JPH0639643B2 - Method for producing magnetic composite material of A1 or A1 alloy - Google Patents
Method for producing magnetic composite material of A1 or A1 alloyInfo
- Publication number
- JPH0639643B2 JPH0639643B2 JP9020087A JP9020087A JPH0639643B2 JP H0639643 B2 JPH0639643 B2 JP H0639643B2 JP 9020087 A JP9020087 A JP 9020087A JP 9020087 A JP9020087 A JP 9020087A JP H0639643 B2 JPH0639643 B2 JP H0639643B2
- Authority
- JP
- Japan
- Prior art keywords
- magnetic
- ferromagnetic material
- composite material
- alloy
- molten metal
- 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.)
- Expired - Lifetime
Links
- 230000005291 magnetic effect Effects 0.000 title claims abstract description 108
- 239000002131 composite material Substances 0.000 title claims abstract description 77
- 238000004519 manufacturing process Methods 0.000 title claims description 35
- 229910045601 alloy Inorganic materials 0.000 title claims description 22
- 239000000956 alloy Substances 0.000 title claims description 22
- 239000003302 ferromagnetic material Substances 0.000 claims abstract description 84
- 239000002184 metal Substances 0.000 claims abstract description 61
- 229910052751 metal Inorganic materials 0.000 claims abstract description 61
- 239000000843 powder Substances 0.000 claims abstract description 17
- 229910000640 Fe alloy Inorganic materials 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 abstract description 18
- 229910052742 iron Inorganic materials 0.000 abstract description 13
- 230000003647 oxidation Effects 0.000 abstract description 8
- 238000007254 oxidation reaction Methods 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 7
- 229910000838 Al alloy Inorganic materials 0.000 abstract description 6
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 230000035699 permeability Effects 0.000 abstract description 4
- 229910052782 aluminium Inorganic materials 0.000 abstract description 2
- 238000003825 pressing Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract 1
- 238000000034 method Methods 0.000 description 44
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 36
- 238000005470 impregnation Methods 0.000 description 33
- 238000006243 chemical reaction Methods 0.000 description 15
- 229910000765 intermetallic Inorganic materials 0.000 description 14
- 230000008569 process Effects 0.000 description 11
- 238000002844 melting Methods 0.000 description 10
- 230000008018 melting Effects 0.000 description 10
- 238000004663 powder metallurgy Methods 0.000 description 9
- 238000007796 conventional method Methods 0.000 description 8
- 239000002775 capsule Substances 0.000 description 7
- 238000010406 interfacial reaction Methods 0.000 description 7
- 239000000696 magnetic material Substances 0.000 description 7
- 230000005294 ferromagnetic effect Effects 0.000 description 6
- 230000004888 barrier function Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 230000004907 flux Effects 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
- 230000002829 reductive effect Effects 0.000 description 5
- 239000012783 reinforcing fiber Substances 0.000 description 5
- 238000007711 solidification Methods 0.000 description 5
- 230000008023 solidification Effects 0.000 description 5
- 229920000049 Carbon (fiber) Polymers 0.000 description 4
- 239000004917 carbon fiber Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000007906 compression Methods 0.000 description 3
- 230000006835 compression Effects 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 230000002401 inhibitory effect Effects 0.000 description 3
- 230000005389 magnetism Effects 0.000 description 3
- 230000036961 partial effect Effects 0.000 description 3
- 230000000717 retained effect Effects 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 229910001209 Low-carbon steel Inorganic materials 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000000536 complexating effect Effects 0.000 description 2
- 238000000748 compression moulding Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 230000009918 complex formation Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000000779 depleting effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000003562 lightweight material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000012768 molten material Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 102200029231 rs11551768 Human genes 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000003832 thermite Substances 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
Landscapes
- Soft Magnetic Materials (AREA)
- Manufacture Of Alloys Or Alloy Compounds (AREA)
Abstract
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は磁気特性、特に初期透磁率の優れる、A▲l▼
またはA▲l▼合金の磁性複合材料の製造に関するもの
である。DETAILED DESCRIPTION OF THE INVENTION [Industrial field of application] The present invention has excellent magnetic properties, particularly excellent initial magnetic permeability.
Alternatively, it relates to the production of a magnetic composite material of A1 alloy.
A▲l▼またはA▲l▼合金(以下「A▲l▼」と略記
する。)は軽量である利点の他に電気伝導性,熱伝導
性,耐蝕性および加工性に優れ、かつ合金化にて強度面
の改善もなされていることにより、近来、特に軽量化・
小型化が急速に進められている電気製品の分野にて鉄鋼
に代替して多用されている。A-1 or A-1 alloy (hereinafter abbreviated as "A-1") is excellent in electrical conductivity, thermal conductivity, corrosion resistance, and workability in addition to being lightweight, and is alloyed. In addition, the strength has been improved in recent years, resulting in particularly lighter weight.
It is widely used as a substitute for steel in the field of electrical products, where miniaturization is proceeding rapidly.
反面「A▲l▼」は非磁性体であつて、モータ類等の磁
性を利用する部品には適用し得ず、これら部品には、強
磁性体のFeまたはFe合金が使用されるのが通常であ
る。On the other hand, "A-1" is a non-magnetic material and cannot be applied to magnetic parts such as motors. For these parts, ferromagnetic Fe or Fe alloy is used. It is normal.
しかし、電気製品の分野においてはこれら磁性部品に関
してもその軽量化が強く望まれており、軽量でかつ磁性
を有す材料が必要とされている。However, in the field of electric products, it is strongly desired to reduce the weight of these magnetic components as well, and a lightweight and magnetic material is required.
こうした要請に対応すべく、「A▲l▼」の特性を保持
しつつ更に磁性を付与した磁性複合材料の開発が進めら
れ、その製造方法についても種々の具体的な提案がなさ
れている。In order to meet such a demand, development of a magnetic composite material having the property of “A (1)” and further magnetism is advanced, and various specific proposals have been made regarding the manufacturing method thereof.
これら「A▲l▼」磁性複合材料の製造方法としては、
大別粉末冶金法によるもの、および溶湯含浸法によ
るものがあつて、粉末冶金法による磁性A▲l▼合金
の製造方法としては、例えば、特開昭57−51231
号公報に開示されたものがある。As a method of manufacturing these "A1" magnetic composite materials,
There are two types, one is a powdered metallurgy method and the other is a molten metal impregnation method. As a method for producing a magnetic Al alloy by a powder metallurgy method, for example, Japanese Patent Application Laid-Open No. 57-51231.
There is one disclosed in the publication.
この従来技術に係る磁性複合材料の製造方法は、「A▲
l▼」の粉末または切粉と、強磁性の金属もしくは合金
の粉末または切粉とを、重量比で20:1〜1:1の割
合で混合し、圧縮成形した後、「A▲l▼」の融点以下
の温度で焼結する、いわゆる粉末冶金法によるもので、
必要に応じて焼結後、前記融点以下の温度にて鍛造,押
出し等の熱間成形加工が加えられるものである。The method of manufacturing a magnetic composite material according to this conventional technique is described in "A ▲
1) powder or cutting powder and ferromagnetic metal or alloy powder or cutting powder are mixed in a weight ratio of 20: 1 to 1: 1 and compression-molded. "Sintering at a temperature equal to or lower than the melting point of" by the so-called powder metallurgy method
If necessary, after sintering, hot forming such as forging and extrusion is added at a temperature of the melting point or lower.
この従来技術は、上記の粉末冶金法にて「A▲l▼中に
鉄粉,低炭鋼切粉等の強磁性材料を混合含有させて、両
者の特性を併せ持つ「A▲l▼」磁性複合材料を製造す
るものである。This prior art is based on the above-mentioned powder metallurgy method, in which "A (1)" magnetism is obtained by mixing and containing "A (1)" with a ferromagnetic material such as iron powder and low carbon steel cutting chips. A composite material is manufactured.
また、溶湯含浸法による「A▲l▼」磁性複合材料の
製造方法としては、例えば、特開昭60−103141
号公報に開示されたものがある。Further, as a method for producing the "A-1" magnetic composite material by the molten metal impregnation method, for example, Japanese Patent Application Laid-Open No. 60-103141
There is one disclosed in the publication.
この従来技術に係るA▲l▼複合材料の製造方法は、A
▲l▼合金と、該A▲l▼合金の融点よりも高い融点を
もつ繊維状または粒子状の補強材(Fe,Ni,Co等の強磁性
金属のウイスカー)にて形成された体積率5〜70%の
予備成形体とを、前記A▲l▼合金よりも高い融点を有
す金属カプセル内に充填し、該カプセル内を真空密封し
た後、加熱してカプセル内のA▲l▼合金を溶融させる
と共に、カプセルを圧力媒体を介して等方圧的に加圧し
て、カプセルを塑性変形させつつ、その内の溶融A▲l
▼合金を予備成形体内に含浸させる、いわゆる溶湯含浸
法にてA▲l▼合金と強磁性金属とを複合体化するもの
である。The manufacturing method of the A1 composite material according to this conventional technique is as follows.
A volume ratio of 5 formed by an alloy (1) and a fibrous or particulate reinforcing material (whisker of a ferromagnetic metal such as Fe, Ni, Co) having a melting point higher than that of the alloy A (1). ~ 70% of the preform is filled in a metal capsule having a melting point higher than that of the Al alloy, the capsule is vacuum-sealed, and then heated to heat the Al alloy in the capsule. Is melted, and the capsule is isotropically pressurized via a pressure medium to plastically deform the capsule, while melting the inside of the capsule.
(3) The alloy (1) is made into a composite with a ferromagnetic metal by a so-called molten metal impregnation method in which a preformed body is impregnated with the alloy.
なお、上記A▲l▼合金の溶湯含浸に際しては、通常、
1000〜2000気圧の含浸圧力が採用され、また、
その処理時間は15〜60分程度とされている。When the molten metal of the Al alloy is used,
An impregnation pressure of 1000-2000 atmospheres is adopted, and
The processing time is about 15 to 60 minutes.
この従来技術は、上記溶湯含浸法にて強磁性金属からな
る予備成形体内にA▲l▼合金の溶湯を圧入含浸させ、
真密度が高く、かつ機械的性質の優れるA▲l▼複合材
料を製造するものである。In this conventional technique, a molten metal of A1 alloy is press-fitted and impregnated into a preformed body made of a ferromagnetic metal by the molten metal impregnation method.
It is intended to produce an Al composite material having high true density and excellent mechanical properties.
そしてまた、A▲l▼溶湯を加圧鋳造してA▲l▼複合
材料を製造する、いわゆる溶湯含浸法にてA▲l▼複
合材料を製造する方法としては、例えば、特公報60−
25222号に開示されたものがある。Further, as a method for producing an A (l) composite material by so-called melt impregnation method for producing an A (l) composite material by pressure casting an A (l) melt, for example, Japanese Patent Application Laid-Open No. 60-
There is one disclosed in No. 25222.
この従来技術に係る複合材料の製造方法は、カーボンフ
ァイバー等の強化用繊維からなる予備成形体を配置した
金型内に、A▲l▼およびMg等の母相金属溶湯を注入
し、該溶湯を加圧して前記予備成形体に圧入含浸させ
る、いわゆる溶湯含浸法によるものであつて、溶湯加圧
について、加圧開始時から第1所定時間内にて第1所定
圧に急激に印加した後、直ちに第1所定圧より低い第2
所定圧に低下させて第2所定時間保持するものである。The method for producing a composite material according to this conventional technique is to inject a molten metal of a parent phase metal such as A (1) and Mg into a mold in which a preformed body made of reinforcing fibers such as carbon fibers is placed, By pressurizing and impregnating into the preform by so-called molten metal impregnation method, in which molten metal pressure is rapidly applied to a first predetermined pressure within a first predetermined time from the start of pressurization. , Immediately the second lower than the first predetermined pressure
The pressure is reduced to a predetermined pressure and is maintained for a second predetermined time.
この従来技術は、上記溶湯含浸法にて、A▲l▼溶湯の
浸透性が低い強化繊維からなる予備成形体についても比
較的に低い圧力にて、A▲l▼溶湯を均一に浸透させ得
るものであつて、A▲l▼とカーボンファイバー等の強
化用繊維とを強固に結合でき、機材的性質の優れる複合
材料、すなわちA▲l▼複合材料を製造するものであ
る。According to this prior art, the molten metal impregnation method allows the molten metal A to be uniformly permeated with a relatively low pressure even for a preform made of reinforcing fibers having a low molten metal permeability. It is intended to produce a composite material having excellent mechanical properties, that is, A1 composite material, in which A1 and reinforcing fibers such as carbon fibers can be firmly bonded.
なお、この従来方法にしたがい、カーボンファイバーか
らなる体積率18%の予備成形体にA▲l▼溶湯を圧入
含浸するについて、前記の第1所定圧を1000〜20
00kg/cm2,第1所定時間を1秒以内,第2所定圧を7
50kg/cm2,第2所定時間を60秒とする溶湯加圧条件
にて良好なるA▲l▼溶湯の含浸結果が得られるとされ
ている。In addition, according to this conventional method, when the preformed body made of carbon fiber and having a volume ratio of 18% was press-impregnated with the molten metal A, the first predetermined pressure was set to 1000 to 20.
00kg / cm 2 , 1st predetermined time within 1 second, 2nd predetermined pressure 7
It is said that good results of impregnation of the molten metal A can be obtained under the molten metal pressurization condition of 50 kg / cm 2 and the second predetermined time of 60 seconds.
「A▲l▼」磁性複合材料の製造においては、その内に
添加・含有される強磁性材料が本来有する磁気特性を十
分発揮し得るようにして、「A▲l▼」と複合体化させ
る必要があるが、そのためには、その複合体化の過程に
て、強磁性材料に歪を付加もしくは残留させないこ
と、および強磁性材料を「A▲l▼」との熱による反
応を抑制することが要点となる。In the production of the "A-1" magnetic composite material, the ferromagnetic material added / contained in the "A-1" is allowed to sufficiently exhibit the inherent magnetic properties, and is compounded with the "A-1". For that purpose, in order to do so, in the process of forming the composite, strain should not be added to or left in the ferromagnetic material, and the reaction of the ferromagnetic material with "A ▲" should be suppressed. Is the point.
これは、強磁性材料の内部に歪があると、この歪が磁
場を印加した際の磁壁の移動を阻害するがため強磁性体
内の磁化率を低下させる、すなわち、磁性複合材料の製
造過程における成形応力にて、その内に添加された強磁
性材料に歪を付加・残留させたとき、この歪が磁性複合
材料の磁化率、特に初期透磁率を低下させるからであ
る。This is because, if there is strain inside the ferromagnetic material, this strain hinders the movement of the domain wall when a magnetic field is applied, and thus reduces the magnetic susceptibility in the ferromagnetic body, that is, in the manufacturing process of the magnetic composite material. This is because when a strain is added to and retained in the ferromagnetic material added therein by the molding stress, the strain lowers the magnetic susceptibility of the magnetic composite material, particularly the initial magnetic permeability.
そして、強磁性材料(FeまたはFe合金)と「A▲
l▼」(A▲l▼またはA▲l▼合金)との界面におけ
る熱による拡散・反応があると、この反応により脆くて
非磁性の金属間化合物(A▲l▼3・Fe等)が生成され
る。すなわち、磁性複合材料の製造過程において加えら
れた熱にて、その内の強磁性材料と「A▲l▼」間に非
磁性の金属間化合物を生成させたとき、強磁性材料が磁
性体としての有効体積を減じ、「A▲l▼」磁性複合材
料はその減損分について単に重量を増すのみで磁気特性
の向上が得られないからである。Then, the ferromagnetic material (Fe or Fe alloy) and “A ▲
When there is thermal diffusion / reaction at the interface with "l ▼" (A ▲ l ▼ or A ▲ l ▼ alloy), brittle and non-magnetic intermetallic compounds (A ▲ l ▼ 3 , Fe, etc.) are generated by this reaction. Is generated. That is, when a non-magnetic intermetallic compound is generated between the ferromagnetic material therein and "A" by the heat applied in the manufacturing process of the magnetic composite material, the ferromagnetic material serves as a magnetic body. This is because the effective volume is reduced, and the magnetic composite material of "A1" is simply increased in weight for the loss, but the magnetic characteristics cannot be improved.
しかし、前述の従来技術に係る磁性複合材料およびA▲
l▼複合材料の製造方法について、上記の観点より検討
したところ、これらは、その内に添加された強磁性材料
がその本来の磁気特性を十分に発揮し得ないものである
ことが判明した。However, the above-mentioned magnetic composite material and A
From the above viewpoints, it was found that the ferromagnetic material added therein cannot sufficiently exhibit its original magnetic characteristics.
すなわち、前述の粉末冶金法による従来技術(特開昭
57−51231号の提案)においては、「A▲l▼」
磁性複合材料は圧縮成形・焼結、およびその後の熱間成
形加工の温度を「A▲l▼」の融点(約480〜650℃)以
下とされてあり、これら比較的に低温なる温度域にて固
化成形ないしは熱間成形加工された「A▲l▼」磁性複
合材料内の強磁性材料は、その成形過程にて付加された
歪を開放し得ず、必然的に、内部に残留させたものとな
る。That is, in the prior art by the above-mentioned powder metallurgy method (proposal of Japanese Patent Laid-Open No. 57-51231), "A.ltoreq."
The temperature of compression molding / sintering and the subsequent hot forming process of the magnetic composite material is set to the melting point of "A1" (about 480 to 650 ° C) or less, and the temperature range is relatively low. The ferromagnetic material in the "A-1" magnetic composite material which has been solidified and hot-molded cannot necessarily release the strain applied during the molding process, and inevitably remains inside. Will be things.
例えば、純A▲l▼粉末と純Fe粉末との混合物を約A
▲l▼の融点(約660℃)以下の600℃にて圧縮固
化するについて、これら粉体間の結合一体化を確実なも
のとするには5000〜8000kg/cm2程度の圧力を加
えることを要すものであつて、この圧力にて純Fe粉末
に加えられる応力は、600℃の温度における純Fの降
伏応力(約3kg/mm2=300kg/cm2)を大巾に超えるもの
で、この圧縮固化過程で加えられた応力にて純Fe内部
に歪が付加され、また、この歪は600℃程度の温度に
ては短時間で開放・除去し得ないものである。For example, a mixture of pure Al powder and pure Fe powder may be mixed with about A
Regarding compression and solidification at 600 ° C, which is lower than the melting point (about 660 ° C) of (1), it is necessary to apply a pressure of about 5000 to 8000 kg / cm 2 in order to ensure the bonding and integration of these powders. The stress applied to pure Fe powder at this pressure greatly exceeds the yield stress of pure F (about 3 kg / mm 2 = 300 kg / cm 2 ) at a temperature of 600 ° C. Strain is added to the inside of pure Fe by the stress applied in the compression solidification process, and this strain cannot be released and removed in a short time at a temperature of about 600 ° C.
従って、これら粉末冶金法による「A▲l▼」磁性複合
材料は、その製造過程の加熱温度が比較的に低温であつ
て、金属間化合物(A▲l▼3・Fe)の生成を抑制する
面では有効なるものであつても、その内に添加された磁
性材料内部に成形過程における応力にて付加された歪が
残留するもので、添加された強磁性材料の量より期待さ
れる磁気特性が得られないものである。Therefore, "A ▲ l ▼" magnetic composite materials of these powder metallurgy, shall apply in a relatively low temperature heating temperature of the manufacturing process, inhibiting the formation of intermetallic compounds (A ▲ l ▼ 3 · Fe ) Even if it is effective in terms of surface, the strain added by the stress in the molding process remains inside the magnetic material added inside it, and the magnetic characteristics expected from the amount of added ferromagnetic material Is something that cannot be obtained.
例えば、純鉄は100エルステツド(Oe)の低磁場内にお
いて、約2万ガウス(G)の磁束密度を示すものであつ
て、この純鉄を純A▲l▼中に体積率にて30%混合添
付してなる磁性複合材料は、混合則に従うと仮定して計
算すると、上記の磁場内において約6千ガウス(G)の磁
束密度を示すことが期待される。For example, pure iron has a magnetic flux density of about 20,000 gauss (G) in a low magnetic field of 100 oersteds (Oe), and this pure iron is 30% in volume ratio in pure A (l). It is expected that the magnetic composite material with the mixed attachment will show a magnetic flux density of about 6,000 gauss (G) in the above magnetic field, when calculated assuming that the mixed rule is obeyed.
しかしながら、例えば、純A▲l▼粉末中に純鉄を体積
率で30%添加した混合物を、600℃,7000気圧
(相当する変形応力≒70kg/mm2)にて熱間圧縮成形した
磁性複合材料は、100エルステツド(Oe)の磁場内にお
ける磁束密度が3500ガウス(G)と、期待値に対し大
巾に低い値を示した。However, for example, a magnetic composite obtained by hot compression molding a mixture obtained by adding pure iron 30% by volume in pure Al powder at 600 ° C. and 7,000 atm (corresponding deformation stress ≈ 70 kg / mm 2 ). The material had a magnetic flux density of 3500 gauss (G) in a magnetic field of 100 Oersted (Oe), which was much lower than the expected value.
なお、上記従来技術による「A▲l▼」磁性複合材料内
の強磁性材料内部の歪は、それぞれ成形完了後におい
て、適切な温度・時間の焼鈍を加えることで除去可能な
るものであるが、しかし、この焼鈍温度は磁性複合材料
の形態を維持するため、該磁性複合材料内の「A▲l
▼」のメルトダウン温度、すなわち「A▲l▼」の融点
以下の温度しか適用し得ず、また、この比較的に低温
(約450〜650℃)なる温度にて強磁性体内部の歪を除去
するにはその所要時間が実用上適用し難い長時間なもの
となる。Although the strain inside the ferromagnetic material in the "A-1" magnetic composite material according to the above-mentioned conventional technique can be removed by applying annealing at an appropriate temperature and time after completion of molding, respectively. However, since this annealing temperature maintains the morphology of the magnetic composite material, “A ▲ l” in the magnetic composite material is maintained.
Only the melt-down temperature of "▼", that is, the temperature below the melting point of "A ▲ l", can be applied, and strain at the relatively low temperature (about 450 to 650 ° C) can reduce strain inside the ferromagnetic material. In order to remove it, the required time becomes a long time which is practically difficult to apply.
一方、前述の溶湯含浸法による従来技術(特開昭60
−103141号の提案)においては、「A▲l▼」は
強磁性材料の予備成形体と共にカプセル内に充填された
状態にて加熱溶融され、しかる後、該カプセルの圧縮変
形に伴い予備成形体内に圧入含浸されるもので、その加
熱溶融,圧入含浸の過程において溶湯である「A▲l
▼」と強磁性材料との界面にて、必然的に反応が起り、
金属間化合物(A▲l▼3・Fe)が生成される。しか
も、「A▲l▼」の加熱溶融のための昇温過程において
も強磁性材料と混在するこの従来技術においては、「A
▲l▼」と強磁性材料(FeまたはFe合金)との界面
における反応(ある時間を与えた場合550℃より認め
られるA▲l▼とFeとの反応)時間を比較的に長く与
えるもので、金属間化合物の生成を助長して、その内に
添加された強磁性材料が磁性体としての有効体積を大き
く減損するものである。On the other hand, the prior art by the above-mentioned molten metal impregnation method (JP-A-60
-103141), "A (1)" is heated and melted in a state where it is filled in a capsule together with a preform of a ferromagnetic material, and thereafter, the preform is compressed and deformed with the preform. It is impregnated into the molten steel and is melted in the process of heat melting and pressure impregnation.
Inevitably a reaction occurs at the interface between the ▼ ”and the ferromagnetic material,
Intermetallic compound (A ▲ l ▼ 3 · Fe ) is generated. In addition, in this conventional technique in which the ferromagnetic material is mixed even in the temperature rising process for heating and melting of "A1", "A
(1) ”and the ferromagnetic material (Fe or Fe alloy) at the interface (reaction between A (1) and Fe observed at 550 ° C. when a certain time is given) gives a relatively long time. The production of intermetallic compounds is promoted, and the ferromagnetic material added therein greatly reduces the effective volume as a magnetic material.
また、前述後者の溶湯含浸法による従来技術(特公昭
60−25222号の提案)においては、カーボンフア
イバー等の強化繊維体にA▲l▼を含浸させて複合体化
するものとされてあり、この複合体化にて母相金属なる
A▲l▼の強化、すなわち機械的特性の改善について言
及されているものの、A▲l▼と強磁性材料との複合化
か、複合体化による強磁性材料の磁気特性への影響等に
ついては一切言及ないしは示唆されていない。Further, in the prior art by the latter molten metal impregnation method (proposal of Japanese Patent Publication No. 60-25222), it is said that a reinforcing fiber body such as a carbon fiber is impregnated with A (1) to form a composite, Although it is mentioned that strengthening A1 as a parent phase metal by this complexing, that is, improving mechanical properties, it is a composite of A1 and a ferromagnetic material, or a ferromagnetic material by complexing. There is no mention or suggestion of any influence on the magnetic properties of the material.
そしてまた、この従来技術にしたがい、強化繊維を強磁
性材料に代替して、「A▲l▼」と強磁性材料(Feま
たはFe合金)の複合体なる磁性複合材料を製造せんと
するとき、含浸圧力は粉末冶金法による固化成形圧力
より比較的に低く、強磁性材料内部に付加もしくは残留
させる歪の面では格段に有利であるとはいえ、また、そ
の含浸・固化時間は比較的に短時間なるとはいえ、溶湯
含浸・凝固の過程におけるA▲l▼とFeとの反応、す
なわち金属間化合物(A▲l▼2・Fe)の生成は避け難
く、強磁性材料は「A▲l▼」との複合体化の過程にて
磁性体としての有効体積を減損する。Further, according to this conventional technique, when the reinforcing fiber is replaced with a ferromagnetic material to produce a magnetic composite material that is a composite of "A1" and a ferromagnetic material (Fe or Fe alloy), The impregnation pressure is comparatively lower than the solidification molding pressure by the powder metallurgy method, and although it is significantly advantageous in terms of strain to be added or retained inside the ferromagnetic material, the impregnation / solidification time is relatively short. Nevertheless becomes time, reaction with a ▲ l ▼ and Fe in the process of melt impregnation and coagulation, namely intermetallic compounds (a ▲ l ▼ 2 · Fe ) difficult generation of avoiding, ferromagnetic material "a ▲ l ▼ In the process of forming a complex with ", the effective volume as a magnetic body is reduced.
従って、これら溶湯含浸法による磁性複合材料は、その
製造過程において強磁性材料と溶湯なる「A▲l▼」と
の界面において金属間化合物(A▲l▼3・Fe)の生成
を伴い、その内に添加した強磁性材料が磁性体としての
有効体積を減損する欠点がある。Therefore, the magnetic composite material according to these melt impregnation method, with the formation of intermetallic compounds (A ▲ l ▼ 3 · Fe ) at the interface of the ferromagnetic material serving as molten metal "A ▲ l ▼" in the manufacturing process, the There is a drawback that the ferromagnetic material added inside reduces the effective volume as a magnetic material.
本発明は上記問題点に鑑み、その製造過程において、そ
の内に添加する強磁性材料(FeまたはFe合金)と
「A▲l▼」(A▲l▼またはA▲l▼合金)との界面
における反応、すなわち非磁性の金属間化合物(A▲l
▼3・Fe)の生成を抑制し得、かつ、強磁性材料内部に
歪を付加ないしは残留させることを軽減し得て、もつて
その内に添加された強磁性材料に本来の磁気特性を十分
に発揮させ得るA▲l▼またはA▲l▼合金の磁性複合
材料の製造方法を提供することを目的とするものであ
る。In view of the above problems, the present invention provides an interface between a ferromagnetic material (Fe or Fe alloy) added therein and "A1" (A1 or A1 alloy) in the manufacturing process. Reaction, that is, a non-magnetic intermetallic compound (A ▲ l
▼ 3・ Fe) generation can be suppressed, and strain added or retained inside the ferromagnetic material can be reduced, and the ferromagnetic material added therein has sufficient original magnetic characteristics. It is an object of the present invention to provide a method for producing a magnetic composite material of A (1) or an alloy of A (1) that can be exhibited in any of the following.
上記問題点を解決するための本発明に係るA▲l▼また
はA▲l▼合金の磁性複合材料の製造方法は、Feまた
はFe合金からなる粉体または繊維体を予備成形した
後、該予備成形体にA▲l▼またはA▲l▼合金の溶湯
を圧入含浸させることにより、前記強磁性材料を体積率
で15〜80%含有する磁性複合材料を製造する方法に
おいて、前記強磁性材料を予備成形の前、もしくは後
に、大気中にて300〜700℃の温度で加熱酸化さ
せ、しかる後、該加熱酸化された強磁性材料からなる予
備成形体に前記溶湯を圧入含浸させることを特徴とする
ものである。The method for producing a magnetic composite material of A1 or A1 alloy according to the present invention for solving the above-mentioned problems includes a method of preforming powder or fibrous body made of Fe or Fe alloy, A method for producing a magnetic composite material containing 15 to 80% by volume of the ferromagnetic material by press-fitting and impregnating a molded body with a molten metal of A1 or A1 alloy, Before or after preforming, it is heated and oxidized in the atmosphere at a temperature of 300 to 700 ° C., and thereafter, the molten metal is press-impregnated into a preformed body made of the heat-oxidized ferromagnetic material. To do.
本発明に係るA▲l▼またはA▲l▼合金の磁性複合材
料の製造方法は、FeまたはFe合金からなる強磁性材
料の粉体または繊維体にて形成されたを予備成形体に、
A▲l▼またはA▲l▼合金の溶湯を圧入含浸させる、
いわゆる溶湯含浸法にて、「A▲l▼」と強磁性材料と
を複合体化させるものであつて、その複合体化に要す圧
力、すなわち「A▲l▼」溶湯の含浸圧力はいわゆる粉
末冶金法による複合体化に要する圧力、すなわち「A▲
l▼」の固相温度域にて圧縮・結合させる圧力に比較し
て低く、その複合体化の過程にて、その内に添加された
強磁性材料内部に歪の付加ないしは残留させることを軽
減し得るものである。A method of manufacturing a magnetic composite material of A (1) or A (1) alloy according to the present invention includes a preformed body formed of powder or fibrous body of ferromagnetic material made of Fe or Fe alloy,
Aℓ or Aℓ alloy melt is press-fitted and impregnated,
The so-called molten metal impregnation method is used to form a composite of "A-1" and a ferromagnetic material, and the pressure required for forming the composite, that is, the impregnation pressure of the "A-1" molten metal is so-called. The pressure required to form a composite by powder metallurgy, that is, "A ▲
It is lower than the pressure to compress and bond in the solid phase temperature range of "l ▼", and it reduces the addition or residual strain inside the ferromagnetic material added in the complex formation process. It is possible.
また、本発明方法においては、前記強磁性材料は予備成
形の前、もしくは後に、大気中にて加熱酸化され、その
表面に酸化被膜を形成させたものであつて、この酸化被
膜を有する強磁性材料からなる予備成形体は前記「A▲
l▼」溶湯の圧入含浸に際して非磁性なる金属間化合物
(A▲l▼2・Fe)の生成を抑制するものである。Further, in the method of the present invention, the ferromagnetic material is one which is heated and oxidized in the atmosphere before or after preforming to form an oxide film on the surface of the ferromagnetic material. The preformed body made of the material is
l ▼ "is intended to suppress the formation of non-magnetic become intermetallic compounds during press-impregnation of the molten metal (A ▲ l ▼ 2 · Fe ).
これは、表面に酸化被膜を形成させた強磁性材料からな
る予備成形体に、「A▲l▼」の溶湯を圧入含浸させる
とき、溶湯と強磁性材料との界面においてA▲l▼とF
eとが反応せんとするが、この界面、すなわち、強磁性
材料の表面には酸化被膜が介在するもので、この酸化被
膜がA▲l▼とFeとの反応を阻害する障壁として作用
して金属間化合物(A▲l▼3・Fe)の生成を抑制する
からである。This is because when a preform made of a ferromagnetic material having an oxide film formed on its surface is press-impregnated with the molten metal of "A1" by impregnation, the molten metal of A1 and F at the interface between the molten material and the ferromagnetic material are used.
Although it reacts with e, an oxide film is present at this interface, that is, on the surface of the ferromagnetic material, and this oxide film acts as a barrier that inhibits the reaction between A and Fe. it is from inhibiting the production of intermetallic compounds (a ▲ l ▼ 3 · Fe ).
上記についてさらに詳しく説明すると、発明者等は磁性
複合材料の製造について、溶湯含浸法を用いるとき、そ
の含浸圧力を予備成形体内のガスを排出するに要する程
度の低い圧力まで低下させても「A▲l▼」と強磁性材
料との複合体化が可能であり、 その内に添加した強磁性材料内部の歪による磁気特性の
低下に関しては大巾に改善し得ることを確認したもので
ある。To explain in more detail, the inventors of the present invention, when using the molten metal impregnation method for the production of the magnetic composite material, even if the impregnation pressure is reduced to a pressure low enough to discharge the gas in the preform, It has been confirmed that it is possible to form a composite of "1""and a ferromagnetic material, and the deterioration of the magnetic properties due to the strain inside the ferromagnetic material added therein can be greatly improved.
しかし、上記溶湯含浸法によるとき、「A▲l▼」溶湯
と強磁性材料との界面反応が不可避的に起り、この反応
による非磁性の金属間化合物(A▲l▼3・Fe)の生成
にて強磁性材料の磁性体としての有効体積を減損すると
いう問題を伴うため、本発明等はこの界面反応につい
て、その抑制方法を種々検討した結果、強磁性材料にあ
る条件下で酸化被膜を形成させたとき、この酸化被膜が
有効なる界面反応の障壁となり得るとの結論に達したも
のである。However, when by the melt impregnation method, the generation of "A ▲ l ▼" interfacial reaction of the molten metal and the ferromagnetic material occurs inevitably, intermetallic compounds of a non-magnetic due to the reaction (A ▲ l ▼ 3 · Fe ) Since this involves the problem of depleting the effective volume of a ferromagnetic material as a magnetic material, the present invention has investigated various methods of suppressing this interfacial reaction, and as a result, an oxide film is formed under certain conditions in the ferromagnetic material. It was concluded that this oxide film, when formed, can be a barrier to effective interfacial reaction.
「A▲l▼」溶湯と強磁性材料との界面反応を防止する
には、強磁性材料の粉末または繊維体の表面に界面反応
を阻害する障壁となり得るものを、例えば蒸着,メツキ
等の方法にて、コーテイングすることが考えられるが、
表面積の大なる粉体または繊維体の表面に有効なるコー
テイングを施すには製造コストの上昇を不可避的に伴
い、また適切かつ有効なるコーテイング材を見いだすの
も必ずしも容易でなかつた。In order to prevent the interfacial reaction between the molten metal "A1" and the ferromagnetic material, a material that can be a barrier to the interfacial reaction on the surface of the powder or fibrous material of the ferromagnetic material, such as vapor deposition or plating, can be used. It is possible to coat at
In order to effectively coat the surface of a powder or fibrous body having a large surface area, the production cost is inevitably increased, and it is not always easy to find an appropriate and effective coating material.
そこで、本発明者等は非常に簡単でかつ低コストなる加
熱酸化による被膜形成に着眼したものであるが、一般に
はFe等の酸化物は熱が介在するとA▲l▼との間にお
いてテルミットという激しい反応を起すものとされてお
り、このような組合せはその実用性について期待され難
いものであつた。Therefore, the inventors of the present invention focused on the formation of a coating by heating oxidation which is very simple and low in cost. Generally, oxides such as Fe are called thermite between A and l when heat intervenes. It is said to cause a violent reaction, and such a combination is difficult to expect for its practicality.
しかし、本発明者等は種々実験の結果、「A▲l▼」の
溶湯含浸法においては、上記のような激しい反応は認め
られず、しかも適切なる温度範囲にて大気中で加熱酸化
されるとき、Fe(またはFe合金)からなる強磁性材
料の表面に形成された酸化被膜は、溶湯含浸の過程にお
いて、「A▲l▼」と強磁性材料との反応を阻害する有
効なる障壁となり得ることを見いだしたものである。However, as a result of various experiments, the inventors of the present invention did not recognize the above-mentioned violent reaction in the molten metal impregnation method of "A (l)", and moreover, it was oxidized by heating in the atmosphere at an appropriate temperature range. At this time, the oxide film formed on the surface of the ferromagnetic material made of Fe (or Fe alloy) can be an effective barrier for inhibiting the reaction between "A1" and the ferromagnetic material in the process of the molten metal impregnation. It was a finding.
これら実験例の内、0.01〜0.02mm径,1〜5mm
長さの低炭素鋼(S15C)短繊維体にて成形された体
積率50%の予備成形体を大気中にて種々の温度・時間
で加熱酸化したる後、純A▲l▼の溶湯を300気圧に
て圧入含浸することで製造した磁性複合材料について、
100エルステツド(Oe)磁場内での磁束密度(ガウス)
を測定した結果を第1図のグラフに示す。Among these experimental examples, 0.01-0.02mm diameter, 1-5mm
A preform with a volume ratio of 50% formed from a low-carbon steel (S15C) short fiber body with a length is heated and oxidized in the atmosphere at various temperatures and times, and then a molten metal of pure A (l) is added. Regarding the magnetic composite material produced by press-fitting and impregnating at 300 atm,
Magnetic Flux Density (Gauss) in 100 Elsted (Oe) Magnetic Field
The result of measurement is shown in the graph of FIG.
なお、第1図のグラフ中に記入した数字は、それぞれの
加熱時間を示すものであり、また、△印および×印でプ
ロツトしたものは対比のために行った実験結果を示すも
ので、△印のものはN2ガス雰囲気下で、×印のものは
Arガス雰囲気下でそれぞれ加熱処理したものである。The numbers entered in the graph of FIG. 1 indicate the respective heating times, and the plots marked with △ and × indicate the results of experiments conducted for comparison. Those marked with X are heat-treated under N 2 gas atmosphere, and those marked with X are heat-treated under Ar gas atmosphere.
これら大気下での磁性材料の加熱温度・時間と磁性複合
材料の磁気特性との関係を示す第1図のグラフで明らか
なように、300〜700℃の加熱温度で加熱酸化され
た強磁性材料からなるものは、それ以外の温度域のもの
より、その磁気特性が遥かに優れている。As is clear from the graph of FIG. 1 showing the relationship between the heating temperature / time of the magnetic material in the atmosphere and the magnetic properties of the magnetic composite material, the ferromagnetic material heated and oxidized at the heating temperature of 300 to 700 ° C. The magnetic properties of the alloys are much better than those of other temperature regions.
そして、その加熱時間は上記温度範囲内では、通常の加
熱処理に適用される範囲(1〜8時間程度)であれば、
効果において大きな差をもたらさないことがわかる。And within the above temperature range, the heating time is within a range (about 1 to 8 hours) applicable to normal heat treatment,
It can be seen that it does not make a big difference in the effect.
これは、300℃未満の温度にて強磁性材料の表面に形
成された酸化被膜は、溶湯含浸に際しA▲l▼との反応
を阻害する有効なる障壁として作用し得ず、反面700
℃を超す温度域では強磁性材料表面における酸化作用が
激しくなり過ぎ、強磁性材料が酸化損耗するからであ
る。This is because the oxide film formed on the surface of the ferromagnetic material at a temperature of less than 300 ° C. cannot act as an effective barrier that inhibits the reaction with A (1) during the impregnation of the molten metal.
This is because the oxidation effect on the surface of the ferromagnetic material becomes too strong in the temperature range exceeding ℃, and the ferromagnetic material is oxidatively worn.
なお、前記予備成形体は強磁性材料を予じめ15〜80
%の体積率となるよう成形してなるものとしたのは、予
備成形体は溶湯の流入圧力に耐える必要があり、15%
未満では溶湯の流入圧力に耐えてその形状を維持し得な
いからであり、また、これが80%を超えるとき、予備
成形体の空隙の連続性が途絶え溶湯が十分に浸透し得な
いからである。The preform is made of a ferromagnetic material in advance of 15-80.
Since the preform has to withstand the inflow pressure of the molten metal, the preform is required to have a volume ratio of 15%.
This is because if it is less than 80%, the inflow pressure of the molten metal cannot be maintained and its shape cannot be maintained, and if it exceeds 80%, the continuity of voids in the preform is interrupted and the molten metal cannot sufficiently permeate. .
上述のように、その表面に酸化被膜を形成させたる強磁
性材料よりなる予備成形体に、「A▲l▼」溶湯を圧入
含浸させる本発明A▲l▼またはA▲l▼合金の磁性複
合材料の製造方法は、粉末冶金法によるものより比較的
に低い応力にて複合体化されるもので、その内に添加さ
れた強磁性材料内部に歪を付加ないしは残留させること
を軽減し得、かつFeまたはFe合金からなる強磁性材
料とA▲l▼またはA▲l▼合金の溶湯との界面反応、
すなわち非磁性の金属間化合物(A▲l▼3・Fe)の生
成を抑制し得、もつてその内に添加された強磁性材料に
本来の磁気特性を十分に発揮させ得るものである。As described above, the magnetic composite of the present invention A-1 or A-1 alloy in which the "A1" molten metal is press-fitted and impregnated into the preformed body made of a ferromagnetic material having an oxide film formed on the surface thereof. The method of manufacturing the material is to form a composite with relatively lower stress than that by the powder metallurgy method, and it is possible to reduce the addition or residual strain inside the ferromagnetic material added therein, And the interfacial reaction between the ferromagnetic material made of Fe or Fe alloy and the molten metal of A (l) or A (l) alloy,
That it is capable enough to exhibit the inherent magnetic properties in the non-magnetic intermetallic compounds (A ▲ l ▼ 3 · Fe ) suppressing give a product of the ferromagnetic material added to them to have.
溶湯含浸法により、種々の組合せ条件下で磁性複合材料
を製造した。Magnetic composite materials were produced under various combined conditions by the molten metal impregnation method.
これら磁性複合材料は、種々の強磁性材料を樹脂等のバ
インダーを用いて所定体積率の予備成形体となし、その
予備成形体を種々の加熱温度・時間、および雰囲気下で
加熱処理した後、所定の金型内に挿入し、該金型内にA
▲l▼溶湯を注入して、加圧含浸・凝固を経て複合体化
させた。These magnetic composite materials form various ferromagnetic materials into preforms having a predetermined volume ratio using a binder such as a resin, and heat-treat the preforms under various heating temperatures / time and atmosphere, Insert into the specified mold and insert A into the mold.
{Circle around (1)} The molten metal was injected and pressure-impregnated and coagulated to form a composite.
第2図は、上記磁性複合材料を製造するに用いられる溶
湯含浸装置の一部を例示しており、円柱状の中空部を有
する金型(3)の上面に、注湯口(4)を設けたプランジヤス
リーブ(5)が密接して配置されている。そしてプランジ
ヤ(6)は前記スリーブ(5)内径に上下動自由に嵌合すると
共に、図外の加圧機構にて駆動されて加圧力を注湯口
(4)より注入されたA▲l▼溶湯(1)に印加する。また、
強磁性材料からなる予備成形体(2)は予じめ所定体積率
にて成形され、金型(3)内に配置されている。FIG. 2 exemplifies a part of the molten metal impregnation apparatus used for producing the magnetic composite material, in which a pouring port (4) is provided on the upper surface of a mold (3) having a cylindrical hollow portion. Plunger sleeves (5) are closely arranged. The plunger (6) is fitted in the inner diameter of the sleeve (5) so that it can move up and down, and is driven by a pressurizing mechanism (not shown) to inject a pressing force.
It is applied to the molten metal (1) injected from (4). Also,
The preform (2) made of a ferromagnetic material is preformed in a predetermined volume ratio and placed in the mold (3).
上記の方法、および装置にて溶湯含浸されて、複合体化
された磁性複合材料それぞれについて、100エルステ
ツド(Oe)の磁場内における磁束密度(ガウス)を測定し
た。The magnetic flux density (gauss) in a magnetic field of 100 Oersteds (Oe) was measured for each of the magnetic composite materials that had been melt-impregnated with the above-described method and apparatus to form a composite.
これら結果を第1表に示す。なお、対比のため、粉末冶
金法による磁性複合材料の例も第1表中に併記したが、
これは所定体積率にてA▲l▼粉末と強磁性材料とを混
合し、A▲l▼の固相温度域の600℃にて、7000
気圧の圧媒ガス下で圧縮固化成形したものである。The results are shown in Table 1. For comparison, an example of the magnetic composite material by the powder metallurgy method is also shown in Table 1.
This is a method in which the A1 powder and the ferromagnetic material are mixed at a predetermined volume ratio, and the temperature is set to 7,000 at 600 ° C. in the solid phase temperature range of A1.
It is formed by compression solidification under a pressure medium gas at atmospheric pressure.
第1表に示すように、本発明方法の条件を満足する範囲
内の条件にて製造された磁性複合材料(表中の備考欄に
おいて○印で示す実施例のもの)は、それ以外の条件に
て製造された磁性複合材料(備考欄において注記したも
の、および×印で示すもの)に比較して大巾に磁気特性
の改善が認められ、その一部はその内に添加した磁性材
料の体積率よりの期待値をほぼ満足するものである。 As shown in Table 1, the magnetic composite materials manufactured in the conditions satisfying the conditions of the method of the present invention (the examples of the examples marked with a circle in the remarks column in the table) are the other conditions. Compared with the magnetic composite materials manufactured in (the ones noted in the remarks column and those marked with x), the magnetic properties were significantly improved, and some of them were It almost satisfies the expected value from the volume ratio.
なお、強磁性材料の体積率を10%としたNo.2に示す
例においては、A▲l▼溶湯を注入した時点で予備成形
体が下方に収縮して所定の形状を得ることができず、ま
た、体積率を90%としたNo.50に示す例において
は、A▲l▼溶湯を予備成形体内に十分浸透させること
ができなかつた。In addition, in the example shown in No. 2 in which the volume ratio of the ferromagnetic material was 10%, the preform was contracted downward at the time of pouring the molten metal, and the predetermined shape could not be obtained. Further, in the example shown in No. 50 in which the volume ratio was 90%, the molten metal A1 could not be sufficiently permeated into the preform.
そして、対比のための粉末冶金法によるもの(製造方法
欄にHと記入の例)は、それぞれと対応する本発明方法
のものと比較(No.7−No.8,No.14−No.15,No.
16−No.17,No.18−No.19,No.44−No.4
5,No.46−No.47)すると、ほぼ半分程度の磁気特
性しか得られなかつた。And the thing by the powder metallurgical method for comparison (the example in which H is entered in the manufacturing method column) is compared with that of the corresponding method of the present invention (No. 7-No. 8, No. 14-No. 15, No.
16-No.17, No.18-No.19, No.44-No.4
No. 5, No. 46-No. 47), only about half the magnetic characteristics could be obtained.
なお、第1表に示す溶湯含浸法によるもの(製造方法欄
にSと記入の例)については、その含浸圧力、すなわち
溶湯圧入圧力は300〜400気圧としたが、これは他
の実験において2気圧以上の圧力であれば予備成形体内
のガスは排除され、A▲l▼溶湯は十分予備成形体に浸
透し得ることが確認されているが、より確実なる浸透を
計るため設定したものである。In the case of the molten metal impregnation method shown in Table 1 (an example in which S is entered in the manufacturing method column), the impregnation pressure, that is, the molten metal injection pressure was 300 to 400 atm. It has been confirmed that if the pressure is equal to or higher than the atmospheric pressure, the gas in the preform is removed, and the molten metal A (l) can sufficiently permeate into the preform, but it is set to measure the permeation more reliably. .
ただし、この含浸圧力は予備成形体を形成する強磁性材
料の注入溶湯温度における降伏応力に相当する圧力以下
であることが望ましい、これは、強磁性材料の降伏応力
以下の応力では該強磁性材料内部に歪を残留さすことが
ないからである。However, it is desirable that the impregnation pressure is equal to or lower than the yield stress of the ferromagnetic material forming the preform at the temperature of the molten metal injected, which is the stress equal to or lower than the yield stress of the ferromagnetic material. This is because no strain remains inside.
溶湯含浸に先立ち、強磁性材料に施す加熱酸化について
は、No.6,No.36,No.48に示す実施例でわかるよ
うに、本発明条件範囲内温度内の570℃にて強磁性材
料を加熱酸化させた磁性複合材料の磁気特性は、その体
積率が15%,50%,80%と変動しても、効果の面
で特異差は認められずその体積率の増加と共に磁気特性
が高くなる。Regarding the thermal oxidation applied to the ferromagnetic material prior to the molten metal impregnation, as shown in Examples shown in No. 6, No. 36, and No. 48, the ferromagnetic material is heated at 570 ° C. within the temperature range of the present invention. Regarding the magnetic properties of the magnetic composite material obtained by heating and oxidizing, even if the volume ratio fluctuates to 15%, 50%, 80%, no singular difference is observed in terms of the effect and the magnetic properties increase as the volume ratio increases. Get higher
そして、No.30,No.36,No.38に示す実施例でわ
かるように、強磁性材料の形態を変えても本発明条件範
囲内温度で加熱酸化された強磁性材料をその内に添下さ
せた磁性複合材料の磁気特性は高い値を示す。As can be seen from the examples shown in No. 30, No. 36, and No. 38, even if the form of the ferromagnetic material is changed, the ferromagnetic material heated and oxidized at the temperature within the range of the conditions of the present invention is added therein. The magnetic properties of the lowered magnetic composite material show high values.
対比のため、大気中における加熱酸化に替り、不活性ガ
ス雰囲気下にて加熱処理したもの(雰囲気欄にてN2ま
たはArと記入の例)は、それと対応する本発明方法の
ものと比較(No.9,10−No.8,No.28,29−No.
27)すると、ほぼ2/3程度の磁気特性しか得られなか
つた。For comparison, the one subjected to heat treatment in an inert gas atmosphere instead of the heating and oxidation in the atmosphere (an example in which N 2 or Ar is entered in the atmosphere column) is compared with that of the corresponding method of the present invention ( No. 9, 10-No. 8, No. 28, 29-No.
27) Then, only about 2/3 of the magnetic characteristics could be obtained.
これら磁性複合材料の内、代表的なものについての断面
を観察したところ、例えばNo.35の実施例のものは、
磁性複合材料の断面模式図である第3図aに示すよう
に、強磁性材料(F)の周囲に酸化被膜(Fo)が認められる
が、A▲l▼(A)との反応相は認められなかつた。When observing the cross section of a typical one of these magnetic composite materials, for example, the one of the example of No. 35 shows that
As shown in Fig. 3a, which is a schematic cross-sectional view of the magnetic composite material, an oxide film (Fo) is recognized around the ferromagnetic material (F), but a reaction phase with A (l) (A) is recognized. I couldn't do it.
一方、大気中において210℃にて加熱酸化されたNo.
21の実施例のもの、および不活性ガス雰囲気下で加熱
処理されたNo.28の例のものにおいては、磁性複合材
料の断面模式図である第3図bに示すように、Fe(F)
とA▲l▼(A)との反応生成物、すなわち金属間化合物
(AF)が存在し、また強磁性材料(F)の損耗が認められ
た。On the other hand, No. was heated and oxidized at 210 ° C in the atmosphere.
In the example of No. 21 and the example of No. 28 heat-treated under an inert gas atmosphere, as shown in FIG. 3b which is a schematic cross-sectional view of the magnetic composite material, Fe (F)
Reaction product of A with Al (A), that is, an intermetallic compound
(AF) was present and wear of the ferromagnetic material (F) was observed.
また、830℃の温度にて加熱酸化されたNo.43の例
のものにおいては、磁性複合材料の断面模式図である第
3図Cに示すように、強磁性材料(F)の周囲に酸化被膜
(Fo)が認められ、かつA▲l▼(A)との反応相は認めら
れなかつたが、しかし、強磁性材料(F)の酸化による損
耗が激しく、強磁性材料がほとんど消失していることが
判明した。Further, in the case of the example of No. 43 which was heated and oxidized at a temperature of 830 ° C., as shown in FIG. 3C which is a schematic sectional view of the magnetic composite material, it was oxidized around the ferromagnetic material (F). Film
(Fo) was observed and the reaction phase with A (l) (A) was not observed, however, the ferromagnetic material (F) was heavily worn due to oxidation, and almost all of the ferromagnetic material disappeared. It has been found.
なお、溶湯含浸に先立っ強磁性材料の加熱酸化につい
て、その実施にあたつてより良く、かつ安定した効果を
得るためには、その加熱温度を400〜600℃の範囲
内に設定されることが望ましい。Regarding the heating and oxidation of the ferromagnetic material prior to the impregnation of the molten metal, in order to obtain a better and stable effect in its implementation, the heating temperature should be set within the range of 400 to 600 ° C. desirable.
上述のように、本発明に係る磁性複合材料はその内に添
加された強磁性材料について、その本来の磁気特性を十
分に発揮させている。As described above, the magnetic composite material according to the present invention sufficiently exhibits the original magnetic characteristics of the ferromagnetic material added therein.
本発明に係るA▲l▼またはA▲l▼合金の磁性複合材
料の製造方法は、その製造過程において、その内に添加
する強磁性材料とA▲l▼(またはA▲l▼合金)との
界面反応、すなわち非磁性の金属間化合物(A▲l▼3
・Fe)の生成を、予じめ強磁性材料に形成させた酸化被
膜にて抑制するを得て、A▲l▼の特性を有してなお高
い磁気特性を有す磁性複合材料の製造を可能とするもの
であつて、本発明方法に係る磁性複合材料は、その優れ
た特性により実用モータ回転子や固定子用の磁性体また
高性能磁気遮蔽体その他、磁性を利用する電気製品の分
野において、その軽量化に大きく寄与し得るものであ
る。A method of manufacturing a magnetic composite material of A1 or A1 alloy according to the present invention comprises a ferromagnetic material and A1 (or A1 alloy) added in the manufacturing process. Interfacial reaction of non-magnetic intermetallic compounds (A ▲ l ▼ 3
The production of Fe) is suppressed in advance by the oxide film formed on the ferromagnetic material, and the production of a magnetic composite material having the characteristics of A (l) and still having high magnetic characteristics is produced. The magnetic composite material according to the method of the present invention enables magnetic fields for practical motor rotors and stators, high-performance magnetic shields, and other fields of electrical products utilizing magnetism due to its excellent characteristics. In the above, it can greatly contribute to the weight reduction.
第1図は本発明の大気下での強磁性材料の加熱温度・時
間と磁性複合材料の磁気特性との関係を示すグラフであ
る。第2図は本発明の磁性複合材料の製造するに用いら
れる溶湯含浸装置を示す正断面図である。第3図aは磁
性複合材料の部分断面を示す模式図である。第3図bは
磁性複合材料の部分断面を示す模式図である。第3図c
は磁性複合材料の部分断面を示す模式図である。 1……A▲l▼溶湯,2……予備成形体、3……金型,
4……注湯口,5……プラジヤスリーブ,6……プラン
ジヤ。FIG. 1 is a graph showing the relationship between the heating temperature / time of a ferromagnetic material and the magnetic characteristics of a magnetic composite material in the atmosphere of the present invention. FIG. 2 is a front sectional view showing a molten metal impregnating apparatus used for manufacturing the magnetic composite material of the present invention. FIG. 3a is a schematic view showing a partial cross section of the magnetic composite material. FIG. 3b is a schematic view showing a partial cross section of the magnetic composite material. Fig. 3c
FIG. 3 is a schematic view showing a partial cross section of a magnetic composite material. 1 …… A ▲ l ▼ Molten metal, 2 …… Preform, 3 …… Mold,
4 ... pouring spout, 5 ... plastic sleeve, 6 ... plungeer.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 元田 高司 兵庫県神崎郡香寺町溝口225−84 (72)発明者 武林 慶樹 愛知県名古屋市西区稲生町字杁先2200− 154 (72)発明者 尾崎 幸一 愛知県瀬戸市北松山町2丁目183番地 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Takashi Motoda 225-84 Mizoguchi, Koji-cho, Kanzaki-gun, Hyogo Prefecture (72) Inventor Keiki Takebayashi 2200-154 (72) Inventor, Inou-cho, Nishi-ku, Nagoya-shi, Aichi Prefecture Koichi Ozaki 2-183 Kitamatsuyama-cho, Seto City, Aichi Prefecture
Claims (1)
粉体または繊維状体を予備成形した後、該予備成形体に
A▲l▼またはA▲l▼合金の溶湯を圧入含浸させるこ
とにより、前記強磁性材料を体積率で15〜80%含有
する磁性複合材料を製造する方法において、前記強磁性
材料を予備成形の前、もしくは後に、大気中にて300
〜700℃の温度で加熱酸化させ、しかる後、該加熱酸
化された強磁性材料からなる予備成形体に前記溶湯を圧
入含浸させることを特徴とするA▲l▼またはA▲l▼
合金の磁性複合材料の製造方法。1. A powder or fibrous body of a ferromagnetic material made of Fe or an Fe alloy is preformed, and then the preformed body is press-impregnated with a molten metal of A (l) or A (l) alloy. In the method for producing a magnetic composite material containing the ferromagnetic material in a volume ratio of 15 to 80%, the ferromagnetic material is heated in the atmosphere at 300 before or after preforming.
A-l ▼ or A-l ▼, which is characterized in that it is heated and oxidized at a temperature of up to 700 ° C., and then the molten metal is press-fitted and impregnated into a preformed body made of the thermally oxidized ferromagnetic material.
Method for producing magnetic composite material of alloy.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9020087A JPH0639643B2 (en) | 1987-04-13 | 1987-04-13 | Method for producing magnetic composite material of A1 or A1 alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9020087A JPH0639643B2 (en) | 1987-04-13 | 1987-04-13 | Method for producing magnetic composite material of A1 or A1 alloy |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63255332A JPS63255332A (en) | 1988-10-21 |
| JPH0639643B2 true JPH0639643B2 (en) | 1994-05-25 |
Family
ID=13991842
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP9020087A Expired - Lifetime JPH0639643B2 (en) | 1987-04-13 | 1987-04-13 | Method for producing magnetic composite material of A1 or A1 alloy |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0639643B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4590633B2 (en) * | 2005-03-17 | 2010-12-01 | 国立大学法人富山大学 | Magnetic aluminum composite |
-
1987
- 1987-04-13 JP JP9020087A patent/JPH0639643B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63255332A (en) | 1988-10-21 |
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