JPH08264360A - Resin-bonded magnet manufacturing method and resin-bonded magnet - Google Patents

Resin-bonded magnet manufacturing method and resin-bonded magnet

Info

Publication number
JPH08264360A
JPH08264360A JP7069685A JP6968595A JPH08264360A JP H08264360 A JPH08264360 A JP H08264360A JP 7069685 A JP7069685 A JP 7069685A JP 6968595 A JP6968595 A JP 6968595A JP H08264360 A JPH08264360 A JP H08264360A
Authority
JP
Japan
Prior art keywords
resin
bonded magnet
powder
magnetic powder
plasma sintering
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.)
Pending
Application number
JP7069685A
Other languages
Japanese (ja)
Inventor
Mitsuru Takei
充 武居
Isato Shirai
勇人 白井
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Seiko Epson Corp
Original Assignee
Seiko Epson Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Seiko Epson Corp filed Critical Seiko Epson Corp
Priority to JP7069685A priority Critical patent/JPH08264360A/en
Publication of JPH08264360A publication Critical patent/JPH08264360A/en
Pending legal-status Critical Current

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Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/06Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys in the form of particles, e.g. powder
    • H01F1/08Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together
    • H01F1/083Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together in a bonding agent

Landscapes

  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Powder Metallurgy (AREA)
  • Hard Magnetic Materials (AREA)
  • Manufacturing Cores, Coils, And Magnets (AREA)

Abstract

(57)【要約】 【目的】 樹脂結合型磁石において短時間または少工程
で品質ばらつきの少ない磁石の製造方法を与えることに
ある。 【構成】 原料粉末として磁性粉末にポリアミド樹脂、
またはポリイミド樹脂、エポキシ樹脂,ポリエチレン,
ポリフェニレンスルフィド,ABS樹脂,アミノ樹脂,
フェノール樹脂,ポリエチレンテレフタレート,ポリカ
ーボネートの何れかを添加したものを使用し放電プラズ
マ焼結法を用いて樹脂結合型磁石を製造する製造方法。
(57) [Summary] [Purpose] To provide a method for manufacturing a resin-bonded magnet in which the quality variation is small in a short time or in a small number of steps. [Structure] Magnetic powder as a raw material powder, polyamide resin,
Or polyimide resin, epoxy resin, polyethylene,
Polyphenylene sulfide, ABS resin, amino resin,
A manufacturing method for manufacturing a resin-bonded magnet using a discharge plasma sintering method using a material to which any one of a phenol resin, polyethylene terephthalate and polycarbonate is added.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【産業上の利用分野】本発明は樹脂結合型磁石の製造方
法および樹脂結合型磁石に関するものである。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a resin-bonded magnet manufacturing method and a resin-bonded magnet.

【0002】[0002]

【従来の技術】現在、生産されている樹脂結合型磁石は
OA機器、カメラ、家電製品等に使用される小型モータ
ーを中心に需要が伸び、その生産数は年10数%の高い
伸び率を示している。樹脂結合型磁石には特公昭50−
18559号公報等に開示されているような熱硬化性樹
脂による圧縮成形法によるものや、特公昭55−331
73号公報あるいは特公昭58−53491公報等に開
示されている射出成形法による磁石、さらに最近は特開
昭61−121307号公報あるいは特開昭62−20
8612号公報等に開示されているような押出成形磁石
がある。
2. Description of the Related Art Demand for resin-bonded magnets currently in production is growing, centering on small motors used in office automation equipment, cameras, home appliances, etc. Shows. For resin-bonded magnets
By a compression molding method using a thermosetting resin as disclosed in Japanese Patent No. 18559 and Japanese Patent Publication No. 55-331.
No. 73 or Japanese Examined Patent Publication No. 58-53491, and the more recent magnets manufactured by the injection molding method, and more recently, Japanese Unexamined Patent Publication No. 61-121307 or Japanese Unexamined Patent Publication No. 62-20.
There is an extruded magnet as disclosed in Japanese Patent No. 8612.

【0003】現在、最も生産量が多いのは熱硬化性樹脂
を用いた磁石であるが、これは少ない樹脂量で磁石を成
形できる為、高性能な磁石が得られるからである。一
方、熱可塑性樹脂を用いた射出成形磁石、押出成形磁石
については複雑な形状、またはパイプ形状の磁石が得ら
れるが、成形時、樹脂と磁性粉末の混合物に対しある程
度の流動性が求められる為、添加する樹脂量が熱硬化性
樹脂の場合に比べ多くなり性能的には熱硬化性樹脂タイ
プにおよばないのが実際である。
At present, the largest amount of production is a magnet using a thermosetting resin. This is because a high performance magnet can be obtained because the magnet can be molded with a small amount of resin. On the other hand, injection-molded magnets and extruded magnets using thermoplastic resins can have magnets with complicated shapes or pipe shapes, but a certain degree of fluidity is required for the mixture of resin and magnetic powder during molding. The amount of resin to be added is larger than that of the thermosetting resin, and in actuality, it does not reach the thermosetting resin type in terms of performance.

【0004】また、熱可塑性樹脂を用いて圧縮成形法で
磁石を成形するには樹脂と磁性粉末を型に入れ加熱しな
がら加圧する必要があり、従来技術ではホットプレスが
これに対応する。
Further, in order to mold a magnet by a compression molding method using a thermoplastic resin, it is necessary to put resin and magnetic powder into a mold and pressurize while heating, and in the prior art, hot pressing corresponds to this.

【0005】[0005]

【発明が解決しようとする課題】しかし、従来技術では
次の様な問題点があった。
However, the prior art has the following problems.

【0006】ホットプレスではその昇温、成形、冷却に
時間がかかり生産性が低くなる上に、加熱が伝熱による
為、成形時に成形体内部に温度差が生じそれが場所によ
る密度差の大きな原因となり、性能ばらつきを引き起こ
している。また、熱硬化性樹脂を使用する場合には成形
後加熱して樹脂を硬化させる必要があり、製品を得るた
めには最低限成形、焼成の2工程を経ることになる。更
に、樹脂を硬化させる前の成型品は機械的強度が弱く変
形、カケなどを起こしやすく取り扱いに充分な注意が必
要となる。
[0006] In the hot press, it takes time to heat up, mold and cool, which lowers the productivity, and since the heating is conducted by heat transfer, a temperature difference occurs inside the molded body during molding, which causes a large density difference depending on the location. It is a cause and causes a variation in performance. Further, when a thermosetting resin is used, it is necessary to heat the resin after molding to cure the resin, and in order to obtain a product, at least two steps of molding and baking are required. Further, the molded product before curing the resin has weak mechanical strength and is liable to be deformed or chipped, so that it is necessary to handle it with sufficient care.

【0007】本発明は、磁性粉末に熱可塑性樹脂または
熱硬化性樹脂を用いた樹脂結合型磁石の製造方法および
樹脂結合型磁石に関わるものであり、その目的とすると
ころは、上記課題を解決するとともに磁性粉末に熱可塑
性樹脂または熱硬化性樹脂を添加して放電プラズマ焼結
法で製造することで効率的かつ品質ばらつきの少ない樹
脂結合型磁石を製造する樹脂結合型磁石の製造方法を与
え、該製造方法で製造された樹脂結合型磁石を与えるも
のである。
The present invention relates to a method for producing a resin-bonded magnet using a thermoplastic resin or a thermosetting resin as magnetic powder and a resin-bonded magnet, and an object of the invention is to solve the above problems. In addition, a thermoplastic resin or thermosetting resin was added to the magnetic powder to produce a resin-bonded magnet that is efficient and has little quality variation by manufacturing by the spark plasma sintering method. The present invention provides a resin-bonded magnet manufactured by the manufacturing method.

【0008】[0008]

【課題を解決するための手段】本発明は、磁性粉末に熱
可塑性樹脂または熱硬化性樹脂を添加し、放電プラズマ
焼結法を用いて製造したことを特徴とする。
The present invention is characterized in that a thermoplastic resin or a thermosetting resin is added to magnetic powder and the magnetic powder is manufactured by a spark plasma sintering method.

【0009】放電プラズマ焼結法とは、プラズマ活性化
焼結法とも呼ばれる方法で加圧下において金属粉末にパ
ルス状の電流を直接通電させることで粒子間に火花放電
とプラズマ発生を引き起こさせ粉末を焼結させるもので
ある。図1にその基本構成を示す。基本構成は成形の為
のプレスと通電の為の電源及び成形型からなっている。
この方法は1960年代に開発され金属間化合物、傾
斜機能材料等の開発に応用されてきた。放電プラズマ焼
結法は放電プラズマの発生を焼結のエネルギーする為に
場所による温度差が生じ難く、均質で高品位の焼結体が
得られる。また、その焼結速度も従来の焼結法に比べ速
い。更にこれまで困難と言われていたセラミックスと金
属の接合や多孔質焼結体の作製が可能なことが特徴とし
て上げられる。
The discharge plasma sintering method is a method also called plasma activated sintering method, in which a pulsed electric current is directly applied to the metal powder under pressure to cause spark discharge and plasma generation between the particles to cause powder generation. It is what is sintered. FIG. 1 shows the basic configuration. The basic structure consists of a press for molding, a power supply for energizing, and a molding die.
This method was developed in the 1960s and has been applied to the development of intermetallic compounds, functionally graded materials and the like. In the discharge plasma sintering method, since the generation of discharge plasma is used as energy for sintering, a temperature difference hardly occurs depending on a place, and a homogeneous and high-quality sintered body can be obtained. Further, the sintering rate is also higher than that of the conventional sintering method. Another feature is that it is possible to bond ceramics and metal, which has been considered difficult until now, and to manufacture a porous sintered body.

【0010】本発明はこの放電プラズマ焼結法を通常の
金属またはセラミックスの焼結ではなく磁性粉末に添加
した結合剤としての樹脂の溶融、または硬化反応を引き
起こす為の加熱手段として応用したものである。
The present invention applies the discharge plasma sintering method as a heating means for inducing a melting or curing reaction of a resin as a binder added to magnetic powder, instead of the usual sintering of metal or ceramics. is there.

【0011】磁性粉末に熱可塑性樹脂または熱硬化性樹
脂を添加し型に充填した後、放電プラズマ焼結の原理に
従い加圧しながらパルス電流を通電し、通電により粉末
が発熱し周囲の樹脂を加熱する。樹脂が熱可塑性樹脂で
あれば溶融し同時に行われる加圧により磁性粉末間の空
隙に進入し、液状滑剤として機能し、成形体を緻密加さ
せる。ある程度緻密化した後型を冷却し、成形体を取り
出す。これにより熱可塑性樹脂を結合剤としながら射出
成形や押出成形に比べ磁性粉末の含有量が多い高性能な
樹脂結合型磁石が得られる。また、樹脂がエポキシ樹脂
の様な熱硬化性樹脂であれば、同様に樹脂が加熱されそ
の昇温過程で一度軟化、または低粘度化が起こる。この
際、加圧により成形体の緻密化が起こる、その後温度の
上昇に伴い硬化反応が起こり硬化する。硬化後冷却し成
形体を取り出す。これによりこれまでは成形と樹脂硬化
の為の焼成の2工程であったものが1工程で行えること
になる。
After adding a thermoplastic resin or a thermosetting resin to the magnetic powder and filling the mold, a pulse current is applied while pressure is applied according to the principle of discharge plasma sintering, and the powder generates heat by heating to heat the surrounding resin. To do. If the resin is a thermoplastic resin, it melts and enters into the voids between the magnetic powders by the pressure applied at the same time, functions as a liquid lubricant, and compacts the compact. After densifying to some extent, the mold is cooled and the molded body is taken out. This makes it possible to obtain a high-performance resin-bonded magnet having a higher content of magnetic powder than that obtained by injection molding or extrusion molding while using a thermoplastic resin as a binder. If the resin is a thermosetting resin such as an epoxy resin, the resin is heated in the same manner, and once the resin is heated, the resin softens or the viscosity decreases. At this time, densification of the molded body occurs due to pressurization, and then a curing reaction occurs and cures as the temperature rises. After curing, it is cooled and the molded product is taken out. As a result, what has heretofore been two steps of molding and baking for curing the resin can be performed in one step.

【0012】請求項12〜14において樹脂の添加量を
0.5〜10wt%としたのは実施例において説明する
通り従来法との比較において本発明品の磁気特性におけ
る優位性が明らかに認められる範囲である為である。
In the twelfth to fourteenth aspects, the amount of the resin added is set to 0.5 to 10% by weight, as will be described in the examples, and the superiority of the magnetic properties of the product of the present invention is clearly recognized in comparison with the conventional method. This is because it is a range.

【0013】[0013]

【実施例】以下、実施例に従い説明する。EXAMPLES Examples will be described below.

【0014】(実施例1)原料粉末としてNd,Fe、
B,Coを主成分とした急冷薄帯法による磁性粉末を用
いた。磁性粉末を振動ボールミルで平均粒径約36μm
に粉砕した後、ふるいで90μm以上のものを取り除い
た。得られた粉末に平均粒径20μmのナイロン12を
1.0,2.0wt%添加し、総重量5kgの粉末を容
量15lの高速流動型混合機(6500RPM)で10
分間混合した。得られた粉末45gを外径20mmのペ
レット成形用金型に充填し、放電プラズマ焼結装置にセ
ットした。焼結条件は昇温速度80度/分,焼結温度
(保持温度)230℃、保持時間3分,冷却温度60℃
/分、加圧力650kgf/cm2,電流値 1000
A〜1500Aとした。
(Example 1) Nd, Fe as raw material powder,
Magnetic powder containing B and Co as the main components by the quenching ribbon method was used. Magnetic powder with a vibrating ball mill has an average particle size of about 36 μm.
After pulverizing into particles, the particles having a size of 90 μm or more were removed by a sieve. Nylon 12 having an average particle size of 20 μm was added to the obtained powder in an amount of 1.0 and 2.0 wt%, and a total weight of 5 kg was mixed with a high-speed flow type mixer (6500 RPM) having a volume of 15 l for 10 times.
Mix for minutes. 45 g of the obtained powder was filled in a pellet molding die having an outer diameter of 20 mm and set in a discharge plasma sintering apparatus. The sintering conditions are a temperature rising rate of 80 degrees / minute, a sintering temperature (holding temperature) of 230 ° C, a holding time of 3 minutes, and a cooling temperature of 60 ° C.
/ Min, pressing force 650 kgf / cm2, current value 1000
It was set to A to 1500A.

【0015】焼結後、外径20mm高さ約30mmの円
柱状の成形体を取り出し、高さ方向に5等分しアルキメ
デス法によりそれぞれの密度の測定を行った。尚、比較
の為に同形状のナイロン12を結合剤とした圧縮成形磁
石をホットプレスにより作製し同様の測定を行った(ナ
イロン12は平均粒径20μm以下の粉末状のもの使用
し、添加量は1.0,2.0wt%とした,また加熱は
昇温速度50℃/分,保持温度230℃,成形保持時間
3分、冷却速度30℃/分,成形圧力は650kgf/
cm2とした)。
After sintering, a cylindrical molded body having an outer diameter of 20 mm and a height of about 30 mm was taken out, divided into 5 equal parts in the height direction, and the respective densities were measured by the Archimedes method. For comparison, a compression-molded magnet having the same shape of nylon 12 as a binder was prepared by hot pressing and the same measurement was performed (nylon 12 was used in the form of powder having an average particle size of 20 μm or less, and the addition amount was Was 1.0, 2.0 wt%, heating was 50 ° C./minute, holding temperature was 230 ° C., molding holding time was 3 minutes, cooling rate was 30 ° C./minute, molding pressure was 650 kgf /
cm2).

【0016】結果を図2に示す。The results are shown in FIG.

【0017】図2から本発明により場所による密度差の
少ない均一な樹脂結合型磁石を得られることが分かる。
It can be seen from FIG. 2 that the present invention can provide a uniform resin-bonded magnet having a small density difference depending on the location.

【0018】(実施例2)原料粉末としてNd,Fe、
B,Coを主成分とした急冷薄帯法による磁性粉末を用
いた。磁性粉末を振動ボールミルで平均粒径約36μm
に粉砕した後、ふるいで90μm以上のものを取り除い
た。得られた粉末に平均粒径20μmのポリイミド樹脂
を1.0,2.0wt%添加し、総重量5kgの粉末を
容量15lの高速流動型混合機(6500RPM)で1
0分間混合した。得られた粉末45gを外径20mmの
ペレット成形用金型に充填し、放電プラズマ焼結装置に
セットした。焼結条件は昇温速度80度/分,焼結温度
(保持温度)270℃、保持時間5分,冷却温度60℃
/分、加圧力650kgf/cm2,電流値 1000
A〜1500Aとした。
(Example 2) Nd, Fe as raw material powder,
Magnetic powder containing B and Co as the main components by the quenching ribbon method was used. Magnetic powder with a vibrating ball mill has an average particle size of about 36 μm.
After pulverizing into particles, the particles having a size of 90 μm or more were removed by a sieve. 1.0 and 2.0 wt% of a polyimide resin having an average particle diameter of 20 μm was added to the obtained powder, and a total weight of 5 kg was mixed with a high-speed flow type mixer (6500 RPM) having a volume of 15 l.
Mix for 0 minutes. 45 g of the obtained powder was filled in a pellet molding die having an outer diameter of 20 mm and set in a discharge plasma sintering apparatus. The sintering conditions are a temperature rising rate of 80 degrees / minute, a sintering temperature (holding temperature) of 270 ° C., a holding time of 5 minutes, and a cooling temperature of 60 ° C.
/ Min, pressing force 650 kgf / cm2, current value 1000
It was set to A to 1500A.

【0019】焼結後、外径20mm高さ約30mmの円
柱状の成形体を取り出し、高さ方向に5等分しアルキメ
デス法によりそれぞれの密度の測定を行った。尚、比較
の為に同形状のポリイミド樹脂を結合剤とした圧縮成形
磁石をホットプレスにより作製し同様の測定を行った
(ポリイミド樹脂は平均粒径20μm以下の粉末状のも
の使用し、添加量は1.0,2.0wt%とした,また
加熱は昇温速度50℃/分,保持温度270℃,成形保
持時間5分、冷却速度30℃/分,成形圧力は650k
gf/cm2とした)。
After sintering, a cylindrical molded body having an outer diameter of 20 mm and a height of about 30 mm was taken out, divided into 5 equal parts in the height direction, and the respective densities were measured by the Archimedes method. For comparison, a compression-molded magnet having the same shape of a polyimide resin as a binder was prepared by hot pressing and the same measurement was carried out (a polyimide resin powder having an average particle size of 20 μm or less was used, and the addition amount was Was 1.0, 2.0 wt%, heating was 50 ° C./min, holding temperature was 270 ° C., molding holding time was 5 minutes, cooling rate was 30 ° C./min, molding pressure was 650 k.
gf / cm2).

【0020】結果を図3に示す。The results are shown in FIG.

【0021】図3から本発明により場所による密度差の
少ない均一な樹脂結合型磁石を得られることが分かる。
It can be seen from FIG. 3 that the present invention can provide a uniform resin-bonded magnet having a small density difference depending on the location.

【0022】(実施例3)原料粉末としてSm、Coを
主成分とし鋳造法により作製された合金を粉砕し作製し
た磁性粉末を用いた。磁性粉末は最終的に振動ボールミ
ルで平均粒径約36μmに粉砕した後、ふるいで90μ
m以上のものを取り除いた。得られた粉末に平均粒径2
0μmのエポキシ樹脂粉末を1.0,2.0wt%添加
し、総重量5kgの粉末を容量15lの高速流動型混合
機(6500RPM)で10分間混合した。得られた粉
末45gを外径20mmのペレット成形用金型に充填
し、放電プラズマ焼結装置にセットした。焼結条件は昇
温速度80度/分,焼結温度(保持温度)230℃、保
持時間3分,冷却温度60℃/分、加圧力650kgf
/cm2,電流値1000A〜1500Aとした。
Example 3 As a raw material powder, a magnetic powder prepared by crushing an alloy containing Sm and Co as main components and prepared by a casting method was used. The magnetic powder is finally crushed with a vibrating ball mill to an average particle size of about 36 μm and then sieved to 90 μm.
Items over m were removed. The obtained powder has an average particle size of 2
1.0 and 2.0 wt% of 0 μm epoxy resin powder was added, and the powder having a total weight of 5 kg was mixed for 10 minutes by a high-speed flow type mixer (6500 RPM) having a volume of 15 l. 45 g of the obtained powder was filled in a pellet molding die having an outer diameter of 20 mm and set in a discharge plasma sintering apparatus. The sintering conditions are a temperature rising rate of 80 degrees / minute, a sintering temperature (holding temperature) of 230 ° C., a holding time of 3 minutes, a cooling temperature of 60 ° C./minute, and a pressing force of 650 kgf.
/ Cm2, and the current value was 1000A to 1500A.

【0023】焼結後、外径20mm高さ約30mmの円
柱状の成形体を取り出し、高さ方向に5等分しアルキメ
デス法によりそれぞれの密度の測定を行った。尚、比較
の為に同形状のエポキシ樹脂を結合剤とした圧縮成形磁
石を作製し同様の測定を行った(エポキシ樹脂は平均粒
径20μm以下の粉末状のもの使用し、添加量は1.
0,2.0wt%とした,成形圧力650kgf/cm
2で成形後、150℃で1時間焼成し樹脂を硬化させ
た)。
After sintering, a cylindrical molded body having an outer diameter of 20 mm and a height of about 30 mm was taken out, divided into 5 equal parts in the height direction, and the respective densities were measured by the Archimedes method. For comparison, a compression-molded magnet having an epoxy resin of the same shape as a binder was prepared and the same measurement was performed (the epoxy resin used was a powder having an average particle size of 20 μm or less, and the addition amount was 1.
Molding pressure of 650 kgf / cm, with 0, 2.0 wt%
After molding at 2, the resin was cured by baking at 150 ° C. for 1 hour).

【0024】結果を図4に示す。The results are shown in FIG.

【0025】図4から本発明により場所による密度差の
少ない均一な樹脂結合型磁石を得られることが分かる。
It can be seen from FIG. 4 that the present invention can provide a uniform resin-bonded magnet with a small density difference depending on the location.

【0026】(実施例4)原料粉末としてSm、Coを
主成分とし鋳造法により作製された合金を粉砕し作製し
た磁性粉末を用いた。磁性粉末は最終的に振動ボールミ
ルで平均粒径約36μmに粉砕した後、ふるいで90μ
m以上のものを取り除いた。得られた粉末に平均粒径2
0μmのポリエチレン粉末を1.0,2.0wt%添加
し、総重量5kgの粉末を容量15lの高速流動型混合
機(6500RPM)で10分間混合した。得られた粉
末45gを外径20mmのペレット成形用金型に充填
し、放電プラズマ焼結装置にセットした。焼結条件は昇
温速度80度/分,焼結温度(保持温度)120℃、保
持時間3分,冷却温度60℃/分、加圧力650kgf
/cm2,電流値1000A〜1500Aとした。
Example 4 As a raw material powder, a magnetic powder prepared by crushing an alloy containing Sm and Co as main components and prepared by a casting method was used. The magnetic powder is finally crushed with a vibrating ball mill to an average particle size of about 36 μm and then sieved to 90 μm.
Items over m were removed. The obtained powder has an average particle size of 2
1.0 and 2.0 wt% of 0 μm polyethylene powder was added, and the powder having a total weight of 5 kg was mixed for 10 minutes by a high-speed flow type mixer (6500 RPM) having a volume of 15 l. 45 g of the obtained powder was filled in a pellet molding die having an outer diameter of 20 mm and set in a discharge plasma sintering apparatus. The sintering conditions are a heating rate of 80 degrees / minute, a sintering temperature (holding temperature) of 120 ° C., a holding time of 3 minutes, a cooling temperature of 60 ° C./minute, and a pressing force of 650 kgf.
/ Cm2, and the current value was 1000A to 1500A.

【0027】焼結後、外径20mm高さ約30mmの円
柱状の成形体を取り出し、高さ方向に5等分しアルキメ
デス法によりそれぞれの密度の測定を行った。尚、比較
の為に同形状のポリエチレンを結合剤とした圧縮成形磁
石を作製し同様の測定を行った(ポリエチレンは平均粒
径20μm以下の粉末状のもの使用し、添加量は1.
0,2.0wt%とした,また加熱は昇温速度50℃/
分,保持温度120℃,成形保持時間5分、冷却速度3
0℃/分,成形圧力は650kgf/cm2とした)。
After sintering, a cylindrical molded body having an outer diameter of 20 mm and a height of about 30 mm was taken out, divided into 5 equal parts in the height direction, and the respective densities were measured by the Archimedes method. For comparison, a compression-molded magnet using polyethylene of the same shape as a binder was prepared and the same measurement was performed (polyethylene powder having an average particle size of 20 μm or less was used, and the addition amount was 1.
0, 2.0 wt% and heating rate is 50 ° C /
Min, holding temperature 120 ° C, molding holding time 5 minutes, cooling rate 3
The molding pressure was 0 ° C./min and the molding pressure was 650 kgf / cm 2.

【0028】結果を図5に示す。The results are shown in FIG.

【0029】図5から本発明により場所による密度差の
少ない均一な樹脂結合型磁石を得られることが分かる。
It can be seen from FIG. 5 that the present invention can provide a uniform resin-bonded magnet having a small density difference depending on the location.

【0030】(実施例5)原料粉末としてSm、Coを
主成分とし鋳造法により作製された合金を粉砕し作製し
た磁性粉末を用いた。磁性粉末は最終的に振動ボールミ
ルで平均粒径約36μmに粉砕した後、ふるいで90μ
m以上のものを取り除いた。得られた粉末に平均粒径2
0μmのポリフェニレンスルフィド粉末を1.0,2.
0wt%添加し、総重量5kgの粉末を容量15lの高
速流動型混合機(6500RPM)で10分間混合し
た。得られた粉末45gを外径20mmのペレット成形
用金型に充填し、放電プラズマ焼結装置にセットした。
焼結条件は昇温速度80度/分,焼結温度(保持温度)
350℃、保持時間3分,冷却温度60℃/分、加圧力
650kgf/cm2,電流値1000A〜1500A
とした。
Example 5 As a raw material powder, a magnetic powder prepared by crushing an alloy containing Sm and Co as main components and prepared by a casting method was used. The magnetic powder is finally crushed with a vibrating ball mill to an average particle size of about 36 μm and then sieved to 90 μm.
Items over m were removed. The obtained powder has an average particle size of 2
0 .mu.m polyphenylene sulfide powder 1.0, 2.
0 wt% was added, and a powder having a total weight of 5 kg was mixed for 10 minutes by a high-speed flow type mixer (6500 RPM) having a volume of 15 l. 45 g of the obtained powder was filled in a pellet molding die having an outer diameter of 20 mm and set in a discharge plasma sintering apparatus.
Sintering conditions are heating rate of 80 degrees / minute, sintering temperature (holding temperature)
350 ° C., holding time 3 minutes, cooling temperature 60 ° C./minute, pressure 650 kgf / cm 2, current value 1000 A to 1500 A
And

【0031】焼結後、外径20mm高さ約30mmの円
柱状の成形体を取り出し、高さ方向に5等分しアルキメ
デス法によりそれぞれの密度の測定を行った。尚、比較
の為に同形状のポリフェニレンスルフィドを結合剤とし
た圧縮成形磁石を作製し同様の測定を行った(ポリフェ
ニレンスルフィドは平均粒径20μm以下の粉末状のも
の使用し、添加量は1.0,2.0wt%とした,また
加熱は昇温速度50℃/分,保持温度350℃,成形保
持時間8分、冷却速度30℃/分,成形圧力は650k
gf/cm2とした)。
After sintering, a cylindrical molded body having an outer diameter of 20 mm and a height of about 30 mm was taken out, divided into 5 equal parts in the height direction, and the respective densities were measured by the Archimedes method. For comparison, a compression-molded magnet having the same shape of polyphenylene sulfide as a binder was prepared and the same measurement was conducted (polyphenylene sulfide was used in the form of powder having an average particle size of 20 μm or less, and the addition amount was 1. The heating rate was 50 ° C./minute, the holding temperature was 350 ° C., the molding holding time was 8 minutes, the cooling rate was 30 ° C./minute, and the molding pressure was 650 k.
gf / cm2).

【0032】結果を図6に示す。The results are shown in FIG.

【0033】図6から本発明により場所による密度差の
少ない均一な樹脂結合型磁石を得られることが分かる。
It can be seen from FIG. 6 that the present invention can provide a uniform resin-bonded magnet with a small density difference depending on the location.

【0034】(実施例6)原料粉末としてNd,Fe、
B,Coを主成分とした急冷薄帯法による磁性粉末を用
いた。磁性粉末を振動ボールミルで平均粒径約36μm
に粉砕した後、ふるいで90μm以上のものを取り除い
た。得られた粉末に平均粒径20μmのABS樹脂を
1.0,2.0wt%添加し、総重量5kgの粉末を容
量15lの高速流動型混合機(6500RPM)で10
分間混合した。得られた粉末45gを外径20mmのペ
レット成形用金型に充填し、放電プラズマ焼結装置にセ
ットした。焼結条件は昇温速度80度/分,焼結温度
(保持温度)130℃、保持時間3分,冷却温度60℃
/分、加圧力650kgf/cm2,電流値 1000
A〜1500Aとした。
Example 6 Nd, Fe as raw material powder,
Magnetic powder containing B and Co as the main components by the quenching ribbon method was used. Magnetic powder with a vibrating ball mill has an average particle size of about 36 μm.
After pulverizing into particles, the particles having a size of 90 μm or more were removed by a sieve. To the obtained powder, 1.0 and 2.0 wt% of ABS resin having an average particle diameter of 20 μm was added, and a total weight of 5 kg was mixed with a high-speed flow type mixer (6500 RPM) having a volume of 15 l for 10 times.
Mix for minutes. 45 g of the obtained powder was filled in a pellet molding die having an outer diameter of 20 mm and set in a discharge plasma sintering apparatus. The sintering conditions are a temperature rising rate of 80 degrees / minute, a sintering temperature (holding temperature) of 130 ° C, a holding time of 3 minutes, and a cooling temperature of 60 ° C.
/ Min, pressing force 650 kgf / cm2, current value 1000
It was set to A to 1500A.

【0035】焼結後、外径20mm高さ約30mmの円
柱状の成形体を取り出し、高さ方向に5等分しアルキメ
デス法によりそれぞれの密度の測定を行った。尚、比較
の為に同形状のABS樹脂を結合剤とした圧縮成形磁石
をホットプレスにより作製し同様の測定を行った(AB
S樹脂は平均粒径20μm以下の粉末状のもの使用し、
添加量は1.0,2.0wt%とした,また加熱は昇温
速度50℃/分,保持温度130℃,成形保持時間3
分、冷却速度30℃/分,成形圧力は650kgf/c
m2とした)。
After sintering, a cylindrical molded body having an outer diameter of 20 mm and a height of about 30 mm was taken out, divided into 5 equal parts in the height direction, and the respective densities were measured by the Archimedes method. For comparison, a compression-molded magnet having the same shape of ABS resin as a binder was prepared by hot pressing and the same measurement was performed (AB
Use the S resin in powder form with an average particle size of 20 μm or less,
The addition amount was 1.0 and 2.0 wt%, and the heating rate was 50 ° C./min, the holding temperature was 130 ° C., and the molding holding time was 3
Min, cooling rate 30 ° C / min, molding pressure 650kgf / c
m2).

【0036】結果を図7に示す。The results are shown in FIG.

【0037】図7から本発明により場所による密度差の
少ない均一な樹脂結合型磁石を得られることが分かる。
It can be seen from FIG. 7 that the present invention makes it possible to obtain a uniform resin-bonded magnet having a small density difference depending on the location.

【0038】(実施例7)原料粉末としてNd,Fe、
B,Coを主成分とした急冷薄帯法による磁性粉末を用
いた。磁性粉末を振動ボールミルで平均粒径約36μm
に粉砕した後、ふるいで90μm以上のものを取り除い
た。得られた粉末に平均粒径20μmのアミノ樹脂を
1.0,2.0wt%添加し、総重量5kgの粉末を容
量15lの高速流動型混合機(6500RPM)で10
分間混合した。得られた粉末45gを外径20mmのペ
レット成形用金型に充填し、放電プラズマ焼結装置にセ
ットした。焼結条件は昇温速度80度/分,焼結温度
(保持温度)240℃、保持時間5分,冷却温度60℃
/分、加圧力650kgf/cm2,電流値 1000
A〜1500Aとした。
Example 7 Nd, Fe as raw material powder,
Magnetic powder containing B and Co as the main components by the quenching ribbon method was used. Magnetic powder with a vibrating ball mill has an average particle size of about 36 μm.
After pulverizing into particles, the particles having a size of 90 μm or more were removed by a sieve. 1.0 and 2.0 wt% of an amino resin having an average particle size of 20 μm was added to the obtained powder, and a powder having a total weight of 5 kg was mixed with a high-speed flow type mixer (6500 RPM) having a volume of 15 l for 10 times.
Mix for minutes. 45 g of the obtained powder was filled in a pellet molding die having an outer diameter of 20 mm and set in a discharge plasma sintering apparatus. The sintering conditions are a temperature rising rate of 80 degrees / minute, a sintering temperature (holding temperature) of 240 ° C, a holding time of 5 minutes, and a cooling temperature of 60 ° C.
/ Min, pressing force 650 kgf / cm2, current value 1000
It was set to A to 1500A.

【0039】焼結後、外径20mm高さ約30mmの円
柱状の成形体を取り出し、高さ方向に5等分しアルキメ
デス法によりそれぞれの密度の測定を行った。尚、比較
の為に同形状のアミノ樹脂を結合剤とした圧縮成形磁石
をホットプレスにより作製し同様の測定を行った(アミ
ノ樹脂は平均粒径20μm以下の粉末状のもの使用し、
添加量は1.0,2.0wt%とした,また加熱は昇温
速度50℃/分,保持温度240℃,成形保持時間20
分、冷却速度30℃/分,成形圧力は650kgf/c
m2とした)。
After sintering, a cylindrical molded body having an outer diameter of 20 mm and a height of about 30 mm was taken out, divided into 5 equal parts in the height direction, and the respective densities were measured by the Archimedes method. For comparison, a compression-molded magnet having the same shape of an amino resin as a binder was prepared by hot pressing and the same measurement was performed (the amino resin used was a powder having an average particle size of 20 μm or less,
The addition amount was 1.0 and 2.0 wt%, and the heating rate was 50 ° C./min, the holding temperature was 240 ° C., and the molding holding time was 20.
Min, cooling rate 30 ° C / min, molding pressure 650kgf / c
m2).

【0040】結果を図8に示す。The results are shown in FIG.

【0041】図8から本発明により場所による密度差の
少ない均一な樹脂結合型磁石を得られることが分かる。
It can be seen from FIG. 8 that the present invention makes it possible to obtain a uniform resin-bonded magnet having a small density difference depending on the location.

【0042】(実施例8)原料粉末としてSm、Coを
主成分とし鋳造法により作製された合金を粉砕し作製し
た磁性粉末を用いた。磁性粉末は最終的に振動ボールミ
ルで平均粒径約36μmに粉砕した後、ふるいで90μ
m以上のものを取り除いた。得られた粉末に平均粒径2
0μmのフェノール樹脂粉末を1.0,2.0wt%添
加し、総重量5kgの粉末を容量15lの高速流動型混
合機(6500RPM)で10分間混合した。得られた
粉末45gを外径20mmのペレット成形用金型に充填
し、放電プラズマ焼結装置にセットした。焼結条件は昇
温速度80度/分,焼結温度(保持温度)250℃、保
持時間3分,冷却温度60℃/分、加圧力650kgf
/cm2,電流値1000A〜1500Aとした。
Example 8 As the raw material powder, a magnetic powder prepared by crushing an alloy containing Sm and Co as main components and prepared by a casting method was used. The magnetic powder is finally crushed with a vibrating ball mill to an average particle size of about 36 μm and then sieved to 90 μm.
Items over m were removed. The obtained powder has an average particle size of 2
1.0 and 2.0 wt% of 0 μm phenol resin powder was added, and the powder having a total weight of 5 kg was mixed for 10 minutes by a high-speed fluid type mixer (6500 RPM) having a volume of 15 l. 45 g of the obtained powder was filled in a pellet molding die having an outer diameter of 20 mm and set in a discharge plasma sintering apparatus. The sintering conditions are a heating rate of 80 degrees / minute, a sintering temperature (holding temperature) of 250 ° C., a holding time of 3 minutes, a cooling temperature of 60 ° C./minute, and a pressing force of 650 kgf.
/ Cm2, and the current value was 1000A to 1500A.

【0043】焼結後、外径20mm高さ約30mmの円
柱状の成形体を取り出し、高さ方向に5等分しアルキメ
デス法によりそれぞれの密度の測定を行った。尚、比較
の為に同形状のフェノール樹脂を結合剤とした圧縮成形
磁石を作製し同様の測定を行った(フェノール樹脂は平
均粒径20μm以下の粉末状のもの使用し、添加量は
1.0,2.0wt%とした,成形圧力650kgf/
cm2で成形後、250℃で1時間焼成し樹脂を硬化さ
せた)。
After sintering, a cylindrical molded body having an outer diameter of 20 mm and a height of about 30 mm was taken out, divided into 5 equal parts in the height direction, and the respective densities were measured by the Archimedes method. For comparison, a compression-molded magnet having the same shape of a phenol resin as a binder was prepared and the same measurement was performed (the phenol resin used was a powder having an average particle size of 20 μm or less, and the addition amount was 1. Molding pressure 650 kgf /
After molding at cm 2, the resin was cured by firing at 250 ° C for 1 hour).

【0044】結果を図9に示す。The results are shown in FIG.

【0045】図9から本発明により場所による密度差の
少ない均一な樹脂結合型磁石を得られることが分かる。
It can be seen from FIG. 9 that the present invention can provide a uniform resin-bonded magnet having a small density difference depending on the location.

【0046】(実施例9)原料粉末としてSm、Coを
主成分とし鋳造法により作製された合金を粉砕し作製し
た磁性粉末を用いた。磁性粉末は最終的に振動ボールミ
ルで平均粒径約36μmに粉砕した後、ふるいで90μ
m以上のものを取り除いた。得られた粉末に平均粒径2
0μmのポリエチレンテレフタレート粉末を1.0,
2.0wt%添加し、総重量5kgの粉末を容量15l
の高速流動型混合機(6500RPM)で10分間混合
した。得られた粉末45gを外径20mmのペレット成
形用金型に充填し、放電プラズマ焼結装置にセットし
た。焼結条件は昇温速度80度/分,焼結温度(保持温
度)130℃、保持時間3分,冷却温度60℃/分、加
圧力650kgf/cm2,電流値1000A〜150
0Aとした。
(Example 9) As a raw material powder, a magnetic powder prepared by crushing an alloy containing Sm and Co as main components and prepared by a casting method was used. The magnetic powder is finally crushed with a vibrating ball mill to an average particle size of about 36 μm and then sieved to 90 μm.
Items over m were removed. The obtained powder has an average particle size of 2
1.0 μm of 0 μm polyethylene terephthalate powder,
2.0 wt% was added, and the total weight of the powder was 5 kg.
The mixture was mixed for 10 minutes using the high speed fluid mixer (6500 RPM). 45 g of the obtained powder was filled in a pellet molding die having an outer diameter of 20 mm and set in a discharge plasma sintering apparatus. The sintering conditions are a temperature rising rate of 80 degrees / minute, a sintering temperature (holding temperature) of 130 ° C., a holding time of 3 minutes, a cooling temperature of 60 ° C./minute, a pressing force of 650 kgf / cm 2, and a current value of 1000 A to 150.
It was set to 0A.

【0047】焼結後、外径20mm高さ約30mmの円
柱状の成形体を取り出し、高さ方向に5等分しアルキメ
デス法によりそれぞれの密度の測定を行った。尚、比較
の為に同形状のポリエチレンテレフタレートを結合剤と
した圧縮成形磁石を作製し同様の測定を行った(ポリエ
チレンテレフタレートは平均粒径20μm以下の粉末状
のもの使用し、添加量は1.0,2.0wt%とした,
また加熱は昇温速度50℃/分,保持温度130℃,成
形保持時間5分、冷却速度30℃/分,成形圧力は65
0kgf/cm2とした)。
After sintering, a cylindrical molded body having an outer diameter of 20 mm and a height of about 30 mm was taken out, divided into 5 equal parts in the height direction, and the respective densities were measured by the Archimedes method. For comparison, a compression-molded magnet having the same shape of polyethylene terephthalate as a binder was prepared and the same measurement was performed (polyethylene terephthalate was used in the form of powder having an average particle size of 20 μm or less, and the addition amount was 1. 0, 2.0 wt%,
The heating rate is 50 ° C./minute, the holding temperature is 130 ° C., the molding holding time is 5 minutes, the cooling rate is 30 ° C./minute, and the molding pressure is 65 minutes.
0 kgf / cm2).

【0048】結果を図10に示す。The results are shown in FIG.

【0049】図10から本発明により場所による密度差
の少ない均一な樹脂結合型磁石を得られることが分か
る。
It can be seen from FIG. 10 that the present invention can provide a uniform resin-bonded magnet having a small density difference depending on the location.

【0050】(実施例10)原料粉末としてSm、Co
を主成分とし鋳造法により作製された合金を粉砕し作製
した磁性粉末を用いた。磁性粉末は最終的に振動ボール
ミルで平均粒径約36μmに粉砕した後、ふるいで90
μm以上のものを取り除いた。得られた粉末に平均粒径
20μmのポリカーボネート粉末を1.0,2.0wt
%添加し、総重量5kgの粉末を容量15lの高速流動
型混合機(6500RPM)で10分間混合した。得ら
れた粉末45gを外径20mmのペレット成形用金型に
充填し、放電プラズマ焼結装置にセットした。焼結条件
は昇温速度80度/分,焼結温度(保持温度)180
℃、保持時間3分,冷却温度60℃/分、加圧力650
kgf/cm2,電流値1000A〜1500Aとし
た。
(Example 10) Sm and Co as raw material powders
A magnetic powder prepared by crushing an alloy containing as a main component and prepared by a casting method was used. The magnetic powder is finally crushed with a vibrating ball mill to an average particle size of about 36 μm and then sieved to 90
Those having a size of μm or more were removed. 1.0, 2.0 wt. Of polycarbonate powder having an average particle size of 20 μm is added to the obtained powder.
%, And the powder having a total weight of 5 kg was mixed for 10 minutes by a high-speed flow type mixer (6500 RPM) having a volume of 15 l. 45 g of the obtained powder was filled in a pellet molding die having an outer diameter of 20 mm and set in a discharge plasma sintering apparatus. The sintering conditions are a temperature rising rate of 80 degrees / minute and a sintering temperature (holding temperature) of 180.
℃, holding time 3 minutes, cooling temperature 60 ℃ / min, pressure 650
The kgf / cm2 and the current value were 1000A to 1500A.

【0051】焼結後、外径20mm高さ約30mmの円
柱状の成形体を取り出し、高さ方向に5等分しアルキメ
デス法によりそれぞれの密度の測定を行った。尚、比較
の為に同形状のポリカーボネートを結合剤とした圧縮成
形磁石を作製し同様の測定を行った(ポリカーボネート
は平均粒径20μm以下の粉末状のもの使用し、添加量
は1.0,2.0wt%とした,また加熱は昇温速度5
0℃/分, 保持温度180℃,成形保持時間5分、冷
却速度30℃/分,成形圧力は650kgf/cm2と
した)。
After sintering, a cylindrical molded body having an outer diameter of 20 mm and a height of about 30 mm was taken out, divided into 5 equal parts in the height direction, and the respective densities were measured by the Archimedes method. For comparison, a compression-molded magnet having a polycarbonate of the same shape as a binder was prepared and the same measurement was performed (the polycarbonate is a powder having an average particle size of 20 μm or less, and the addition amount is 1.0, 2.0 wt% and heating rate is 5
0 ° C./minute, holding temperature 180 ° C., molding holding time 5 minutes, cooling rate 30 ° C./minute, molding pressure 650 kgf / cm 2).

【0052】結果を図11に示す。The results are shown in FIG.

【0053】図12から本発明により場所による密度差
の少ない均一な樹脂結合型磁石を得られることが分か
る。
It can be seen from FIG. 12 that the present invention can provide a uniform resin-bonded magnet having a small density difference depending on the location.

【0054】(実施例11)原料粉末としてNd,F
e、B,Coを主成分とした急冷薄帯法による磁性粉末
を用いた。磁性粉末を振動ボールミルで平均粒径約36
μmに粉砕した後、ふるいで90μm以上のものを取り
除いた。得られた粉末に平均粒径20μmのナイロン6
を0.2wt%間隔で0.3〜12wt%の範囲で添加
し、総重量5kgの粉末を容量15lの高速流動型混合
機(6500RPM)で10分間混合した。得られた粉
末15gを外径20mmのペレット成形用金型に充填
し、放電プラズマ焼結装置にセットした。焼結条件は昇
温速度80度/分,焼結温度(保持温度)230℃、保
持時間3分,10分,冷却温度60℃/分、加圧力65
0kgf/cm2,電流値 1000A〜1500Aと
した。
(Example 11) Nd, F as raw material powder
A magnetic powder containing e, B, and Co as the main components by the quenching ribbon method was used. Magnetic powder with a vibrating ball mill has an average particle size of about 36
After pulverizing to a size of μm, the particles having a size of 90 μm or more were removed by a sieve. Nylon 6 with an average particle size of 20 μm was added to the obtained powder.
Was added at intervals of 0.2 wt% in the range of 0.3 to 12 wt%, and the powder having a total weight of 5 kg was mixed for 10 minutes by a high-speed flow type mixer (6500 RPM) having a volume of 15 l. 15 g of the obtained powder was filled in a pellet molding die having an outer diameter of 20 mm and set in a discharge plasma sintering apparatus. The sintering conditions are a heating rate of 80 degrees / minute, a sintering temperature (holding temperature) of 230 ° C., a holding time of 3 minutes and 10 minutes, a cooling temperature of 60 ° C./minute, and a pressing force of 65.
The current value was 0 kgf / cm2 and the current value was 1000A to 1500A.

【0055】焼結後、外径20mm高さ約10mmの円
柱状の成形体を取り出し、磁気性能測定を行った。尚、
比較の為に同形状のナイロン6を結合剤とした圧縮成形
磁石をホットプレスにより作製し同様の測定を行った
(ナイロン12は平均粒径20μm以下の粉末状のもの
使用し、添加量は1.0,2.0wt%とした,また加
熱は昇温速度50℃/分,保持温度230℃,成形保持
時間3分、10分,冷却速度30℃/分,成形圧力は6
50kgf/cm2とした)。
After sintering, a cylindrical molded body having an outer diameter of 20 mm and a height of about 10 mm was taken out, and its magnetic performance was measured. still,
For comparison, a compression-molded magnet having the same shape of nylon 6 as a binder was prepared by hot pressing and the same measurement was performed (nylon 12 was used in the form of powder having an average particle size of 20 μm or less, and the addition amount was 1 The heating rate was 50 ° C / minute, the holding temperature was 230 ° C, the molding holding time was 3 minutes and 10 minutes, the cooling rate was 30 ° C / minute, and the molding pressure was 6%.
50 kgf / cm2).

【0056】結果を図12に示す。The results are shown in FIG.

【0057】図12から本発明品はにおいて保持時間3
分で性能的に飽和状態となるが従来法では保持時間10
分にならないと本発明品に追いつかないことが分かる。
また性能的には保持時間3分の場合,ナイロン12の添
加量0.5〜10wt%の範囲では本発明品の方が優れ
ていることが分かる。
From FIG. 12, the product of the present invention has a retention time of 3
The performance is saturated in minutes, but the retention time is 10 in the conventional method.
It can be seen that the product of the present invention cannot be caught up unless it is understood.
In terms of performance, it can be seen that when the holding time is 3 minutes, the product of the present invention is superior when the amount of nylon 12 added is in the range of 0.5 to 10 wt%.

【0058】(実施例12)原料粉末としてNd,F
e、B,Coを主成分とした急冷薄帯法による磁性粉末
を用いた。磁性粉末を振動ボールミルで平均粒径約36
μmに粉砕した後、ふるいで90μm以上のものを取り
除いた。得られた粉末に平均粒径20μmのポリイミド
樹脂を0.2wt%間隔で0.3〜12wt%の範囲で
添加し、総重量5kgの粉末を容量15lの高速流動型
混合機(6500RPM)で10分間混合した。得られ
た粉末15gを外径20mmのペレット成形用金型に充
填し、放電プラズマ焼結装置にセットした。焼結条件は
昇温速度80度/分,焼結温度(保持温度)270℃、
保持時間5分,10分,冷却温度84℃/分、加圧力6
50kgf/cm2,電流値 1000A〜1500A
とした。
(Example 12) Nd, F as raw material powder
A magnetic powder containing e, B, and Co as the main components by the quenching ribbon method was used. Magnetic powder with a vibrating ball mill has an average particle size of about 36
After pulverizing to a size of μm, the particles having a size of 90 μm or more were removed by a sieve. Polyimide resin having an average particle size of 20 μm was added to the obtained powder at intervals of 0.2 wt% in the range of 0.3 to 12 wt%, and a total weight of 5 kg was added to a high-speed flow mixer (6500 RPM) having a volume of 15 l for 10 times. Mix for minutes. 15 g of the obtained powder was filled in a pellet molding die having an outer diameter of 20 mm and set in a discharge plasma sintering apparatus. The sintering conditions are a heating rate of 80 degrees / minute, a sintering temperature (holding temperature) of 270 ° C.,
Holding time 5 minutes, 10 minutes, cooling temperature 84 ° C / minute, pressure 6
50kgf / cm2, current value 1000A-1500A
And

【0059】焼結後、外径20mm高さ約10mmの円
柱状の成形体を取り出し、磁気性能測定を行った。尚、
比較の為に同形状のポリイミド樹脂を結合剤とした圧縮
成形磁石をホットプレスにより作製し同様の測定を行っ
た(ポリイミド樹脂は平均粒径20μm以下の粉末状の
もの使用し、添加量は0.3〜12wt%とした,また
加熱は昇温速度50℃/分,保持温度270℃,成形保
持時間5分、10分,冷却速度30℃/分,成形圧力は
650kgf/cm2とした)。
After sintering, a columnar molded body having an outer diameter of 20 mm and a height of about 10 mm was taken out and its magnetic performance was measured. still,
For comparison, a compression-molded magnet having a polyimide resin of the same shape as a binder was prepared by hot pressing and the same measurement was performed (the polyimide resin used was a powder having an average particle size of 20 μm or less, and the addition amount was 0). The heating rate was 50 ° C./minute, the holding temperature was 270 ° C., the molding holding time was 5 minutes and 10 minutes, the cooling rate was 30 ° C./minute, and the molding pressure was 650 kgf / cm 2.

【0060】結果を図13に示す。The results are shown in FIG.

【0061】図13から本発明品はにおいて保持時間5
分で性能的に飽和状態となるが従来法では保持時間10
分にならないと本発明品に追いつかないことが分かる。
また性能的には保持時間5分の場合,ポリイミド樹脂の
添加量0.5〜10wt%の範囲では本発明品の方が優
れていることが分かる。
From FIG. 13, the product of the present invention has a retention time of 5
The performance is saturated in minutes, but the retention time is 10 in the conventional method.
It can be seen that the product of the present invention cannot be caught up unless it is understood.
In terms of performance, it can be seen that when the holding time is 5 minutes, the product of the present invention is superior when the amount of polyimide resin added is in the range of 0.5 to 10 wt%.

【0062】(実施例13)原料粉末としてSm、Co
を主成分とし鋳造法により作製された合金を粉砕し作製
した磁性粉末を用いた。磁性粉末は最終的に振動ボール
ミルで平均粒径約36μmに粉砕した後、ふるいで90
μm以上のものを取り除いた。得られた粉末に平均粒径
20μmのエポキシ樹脂粉末を0.2wt%間隔で0.
3〜12wt%の範囲で添加し、総重量5kgの粉末を
容量15lの高速流動型混合機(6500RPM)で1
0分間混合した。得られた粉末15gを外径20mmの
ペレット成形用金型に充填し、放電プラズマ焼結装置に
セットした。焼結条件は昇温速度80度/分,焼結温度
(保持温度)230℃、保持時間3分,冷却温度84℃
/分、加圧力650kgf/cm2,電流値 1000
A〜1500Aとした。
Example 13 Sm and Co as raw material powders
A magnetic powder prepared by crushing an alloy containing as a main component and prepared by a casting method was used. The magnetic powder is finally crushed with a vibrating ball mill to an average particle size of about 36 μm and then sieved to 90
Those having a size of μm or more were removed. Epoxy resin powder having an average particle diameter of 20 μm was added to the obtained powder at 0.2 wt% intervals.
3 to 12 wt% is added, and the total weight of 5 kg of powder is 1 with a high-speed flow type mixer (6500 RPM) having a volume of 15 l.
Mix for 0 minutes. 15 g of the obtained powder was filled in a pellet molding die having an outer diameter of 20 mm and set in a discharge plasma sintering apparatus. The sintering conditions are a heating rate of 80 degrees / minute, a sintering temperature (holding temperature) of 230 ° C, a holding time of 3 minutes, and a cooling temperature of 84 ° C.
/ Min, pressing force 650 kgf / cm2, current value 1000
It was set to A to 1500A.

【0063】焼結後、外径20mm高さ約10mmの円
柱状の成形体を取り出し磁気性能測定を行った。尚、比
較の為に同形状のエポキシ樹脂を結合剤とした圧縮成形
磁石を作製し同様の測定を行った(エポキシ樹脂は平均
粒径20μm以下の粉末状のもの使用し、添加量は0.
3〜12wt%とした,成形圧力650kgf/cm2
で成形後、150℃で1時間焼成し樹脂を硬化させ
た)。
After sintering, a cylindrical molded body having an outer diameter of 20 mm and a height of about 10 mm was taken out and magnetic performance was measured. For comparison, a compression-molded magnet having an epoxy resin of the same shape as a binder was prepared and the same measurement was carried out (the epoxy resin used was a powder having an average particle size of 20 μm or less, and the addition amount was 0.
Molding pressure of 650 kgf / cm2, 3-12 wt%
After molding, the resin was baked by baking at 150 ° C. for 1 hour).

【0064】結果を図14に示す。The results are shown in FIG.

【0065】図14から本発明品の方が従来法に比べ性
能が高くなっているのが分かるが、エポキシ添加量0.
5〜12wt%の範囲においてはその差が明らかに認め
られる。
It can be seen from FIG. 14 that the product of the present invention has higher performance than the conventional method, but the amount of epoxy added is 0.
The difference is clearly recognized in the range of 5 to 12 wt%.

【0066】[0066]

【発明の効果】以上述べたように本発明による製造方法
を用いることにより密度バラツキの少ない均一な樹脂結
合型磁石が得られ、且つ従来2工程であった成形、焼成
が1工程で可能となるため製造に費やす時間が大幅に短
縮できる。
As described above, by using the manufacturing method according to the present invention, a uniform resin-bonded magnet with less density variation can be obtained, and molding and firing which were conventionally two steps can be performed in one step. Therefore, the time spent for manufacturing can be significantly reduced.

【図面の簡単な説明】[Brief description of drawings]

【図1】本発明の実施例における放電プラズマ焼結装置
の基本構成図である。
FIG. 1 is a basic configuration diagram of a spark plasma sintering apparatus in an example of the present invention.

【図2】本発明によるポリアミド樹脂を用いた圧縮成形
型磁石の場所による密度変化。
FIG. 2 is a density change depending on a location of a compression molding magnet using the polyamide resin according to the present invention.

【図3】本発明によるポリイミド樹脂を用いた圧縮成形
型磁石の場所による密度変化。
FIG. 3 is a density change depending on a location of a compression molding magnet using a polyimide resin according to the present invention.

【図4】本発明によるエポキシ樹脂を用いた圧縮成形型
磁石の場所による密度変化。
FIG. 4 is a density change depending on a place of a compression molding type magnet using an epoxy resin according to the present invention.

【図5】本発明によるポリエチレンを用いた圧縮成形型
磁石の場所による密度変化。
FIG. 5 shows the density change depending on the location of a compression molding magnet using polyethylene according to the present invention.

【図6】本発明によるポリフェニレンスルフィドを用い
た圧縮成形型磁石の場所による密度変化。
FIG. 6 shows the density change with time of the compression-molded magnet using the polyphenylene sulfide according to the present invention.

【図7】本発明によるABS樹脂を用いた圧縮成形型磁
石の場所による密度変化。
FIG. 7 is a density change depending on a location of a compression molding type magnet using the ABS resin according to the present invention.

【図8】本発明によるアミノ樹脂を用いた圧縮成形型磁
石の場所による密度変化。
FIG. 8 is a density change depending on a location of a compression molding magnet using an amino resin according to the present invention.

【図9】本発明によるフェノール樹脂を用いた圧縮成形
型磁石の場所による密度変化。
FIG. 9 is a density change depending on a location of a compression molding magnet using a phenol resin according to the present invention.

【図10】本発明によるポリエチレンテレフタレートを
用いた圧縮成形型磁石の場所による密度変化。
FIG. 10 shows the density change depending on the location of a compression molding magnet using polyethylene terephthalate according to the present invention.

【図11】本発明によるポリカーボネートを用いた圧縮
成形型磁石の場所による密度変化。
FIG. 11 is a density change depending on a location of a compression molding magnet using the polycarbonate according to the present invention.

【図12】本発明によるポリアミド樹脂を用いた圧縮成
形型磁石の樹脂量及び保持時間による磁気性能変化。
FIG. 12 is a graph showing changes in magnetic performance of a compression molding magnet using the polyamide resin according to the present invention depending on the resin amount and holding time.

【図13】本発明によるポリイミド樹脂を用いた圧縮成
形型磁石の樹脂量及び保持時間による磁気性能変化。
FIG. 13 shows changes in magnetic performance of a compression molding magnet using a polyimide resin according to the present invention depending on the resin amount and holding time.

【図14】本発明によるエポキシ樹脂を用いた圧縮成形
型磁石の樹脂量及び保持時間による磁気性能変化。
FIG. 14 is a graph showing changes in magnetic performance of a compression-molded magnet using an epoxy resin according to the present invention depending on the resin amount and holding time.

【符号の説明】[Explanation of symbols]

1 上電極 2 下電極 3 上パンチ 4 下パンチ 5 型 6 粉末 7 熱電対 8 電源 1 Upper electrode 2 Lower electrode 3 Upper punch 4 Lower punch 5 Type 6 Powder 7 Thermocouple 8 Power supply

Claims (15)

【特許請求の範囲】[Claims] 【請求項1】 樹脂結合型磁石の製造方法において、磁
性粉末に熱可塑性樹脂または熱硬化性樹脂を添加し、放
電プラズマ焼結法を用いて製造することを特徴とする樹
脂結合型磁石の製造方法。
1. A method of manufacturing a resin-bonded magnet, comprising adding a thermoplastic resin or a thermosetting resin to magnetic powder and manufacturing the resin-bonded magnet by a discharge plasma sintering method. Method.
【請求項2】 樹脂結合型磁石の製造方法において、磁
性粉末にポリアミド樹脂を添加し、放電プラズマ焼結法
を用いて製造することを特徴とする請求項1記載の樹脂
結合型磁石の製造方法。
2. The method for producing a resin-bonded magnet according to claim 1, wherein the resin powder is produced by adding a polyamide resin to the magnetic powder and using a spark plasma sintering method. .
【請求項3】 樹脂結合型磁石の製造方法において、磁
性粉末にポリイミド樹脂を添加し、放電プラズマ焼結法
を用いて製造することを特徴とする請求項1記載の樹脂
結合型磁石の製造方法。
3. The method for producing a resin-bonded magnet according to claim 1, wherein the resin powder is produced by adding a polyimide resin to the magnetic powder and using a discharge plasma sintering method. .
【請求項4】 樹脂結合型磁石の製造方法において、磁
性粉末にエポキシ樹脂を添加し、放電プラズマ焼結法を
用いて製造することを特徴とする請求項1記載の樹脂結
合型磁石の製造方法。
4. The method for producing a resin-bonded magnet according to claim 1, wherein an epoxy resin is added to the magnetic powder and the resin-bonded magnet is produced by a spark plasma sintering method. .
【請求項5】 樹脂結合型磁石の製造方法において、磁
性粉末にポリエチレンを添加し、放電プラズマ焼結法を
用いて製造することを特徴とする請求項1記載の樹脂結
合型磁石の製造方法。
5. The method for producing a resin-bonded magnet according to claim 1, wherein polyethylene is added to the magnetic powder and the resin-bonded magnet is produced by a discharge plasma sintering method.
【請求項6】 樹脂結合型磁石の製造方法において、磁
性粉末にポリフェニレンスルフィドを添加し、放電プラ
ズマ焼結法を用いて製造することを特徴とする請求項1
記載の樹脂結合型磁石の製造方法。
6. The method for producing a resin-bonded magnet according to claim 1, wherein polyphenylene sulfide is added to the magnetic powder and the magnet is produced by a spark plasma sintering method.
A method for producing the resin-bonded magnet described.
【請求項7】 樹脂結合型磁石の製造方法において、磁
性粉末にABS樹脂を添加し、放電プラズマ焼結法を用
いて製造することを特徴とする請求項1記載の樹脂結合
型磁石の製造方法。
7. The method for producing a resin-bonded magnet according to claim 1, wherein ABS resin is added to the magnetic powder and the resin-bonded magnet is produced by a spark plasma sintering method. .
【請求項8】 樹脂結合型磁石の製造方法において、磁
性粉末にアミノ樹脂を添加し、放電プラズマ焼結法を用
いて製造することを特徴とする請求項1記載の樹脂結合
型磁石の製造方法。
8. The method for producing a resin-bonded magnet according to claim 1, wherein the resin powder is produced by adding an amino resin to the magnetic powder and using a discharge plasma sintering method. .
【請求項9】 樹脂結合型磁石の製造方法において、磁
性粉末にフェノール樹脂を添加し、放電プラズマ焼結法
を用いて製造することを特徴とする請求項1記載の樹脂
結合型磁石の製造方法。
9. The method for producing a resin-bonded magnet according to claim 1, wherein phenol resin is added to the magnetic powder and the resin-bonded magnet is produced by a discharge plasma sintering method. .
【請求項10】 樹脂結合型磁石の製造方法において、
磁性粉末にポリエチレンテレフタレートを添加し、放電
プラズマ焼結法を用いて製造することを特徴とする請求
項1記載の樹脂結合型磁石の製造方法。
10. A method of manufacturing a resin-bonded magnet, comprising:
The method for producing a resin-bonded magnet according to claim 1, wherein polyethylene terephthalate is added to the magnetic powder and the magnetic powder is produced by a discharge plasma sintering method.
【請求項11】 樹脂結合型磁石の製造方法において、
磁性粉末にポリカーボネートを添加し、放電プラズマ焼
結法を用いて製造することを特徴とする請求項1記載の
樹脂結合型磁石の製造方法。
11. A method of manufacturing a resin-bonded magnet, comprising:
2. The method for producing a resin-bonded magnet according to claim 1, wherein polycarbonate is added to the magnetic powder and the magnetic powder is produced by a discharge plasma sintering method.
【請求項12】 樹脂結合型磁石の製造方法において、
磁性粉末にポリアミド樹脂を0.5〜10wt%添加
し、放電プラズマ焼結法を用いて製造したことを特徴と
する請求項2記載の樹脂結合型磁石の製造方法。
12. A method for manufacturing a resin-bonded magnet, comprising:
The method for producing a resin-bonded magnet according to claim 2, wherein 0.5 to 10 wt% of polyamide resin is added to the magnetic powder and the magnetic powder is produced by a discharge plasma sintering method.
【請求項13】 樹脂結合型磁石の製造方法において、
磁性粉末にポリイミド樹脂を0.5〜10wt%添加
し、放電プラズマ焼結法を用いて製造したことを特徴と
する請求項3記載の樹脂結合型磁石の製造方法。
13. A method of manufacturing a resin-bonded magnet, comprising:
The method for producing a resin-bonded magnet according to claim 3, wherein 0.5 to 10 wt% of a polyimide resin is added to the magnetic powder and the magnetic powder is produced by a discharge plasma sintering method.
【請求項14】 樹脂結合型磁石の製造方法において、
磁性粉末にエポキシ樹脂を0.5〜10wt%添加し、
放電プラズマ焼結法を用いて製造したことを特徴とする
請求項4記載の樹脂結合型磁石の製造方法。
14. A method of manufacturing a resin-bonded magnet, comprising:
Add 0.5 to 10 wt% of epoxy resin to magnetic powder,
The method of manufacturing a resin-bonded magnet according to claim 4, wherein the resin-bonded magnet is manufactured by using a discharge plasma sintering method.
【請求項15】 樹脂結合型磁石において、請求項1乃
至14のいずれかに記載された放電プラズマ焼結法を用
いて製造したことを特徴とする樹脂結合型磁石。
15. A resin-bonded magnet manufactured by using the spark plasma sintering method according to claim 1 in a resin-bonded magnet.
JP7069685A 1995-03-28 1995-03-28 Resin-bonded magnet manufacturing method and resin-bonded magnet Pending JPH08264360A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP7069685A JPH08264360A (en) 1995-03-28 1995-03-28 Resin-bonded magnet manufacturing method and resin-bonded magnet

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP7069685A JPH08264360A (en) 1995-03-28 1995-03-28 Resin-bonded magnet manufacturing method and resin-bonded magnet

Publications (1)

Publication Number Publication Date
JPH08264360A true JPH08264360A (en) 1996-10-11

Family

ID=13409980

Family Applications (1)

Application Number Title Priority Date Filing Date
JP7069685A Pending JPH08264360A (en) 1995-03-28 1995-03-28 Resin-bonded magnet manufacturing method and resin-bonded magnet

Country Status (1)

Country Link
JP (1) JPH08264360A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004146542A (en) * 2002-10-23 2004-05-20 Asahi Kasei Chemicals Corp Solid material for magnet and method for producing the same
JP2019536909A (en) * 2016-11-18 2019-12-19 アルケマ フランス Sinterable magnetic powder composition and three-dimensional article made by sintering this composition
CN116278023A (en) * 2023-02-14 2023-06-23 清华大学 A kind of self-lubricating sliding bearing and its preparation method

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004146542A (en) * 2002-10-23 2004-05-20 Asahi Kasei Chemicals Corp Solid material for magnet and method for producing the same
JP2019536909A (en) * 2016-11-18 2019-12-19 アルケマ フランス Sinterable magnetic powder composition and three-dimensional article made by sintering this composition
CN116278023A (en) * 2023-02-14 2023-06-23 清华大学 A kind of self-lubricating sliding bearing and its preparation method

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