する混合物製造工程と；前記スラリー状混合物を加熱して、前記低沸点溶剤を蒸発させ、ペースト状混合物を製造する第１乾燥工程と；前記ペースト状混合物を、メッシュを通して解砕することによって製粒し、粒子を得る整粒工程と；前記粒子を加熱して前記高沸点溶剤を蒸発させて、磁性粒子を得る第２乾燥工程と；
を備え、前記低沸点溶剤は、沸点が９０℃以下の有機溶剤であり、メチルエチルケトン、アセトン、酢酸エチル、ベンゼン、メタノール、エタノール、及びイソプロパノールからなる群から選ばれるいずれかのものであり、前記高沸点溶剤は、沸点が１１０〜２００℃の範囲内にある有機溶剤であり、ブチルセロソルブ、ジイソブチルケトン、ペンタノール、イソペンタノール、キシレン、及び酢酸ｎ−ブチルからなる群から選ばれるいずれかのものであり、前記樹脂は、その硬化温度が前記低沸点溶剤の沸点よりも高い、造粒物の製造方法。である。
The inventor of the present invention has completed the present invention by carrying out diligent research under the above circumstances.
That is, in the first aspect of the present invention, a magnetic powder, a resin, a low boiling point solvent, a high boiling point solvent are mixed to produce a slurry-like mixture, and the slurry-like mixture is heated; A first drying step of evaporating the low boiling point solvent to produce a pasty mixture; a granulating step of granulating the pasty mixture by crushing through a mesh to obtain particles; and heating the particles A second drying step of evaporating the high boiling point solvent to obtain magnetic particles;
The low-boiling solvent is an organic solvent having a boiling point of 90 ° C. or less , and is selected from the group consisting of methyl ethyl ketone, acetone, ethyl acetate, benzene, methanol, ethanol, and isopropanol, The boiling point solvent is an organic solvent having a boiling point in the range of 110 to 200 ° C. , and is any one selected from the group consisting of butyl cellosolve, diisobutyl ketone, pentanol, isopentanol, xylene, and n-butyl acetate. Yes, the resin has a curing temperature higher than the boiling point of the low- boiling solvent, and is a method for producing a granulated product. It is.
ここで、前記磁性粉末は、カルボニル鉄粉、アモルファス鉄粉、ケイ素鋼、パーマロイ及びセンダストからなる群から選ばれるいずれかであることが好ましい。また、前記樹脂は、硬化温度が１５０℃以上の樹脂であることが好ましい。さらにまた、前記高沸点溶剤は、前記樹脂量に対して、１０〜６０重量％であることが好ましく、１０〜４５重量％（以下、「ｗｔ％」ということがある。）であることが、さらに好ましい。 Here, the magnetic powder is preferably any one selected from the group consisting of carbonyl iron powder, amorphous iron powder, silicon steel, permalloy, and sendust. Further, the resin is preferably a resin having a curing temperature of 150 ° C. or higher. Furthermore, the high boiling point solvent is preferably 10 to 60% by weight, and preferably 10 to 45% by weight (hereinafter sometimes referred to as “wt%”) with respect to the resin amount. Further preferred.
前記樹脂は、エポキシ樹脂、フェノール樹脂、シリコン樹脂、不飽和ポリエステル樹脂及びアミド樹脂からなる群から選ばれるものであることが好ましい。
前記低沸点溶剤は、沸点が９０℃以下の有機溶剤であることが好ましく、前記低沸点溶剤は、メチルエチルケトン、アセトン、トルエン、酢酸エチル、ベンゼン、メタノール、エタノール、及びイソプロパノールからなる群から選ばれるいずれかのものであることが好ましい。
The resin is preferably selected from the group consisting of an epoxy resin, a phenol resin, a silicon resin, an unsaturated polyester resin, and an amide resin.
The low boiling point solvent is preferably an organic solvent having a boiling point of 90 ° C. or less, and the low boiling point solvent is any selected from the group consisting of methyl ethyl ketone, acetone, toluene, ethyl acetate, benzene, methanol, ethanol, and isopropanol. These are preferable.
前記高沸点溶剤は、沸点が１１０〜２００℃の範囲内にある有機溶剤であることが好ましく、前記高沸点溶剤は、ブチルセロソルブ、ジイソブチルケトン、テルピネオール、ペンタノール、イソペンタノール、キシレン、及び酢酸ｎ−ブチルからなる群から選ばれるいずれかのものであることが好ましい。
また、前記第１乾燥工程は、５０〜６０℃で加熱することが好ましく、前記第２乾燥工程は、１１０〜１３０℃で加熱することが好ましい。前記整粒工程で使用するメッシュは、前記造粒物の粒子径よりも２〜５倍大きな目開き径を有するメッシュであることが好ましい。
スラリー状混合物は、スラリーの総重量に対して、８０〜９５重量％の磁性粉末と、４〜１５重量％の低沸点溶剤と、０．２〜１．５重量％の高沸点溶剤と、１．５〜３．５重量％の樹脂とを使用することが好ましい。
The high boiling point solvent is preferably an organic solvent having a boiling point in the range of 110 to 200 ° C., and the high boiling point solvent is butyl cellosolve, diisobutyl ketone, terpineol, pentanol, isopentanol, xylene, and n-acetate. It is preferably any one selected from the group consisting of butyl.
The first drying step is preferably heated at 50 to 60 ° C, and the second drying step is preferably heated at 110 to 130 ° C. The mesh used in the granulation step is preferably a mesh having an opening diameter 2 to 5 times larger than the particle diameter of the granulated product.
The slurry mixture consists of 80 to 95 wt% magnetic powder, 4 to 15 wt% low boiling point solvent, 0.2 to 1.5 wt% high boiling point solvent, 1 It is preferable to use 5 to 3.5% by weight of resin.
本発明の第２の態様は、上述したいずれかの方法によって製造され、以下の特性を有する造粒物である：
（１）粒径が７５μｍ未満である造粒物の割合が１０％以下；
（２）粒径が５００μｍを超える造粒物の割合が２０％以下；
（３）第１乾燥温度及び第２乾燥温度における乾燥性が良好。
また、本発明の第３の態様は、上記のようにして得られた造粒物中に、巻線が組み入れられたインダクタである。ここで、上記インダクタは、組み入れられた巻き線を含む前記造粒物を１５０〜２００℃で硬化させたものであることが好ましい。
A second aspect of the present invention is a granulated product produced by any of the methods described above and having the following characteristics:
(1) The proportion of the granulated product having a particle size of less than 75 μm is 10% or less;
(2) The proportion of the granulated product having a particle size exceeding 500 μm is 20% or less;
(3) Good drying at the first drying temperature and the second drying temperature.
The third aspect of the present invention is an inductor in which a winding is incorporated in the granulated material obtained as described above. Here, it is preferable that the said inductor is what hardened | cured the said granulated material containing the incorporated winding at 150-200 degreeC .
本発明によれば、磁性体と樹脂とが強固に凝集することを防ぎつつ、メッシュによる安定した解砕が可能となる。それによって、均一な粒径を有する造粒物（以下、「造粒粉」ということがある。）を、効率良く製造することができる。
さらに、こうして得られた造粒粉は、流れがよく、成形不良を起こさないばかりでなく、成形金型を傷めることもなく、生産効率を挙げることができる。
According to the present invention, stable crushing with a mesh is possible while preventing the magnetic body and the resin from agglomerating firmly. Thereby, a granulated product having a uniform particle size (hereinafter sometimes referred to as “granulated powder”) can be produced efficiently.
Furthermore, the granulated powder thus obtained has a good flow and does not cause defective molding, and can increase production efficiency without damaging the molding die.
以下に、本発明をより具体的に説明する。上述した通り、本発明は、（Ａ）混合物製造工程と；（Ｂ）第１乾燥工程と；（Ｃ）整粒工程と；（Ｄ）第２乾燥工程と；を備える造粒物の製造方法である。
ここで、上記混合物製造工程では、(a1)磁性粉末と、(a2)樹脂と、(a3)低沸点溶剤、(a4)高沸点溶剤とを混合し、スラリー状混合物を製造する。また、上記第１乾燥工程では、(b1)前記スラリー状混合物を加熱して、(b2)前記低沸点溶剤を蒸発させ、(b3)ペースト状混合物を製造する。次いで上記整粒工程では、(c1)前記ペースト状混合物を、メッシュを通して解砕し、(c2)整粒して粒子を得る。最後に、上記第２乾燥工程では、(d1)前記粒子を加熱し、(d2)前記高沸点溶剤を蒸発させて、磁性粒子を得る。
Hereinafter, the present invention will be described more specifically. As described above, the present invention provides (A) a mixture production process; (B) a first drying process; (C) a granulating process; and (D) a second drying process. It is.
Here, in the above-mentioned mixture production step, (a1) magnetic powder, (a2) resin, (a3) low boiling point solvent, and (a4) high boiling point solvent are mixed to produce a slurry mixture. In the first drying step, (b1) the slurry mixture is heated, (b2) the low boiling point solvent is evaporated, and (b3) a paste mixture is produced. Next, in the sizing step, (c1) the paste-like mixture is crushed through a mesh, and (c2) sizing is performed to obtain particles. Finally, in the second drying step, (d1) the particles are heated and (d2) the high boiling point solvent is evaporated to obtain magnetic particles.
ここで、上記磁性粉末としては、カルボニル鉄粉（Carbonyl Iron Powder、以下、「CIP」ということがある。）、アモルファス純鉄粉、ケイ素鋼、パーマロイ、センダスト等を使用することができる。
CIPは、真球状の均質な鉄粉であり、直径１〜８μｍの粒度分布を有する。アモルファス純鉄粉は、結晶構造を持たない低損失な金属材料の一種であり、Feを主成分とするFe基アモルファス金属材料は、方向性ケイ素鋼板に比べて、無負荷損が小さいという特性を有する。
ケイ素鋼は、鉄にケイ素が３％前後含まれた軟質磁性材料であり、透磁率・電気抵抗が高く、磁気ヒステリシス損失が少ないという特性を有する。
Here, as the magnetic powder, carbonyl iron powder (Carbonyl Iron Powder, hereinafter referred to as “CIP”), amorphous pure iron powder, silicon steel, permalloy, Sendust, or the like can be used.
CIP is a true spherical homogeneous iron powder and has a particle size distribution with a diameter of 1 to 8 μm. Amorphous pure iron powder is a type of low-loss metal material that does not have a crystal structure, and Fe-based amorphous metal material, which contains Fe as its main component, has the characteristic of low no-load loss compared to oriented silicon steel sheets. Have.
Silicon steel is a soft magnetic material in which about 3% of silicon is contained in iron, and has characteristics of high magnetic permeability and electrical resistance and low magnetic hysteresis loss.
パーマロイは、鉄ニッケル合金であり、軟磁性合金であるとともに強磁性材である。透磁性が非常に高く、磁気を通し易い性質を有する。
センダストは、高透磁率合金の１つである。ケイ素９．５％，アルミニウム５５．５％を含む鉄合金で，パーマロイに匹敵する高い透磁率を示す。また飽和磁束密度も高い。非常に硬くて脆いため、鍛造や圧延などの加工はできないという特性を有する。
上記の磁性粉末のうち、CIPを主として使用することが、透磁率が高く、直流重畳特性が上がるために好ましい。
Permalloy is an iron-nickel alloy, a soft magnetic alloy and a ferromagnetic material. It has very high magnetic permeability and is easy to pass magnetism.
Sendust is one of high permeability alloys. It is an iron alloy containing 9.5% silicon and 55.5% aluminum, and exhibits high permeability comparable to permalloy. The saturation magnetic flux density is also high. Since it is very hard and brittle, it has a characteristic that it cannot be processed by forging or rolling.
Of the above magnetic powders, CIP is mainly used because of its high magnetic permeability and improved direct current superposition characteristics.
上述した樹脂は、磁性粉同士をつなぎ合わせるバインダーとして使用される。こうした樹脂としては、硬化温度が１５０℃以上の熱硬化性樹脂を、耐熱性があり、強度が高いことから好適に使用することができる。具体的には、エポキシ樹脂、シリコン樹脂、フェノール樹脂、不飽和ポリエステル樹脂、アミノ樹脂等を使用することができる。 The above-described resin is used as a binder for joining magnetic powders together. As such a resin, a thermosetting resin having a curing temperature of 150 ° C. or higher can be suitably used because it has heat resistance and high strength. Specifically, an epoxy resin, a silicon resin, a phenol resin, an unsaturated polyester resin, an amino resin, or the like can be used.
上述した低沸点溶剤は、磁性粉に対する樹脂の分散を向上させるために使用する。沸点が９０℃以下の有機溶剤であることが、低沸点溶剤として使用することができる溶剤の種類が多くなることから好ましい。
こうした低沸点溶剤としては、メチルエチルケトン、アセトン、トルエン、酢酸エチル、ベンゼン、メタノール、エタノール、及びイソプロパノールからなる群から選ばれるいずれかのものであることが、取り扱いの容易さ及び安全性の面から好ましい。これらの中でも、メチルエチルケトン及びアセトンを使用することが、揮発性が高く工程時間の短縮ができることからさらに好ましい。
The low boiling point solvent mentioned above is used in order to improve the dispersion of the resin with respect to the magnetic powder. An organic solvent having a boiling point of 90 ° C. or less is preferable because the number of types of solvents that can be used as the low boiling point solvent is increased.
Such a low boiling point solvent is preferably one selected from the group consisting of methyl ethyl ketone, acetone, toluene, ethyl acetate, benzene, methanol, ethanol, and isopropanol from the viewpoint of ease of handling and safety. . Among these, it is more preferable to use methyl ethyl ketone and acetone because they have high volatility and can shorten the process time.
上述した高沸点溶剤は、均一な粒度分布の造粒粉を製造するために使用する。沸点が１１０〜２００℃の範囲内にある有機溶剤であることが、第１乾燥工程で揮発せず、樹脂の硬化が開始されない温度であることから好ましい。１４５〜１７５℃の範囲にある溶剤を使用することが、さらに好ましい。
こうした高沸点溶剤としては、ブチルセロソルブ、ジイソブチルケトン、テルピネオール、ペンタノール、イソペンタノール、キシレン、及び酢酸ｎ−ブチルからなる群から選ばれるいずれかのものであることが、取り扱いの容易さ及び安全性の面から好ましい。これらの中でも、ブチルセロソルブ及びジイソブチルケトンを使用することが、蒸気圧が高く、１１０〜１３０℃前後の低い温度で乾燥造粒粉を乾燥させることができるため、さらに好ましい。
The high boiling point solvent described above is used to produce a granulated powder having a uniform particle size distribution. An organic solvent having a boiling point in the range of 110 to 200 ° C. is preferable because it is a temperature at which the resin does not volatilize in the first drying step and the curing of the resin is not started. More preferably, a solvent in the range of 145 to 175 ° C is used.
Such a high boiling point solvent is any one selected from the group consisting of butyl cellosolve, diisobutyl ketone, terpineol, pentanol, isopentanol, xylene, and n-butyl acetate. From the viewpoint of Among these, it is more preferable to use butyl cellosolve and diisobutyl ketone since the dried granulated powder can be dried at a low temperature of about 110 to 130 ° C. because of high vapor pressure.
上述した樹脂、低沸点溶剤及び高沸点溶剤の混合物を磁性粉と混合して、スラリーを製造する。樹脂と磁性粉とが均一に混ざり合って分散するようにするために、このスラリー中の樹脂濃度は、スラリーの総重量の１．５〜３．５重量％とすることが好ましい。この範囲で使用することによって、磁性粉に対して樹脂を十分に分散させることができるからである。
さらに、スラリー中の樹脂濃度は、スラリー総重量の２．６〜３．４重量％であることが、均質な造粒粉を得ることができるため、より好ましい。
また、スラリー中の高沸点溶剤と低沸点溶剤の総重量は、樹脂の重量の４００〜５００重量％であることが、スラリーに対する樹脂の分散性が向上すること、及び工程時間が短縮されることから好ましい。
A mixture of the resin, low boiling point solvent and high boiling point solvent described above is mixed with magnetic powder to produce a slurry. In order to uniformly mix and disperse the resin and the magnetic powder, the resin concentration in the slurry is preferably 1.5 to 3.5% by weight of the total weight of the slurry. It is because resin can fully be disperse | distributed with respect to magnetic powder by using in this range.
Further, the resin concentration in the slurry is more preferably 2.6 to 3.4% by weight of the total weight of the slurry because homogeneous granulated powder can be obtained.
In addition, the total weight of the high-boiling solvent and the low-boiling solvent in the slurry is 400 to 500% by weight of the weight of the resin, which improves the dispersibility of the resin in the slurry and shortens the process time. To preferred.
後述する状態のペーストを得るために、スラリーを製造する際に使用する高沸点溶剤の量は、樹脂の重量に対して１０〜４５重量％であることが、後述するペーストを、造粒の際に柔らかい状態に保つことができるため、好ましい。
さらに、高沸点溶剤の量は、樹脂の重量に対して２０〜３０重量％であることが、均質な造粒粉を得ることができるため、より好ましい。
換言すると、このスラリー状混合物は、スラリーの総重量に対して、８０〜９５重量％の磁性粉末と、４〜１５重量％の低沸点溶剤と、０．２〜１．５重量％の高沸点溶剤と、１．５〜３．５重量％の樹脂とを使用して製造することが好ましい。
さらに、このスラリーは、８０〜９０重量％の磁性粉末と、６．９〜１４．２重量％の低沸点溶剤と、０．５〜１．０重量％の高沸点溶剤と、２．６〜３．４重量％の樹脂とを使用することが、均質な造粒粉を得ることができるために、さらに好ましい。
In order to obtain a paste in a state described later, the amount of the high boiling point solvent used in producing the slurry is 10 to 45% by weight based on the weight of the resin. It is preferable because it can be kept soft.
Further, the amount of the high boiling point solvent is more preferably 20 to 30% by weight with respect to the weight of the resin, since a homogeneous granulated powder can be obtained.
In other words, the slurry-like mixture has 80 to 95% by weight of magnetic powder, 4 to 15% by weight of low boiling point solvent, and 0.2 to 1.5% by weight of high boiling point based on the total weight of the slurry. It is preferable to manufacture using a solvent and 1.5 to 3.5 weight% of resin.
Further, the slurry comprises 80 to 90% by weight of magnetic powder, 6.9 to 14.2% by weight of low boiling point solvent, 0.5 to 1.0% by weight of high boiling point solvent, 2.6 to It is more preferable to use 3.4% by weight of resin because a homogeneous granulated powder can be obtained.
以上のようにして製造したスラリーを、約５０〜６０℃にて１５〜３０分乾燥させ、低沸点溶剤を蒸発させてペーストとする。すなわち、ペーストは、磁性粉と樹脂と高沸点溶剤とを含み、磁性粉同士が強固に凝集しないようになっている。
このペーストをメッシュ（金網）に擦りつけて解砕し、整粒する。目標とする造粒粉の粒径の２〜５倍の目開き径を有する上記メッシュを使用することが好ましい。さらに、目標とする造粒粉の粒径の２〜４倍の目開き径を有するものであることが、均質な所望の粒径の造粒粉が得られることから、より好ましい。
例えば、目開き径が約２００〜５００μｍの篩を用いると、約１００μｍの粒径の造粒粉を得ることができる。
The slurry produced as described above is dried at about 50 to 60 ° C. for 15 to 30 minutes, and the low boiling point solvent is evaporated to obtain a paste. That is, the paste contains magnetic powder, a resin, and a high boiling point solvent so that the magnetic powders do not aggregate firmly.
The paste is crushed by rubbing it on a mesh (metal mesh) and sized. It is preferable to use the mesh having an opening diameter of 2 to 5 times the particle diameter of the target granulated powder. Furthermore, it is more preferable to have an opening diameter of 2 to 4 times the particle diameter of the target granulated powder because a granulated powder having a uniform desired particle diameter can be obtained.
For example, when a sieve having an opening size of about 200 to 500 μm is used, a granulated powder having a particle size of about 100 μm can be obtained.
解砕され、整粒されたペーストを、上記ペースト中の樹脂が硬化しない程度に加熱して高沸点溶剤を蒸発させ、造粒する。具体的には、１１０〜１３０℃の範囲の温度で加熱することが好ましい。以上のようにして、均一な粒径を有する造粒粉を得ることができる。また、本発明の方法で得られた造粒粉は、磁性粉が樹脂で被覆されているため、熱硬化後の強度が向上するとともに、絶縁性も向上する。さらに、防錆効果も高い。 The crushed and sized paste is heated to such an extent that the resin in the paste is not cured to evaporate the high boiling point solvent and granulate. Specifically, it is preferable to heat at a temperature in the range of 110 to 130 ° C. As described above, a granulated powder having a uniform particle size can be obtained. Moreover, since the granulated powder obtained by the method of the present invention is coated with a magnetic powder, the strength after thermosetting is improved and the insulation is also improved. Furthermore, the rust prevention effect is also high.
次いで、以上のようにして得られた造粒粉を用いて、電子部品を製造する。以下に、インダクタを製造する場合を例に挙げて説明する。
まず、金型に、上述したようにして得た造粒粉を所定の量で入れる。ここに、所望の数で巻いた巻線を組み入れ、さらに造粒粉を入れて、巻線を覆う。金型をプレスし、造粒粉中の樹脂が硬化する温度以上の温度で、所望の時間加熱して、樹脂を硬化させる。
加熱温度は１５０〜２００℃が好ましい。さらに、樹脂がエポキシ樹脂では１５０℃、樹脂がシリコン樹脂では２００℃が、より好ましい。
Next, an electronic component is manufactured using the granulated powder obtained as described above. Hereinafter, a case where an inductor is manufactured will be described as an example.
First, the granulated powder obtained as described above is put into a mold in a predetermined amount. Here, a winding wound in a desired number is incorporated, and further granulated powder is put to cover the winding. The mold is pressed and heated for a desired time at a temperature equal to or higher than the temperature at which the resin in the granulated powder is cured to cure the resin.
The heating temperature is preferably 150 to 200 ° C. Further, 150 ° C. is more preferable when the resin is an epoxy resin, and 200 ° C. is more preferable when the resin is a silicon resin.
本発明の造粒粉は流れが良く、分散状態も向上しているため、金型に入れたときの充填密度を高くすることができる。これによって、透磁率の向上を図ることができるとともに、上記のような電子部品を製造したときの歩留まりも良くなるという利点がある。 Since the granulated powder of the present invention has a good flow and improved dispersion, the packing density when placed in a mold can be increased. As a result, the magnetic permeability can be improved and the yield can be improved when the electronic parts as described above are manufactured.
以下に、実施例を用いて、本発明をさらに詳細に説明する。なお、本発明は、以下の実施例に何等限定されるものではない。
（実施例１）本発明例１〜３の造粒粉の製造
本発明では、磁性粉として、粒子径が３〜５μｍのカルボニル鉄粉を使用した。この鉄粉の組成は、Ｆｅ：Ｓｉ：Ｃｒ＝１００：０：０であった。この磁性粉を、目開き径２５５〜５００μｍの篩で分級して使用した。
ガラス転移点が１３０〜１４０℃である熱硬化性エポキシ樹脂を使用した。低沸点溶剤としてはメチルエチルケトンを、また、高沸点溶剤としてはブチルセロソルブを、それぞれ使用した。
Hereinafter, the present invention will be described in more detail with reference to examples. The present invention is not limited to the following examples.
Example 1 Production of Granulated Powder of Invention Examples 1 to 3 In the present invention, carbonyl iron powder having a particle diameter of 3 to 5 μm was used as the magnetic powder. The composition of this iron powder was Fe: Si: Cr = 100: 0: 0. This magnetic powder was classified and used with a sieve having an opening diameter of 255 to 500 μm.
A thermosetting epoxy resin having a glass transition point of 130 to 140 ° C. was used. Methyl ethyl ketone was used as the low boiling point solvent, and butyl cellosolve was used as the high boiling point solvent.
１５．０ｇのメチルエチルケトンと、１．０ｇのブチルセロソルブと、３．２ｇのエポキシ樹脂とを高分子製カップの中で混合し、十分に撹拌して混合液とした。（これらの混合の割合は、スラリーの総重量に対して、メチルエチルケトンが１２％（w/w）、ブチルセロソルブが約１％（w/w）、エポキシ樹脂が約２％（w/w）であった。）
次いで、１００ｇのカルボニル鉄粉と、上記の混合液の全量とを混合し、十分に撹拌してエポキシ樹脂をカルボニル鉄粉に対して十分に分散させ、スラリーを製造した。カルボニル鉄粉の混合割合は、スラリーの総重量に対して、約８５％（w/w）であった。
15.0 g of methyl ethyl ketone, 1.0 g of butyl cellosolve, and 3.2 g of an epoxy resin were mixed in a polymer cup and sufficiently stirred to obtain a mixed solution. (The mixing ratios were 12% (w / w) for methyl ethyl ketone, about 1% (w / w) for butyl cellosolve, and about 2% (w / w) for epoxy resin based on the total weight of the slurry. )
Next, 100 g of carbonyl iron powder and the total amount of the above mixed solution were mixed and sufficiently stirred to sufficiently disperse the epoxy resin in the carbonyl iron powder to produce a slurry. The mixing ratio of the carbonyl iron powder was about 85% (w / w) based on the total weight of the slurry.
次いで、このスラリーを高温槽に入れて約５０℃（第１乾燥温度）で３０分加熱してメチルエチルケトンを蒸発させ、柔らかい固体状態のペーストを製造した。
次いで、目開き径３５５μｍのメッシュ（篩）に、このペーストを擦りつけて解砕し、粒子を得た。
引き続き、上記で得られた粒子を高温槽に入れて１１０℃（第２乾燥温度）で２５〜３５分加熱してメチルセロソルブを蒸発させて整粒し、造粒粉を得た。以上のようにして、本発明例１の造粒粉を得た。
以上のようにして得られた本発明例１の造粒粉の粒径を、ふるいを用いて測定したところ、粒径が７５μｍ未満の粒子（ＤＳ）の含有量は約５％、５００μｍを越える粒子（ＤＬ）の含有量は約１０％、平均粒径は約１００μｍであった。
Next, this slurry was put in a high temperature bath and heated at about 50 ° C. (first drying temperature) for 30 minutes to evaporate methyl ethyl ketone, thereby producing a soft solid paste.
Next, the paste was rubbed against a mesh (sieve) having an opening diameter of 355 μm to break up particles.
Subsequently, the particles obtained above were put in a high-temperature bath and heated at 110 ° C. (second drying temperature) for 25 to 35 minutes to evaporate methyl cellosolve and sized to obtain granulated powder. As described above, the granulated powder of Invention Example 1 was obtained.
When the particle size of the granulated powder of Example 1 of the present invention obtained as described above was measured using a sieve, the content of particles having a particle size of less than 75 μm (D S ) was about 5%, 500 μm. The content of particles exceeding (D L ) was about 10%, and the average particle size was about 100 μm.
（実施例２）本発明例２の造粒粉の製造
実施例１における第２乾燥温度を１２０℃に変更した以外は実施例１と同様にして、本発明例２の造粒粉を得た。得られた本発明例２の造粒粉中のＤＳ及びＤＬの割合、及び平均粒径は実施例１と同様であった。
（実施例３）本発明例３の造粒粉の製造
実施例１における第２乾燥温度を１３０℃に変更した以外は実施例１と同様にして、本発明例３の造粒粉を得た。得られた本発明例３の造粒粉中のＤＳ及びＤＬの割合、及び平均粒径は実施例１と同様であった。
(Example 2) Production of granulated powder of Invention Example 2 Granulated powder of Invention Example 2 was obtained in the same manner as in Example 1 except that the second drying temperature in Example 1 was changed to 120 ° C. . D ratio of S and D L of the resulting granulated powder of the present invention Example 2, and the average particle size was the same as in Example 1.
(Example 3) Production of granulated powder of Example 3 of the present invention Granulated powder of Example 3 of the present invention was obtained in the same manner as in Example 1 except that the second drying temperature in Example 1 was changed to 130 ° C. . D ratio of S and D L of the granulated powder in the present invention obtained Example 3, and the average particle size was the same as in Example 1.
（実施例４）本発明例４の造粒粉の製造
実施例１で約５０℃とした第１乾燥工程の温度を約６０℃に上げた以外は実施例１と同様にして、本発明例４の造粒粉を製造した。得られた本発明例４の造粒粉中のＤＳ及びＤＬの割合、及び平均粒径は実施例１と同様であった。
（実施例５）本発明例５の造粒粉の製造
実施例２で約５０℃とした第１乾燥工程の温度を約６０℃に上げた以外は実施例２と同様にして、本発明例５の造粒粉を製造した。得られた本発明例５の造粒粉中のＤＳ及びＤＬの割合、及び平均粒径は実施例１と同様であった。
(Example 4) Production of granulated powder of Example 4 of the present invention Example of the present invention was carried out in the same manner as Example 1 except that the temperature of the first drying step, which was about 50 ° C in Example 1, was raised to about 60 ° C. 4 granulated powder was produced. D ratio of S and D L of the granulated powder of the present invention example 4 obtained, and the average particle size was the same as in Example 1.
(Example 5) Production of granulated powder of Example 5 of the invention Example of the invention was carried out in the same manner as Example 2 except that the temperature of the first drying step, which was about 50 ° C in Example 2, was raised to about 60 ° C. 5 granulated powder was produced. D ratio of S and D L of the granulated powder in the present invention obtained Example 5, and the average particle size was the same as in Example 1.
（実施例６）本発明例６の造粒粉の製造
実施例３で約５０℃とした第１乾燥工程の温度を約６０℃に上げた以外は実施例３と同様にして、本発明例６の造粒粉を製造した。得られた本発明例６の造粒粉中のＤＳ及びＤＬの割合、及び平均粒径は実施例１と同様であった。
（実施例７）本発明例７の造粒粉の製造
実施例２で、樹脂量に対して３０ｗｔ％とした高沸点溶剤の添加量を、１０ｗｔ％にした以外は実施例２と同様にして、本発明例７の造粒粉を得た。得られた本発明例７の造粒粉中のＤＳの割合は約９％、ＤＬの割合は約１１％であった。
(Example 6) Production of granulated powder of Example 6 of the present invention Example of the present invention was carried out in the same manner as Example 3 except that the temperature of the first drying step, which was about 50 ° C in Example 3, was raised to about 60 ° C. 6 granulated powder was produced. D ratio of S and D L of the granulated powder in the obtained present invention Example 6, and the average particle size was the same as in Example 1.
(Example 7) Production of granulated powder of Invention Example 7 In Example 2, the same procedure as in Example 2 was conducted except that the amount of the high-boiling solvent added was 30 wt% relative to the amount of resin, and the addition amount was 10 wt%. The granulated powder of Invention Example 7 was obtained. D ratio of S of the present invention obtained in Example 7 granulated powder in about 9%, the ratio of D L was approximately 11%.
（実施例８）本発明例８の造粒粉の製造
実施例２で、樹脂量に対して３０ｗｔ％とした高沸点溶剤の添加量を、２０ｗｔ％にした以外は実施例２と同様にして、本発明例８の造粒粉を得た。得られた本発明例８の造粒粉中のＤＳの割合は約７％、ＤＬの割合は約１１％であった。本発明例８の造粒粉の性質は実施例１で得られた造粒粉１とほぼ同等であった
（実施例９）本発明例９の造粒粉の製造
実施例２で、樹脂量に対して３０ｗｔ％とした高沸点溶剤の添加量を、４０ｗｔ％にした以外は実施例２と同様にして、本発明例９の造粒粉を得た。得られた本発明例９の造粒粉中のＤＳの割合は約４％、ＤＬの割合は約１４％であった。
(Example 8) Production of granulated powder of Invention Example 8 In the same manner as in Example 2 except that the amount of the high-boiling solvent added in Example 2 was 30 wt% with respect to the amount of resin was 20 wt%. The granulated powder of Invention Example 8 was obtained. D ratio of S of granulated powder in the obtained Inventive Example 8 was about 7%, the ratio of D L was approximately 11%. The properties of the granulated powder of Invention Example 8 were almost equivalent to the granulated powder 1 obtained in Example 1 (Example 9) Production of Granulated Powder of Example 9 of the Invention In Example 2, the amount of resin A granulated powder of Invention Example 9 was obtained in the same manner as in Example 2 except that the amount of the high-boiling solvent added was 30 wt% with respect to 40 wt%. D ratio of S obtained in granulated powder of the present invention Example 9 was about 4%, the ratio of D L was about 14%.
（実施例10）本発明例10の造粒粉の製造
実施例２で、樹脂量に対して３０ｗｔ％とした高沸点溶剤の添加量を、４５ｗｔ％にした以外は実施例２と同様にして、本発明例８の造粒粉を得た。得られた本発明例８の造粒粉中のＤＳの割合は約４％、ＤＬの割合は約１８％であった。
（実施例11）本発明例11の造粒粉の製造
実施例２で、樹脂量に対して３５０ｗｔ％とした低沸点溶剤添加量を、２５０ｗｔ％にした以外は、実施例２と同様にして本発明例11の造粒粉を得た。
(Example 10) Production of granulated powder of Invention Example 10 In Example 2, the same procedure as in Example 2 was conducted except that the amount of the high-boiling solvent added was 30 wt% with respect to the resin amount was 45 wt%. The granulated powder of Invention Example 8 was obtained. D ratio of S of granulated powder in the obtained Inventive Example 8 was about 4%, the ratio of D L was about 18%.
(Example 11) Production of granulated powder of Example 11 of the present invention In Example 2, except that the amount of the low boiling point solvent added to 350 wt% with respect to the resin amount was changed to 250 wt%, the same as in Example 2 A granulated powder of Invention Example 11 was obtained.
（実施例12）本発明例12の造粒粉の製造
実施例２で、樹脂量に対して３５０ｗｔ％とした低沸点溶剤添加量を、４５０ｗｔ％にした以外は実施例２と同様にして、本発明例12の造粒粉を得た。
（実施例13）本発明例13の造粒粉の製造
実施例２で使用した高沸点溶剤をブチルセロソルブからプロピレングリコールモノメチルエーテルアセテートに代えた以外は、実施例２と同様にして、本発明例13の造粒粉を得た。
(Example 12) Production of granulated powder of Invention Example 12 In Example 2, except that the amount of low boiling point solvent added to 350 wt% with respect to the resin amount was changed to 450 wt%, the same as in Example 2, A granulated powder of Invention Example 12 was obtained.
(Example 13) Production of granulated powder of Example 13 of the present invention Example 13 of the present invention was carried out in the same manner as Example 2 except that the high boiling point solvent used in Example 2 was changed from butyl cellosolve to propylene glycol monomethyl ether acetate. Of granulated powder was obtained.
（実施例14）本発明例14の造粒粉の製造
実施例２で使用した高沸点溶剤をブチルセロソルブからシクロヘキサンに代えた以外は実施例２と同様にして、本発明例14の造粒粉を得た。
（実施例15）本発明例15の造粒粉の製造
実施例２で使用した高沸点溶剤をブチルセロソルブからジイソブチルケトンにした以外は実施例２と同様にして、本発明例15の造粒粉を得た。
(Example 14) Production of granulated powder of Invention Example 14 The granulated powder of Invention Example 14 was prepared in the same manner as in Example 2 except that the high-boiling solvent used in Example 2 was changed from butyl cellosolve to cyclohexane. Obtained.
(Example 15) Production of granulated powder of Invention Example 15 The granulated powder of Invention Example 15 was prepared in the same manner as in Example 2 except that the high boiling point solvent used in Example 2 was changed from butyl cellosolve to diisobutyl ketone. Obtained.
（実施例16）本発明例16の造粒粉の製造
実施例２で使用した低沸点溶剤をメチルエチルケトンからアセトンに代え、低沸点溶剤の対樹脂重量を２５０ｗｔ％とした以外は、実施例２と同様にして本発明例16の造粒粉を得た。
（実施例17）本発明例17の造粒粉の製造
実施例２で使用した低沸点溶剤をメチルエチルケトンからアセトンに代えた以外は、実施例２と同様にして本発明例17の造粒粉を得た。
(Example 16) Production of granulated powder of Example 16 of the present invention Example 2 except that the low boiling point solvent used in Example 2 was changed from methyl ethyl ketone to acetone, and the weight of the low boiling point solvent relative to the resin was 250 wt%. Similarly, the granulated powder of Invention Example 16 was obtained.
(Example 17) Production of granulated powder of Invention Example 17 The granulated powder of Invention Example 17 was prepared in the same manner as in Example 2 except that the low boiling point solvent used in Example 2 was changed from methyl ethyl ketone to acetone. Obtained.
（実施例18）本発明例17の造粒粉の製造
実施例２で使用した低沸点溶剤をメチルエチルケトンからアセトンに代え、低沸点溶剤の対樹脂重量を４５０ｗｔ％とした以外は、実施例２と同様にして本発明例18の造粒粉を得た。
（実施例19）本発明例19の造粒粉の製造
実施例２で造粒粉に対して３．５ｗｔ％としたエポキシ樹脂添加量を２．０ｗｔ％とした以外は、実施例２と同様にして、本発明例19の造粒粉を得た。
（実施例20）本発明例20の造粒粉の製造
実施例２で造粒粉に対して３．５ｗｔ％としたエポキシ樹脂添加量を２．５ｗｔ％とした以外は、実施例２と同様にして、本発明例20の造粒粉を得た。
(Example 18) Production of granulated powder of Example 17 of the present invention Example 2 except that the low boiling point solvent used in Example 2 was changed from methyl ethyl ketone to acetone, and the weight of the low boiling point solvent relative to the resin was changed to 450 wt%. Similarly, a granulated powder of Invention Example 18 was obtained.
(Example 19) Production of granulated powder of Invention Example 19 The same as Example 2 except that the amount of the epoxy resin added to 3.5 wt% of the granulated powder in Example 2 was 2.0 wt%. Thus, a granulated powder of Invention Example 19 was obtained.
(Example 20) Production of granulated powder of Invention Example 20 The same as Example 2 except that the amount of epoxy resin added to 3.5 wt% of the granulated powder in Example 2 was 2.5 wt%. Thus, a granulated powder of Invention Example 20 was obtained.
（実施例21）本発明例21の造粒粉の製造
実施例２で造粒粉に対して３．５ｗｔ％としたエポキシ樹脂添加量を３．０ｗｔ％とした以外は、実施例２と同様にして、本発明例21の造粒粉を得た。
（実施例22）本発明例22の造粒粉の製造
実施例２で使用したエポキシ樹脂をシリコン樹脂に代えるとともに樹脂添加量を３．５重量％から３．７重量％にした以外は実施例２と同様にして、本発明例22の造粒粉を得た。
(Example 21) Production of granulated powder of Invention Example 21 The same as Example 2 except that the amount of epoxy resin added to 3.5 wt% of the granulated powder in Example 2 was changed to 3.0 wt%. Thus, a granulated powder of Invention Example 21 was obtained.
(Example 22) Production of granulated powder of Example 22 of the present invention Example except that the epoxy resin used in Example 2 was replaced with silicon resin and the resin addition amount was changed from 3.5 wt% to 3.7 wt% In the same manner as in Example 2, a granulated powder of Inventive Example 22 was obtained.
（実施例23）本発明例23の造粒粉の製造
実施例22で使用した高沸点溶剤をブチルセロソルブからプロピレングリコールモノメチルエーテルアセテートに代えた以外は実施例22と同様にして、本発明例23の造粒粉を得た。
（実施例24）本発明例24の造粒粉の製造
実施例22で使用した高沸点溶剤をブチルセロソルブからシクロヘキサンに代えた以外は実施例22と同様にして、本発明例24の造粒粉を得た。
（実施例25）本発明例25の造粒粉の製造
実施例22で使用した高沸点溶剤をブチルセロソルブからジイソブチルケトンに代えた以外は実施例22と同様にして本発明例25の造粒粉を得た。
(Example 23) Production of granulated powder of Inventive Example 23 In the same manner as in Example 22, except that the high boiling point solvent used in Example 22 was changed from butyl cellosolve to propylene glycol monomethyl ether acetate. Granulated powder was obtained.
(Example 24) Production of granulated powder of Invention Example 24 The granulated powder of Invention Example 24 was obtained in the same manner as in Example 22 except that the high-boiling solvent used in Example 22 was changed from butyl cellosolve to cyclohexane. Obtained.
(Example 25) Production of granulated powder of Invention Example 25 The granulated powder of Invention Example 25 was obtained in the same manner as in Example 22 except that the high-boiling solvent used in Example 22 was changed from butyl cellosolve to diisobutyl ketone. Obtained.
（比較例１）比較例１の造粒粉の製造
実施例１で使用したブチルセロソルブをメチルエチルケトンに代えてメチオルエチルケトンのみとした以外は実施例１と同様にして、比較例１の造粒粉を得た。
（比較例２）比較例２の造粒粉の製造
実施例１で１１０℃とした第２乾燥温度を１００℃にした以外は実施例１と同様にして、比較例２の造粒粉を得た。
(Comparative Example 1) Production of granulated powder of Comparative Example 1 Granulated powder of Comparative Example 1 in the same manner as in Example 1, except that butyl cellosolve used in Example 1 was replaced with methyl ethyl ketone and only methyol ethyl ketone was used. Got.
Comparative Example 2 Production of Granulated Powder of Comparative Example 2 A granulated powder of Comparative Example 2 was obtained in the same manner as in Example 1 except that the second drying temperature of 110 ° C. in Example 1 was changed to 100 ° C. It was.
（比較例３）比較例３の造粒粉の製造
実施例１で、１１０℃とした第２乾燥温度を１４０℃にした以外は実施例１と同様にして、比較例３の造粒粉を得た。
（比較例４）比較例４の造粒粉の製造
実施例２で樹脂量に対して３０ｗｔ％とした高沸点溶剤の添加量を８ｗｔ％にした以外は実施例２と同様にして、比較例４の造粒粉を得た。
Comparative Example 3 Production of Granulated Powder of Comparative Example 3 The granulated powder of Comparative Example 3 was prepared in the same manner as in Example 1 except that the second drying temperature at 110 ° C. was changed to 140 ° C. in Example 1. Obtained.
(Comparative Example 4) Production of granulated powder of Comparative Example 4 Comparative Example was made in the same manner as in Example 2 except that the amount of high-boiling solvent added in Example 2 was 30 wt% with respect to the amount of resin was 8 wt%. 4 granulated powder was obtained.
（比較例５）比較例５の造粒粉の製造
実施例２で樹脂量に対して３０ｗｔ％とした高沸点溶剤の添加量を、５０ｗｔ％にした以外は実施例２と同様にして、比較例５の造粒粉を得た。
（比較例６）比較例６の造粒粉の製造
実施例２で使用した高沸点溶剤をブチルセロソルブからメチルイソブチルケトンに代えた以外は実施例２と同様にして、比較例６の造粒粉を得た。
(Comparative Example 5) Production of granulated powder of Comparative Example 5 Comparison was made in the same manner as in Example 2 except that the amount of the high-boiling solvent added in Example 2 was 30 wt% with respect to the resin amount was 50 wt%. The granulated powder of Example 5 was obtained.
Comparative Example 6 Production of Granulated Powder of Comparative Example 6 The granulated powder of Comparative Example 6 was prepared in the same manner as in Example 2 except that the high boiling point solvent used in Example 2 was changed from butyl cellosolve to methyl isobutyl ketone. Obtained.
（比較例７）比較例７の造粒粉の製造
実施例２で使用した高沸点溶剤をブチルセロソルブからn-ブチルアルコールに代えた以外は、実施例２と同様にして比較例７の造粒粉を得た。
（比較例８）比較例８の造粒粉の製造
実施例２で使用した高沸点溶剤をブチルセロソルブから2-2ブトキシエトキシエタノールに代えた以外は、実施例２と同様にして比較例８の造粒粉を得た。
Comparative Example 7 Production of Granulated Powder of Comparative Example 7 Granulated powder of Comparative Example 7 in the same manner as in Example 2 except that the high boiling point solvent used in Example 2 was changed from butyl cellosolve to n-butyl alcohol. Got.
Comparative Example 8 Production of Granulated Powder of Comparative Example 8 Comparative Example 8 was prepared in the same manner as in Example 2 except that the high boiling point solvent used in Example 2 was changed from butyl cellosolve to 2-2 butoxyethoxyethanol. Granules were obtained.
（比較例９）比較例９の造粒粉の製造
実施例２で３．５重量％としていた樹脂添加量を１．５％重量にした以外は、実施例２と同様にして比較例９の造粒粉を得た。
（比較例10）比較例10の造粒粉の製造
実施例２で使用した樹脂をエポキシからシリコンとし、高沸点溶剤をブチルセロソルブからメチルイソブチルケトンとした以外は、実施例２と同様にして比較例10の造粒粉を得た。
(Comparative Example 9) Production of granulated powder of Comparative Example 9 Comparative Example 9 was prepared in the same manner as in Example 2 except that the resin addition amount which was 3.5% by weight in Example 2 was changed to 1.5% by weight. Granulated powder was obtained.
Comparative Example 10 Production of Granulated Powder of Comparative Example 10 Comparative Example as in Example 2 except that the resin used in Example 2 was changed from epoxy to silicon and the high boiling point solvent was changed from butyl cellosolve to methyl isobutyl ketone. Ten granulated powders were obtained.
（比較例11）比較例11の造粒粉の製造
比較例10で使用した高沸点溶剤をブチルセロソルブからn-ブチルアルコールとした以外は、比較例10と同様にして比較例11の造粒粉を得た。
（比較例12）比較例12の造粒粉の製造
比較例10で使用した高沸点溶剤をブチルセロソルブから2-2ブトキシエトキシエタノールとした以外は、比較例10と同様にして比較例12の造粒粉を得た。
本発明例１〜25及び比較例１〜12の造粒粉の製造条件を各造粒粉の物性とともに表１及び表２に示す。
(Comparative Example 11) Production of granulated powder of Comparative Example 11 The granulated powder of Comparative Example 11 was prepared in the same manner as Comparative Example 10 except that the high boiling point solvent used in Comparative Example 10 was changed from n-butyl alcohol to butyl cellosolve. Obtained.
(Comparative Example 12) Production of granulated powder of Comparative Example 12 Granulation of Comparative Example 12 in the same manner as Comparative Example 10 except that the high boiling point solvent used in Comparative Example 10 was changed from butyl cellosolve to 2-2 butoxyethoxyethanol. I got a powder.
The production conditions of the granulated powders of Invention Examples 1 to 25 and Comparative Examples 1 to 12 are shown in Tables 1 and 2 together with the physical properties of each granulated powder.
表１及び表２中の略号等は下記の通りである。
*1：対造粒粉重量
*2：MEK:メチルエチルケトン
BCS:ブチルセロソルブ
PGM: プロピレングリコールモノエチルエーテルアセテート
CHEX: シクロヘキサン
DIB: ジイソブチルケトン
ACT: アセトン
MIB: メチルイソブチルケトン
NBA: n-ブチルアルコール
BEE: 2-2ブトキシエトキシエタノール
Abbreviations in Table 1 and Table 2 are as follows.
* 1: Weight of granulated powder
* 2: MEK: Methyl ethyl ketone
BCS: Butyl cellosolve
PGM: Propylene glycol monoethyl ether acetate
CHEX: cyclohexane
DIB: Diisobutylketone
ACT: Acetone
MIB: Methyl isobutyl ketone
NBA: n-butyl alcohol
BEE: 2-2 Butoxyethoxyethanol
*3：低沸点溶剤（LBS）/高沸点溶剤（HBS）
*4：粒径が75μｍ未満の粒子の量（ＤＳ）及び500μｍの粒子の量（ＤＬ）の粒子全体に占める割合で評価した。
Ａｒ＝ＤＳが５％以下、かつＤＬが10％以下
Ｂｒ＝ＤＳが10％以下、かつＤＬが10％以上、20％以下
Ｃｒ＝ＤＳが10％以上、かつＤＬが20％超
*5：透磁率は、100kHzで測定した。成形圧は4ton/cm2とした。
*6：直流重畳特性は、100kHzで測定した（Δμ-20％）
*7：Pcvは100kHz、50ｍTの条件で測定した。
* 3: Low boiling point solvent (LBS) / High boiling point solvent (HBS)
* 4: Evaluated based on the ratio of the amount of particles having a particle size of less than 75 μm (D S ) and the amount of particles having a particle size of 500 μm (D L ) to the whole particles.
A r = D S is 5% or less and D L is 10% or less B r = D S is 10% or less and D L is 10% or more and 20% or less C r = D S is 10% or more and D L is over 20%
* 5: Permeability was measured at 100kHz. The molding pressure was 4 ton / cm 2 .
* 6: DC superposition characteristics were measured at 100kHz (Δμ-20%)
* 7: Pcv was measured under the conditions of 100kHz and 50mT.
乾燥性は、Ａｄ（良好）、Ｂｄ（やや良好）、又はＣｄ（不良）で評価した。
透磁率は、Ａｍ（良好）、Ｂｍ（やや良好）、又はＣｍ（不良）で評価した。
直流重畳性は、Ａｈ（良好）、Ｂｈ（やや良好）、又はＣｈ（不良）で評価した。
Ｐｃｖは、Ａｐ（良好）、Ｂｐ（やや良好）、又はＣｐ（不良）で評価した。
The drying property was evaluated by A d (good), B d (slightly good), or C d (poor).
The magnetic permeability was evaluated by A m (good), B m (slightly good), or C m (bad).
The direct current superimposition was evaluated by A h (good), B h (slightly good), or C h (bad).
Pcv was evaluated by A p (good), B p (slightly good), or C p (bad).
製造された各造粒粉の評価
本発明例１〜25の造粒粉はいずれも、ＤＳが10％以下かつＤＬが20％以下という粒径範囲にあり、粒径のばらつきは少なかった。
これに対し、比較例１〜１２の造粒粉は、第１乾燥工程での乾燥は良好であったが、比較例１及び９の造粒粉を除き、第２乾燥工程での乾燥状態が不良であった。第２乾燥工程の温度が100℃の場合には高沸点溶剤の残留が多く、製造されたペーストをメッシュに通すことができなかった。このことは、所望の粒径の造粒粉を得ることができないことを示す。
Any granulated powder Evaluation Invention Example 1-25 of each granulated powder was produced, D S is in the size range of 10% or less and D L is less than 20%, variation in the particle size was less .
On the other hand, although the granulated powder of Comparative Examples 1-12 was favorable in the 1st drying process, the dry state in the 2nd drying process except the granulated powder of Comparative Examples 1 and 9. It was bad. When the temperature of the second drying step was 100 ° C., the high boiling point solvent remained so much that the produced paste could not be passed through the mesh. This indicates that a granulated powder having a desired particle size cannot be obtained.
また、第２乾燥工程の温度が140℃の場合には、エポキシ樹脂が硬化した状態となっており、プレス成形時の成形性が悪くなり、透磁率が低下することが予想された。
比較例１、４、６、７、10及び11の造粒粉は、乾燥工程でペーストの乾燥が進み過ぎ、粒径にバラつきが大きくなっていた。また、比較例５、８及び12の造粒粉は高沸点溶剤の残存量が多く、メッシュを通すことができなかったため、後述する成形を行うことができなかった。
Further, when the temperature of the second drying step was 140 ° C., the epoxy resin was in a cured state, and it was expected that the moldability at the time of press molding deteriorated and the magnetic permeability decreased.
In the granulated powders of Comparative Examples 1, 4, 6, 7, 10, and 11, the drying of the paste progressed excessively in the drying process, and the particle size was greatly varied. Moreover, since the granulated powder of Comparative Examples 5, 8 and 12 had a large amount of residual high boiling point solvent and could not pass through the mesh, it was not possible to perform the molding described later.
（実施例26）電子部品の製造
本発明例１と一般的な磁性粉（Ｆｅ：Ｓｉ：Ｃｒ＝９２：４：４）を用いて、以下の条件でトロイダルコアを製造し、特性を比較した。
（１）材料
本発明例１と引用文献２と似たような造粒粉で、それぞれトロイダルコアを作製し、比透磁率、μ周波数、直流重畳特性及びコアロス特性を測定し比較した。
トロイダルコア：φ15mm×2.5mmt（成形圧力 4t/cm2）
巻数：本発明例１の磁性粉末（CIP）＝19T
一般的な磁性粉末（Fe-Si-Cr）＝10T
(Example 26) Manufacture of electronic parts Using Invention Example 1 and general magnetic powder (Fe: Si: Cr = 92: 4: 4), toroidal cores were manufactured under the following conditions, and the characteristics were compared. .
(1) Material Toroidal cores were produced from granulated powders similar to those of Invention Example 1 and Reference Document 2, respectively, and relative magnetic permeability, μ frequency, DC superposition characteristics, and core loss characteristics were measured and compared.
Toroidal core: φ15mm × 2.5mmt (molding pressure 4t / cm 2 )
Number of turns: Magnetic powder (CIP) of Invention Example 1 = 19T
General magnetic powder (Fe-Si-Cr) = 10T
透磁率は、成形圧力（トン/cm2）と１００ｋＨｚにおける透磁率との関係を、インピーダンスアナライザを用いて、測定した。また、μ周波数は、周波数と１００ｋＨｚにおける透磁率の変化を、インピーダンスアナライザを用いて、周波数を１００ｋＨｚ〜１０ＭＨｚまでの間で、調べた。直流重畳特性は、印加磁界と透磁率との変化を、インピーダンスアナライザを用いて、コイルに供給する直流電流を除除に加えるようにして調べた。
コアロスは、Ｂ−Ｈアナライザを用いて、周波数を１００ｋＨｚ〜１０ＭＨｚまでの間で調べた。結果を、上記表１及び２、並びに図１〜図４に示す。
For the magnetic permeability, the relationship between the molding pressure (ton / cm 2 ) and the magnetic permeability at 100 kHz was measured using an impedance analyzer. As for the μ frequency, the change in the magnetic permeability at the frequency and 100 kHz was examined using an impedance analyzer between 100 kHz and 10 MHz. The direct current superimposition characteristics were examined by changing the applied magnetic field and the magnetic permeability by using an impedance analyzer so that the direct current supplied to the coil was added to the removal.
The core loss was examined using a BH analyzer between 100 kHz and 10 MHz. The results are shown in Tables 1 and 2 and FIGS.
図１に示すように、上記２つのトロイダルコアの透磁率は、成形圧力２トン/cm2の時点で一般的な磁性粉末を使用した方が高く、成形圧が高くなっても、その差は縮まらなかった。
このことから、製品として同じインダクタンス（L）を得るためには、巻数を多くするか、より高い成形圧を欠けることが必要になることが示された。
一方、図４に示すように、コアロスについては、１００ｋＨｚの時点における本発明例１の磁性粉末を用いたトロイダルコアの方が、一般的な磁性粉末を用いたトロイダルコアよりも、コアロスが少なく、周波数が高くなると、その差が大きくなることが示された。
このことから、図２に示すように１．５ＭＨｚを越える領域では、本発明例１の磁性粉末を用いたトロイダルコアの方が、コアロスが少ないため、コイルの自己共振周波数の近傍で比透磁率が大きく上昇したが、一般的な磁性粉末を用いたトロイダルコアでは、コアロスが大きいため逆に低下傾向が認められた。
As shown in FIG. 1, the magnetic permeability of the above two toroidal cores is higher when a general magnetic powder is used at a molding pressure of 2 ton / cm 2 , and even if the molding pressure increases, the difference is It did not shrink.
This indicates that in order to obtain the same inductance (L) as a product, it is necessary to increase the number of turns or to lack a higher molding pressure.
On the other hand, as shown in FIG. 4, for core loss, the toroidal core using the magnetic powder of Example 1 of the present invention at 100 kHz has less core loss than the toroidal core using a general magnetic powder, It was shown that the difference increases as the frequency increases.
From this, as shown in FIG. 2, in the region exceeding 1.5 MHz, the toroidal core using the magnetic powder of Example 1 of the present invention has less core loss, and therefore the relative permeability near the self-resonant frequency of the coil. However, in the toroidal core using a general magnetic powder, the core loss was large, and a downward trend was observed.
図３（Ａ）及び（Ｂ）で示すように、直流重畳特性は、本発明例１の磁性粉末を用いたトロイダルコアの方が、一般的な磁性粉末を用いたトロイダルコアよりもよい結果が得られた。
図３（Ａ）は、上述したFe-Si-Crの巻数を10T、CIPの巻数を19Tとして測定したため、初期透磁率に相違がみられた。しかし、透磁率が同じであると想定した場合でも、本発明例１の磁性粉末と一般的な磁性粉末の透磁率の差は約１．３倍であるので、磁性粉末を用いたトロイダルコアの方が良好な直流重畳特性を得られると考えられた。
以上より、本発明の方法で製造された磁性粉末は、比透磁率を除き、良好な特性を示した。
As shown in FIGS. 3 (A) and 3 (B), the direct current superimposition characteristics of the toroidal core using the magnetic powder of Example 1 of the present invention are better than the toroidal core using the general magnetic powder. Obtained.
In FIG. 3A, since the Fe—Si—Cr winding described above was measured with 10T and the CIP winding with 19T, the initial permeability was different. However, even when it is assumed that the magnetic permeability is the same, the magnetic permeability difference between the magnetic powder of Example 1 of the present invention and a general magnetic powder is about 1.3 times, so that the toroidal core using the magnetic powder has the same magnetic permeability. It is thought that better direct current superposition characteristics can be obtained.
From the above, the magnetic powder produced by the method of the present invention showed good characteristics except for the relative magnetic permeability.
本発明は、電子部品の製造の分野において有用である。 The present invention is useful in the field of manufacturing electronic components.
Claims (12)
前記スラリー状混合物を加熱して、前記低沸点溶剤を蒸発させ、ペースト状混合物を製造する第１乾燥工程と；
前記ペースト状混合物を、メッシュを通して解砕することによって製粒し、粒子を得る整粒工程と；
前記粒子を加熱して前記高沸点溶剤を蒸発させて、磁性粒子を得る第２乾燥工程と；
を備え、
前記低沸点溶剤は、沸点が９０℃以下の有機溶剤であり、メチルエチルケトン、アセトン、酢酸エチル、ベンゼン、メタノール、エタノール、及びイソプロパノールからなる群から選ばれるいずれかのものであり、
前記高沸点溶剤は、沸点が１１０〜２００℃の範囲内にある有機溶剤であり、ブチルセロソルブ、ジイソブチルケトン、ペンタノール、イソペンタノール、キシレン、及び酢酸ｎ−ブチルからなる群から選ばれるいずれかのものであり、
前記樹脂は、その硬化温度が前記低沸点溶剤の沸点よりも高い、造粒物の製造方法。
造粒物の製造方法。 A mixture production process for producing a slurry mixture by mixing magnetic powder, resin, low boiling point solvent, and high boiling point solvent;
A first drying step of heating the slurry mixture to evaporate the low boiling point solvent to produce a paste mixture;
Sizing the pasty mixture by crushing through a mesh to obtain particles;
A second drying step of heating the particles to evaporate the high boiling point solvent to obtain magnetic particles;
With
The low boiling point solvent is an organic solvent having a boiling point of 90 ° C. or less , and is any one selected from the group consisting of methyl ethyl ketone, acetone, ethyl acetate, benzene, methanol, ethanol, and isopropanol,
The high boiling point solvent is an organic solvent having a boiling point in the range of 110 to 200 ° C. , and any one selected from the group consisting of butyl cellosolve, diisobutyl ketone, pentanol, isopentanol, xylene, and n-butyl acetate. Is,
The method for producing a granulated product, wherein the resin has a curing temperature higher than the boiling point of the low- boiling solvent.
A method for producing a granulated product.
（１）粒径が７５μｍ未満である造粒物の割合が１０％以下；
（２）粒径が５００μｍを超える造粒物の割合が２０％以下；
（３）第１乾燥温度及び第２乾燥温度における乾燥性が良好。 Produced by the method according to any one of claims 1 to 9, granules having the following properties:
(1) The proportion of the granulated product having a particle size of less than 75 μm is 10% or less;
(2) The proportion of the granulated product having a particle size exceeding 500 μm is 20% or less;
(3) Good drying at the first drying temperature and the second drying temperature.
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