JP2001303111A - Method for producing flat soft magnetic metal powder - Google Patents
Method for producing flat soft magnetic metal powderInfo
- Publication number
- JP2001303111A JP2001303111A JP2000123417A JP2000123417A JP2001303111A JP 2001303111 A JP2001303111 A JP 2001303111A JP 2000123417 A JP2000123417 A JP 2000123417A JP 2000123417 A JP2000123417 A JP 2000123417A JP 2001303111 A JP2001303111 A JP 2001303111A
- Authority
- JP
- Japan
- Prior art keywords
- metal powder
- soft magnetic
- powder
- magnetic metal
- flat
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
Landscapes
- Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
- Crushing And Grinding (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
- Hard Magnetic Materials (AREA)
- Soft Magnetic Materials (AREA)
Abstract
(57)【要約】
【課題】 粉砕時間が短く、粉砕工程が簡単で、しかも
粉砕時間を調整するだけで、盤状から薄い扁平状軟磁性
金属粉末が製造できる方法を提供する。
【解決手段】 アトマイズ法による軟磁性金属粉末を粉
砕媒体を用いた粉砕機で機械的に扁平加工する製造方法
において、前記軟磁性金属粉末のすきま容量の１／２〜
２倍のアルコール系有機溶剤と、金属粉末１００重量部
に対して０．１〜２重量部の脂肪酸を混入して、粉砕す
ることを特徴とする扁平状軟磁性金属粉末の製造方法。PROBLEM TO BE SOLVED: To provide a method capable of producing a thin flat soft magnetic metal powder from a disc shape by simply adjusting a pulverizing time, a pulverizing time is short, and a pulverizing step is simple. SOLUTION: In the manufacturing method of softening a soft magnetic metal powder by an atomizing method by mechanical flattening with a pulverizer using a pulverizing medium, the soft magnetic metal powder has a clearance of 1/2 to 1/2 of a clearance capacity of the soft magnetic metal powder.
A method for producing a flat soft magnetic metal powder, comprising mixing and pulverizing a double-fold alcohol-based organic solvent and 0.1 to 2 parts by weight of a fatty acid with respect to 100 parts by weight of a metal powder.
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、磁気シールド材に
用いられる扁平状軟磁性金属粉末の製造方法に関するも
のである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a flat soft magnetic metal powder used for a magnetic shielding material.
【０００２】[0002]
【従来の技術】磁気シールド材として扁平状軟磁性金属
粉末を基板に塗布して用いる方法では、粉末に樹脂、溶
剤等を混合して塗料とし、これを基板に塗布し、乾燥し
てシールド膜が形成される。これにはパーマロイと総称
されているＦｅ−Ｎｉ系、センダストに代表されるケイ
素鋼Ｆｅ−Ｓｉ系などの軟磁性合金粉末がある。このよ
うな軟磁性合金粉末はインゴットを溶解し、水アトマイ
ズ法やガスアトマイズ法で製造するため球状の粉末であ
る。2. Description of the Related Art In a method of applying a flat soft magnetic metal powder to a substrate as a magnetic shield material, a resin, a solvent and the like are mixed with the powder to form a paint, which is applied to the substrate and dried to form a shield film. Is formed. This includes soft magnetic alloy powders such as Fe-Ni-based alloys generally referred to as permalloy and silicon steel Fe-Si-based alloys represented by Sendust. Such a soft magnetic alloy powder is a spherical powder obtained by melting an ingot and producing it by a water atomization method or a gas atomization method.
【０００３】しかし、塗料用金属粉末としては粉末形状
が扁平状であることが求められ、アトマイズ法による粉
末を機械的に湿式粉砕することにより扁平化する方法が
行われている（特公平６−６８１２２号公報）。しか
し、この方法では粉砕時間が長くかかるため、あらかじ
め圧延処理した盤状粉を粉砕する方法（特開平４−１３
８０１号公報）、湿式粉砕した粉末を乾燥し気流粉砕機
で微粉化する方法（特開平５−９８３０１号公報）、粉
砕中の粒子の拡大に応じて潤滑剤を添加し効率よく扁平
化する方法（特開平６−２５６８０３号公報）などが開
示されている。However, metal powders for paints are required to have a flat powder shape, and a method of flattening the powder by mechanically wet pulverizing the powder by an atomizing method has been used (Japanese Patent Publication No. Hei 6-1994). No. 68122). However, this method requires a long pulverizing time. Therefore, a method of pulverizing a plate-like powder that has been rolled in advance (Japanese Patent Laid-Open No. 4-13 / 1990)
801), a method in which wet-pulverized powder is dried and pulverized with an air current pulverizer (JP-A-5-98301), and a method in which a lubricant is added according to the expansion of particles during pulverization to efficiently flatten the powder. (JP-A-6-256803).
【０００４】また、最近ではより高い磁気シールド特性
を有する扁平状軟磁性金属粉末の要求もあり、有機溶剤
中にレシチンを混合して粉砕し磁気特性劣化が少ない扁
平状金属粉末を製造する方法（特開平７−１０２３０１
号公報）、湿式粉砕に使用する粉砕媒体の表面粗さを小
さくして粉砕中に粉末の破砕を抑える方法（特開平５−
２５５７１０号公報）などが開示されている。しかし、
これらの方法はいずれも粉砕時間が長く、かつ粉砕工程
も複雑であり、連続生産には不適当なものであった。[0004] Recently, there has been a demand for a flat soft magnetic metal powder having higher magnetic shielding properties, and a method of producing a flat metal powder with little deterioration in magnetic properties by mixing and pulverizing lecithin in an organic solvent (pulverization). JP-A-7-102301
Japanese Patent Application Laid-Open No. H05-205, and a method of reducing the surface roughness of a grinding medium used for wet grinding to suppress powder crushing during grinding.
No. 255710) and the like. But,
All of these methods have long grinding times and complicated grinding steps, and are unsuitable for continuous production.
【０００５】[0005]
【発明が決しようとする課題】本発明は、粉砕時間が短
く、かつ粉砕工程も簡単で、しかも粉砕時間を調整する
だけで盤状から厚みの薄い扁平状粉が製造できる粉砕方
法を提供するものである。DISCLOSURE OF THE INVENTION The present invention provides a pulverizing method in which a pulverizing time is short, a pulverizing step is simple, and a flat powder having a small thickness from a disk shape can be produced only by adjusting the pulverizing time. Things.
【０００６】[0006]
【課題を解決するための手段】即ち本発明は、アトマイ
ズ法による軟磁性金属粉末を粉砕媒体を用いた粉砕機で
機械的に扁平加工する製造方法において、前記軟磁性金
属粉末のすきま容量の１／２〜２倍の有機溶剤と、金属
粉末１００重量部に対して０．１〜２重量部の脂肪酸を
混入して、粉砕することを特徴とする扁平状軟磁性金属
粉末の製造方法である。That is, the present invention provides a method for mechanically flattening a soft magnetic metal powder by an atomizing method using a pulverizer using a pulverizing medium. A method for producing a flat soft magnetic metal powder comprising mixing and pulverizing an organic solvent in an amount of 1/2 to 2 times and a fatty acid in an amount of 0.1 to 2 parts by weight based on 100 parts by weight of the metal powder. .
【０００７】本発明の軟磁性金属粉末とは高透磁率材料
の合金粉末である。具体的にはパーマロイと総称される
Ｆｅ-Ｎｉ系合金粉末で、３６パーマロイ(３６Ｎｉ-
０．３Ｍｎ-Ｆｅ)４５パーマロイ(４５Ｎｉ-０．３Ｍｎ
-Ｆｅ)７８パーマロイ(７８．５Ｎｉ-０．３Ｍｎ-Ｆｅ)
などが挙げられる。ケイ素鋼のＦｅ-Ｓｉ系合金粉末で
は、ケイ素含有量の違う合金が有り、具体的には６．５
％Ｓｉ-Ｆｅ、１１％Ｓｉ-Ｆｅ、センダスト(９．６％
Ｓｉー５．４％Ａｌ-Ｆｅ)などが挙げられる。The soft magnetic metal powder of the present invention is an alloy powder of a material having a high magnetic permeability. Specifically, it is a Fe-Ni alloy powder generally called permalloy, and is made of 36 permalloy (36Ni-
0.3Mn-Fe) 45 permalloy (45Ni-0.3Mn
-Fe) 78 permalloy (78.5Ni-0.3Mn-Fe)
And the like. Among Fe—Si alloy powders of silicon steel, there are alloys having different silicon contents, specifically, 6.5.
% Si-Fe, 11% Si-Fe, Sendust (9.6%
Si-5.4% Al-Fe).
【０００８】本発明の有機溶剤とはアルコール系溶剤
で、具体的にはメタノール、エタノール、イソプロパノ
ール、ブタノールなどが挙げられる。アルコール系溶剤
でも、臭いの強い溶剤や１００℃以上の高沸点溶剤は作
業性が悪く好ましくない。石油スピリットやトルエンな
どの炭化水素系溶剤では粉砕中に扁平粉末の色調が黒く
なり、カード印刷用途には良くない。[0008] The organic solvent of the present invention is an alcoholic solvent, and specific examples thereof include methanol, ethanol, isopropanol and butanol. Among alcohol solvents, solvents having a strong smell and high boiling solvents having a temperature of 100 ° C. or higher are not preferable because of poor workability. With hydrocarbon solvents such as petroleum spirit and toluene, the color of the flat powder becomes black during grinding, which is not good for card printing applications.
【０００９】軟磁性金属粉末に対する有機溶剤量は軟磁
性金属粉末のすきま容量の１／２〜２倍の量であること
が重要である。すきま容量とは金属粉末を容器に入れた
時の空隙の事である。我々の実験では、約１０μｍのパ
ーマロイ球状微粉末の場合約３７．５％の空隙が有る事
が判明した。It is important that the amount of the organic solvent relative to the soft magnetic metal powder is 1/2 to 2 times the clearance capacity of the soft magnetic metal powder. The clearance capacity is a gap when metal powder is put in a container. In our experiments, it was found that about 10 μm permalloy spherical fine powder had about 37.5% voids.
【００１０】具体的に必要な有機溶剤重量を計算する
と、見掛け密度４〜５ｇ／ｃｍ3のアトマイズ法による
軟磁性金属粉末を本発明の方法で粉砕する場合、重量４
００〜５００ｇの金属粉末に対して、すきま容量は３
７．５ｃｃとなる。比重０．８のアルコールを使用する
と約３０ｇが金属粉末のすきまを充填する重量になる。The specific required weight of the organic solvent is calculated as follows. When the soft magnetic metal powder having an apparent density of 4 to 5 g / cm 3 by the atomizing method is pulverized by the method of the present invention, the weight is 4%.
Clearance capacity is 3 for 100-500g of metal powder.
It becomes 7.5cc. When an alcohol having a specific gravity of 0.8 is used, about 30 g becomes a weight for filling the gap of the metal powder.
【００１１】すきま充填量と同じ溶剤量で粉砕する事が
一番好ましいが、最小１／２から、最大２倍の容量まで
本発明の効果がある。従って約４００〜５００ｇの金属
粉末に対して有機溶剤量は重量で約１５〜６０ｇとな
る。それよりも少ないと、粉砕中に金属粉末の流動性が
悪くなり、良くない。また有機溶剤量を２倍より多くす
ると、粉砕効率が悪くなり粉砕に長時間必要になり、粉
砕されない球状粉末が混在したり、微粉が発生し磁気特
性や色調に悪影響を与える。It is most preferable to pulverize with the same amount of solvent as the gap filling amount, but the effect of the present invention is from a minimum of 1/2 to a maximum of twice the capacity. Therefore, the amount of the organic solvent is about 15 to 60 g by weight with respect to about 400 to 500 g of the metal powder. If it is less than this, the fluidity of the metal powder during pulverization becomes poor, which is not good. On the other hand, if the amount of the organic solvent is more than twice, the pulverization efficiency is deteriorated and the pulverization is required for a long time, and spherical powder that is not pulverized is mixed or fine powder is generated, which adversely affects magnetic properties and color tone.
【００１２】本発明の脂肪酸は直鎖飽和脂肪酸が好まし
くラウリン酸、ミリスチン酸、パルミチン酸、ステアリ
ン酸、ベヘン酸などが挙げられる。金属粉末に対する混
入量は０．１％以上必要で、それより少ないと粉砕中に
粉末が凝集し扁平状に加工されない。また２％以上だ
と、細かくなるが扁平状に加工できなくなる。The fatty acids of the present invention are preferably straight-chain saturated fatty acids, and include lauric acid, myristic acid, palmitic acid, stearic acid, behenic acid and the like. The mixing amount with the metal powder is required to be 0.1% or more. If the amount is less than 0.1%, the powder is agglomerated during pulverization and is not processed into a flat shape. If it is 2% or more, it becomes fine, but cannot be processed into a flat shape.
【００１３】粉砕機はボールミル、振動ミル、媒体撹拌
ミルなど市販の粉砕機が使用できる。粉砕方法はこれら
粉砕機に軟磁性金属粉末を投入し、有機溶剤と脂肪酸を
規定量入れ、粉砕すれば良い。目的とする粒度や扁平度
になるまで粉砕し、その後加工した扁平粉末を粉砕室か
ら排出し、乾燥、篩などの処理をして扁平状軟磁性材料
として使用すれば良い。As the pulverizer, a commercially available pulverizer such as a ball mill, a vibration mill and a medium stirring mill can be used. The pulverization method may be such that a soft magnetic metal powder is charged into these pulverizers, a predetermined amount of an organic solvent and a fatty acid are charged, and pulverization is performed. The powder may be pulverized to a desired particle size or flatness, and then the processed flat powder may be discharged from the pulverizing chamber, dried, sieved, or the like and used as a flat soft magnetic material.
【００１４】球状微粉末から扁平状の金属粉末を製造す
る場合、アルミニウムのような軟らかい、展延性の良い
金属組成の場合、有機溶剤中で粉砕する湿式粉砕方法で
も短時間に扁平状に加工できる。しかし軟磁性金属のよ
うな硬い、展延加工性の悪い金属は湿式粉砕では粉砕時
間が非常に長くなる。In the case of producing a flat metal powder from a spherical fine powder, in the case of a soft and extensible metal composition such as aluminum, it can be processed into a flat shape in a short time even by a wet pulverization method of pulverizing in an organic solvent. . However, hard metals having poor spreadability, such as soft magnetic metals, require very long grinding times in wet grinding.
【００１５】従来まで考案されている方法は、アルミニ
ウム粉などを粉砕する湿式粉砕方法と呼ばれているもの
で、開示例でも示されているように金属粉末重量の３〜
２０倍のイソプロピルアルコール（特開平５−９８３０
１号公報、特開平５−２５５７１０号公報、特開平６−
２５６８０３号公報）、１．８倍のトルエン（特公平６
−６８１２２号公報）など、いずれも有機溶剤中で金属
粉末を粉砕加工するものである。The method devised up to now is called a wet pulverization method for pulverizing aluminum powder or the like, and as shown in the disclosed examples, 3 to 3 times the weight of the metal powder.
20-fold isopropyl alcohol (JP-A-5-9830)
No. 1, JP-A-5-255710, JP-A-5-255710
No. 256803), 1.8 times toluene (Japanese Patent Publication No.
All of these methods grind metal powder in an organic solvent.
【００１６】本発明でも有機溶剤を使用しているが、粉
砕機構は従来の湿式粉砕法とは全く違うものである。本
発明では、すきま容量を充填する事が重要なので容量で
規定したが、金属粉末に対する重量で計算すると、金属
粉末の１５／５００〜６０／４００倍重量、つまり金属
粉末に対して溶剤混入重量は０．０３〜０．１５倍であ
る。粉砕媒体として通常スチールボールなどが使用され
るが、本発明の方法はスチールボールのエネルギーが粉
砕する金属粉末に直接伝わり、球状粉末が短時間に扁平
状に加工される。Although an organic solvent is used in the present invention, the pulverization mechanism is completely different from the conventional wet pulverization method. In the present invention, it is important to fill the clearance volume, so it is defined by the volume. However, when calculated by the weight with respect to the metal powder, the weight of the solvent mixed with the metal powder is 15/500 to 60/400 times, that is, It is 0.03 to 0.15 times. Steel balls or the like are usually used as a grinding medium. In the method of the present invention, the energy of the steel balls is directly transmitted to the metal powder to be ground, and the spherical powder is processed into a flat shape in a short time.
【００１７】空気中で粉砕すると、粉砕ボールの移動エ
ネルギーの減衰は少ないが、スチールボールと金属粉末
が直接衝突するために微粉が多く発生し、また空気中だ
と発火燃焼したり、均一に扁平加工ができない。湿式粉
砕方法では有機溶剤中で粉砕ボールが移動するため、衝
撃エネルギーが移動する事で減衰し粉砕物に伝わらなく
なり、非常に時間がかかる。When pulverized in the air, the transfer energy of the pulverized ball is less attenuated, but a large amount of fine powder is generated due to direct collision between the steel ball and the metal powder. Cannot be processed. In the wet pulverization method, since the pulverized ball moves in the organic solvent, the impact energy is attenuated due to the transfer and is not transmitted to the pulverized material, which takes a very long time.
【００１８】しかし本発明の方法は粉砕ボールは空気中
を移動し、しかも金属粉末には有機溶剤を介して接触す
るため均一な圧力が粉末にかかり、早く均一な扁平加工
ができるのであろう。また湿式粉砕方法ではボール間の
金属粉末濃度が少ないため、ボール同士が衝突する機会
が多くなり、ボール摩耗も激しく、ボール表面が粗にな
ることにより粗大粒子発生も多くなる。さらに本発明の
方法では、たとえ脂肪酸などの潤滑剤量が展延加工中に
不足してきても、少量の有機溶剤が存在するため、粉末
同士の凝集が防止でき、連続生産も可能となった。However, according to the method of the present invention, since the crushed ball moves in the air and comes into contact with the metal powder via the organic solvent, a uniform pressure is applied to the powder, so that a uniform flattening process can be performed quickly. Further, in the wet pulverization method, since the metal powder concentration between the balls is low, the chances of collision between the balls increase, the ball wear is severe, and the generation of coarse particles increases due to the rough surface of the ball. Furthermore, according to the method of the present invention, even if the amount of a lubricant such as a fatty acid becomes insufficient during the spreading process, a small amount of an organic solvent is present, so that aggregation of the powders can be prevented and continuous production has become possible.
【００１９】[0019]
【発明の実施の形態】本発明の構成を詳しく説明すれば
次の通りである。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The construction of the present invention will be described in detail as follows.
【００２０】[0020]
【実施例】（実施例１）合金組成Ｎｉ７８．５％、残部
Ｆｅからなる７８パーマロイの軟磁性金属をアトマイズ
法により噴霧し、見掛密度４ｇ／ｃｍ3、平均粒径１０
μｍ、ＢＥＴ法比表面積値２１００ｃｍ2／ｇの球状金
属粉末を得た。次いでこの粉末を材質ＳＵＪ−２の１／
４インチボールを粉砕媒体とする、媒体撹拌ミルを用い
て粉砕した。粉砕条件は粉砕媒体の鋼球を４０００ｇ、
軟磁性金属粉末を４００ｇ、有機溶剤としてメタノール
を軟磁性金属粉末のすきま容量相当量の３０ｇ、ステア
リン酸を４ｇ加え、回転数５００ｒｐｍで粉砕した。１
０分、３０分、６０分後に粉砕機を停止しサンプリング
した。本発明の方法で製造した扁平状軟磁性金属粉末の
形状を電子顕微鏡と粒度測定器で調査した結果、１０分
後には明らかに扁平状であり、平均粒径２０μｍ、ＢＥ
Ｔ法比表面積値２２００ｃｍ2／ｇの盤状形状粉末が得
られた。３０分後には平均粒径２５μｍ、ＢＥＴ法比表
面積値３０００ｃｍ2／ｇの扁平状粉が得られた。６０
分後には平均粒径２８μｍ、ＢＥＴ法比表面積値５００
０ｃｍ2／ｇの良く展延された扁平状粉が得られた。い
ずれも均一で粗大粉や微粉も少なく、磁気シールド材と
して最適な形状であった。(Example 1) 78 permalloy soft magnetic metal composed of 78.5% of alloy composition Ni and the balance of Fe was sprayed by an atomizing method, and had an apparent density of 4 g / cm 3 and an average particle size of 10%.
A spherical metal powder having a specific surface area of 2100 cm 2 / g with a BET method was obtained. Next, this powder was mixed with 1 / of the material SUJ-2.
Grinding was performed using a medium stirring mill using a 4-inch ball as a grinding medium. The grinding conditions were 4000 g of steel balls as grinding media,
400 g of the soft magnetic metal powder, 30 g of methanol as an organic solvent corresponding to the clearance volume of the soft magnetic metal powder, and 4 g of stearic acid were added, and the mixture was pulverized at 500 rpm. 1
After 0, 30, and 60 minutes, the pulverizer was stopped and sampling was performed. The shape of the flat soft magnetic metal powder produced by the method of the present invention was examined with an electron microscope and a particle size analyzer. As a result, it was clearly flat after 10 minutes, the average particle size was 20 μm, and BE
A disk-shaped powder having a T method specific surface area of 2200 cm 2 / g was obtained. After 30 minutes, a flat powder having an average particle size of 25 μm and a BET specific surface area of 3000 cm 2 / g was obtained. 60
After a minute, the average particle diameter is 28 μm, and the specific surface area of the BET method is 500.
A well spread flat powder of 0 cm 2 / g was obtained. Each of them was uniform and had little coarse powder or fine powder, and had optimal shapes as magnetic shielding materials.
【００２１】（実施例２）合金組成Ｎｉ７８．５％、残
部Ｆｅからなる７８パーマロイの軟磁性金属をアトマイ
ズ法により噴霧し、見掛密度４ｇ／ｃｍ3、平均粒径１
０μｍ、ＢＥＴ法比表面積値２１００ｃｍ2／ｇの球状
金属粉末を得た。次いでこの粉末を材質ＳＵＪ−２の１
／４インチボールを粉砕媒体とする、媒体撹拌ミルを用
いて粉砕した。粉砕条件は粉砕媒体の鋼球を４０００
ｇ、軟磁性金属粉末を４００ｇ、有機溶剤としてメタノ
ールを軟磁性金属粉末のすきま容量の約１／２相当量の
１５ｇ、ステアリン酸を４ｇ加え、回転数５００ｒｐｍ
で粉砕した。１０分、３０分、６０分後に粉砕機を停止
しサンプリングした。本発明の方法で製造した扁平状軟
磁性金属粉末の形状を電子顕微鏡と粒度測定器で調査し
た結果、１０分後には明らかに扁平状であり、平均粒径
２２μｍ、ＢＥＴ法比表面積値２３００ｃｍ2／ｇの盤
状形状粉末が得られた。３０分後には平均粒径２６μ
ｍ、ＢＥＴ法比表面積値３１００ｃｍ2／ｇの扁平状粉
が得られた。６０分後には平均粒径３０μｍ、ＢＥＴ法
比表面積値５５００ｃｍ2／ｇの良く展延された扁平状
粉が得られた。いずれも均一で粗大粉や微粉も少なく、
磁気シールド材として最適な形状であった。(Example 2) 78 Permalloy soft magnetic metal consisting of 78.5% of alloy composition Ni and the balance of Fe was sprayed by an atomizing method, and had an apparent density of 4 g / cm 3 and an average particle size of 1.
A spherical metal powder having a specific surface area of 0 μm and a BET method specific surface value of 2100 cm 2 / g was obtained. Next, this powder was used as SUJ-2 material 1
This was pulverized using a medium stirring mill using a / 4 inch ball as a pulverizing medium. The grinding conditions were as follows.
g, 400 g of soft magnetic metal powder, 15 g of methanol as an organic solvent, equivalent to about 1/2 of the clearance capacity of the soft magnetic metal powder, and 4 g of stearic acid.
And crushed. After 10 minutes, 30 minutes, and 60 minutes, the pulverizer was stopped and sampling was performed. The shape of the flat soft magnetic metal powder produced by the method of the present invention was examined with an electron microscope and a particle size analyzer. As a result, it was clearly flat after 10 minutes, the average particle size was 22 μm, and the BET specific surface area was 2300 cm 2. / G of a disc-shaped powder was obtained. After 30 minutes, the average particle size is 26μ.
m, a flat powder having a BET specific surface area of 3,100 cm 2 / g was obtained. After 60 minutes, a well spread flat powder having an average particle size of 30 μm and a BET specific surface area of 5,500 cm 2 / g was obtained. All are uniform and have few coarse and fine powders,
The shape was optimal as a magnetic shield material.
【００２２】（実施例３）合金組成Ｎｉ７８．５％、残
部Ｆｅからなる７８パーマロイの軟磁性金属をアトマイ
ズ法により噴霧し、見掛密度４ｇ／ｃｍ3、平均粒径１
０μｍ、ＢＥＴ法比表面積値２１００ｃｍ2／ｇの球状
金属粉末を得た。次いでこの粉末を材質ＳＵＪ−２の１
／４インチボールを粉砕媒体とする、媒体撹拌ミルを用
いて粉砕した。粉砕条件は粉砕媒体の鋼球を４０００
ｇ、軟磁性金属粉末を４００ｇ、有機溶剤としてメタノ
ールを軟磁性金属粉末のすきま容量の約２倍相当量の６
０ｇ、ステアリン酸を４ｇ加え、回転数５００ｒｐｍで
粉砕した。１０分、３０分、６０分後に粉砕機を停止し
サンプリングした。本発明の方法で製造した扁平状軟磁
性金属粉末の形状を電子顕微鏡と粒度測定器で調査した
結果、１０分後には明らかに扁平状であり、平均粒径１
８μｍ、ＢＥＴ法比表面積値２２００ｃｍ2／ｇの盤状
形状粉末が得られた。３０分後には平均粒径２２μｍ、
ＢＥＴ法比表面積値２７００ｃｍ2／ｇの扁平状粉が得
られた。６０分後には平均粒径２５μｍ、ＢＥＴ法比表
面積値４０００ｃｍ2／ｇの良く展延された扁平状粉が
得られた。いずれも均一で粗大粉や微粉も少なく、磁気
シールド材として最適な形状であった。Example 3 78 Permalloy soft magnetic metal consisting of 78.5% of alloy composition Ni and the balance of Fe was sprayed by an atomizing method, and had an apparent density of 4 g / cm 3 and an average particle size of 1
A spherical metal powder having a specific surface area of 0 μm and a BET method specific surface value of 2100 cm 2 / g was obtained. Next, this powder was used as SUJ-2 material 1
This was pulverized using a medium stirring mill using a / 4 inch ball as a pulverizing medium. The grinding conditions were as follows.
g of the soft magnetic metal powder, 400 g of the soft magnetic metal powder, and methanol as an organic solvent.
0 g and stearic acid (4 g) were added, and pulverized at a rotation speed of 500 rpm. After 10 minutes, 30 minutes, and 60 minutes, the pulverizer was stopped and sampling was performed. The shape of the flat soft magnetic metal powder produced by the method of the present invention was examined with an electron microscope and a particle size analyzer. As a result, the powder was clearly flat after 10 minutes and had an average particle size of 1
A disc-shaped powder having a specific surface area of 8 μm and a BET specific surface area of 2200 cm 2 / g was obtained. After 30 minutes, the average particle size is 22 μm,
A flat powder having a BET specific surface area of 2700 cm 2 / g was obtained. After 60 minutes, a well spread flat powder having an average particle size of 25 μm and a BET specific surface area of 4000 cm 2 / g was obtained. Each of them was uniform and had little coarse powder or fine powder, and had optimal shapes as magnetic shielding materials.
【００２３】（実施例４）合金組成Ｓｉ６．５％、残部
Ｆｅからなる軟磁性金属をアトマイズ法により噴霧し、
見掛密度５ｇ／ｃｍ3、平均粒径２０μｍ、ＢＥＴ法比
表面積値１２００ｃｍ2／ｇの球状金属粉末を得た。次
いでこの粉末を材質ＳＵＪ−２の３／８インチボールを
粉砕媒体とする、媒体撹拌ミルを用いて粉砕した。粉砕
条件は粉砕媒体の鋼球を４０００ｇ、軟磁性金属粉末を
５００ｇ、有機溶剤としてイソプロピルアルコールを軟
磁性金属粉末のすきま容量相当量の３０ｇ、ステアリン
酸を５ｇ加え、回転数６００ｒｐｍで粉砕した。３０
分、６０分後に粉砕機を停止しサンプリングした。本発
明の方法で製造した扁平状軟磁性金属粉末の形状を電子
顕微鏡と粒度測定器で調査した結果、３０分後には明ら
かに扁平状であり、平均粒径３０μｍ、ＢＥＴ法比表面
積値２２００ｃｍ2／ｇの盤状形状粉末が得られた。６
０分後には平均粒径５０μｍ、ＢＥＴ法比表面積値４０
００ｃｍ2／ｇの扁平状粉が得られた。いずれも均一で
粗大粉や微粉も少なく、磁気シールド材として最適な形
状であった。(Example 4) A soft magnetic metal composed of 6.5% of alloy composition Si and the balance of Fe was sprayed by an atomizing method.
A spherical metal powder having an apparent density of 5 g / cm 3 , an average particle size of 20 μm, and a BET specific surface area of 1200 cm 2 / g was obtained. Next, this powder was pulverized using a medium stirring mill using 3/8 inch balls of material SUJ-2 as a pulverizing medium. The grinding conditions were as follows: 4000 g of a steel ball as a grinding medium, 500 g of a soft magnetic metal powder, 30 g of isopropyl alcohol as an organic solvent corresponding to the clearance capacity of the soft magnetic metal powder, and 5 g of stearic acid, and pulverized at a rotation speed of 600 rpm. 30
After 60 minutes, the mill was stopped and sampling was performed. As a result of examining the shape of the flat soft magnetic metal powder produced by the method of the present invention with an electron microscope and a particle size analyzer, it was clearly flat after 30 minutes, the average particle diameter was 30 μm, and the BET specific surface area was 2200 cm 2. / G of a disc-shaped powder was obtained. 6
After 0 minute, the average particle size is 50 μm, and the BET specific surface area value is 40.
A flat powder of 00 cm 2 / g was obtained. Each of them was uniform and had little coarse powder or fine powder, and had optimal shapes as magnetic shielding materials.
【００２４】（実施例５）合金組成Ｓｉ６．５％、残部
Ｆｅからなる軟磁性金属をアトマイズ法により噴霧し、
見掛密度５ｇ／ｃｍ3、平均粒径２０μｍ、ＢＥＴ法比
表面積値１２００ｃｍ2／ｇの球状金属粉末を得た。次
いでこの粉末を材質ＳＵＪ−２の３／８インチボールを
粉砕媒体とする、媒体撹拌ミルを用いて粉砕した。粉砕
条件は粉砕媒体の鋼球を４０００ｇ、軟磁性金属粉末を
５００ｇ、有機溶剤としてイソプロピルアルコールを軟
磁性金属粉末のすきま容量相当量の３０ｇ、ステアリン
酸を０．５ｇ加え、回転数６００ｒｐｍで粉砕した。３
０分、６０分後に粉砕機を停止しサンプリングした。本
発明の方法で製造した扁平状軟磁性金属粉末の形状を電
子顕微鏡と粒度測定器で調査した結果、３０分後には明
らかに扁平状であり、平均粒径３３μｍ、ＢＥＴ法比表
面積値２０００ｃｍ2／ｇの盤状形状粉末が得られた。
６０分後には平均粒径４０μｍ、ＢＥＴ法比表面積値３
５００ｃｍ2／ｇの扁平状粉が得られた。いずれも均一
で粗大粉や微粉も少なく、磁気シールド材として最適な
形状であった。(Example 5) A soft magnetic metal consisting of an alloy composition of 6.5% Si and the balance of Fe was sprayed by an atomizing method.
A spherical metal powder having an apparent density of 5 g / cm 3 , an average particle size of 20 μm, and a BET specific surface area of 1200 cm 2 / g was obtained. Next, this powder was pulverized using a medium stirring mill using 3/8 inch balls of material SUJ-2 as a pulverizing medium. The grinding conditions were as follows: 4000 g of a steel ball as a grinding medium, 500 g of a soft magnetic metal powder, 30 g of isopropyl alcohol as an organic solvent corresponding to the clearance capacity of the soft magnetic metal powder, and 0.5 g of stearic acid were added, followed by grinding at 600 rpm. . Three
After 0 minute and 60 minutes, the pulverizer was stopped and sampling was performed. As a result of examining the shape of the flat soft magnetic metal powder produced by the method of the present invention with an electron microscope and a particle size analyzer, it was clearly flat after 30 minutes, the average particle diameter was 33 μm, and the BET specific surface area value was 2000 cm 2. / G of a disc-shaped powder was obtained.
After 60 minutes, the average particle size is 40 μm, and the BET specific surface area value is 3.
A flat powder of 500 cm 2 / g was obtained. Each of them was uniform and had little coarse powder or fine powder, and had optimal shapes as magnetic shielding materials.
【００２５】（実施例６）合金組成Ｓｉ６．５％、残部
Ｆｅからなる軟磁性金属をアトマイズ法により噴霧し、
見掛密度５ｇ／ｃｍ3、平均粒径２０μｍ、ＢＥＴ法比
表面積値１２００ｃｍ2／ｇの球状金属粉末を得た。次
いでこの粉末を材質ＳＵＪ−２の３／８インチボールを
粉砕媒体とする、媒体撹拌ミルを用いて粉砕した。粉砕
条件は粉砕媒体の鋼球を４０００ｇ、軟磁性金属粉末を
５００ｇ、有機溶剤としてイソプロピルアルコールを軟
磁性金属粉末のすきま容量相当量の３０ｇ、ステアリン
酸を１０ｇ加え、回転数６００ｒｐｍで粉砕した。３０
分、６０分後に粉砕機を停止しサンプリングした。本発
明の方法で製造した扁平状軟磁性金属粉末の形状を電子
顕微鏡と粒度測定器で調査した結果、３０分後には明ら
かに扁平状であり、平均粒径３０μｍ、ＢＥＴ法比表面
積値２４００ｃｍ2／ｇの盤状形状粉末が得られた。６
０分後には平均粒径４５μｍ、ＢＥＴ法比表面積値４８
００ｃｍ2／ｇの扁平状粉が得られた。いずれも均一で
粗大粉や微粉も少なく、磁気シールド材として最適な形
状であった。(Example 6) A soft magnetic metal comprising 6.5% of alloy composition and the balance of Fe was sprayed by an atomizing method.
A spherical metal powder having an apparent density of 5 g / cm 3 , an average particle size of 20 μm, and a BET specific surface area of 1200 cm 2 / g was obtained. Next, this powder was pulverized using a medium stirring mill using 3/8 inch balls of material SUJ-2 as a pulverizing medium. The grinding conditions were as follows: 4000 g of a steel ball as a grinding medium, 500 g of a soft magnetic metal powder, 30 g of isopropyl alcohol as an organic solvent corresponding to the clearance capacity of the soft magnetic metal powder, and 10 g of stearic acid, and pulverized at 600 rpm. 30
After 60 minutes, the mill was stopped and sampling was performed. As a result of examining the shape of the flat soft magnetic metal powder produced by the method of the present invention with an electron microscope and a particle size analyzer, the powder was clearly flat after 30 minutes, had an average particle size of 30 μm, and a BET specific surface area of 2400 cm 2. / G of a disc-shaped powder was obtained. 6
After 0 minute, the average particle size is 45 μm, and the BET specific surface area value is 48.
A flat powder of 00 cm 2 / g was obtained. Each of them was uniform and had little coarse powder or fine powder, and had optimal shapes as magnetic shielding materials.
【００２６】[0026]
【比較例】（比較例１）合金組成Ｎｉ７８．５％、残部
Ｆｅからなる７８パーマロイの軟磁性金属をアトマイズ
法により噴霧し、見掛密度４ｇ／ｃｍ3、平均粒径１０
μｍ、ＢＥＴ法比表面積値２１００ｃｍ2／ｇの球状金
属粉末を得た。次いでこの粉末を材質ＳＵＪ−２の１／
４インチボールを粉砕媒体とする、媒体撹拌ミルを用い
て湿式粉砕した。粉砕条件は粉砕媒体の鋼球を４０００
ｇ、軟磁性金属粉末を４００ｇ、有機溶剤としてメタノ
ールを金属粉末の２０倍の８０００ｇ、ステアリン酸を
４ｇ加え、回転数５００ｒｐｍで湿式粉砕した。６０分
毎に粉砕機を停止しサンプリングし軟磁性金属粉末の形
状を電子顕微鏡と粒度測定器で調査した。その結果、６
０分後に扁平状粉が多く見られるが粉砕されていない球
状粉も混在していた。１２０粉後で球状粉は無くなり全
て扁平粉となったが、５μｍ以下の微粉から１５０μｍ
の粗大粉が混在し、篩い分けや再粉砕が必要で、そのま
ま磁気シールド材としては使用できない粉末であった。[Comparative Example] (Comparative Example 1) 78 permalloy soft magnetic metal composed of 78.5% of alloy composition Ni and the balance of Fe was sprayed by an atomizing method to have an apparent density of 4 g / cm 3 and an average particle size of 10
A spherical metal powder having a specific surface area of 2100 cm 2 / g with a BET method was obtained. Next, this powder was mixed with 1 / of the material SUJ-2.
Wet pulverization was performed using a medium stirring mill using a 4-inch ball as a pulverizing medium. The grinding conditions were as follows.
g, 400 g of soft magnetic metal powder, 8000 g of methanol as an organic solvent, 20 times that of the metal powder, and 4 g of stearic acid, and wet pulverized at 500 rpm. The pulverizer was stopped every 60 minutes, sampled, and the shape of the soft magnetic metal powder was examined with an electron microscope and a particle size analyzer. As a result, 6
At 0 minutes, many flat powders were observed, but spherical powders that were not pulverized were also present. After 120 powders, the spherical powders disappeared and all became flat powders, but from fine powders of 5 μm or less to 150 μm
Coarse powder was mixed, sieving and re-crushing were necessary, and the powder could not be used as a magnetic shielding material as it was.
【００２７】[0027]
【発明の効果】本発明の製造方法により、従来まで製造
が難しかった扁平状軟磁性金属粉末が簡単に製造できる
ようになった。しかも得られる扁平状粉末は微粉が少な
く、粒径も均一で、塗料用磁気シールド材料として最適
なものである。さらに近年、内部歪みのない磁気シール
ド特性の良い扁平状軟磁性金属粉末の要求もあり、それ
らへの使用も可能となった。本発明の製造方法は従来の
湿式粉砕方法と違い、エネルギー効率が良い方法である
とともに、有機溶剤使用量の少ない環境にも優しい新し
い製造方法である。According to the production method of the present invention, it is possible to easily produce a flat soft magnetic metal powder which has been difficult to produce until now. Moreover, the obtained flat powder has a small amount of fine powder and a uniform particle size, and is optimal as a magnetic shielding material for paint. Furthermore, in recent years, there has been a demand for a flat soft magnetic metal powder having good magnetic shielding characteristics without internal distortion, and it has become possible to use them. The production method of the present invention is different from the conventional wet pulverization method in that it is a method with good energy efficiency and is a new production method that is environmentally friendly and uses little organic solvent.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｈ０１Ｆ 1/00 Ｈ０１Ｆ 1/20 1/20 1/00 Ｃ Ｆターム(参考） 4D063 FF02 FF13 FF34 GA02 GD28 4K017 AA04 BA03 BA06 BB06 BB16 CA09 DA02 DA07 EA13 EK01 4K018 AA08 AA26 BD05 KA43 5E040 CA13 5E041 AA04 AA07 CA06 HB17 ──────────────────────────────────────────────────の Continued on the front page (51) Int.Cl. 7 Identification symbol FI Theme coat ゛ (Reference) H01F 1/00 H01F 1/20 1/20 1/00 CF term (Reference) 4D063 FF02 FF13 FF34 GA02 GD28 4K017 AA04 BA03 BA06 BB06 BB16 CA09 DA02 DA07 EA13 EK01 4K018 AA08 AA26 BD05 KA43 5E040 CA13 5E041 AA04 AA07 CA06 HB17
Claims (2)
砕媒体を用いた粉砕機で機械的に扁平加工する製造方法
において、前記軟磁性金属粉末のすきま容量の1/2〜２
倍の有機溶剤と、金属粉末１００重量部に対して０．１
〜２重量部の脂肪酸を混入して、粉砕することを特徴と
する扁平状軟磁性金属粉末の製造方法。1. A method for mechanically flattening a soft magnetic metal powder by an atomizing method using a pulverizer using a pulverizing medium, wherein the soft magnetic metal powder has a clearance of 1/2 to 2 times the clearance capacity of the soft magnetic metal powder.
Twice the amount of the organic solvent and 0.1 parts by weight with respect to 100 parts by weight of the metal powder.
A method for producing a flat soft magnetic metal powder, comprising mixing and pulverizing up to 2 parts by weight of a fatty acid.
徴とする特許請求項１記載の扁平状軟磁性金属粉末の製
造方法。2. The method for producing a flat soft magnetic metal powder according to claim 1, wherein the organic solvent is an alcohol solvent.
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|---|---|---|---|
| JP2000123417A JP2001303111A (en) | 2000-04-25 | 2000-04-25 | Method for producing flat soft magnetic metal powder |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000123417A JP2001303111A (en) | 2000-04-25 | 2000-04-25 | Method for producing flat soft magnetic metal powder |
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|---|---|
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Family
ID=18633721
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004140335A (en) * | 2002-08-19 | 2004-05-13 | Sumitomo Electric Ind Ltd | Electromagnetic wave absorber |
| JP2004156134A (en) * | 2002-09-11 | 2004-06-03 | Alps Electric Co Ltd | Amorphous soft magnetic alloy powder, and green compact core and radio wave absorber using the same |
| JP2005307291A (en) * | 2004-04-22 | 2005-11-04 | Alps Electric Co Ltd | Amorphous soft-magnetic alloy powder, and powder magnetic core and electromagnetic wave absorber using it |
| WO2008041588A1 (en) * | 2006-09-26 | 2008-04-10 | Mitsubishi Materials Corporation | Soft-magnetic iron composite powder for producing soft-magnetic composite material with high resistivity and low iron loss |
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| WO2008041588A1 (en) * | 2006-09-26 | 2008-04-10 | Mitsubishi Materials Corporation | Soft-magnetic iron composite powder for producing soft-magnetic composite material with high resistivity and low iron loss |
| JP2008308758A (en) * | 2006-09-26 | 2008-12-25 | Mitsubishi Materials Corp | Composite soft magnetic iron powder for producing composite soft magnetic material having high specific resistance and low iron loss |
| EP2117017A1 (en) | 2008-04-23 | 2009-11-11 | TDK Corporation | Flat soft magnetic material and process for its production |
| US8038808B2 (en) | 2008-04-23 | 2011-10-18 | Tdk Corporation | Flat soft magnetic material and process for its production |
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| JP2017188646A (en) * | 2016-03-31 | 2017-10-12 | Tdk株式会社 | Composite magnetic sealing material |
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