JPS6389608A - Production of rare earth magnet alloy powder - Google Patents
Production of rare earth magnet alloy powderInfo
- Publication number
- JPS6389608A JPS6389608A JP61235801A JP23580186A JPS6389608A JP S6389608 A JPS6389608 A JP S6389608A JP 61235801 A JP61235801 A JP 61235801A JP 23580186 A JP23580186 A JP 23580186A JP S6389608 A JPS6389608 A JP S6389608A
- Authority
- JP
- Japan
- Prior art keywords
- rare earth
- org
- acid
- earth magnet
- magnet alloy
- 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
Links
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 26
- 239000000956 alloy Substances 0.000 title claims abstract description 26
- 239000000843 powder Substances 0.000 title claims abstract description 23
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 17
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 239000004033 plastic Substances 0.000 claims abstract description 18
- 229920003023 plastic Polymers 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 238000010298 pulverizing process Methods 0.000 claims abstract description 4
- 150000007524 organic acids Chemical class 0.000 claims description 7
- 239000003960 organic solvent Substances 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 abstract description 21
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 abstract description 12
- 239000000203 mixture Substances 0.000 abstract description 9
- 230000004907 flux Effects 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 7
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 abstract description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 abstract description 6
- 239000002245 particle Substances 0.000 abstract description 6
- 239000002253 acid Substances 0.000 abstract description 5
- 229910001172 neodymium magnet Inorganic materials 0.000 abstract description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 abstract description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 abstract description 2
- 235000006408 oxalic acid Nutrition 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract 3
- 239000002904 solvent Substances 0.000 abstract 3
- 230000000052 comparative effect Effects 0.000 description 9
- 239000007789 gas Substances 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 2
- 229920005992 thermoplastic resin Polymers 0.000 description 2
- 238000001238 wet grinding Methods 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910001004 magnetic alloy Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 235000011888 snacks Nutrition 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
Landscapes
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Hard Magnetic Materials (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明はグラスチック又はゴム磁石用の希土類磁石合金
粉末の製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for producing rare earth magnet alloy powder for glass or rubber magnets.
Ｎｄ （ネオジム） −Ｆｅ ｃ鉄）−Ｂ（ホウ素）系
希土類磁石合金粉未使用のプラスチック磁石を炸裂する
ために、ｒｌｌｉｄ−Ｆｅ−Ｂ系希土類磁石の原料を溶
解し、得られたインゴットを微粉砕し、磁場中成形し、
得られた成形体を不活性ガス雰囲気中で焼成し之のち急
冷し、再び熱処理し、ジェットミルで微粉砕し、ボール
ミルで湿式粉砕してプラスナックマグネット用Ｎｄ −
Ｆｅ −Ｂ 系希土類磁石合金粉末を得、この合金粉末
に熱可型性樹脂を加えて磁場中にて射出成形すること、
！！０ち後述の比較試料１の製造工程（１）〜Ｑ４１で
プラスチック磁石を作ることは既に知られている。Nd (neodymium) - Fe c iron) - B (boron) based rare earth magnet alloy powder In order to explode an unused plastic magnet, the raw material for the rllid -Fe-B based rare earth magnet was melted and the resulting ingot was finely milled. Crush it, form it in a magnetic field,
The obtained molded body is fired in an inert gas atmosphere, then rapidly cooled, heat treated again, finely pulverized with a jet mill, and wet pulverized with a ball mill to obtain Nd − for plastic snack magnets.
Obtaining a Fe-B rare earth magnet alloy powder, adding a thermoplastic resin to the alloy powder and injection molding it in a magnetic field,
! ! It is already known that plastic magnets can be made in the manufacturing steps (1) to Q41 of Comparative Sample 1, which will be described later.
ところが、従来のＮｄ −Ｆｅ −Ｂ系希土類磁石合金
粉末は、粉砕時に発生する熱等によシその表面が酸化さ
れてしまう為、このような合金粉末を用いて、高い残留
磁束密度（Ｂ「）と、高い固有保磁力（）Ｉ、ｉ）ヲ有
−するプラスチック又はゴム磁石を得ることが困難であ
つ念。However, the surface of conventional Nd-Fe-B rare earth magnet alloy powders is oxidized by the heat generated during crushing. ) and high intrinsic coercive force (i), it is difficult to obtain plastic or rubber magnets.
従って１本発明の目的は、高い残留磁束密度と高い保磁
力を有するプラスチック又はゴム磁石を得ることができ
る希土類合金粉末を提併することにある。Therefore, one object of the present invention is to provide a rare earth alloy powder from which a plastic or rubber magnet having a high residual magnetic flux density and a high coercive force can be obtained.
上記問題点を解決し、上記目的を達成するための本発明
は、熱処理後の希土類磁石合金を湿式粉砕スる際に、ト
ルエン、エタノール、メタノール、メチルエチルケトン
等の有機溶剤と、酢酸、シュう酸、アクリル酸等から選
ばれた３２１以上の有機酸との混合液を用いることを特
徴とするものである。In order to solve the above problems and achieve the above objects, the present invention uses an organic solvent such as toluene, ethanol, methanol, methyl ethyl ketone, acetic acid, oxalic acid, etc. when wet-pulverizing a rare earth magnetic alloy after heat treatment. It is characterized by using a mixed solution with 321 or more organic acids selected from , acrylic acid, and the like.
上述の如く有機酸を用いて湿式粉砕すると、希土類磁石
合金の粒子表面に形成されていた酸化被膜が、有機酸に
よシ除去され、プラスチック又はゴム磁石に好適な粉末
を得ることができる。When wet-pulverized using an organic acid as described above, the oxide film formed on the surface of the rare earth magnet alloy particles is removed by the organic acid, and a powder suitable for plastic or rubber magnets can be obtained.
次に本発明の実施例（比較例も含む）に係わるＮｄ −
Ｆｅ −Ｂ系希土類磁石合金粉末及びこれを使用し念プ
ラスチック磁石の製造方法を説明する。Next, Nd − related to Examples (including comparative examples) of the present invention
A Fe-B rare earth magnet alloy powder and a method for producing a plastic magnet using the powder will be described.
第】表の試料Ａ１の比較例のＮｄ −Ｆｅ −Ｂ系希土
類プラスチック磁石を次のｆｉｌ −α４１の工程で作
製した。A Nd-Fe-B rare earth plastic magnet as a comparative example of sample A1 in Table 1 was produced in the following process of fil-α41.
（１１原料をＮｄ１５Ｆｅ７７Ｂ１組成になるように配
合した０
（２）上記原料を高周波溶解し、しかる後冷却すること
によってインゴットを作製した。(11 raw materials were blended to have a composition of Nd15Fe77B1) (2) An ingot was produced by high-frequency melting of the above raw materials and then cooling.
１３１４うれたインゴットをスタンプミルによりＮ、ガ
ス雰囲気中で平均粒径５ｍｍ程度に解砕し。The obtained ingot of 1314 was crushed to an average particle size of about 5 mm using a stamp mill in a N gas atmosphere.
更にＮ２ガス雰囲気中でディスクミルによシ０．】〜１
、Ｏｍｍ ｉｃ粗粉砕した。Furthermore, the disk mill was used in a N2 gas atmosphere to reduce the temperature to zero. ]~1
, Omm ic coarsely pulverized.
１４）得られｔ粉末なＮ２ガス雰囲気中でジェットミル
により平均粒径４μｍになるように微粉砕し几。14) The obtained powder was pulverized by a jet mill in a N2 gas atmosphere to an average particle size of 4 μm.
（５）得られ次粉末を磁場中成形した。(5) The obtained powder was compacted in a magnetic field.
（６１得られた成形体をＡｒガス雰囲気中で１０００〜
１２００℃で１時間焼成したのち急冷した。(61) The obtained molded body was heated to 1,000 ~
After firing at 1200°C for 1 hour, it was rapidly cooled.
（７１得られた焼成物をＡｒガス雰囲気中で５００〜１
０００℃で１時間再度熱処理し念。(71) The obtained fired product was heated to 500 to 1
Heat-treated again at 000℃ for 1 hour.
（８１再熱処理したものをＮ２ガス雰囲気中でジェット
ミルによシ粉砕し、３〜２０μｍの合金粉末を得た◎
（９； 直径３ｍｍの鉄球を３０ ｖａｔ％充填し之
内容積］リットルのボールミルに、得られた合金粉末を
３００ｇ入れた。(81) The reheat-treated product was pulverized by a jet mill in a N2 gas atmosphere to obtain an alloy powder of 3 to 20 μm. 300 g of the obtained alloy powder was placed in a ball mill.
推 該ボールミルに静かにトルエンを満たし。Gently fill the ball mill with toluene.
密封し几。Sealed.
ａｌＪ 該ボールミルを］ ００ ｒｐｍ、で２０分
間攪拌し之＠
α２ 液中よシ合金粉末を分離し、さらにトルエンで十
分に洗浄した。The ball mill was stirred at 00 rpm for 20 minutes to separate the alloy powder from the α2 solution, which was then thoroughly washed with toluene.
ａ３ 洗浄後の合金粉末にナイロン系熱可塑性樹脂を
５ｗｔ％添加し、混合し念。a3 Add 5wt% of nylon thermoplastic resin to the washed alloy powder, mix thoroughly.
α４１ 得られ念混合粉末を磁場中で射出成形し。α41 The obtained mixed powder was injection molded in a magnetic field.
試料Ａ】のプラスチック磁石を得九。Obtain a plastic magnet of sample A.
上述の方法で作製したプラスチック磁石の残留磁束密度
（Ｂｒ）、固有保磁力（Ｈ，ｉ）、最大エネルギー積（
ＢＨ＞ｍａｘを求めたところ、第２表に示す通シであつ
几。Residual magnetic flux density (Br), intrinsic coercive force (H, i), maximum energy product (
When we calculated BH>max, we found that it was the same as shown in Table 2.
次に１本発明に従う第１表の試料ぷ２のグラスチック磁
石を得る之めに、上記比較試料の作製工程ａαにおいて
、ボールミルにトルエンを入れる代シに、トルエン９９
ｖ０１％と酢酸］ ｖｏ１％とから成る混合液を入れ
た他は、比較試料Ｊと同一の方法でプラスチック磁石を
作り、その残留磁束密度（Ｂｒ ） 、保磁力（）Ｉｏ
ｉ）、＃大エネルギー積（ＢＨ）ｍ３ｘを測足し、第２
表の結果を得た。Next, in order to obtain the glass magnet of sample P2 in Table 1 according to the present invention, in the preparation step aα of the comparative sample, toluene 99% was added to the ball mill instead of toluene.
A plastic magnet was made in the same manner as Comparative Sample J, except that a mixed solution consisting of V01% and acetic acid] was added, and its residual magnetic flux density (Br) and coercive force (Io) were
i), #Measure the large energy product (BH) m3x, and calculate the second
Obtained the results in the table.
有ａ酸と有機溶剤との混合比及び種類をマえても１本発
明の作用効果が得られることを確かめるために、これ等
を第１表の試料鳥３〜Ｊ４に示す如く堂化嘔七次他は、
試料Ａ２と同一の方法で本発明に従うプラスチック磁石
を作り、その残留磁束密度（Ｂｒ）、保磁力（Ｈｃｉ
） 、最大エネルギー積（ＢＨ）ｍａｘを測定し次。In order to confirm that the effects of the present invention can be obtained even if the mixing ratio and type of the aerobic acid and organic solvent are changed, these samples were prepared as shown in Samples 3 to J4 in Table 1. The next one is
A plastic magnet according to the present invention was made in the same manner as Sample A2, and its residual magnetic flux density (Br) and coercive force (Hci) were
), measure the maximum energy product (BH)max and then.
また、合金粉末の組成を変えても本発明の作用効果が得
られることを確かめるために、試料Ｊ５及び１６ＩＣ示
すＮｄ Ｈｓ、ｌ！ Ｄｙ １．５ Ｆｅ ７７ Ｂ、
Ｉ）組成の合金粉末が得られるように原料を用意し、
比較試料Ｊ５の場合は、比較試料１の（２１〜α七と同
一の工程でプラスチック磁石を作り、一方１本発明に従
う試料Ｊ６の場合には、比較試料１の工程０１のトルエ
ンの代シに、酢酸］０ｖｏ１％とトルエン９０ ｖｏ１
％との混合液を使用する他は比較試料Ｊと同一の方法で
プラスチックを作り、それぞれのＢｒ 、 Ｈｃｉ、（
ＢＨ）ｍａＸを測定した。In addition, in order to confirm that the effects of the present invention can be obtained even if the composition of the alloy powder is changed, samples J5 and 16IC shown in Nd Hs, l! Dy 1.5 Fe 77 B,
I) Prepare raw materials so as to obtain alloy powder of the composition,
In the case of comparative sample J5, a plastic magnet was made using the same process as (21 to , acetic acid] 0 vol 1% and toluene 90 vol
Plastics were made in the same manner as Comparative Sample J except for using a mixture with Br, Hci, (
BH) maX was measured.
第】表ｃ次だし朱印は比較例）
第２表
第２表の比較試料Ｊと本発明に従う試料２〜Ｊ４との磁
気特性の差、及び比較試料】５と本発明に従う試料】６
との磁気特性の差から明らかな如く。Table 2 shows the difference in magnetic properties between Comparative Sample J in Table 2 and Samples 2 to J4 according to the present invention, and Comparative Sample] 5 and Sample according to the present invention] 6
As is clear from the difference in magnetic properties between
有機酸と有機溶剤との混合液を使用して湿式粉砕した本
発明に従う合金粉末を用いると、有機溶剤のみを使用し
て湿式粉砕し之従来の合金粉末を用いる場合に比べて、
高い残留磁束密度（Ｂｒ ）及び保磁力（Ｈ，ｉ）を有
するプラスチック磁石を得ることができる。これは１合
金粒子の表面に形成されてい次酸化被膜が有機酸によっ
て除去される次めである。When the alloy powder according to the present invention is wet-milled using a mixture of an organic acid and an organic solvent, compared to the conventional alloy powder that is wet-milled using only an organic solvent,
A plastic magnet with high residual magnetic flux density (Br 2 ) and coercive force (H,i) can be obtained. This occurs after the secondary oxide film formed on the surface of the alloy particles is removed by the organic acid.
上述から明らかな如く、本発明によれば、湿式粉砕の工
程に左いて、有機酸と有機溶剤との混合液を用いること
によシ１合金粒子の表面に形成されてい次酸化被膜が除
去てれ、これをプラスチック磁石又はゴムに使用すると
残留磁束密度（Ｓｒ） 。As is clear from the above, according to the present invention, the secondary oxide film formed on the surface of the Si1 alloy particles is removed by using a mixed solution of an organic acid and an organic solvent during the wet grinding process. When this is used in plastic magnets or rubber, the residual magnetic flux density (Sr) increases.
保磁力（）ｌｃｊ ）が向上する。なＳ、酸化被膜の除
去は特別な工程を設けることな（、湿式粉砕の工程で達
成することができる。Coercive force () lcj ) is improved. The removal of the oxide film can be achieved by a wet grinding process without any special process.
Claims (1)
溶剤と有機酸との混合液を用いることを特徴とするプラ
スチック又はゴム磁石用希土類磁石合金粉末の製造方法
。A method for producing rare earth magnet alloy powder for plastic or rubber magnets, which comprises using a mixed solution of an organic solvent and an organic acid when wet-pulverizing the rare earth magnet alloy after heat treatment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61235801A JPS6389608A (en) | 1986-10-03 | 1986-10-03 | Production of rare earth magnet alloy powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61235801A JPS6389608A (en) | 1986-10-03 | 1986-10-03 | Production of rare earth magnet alloy powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6389608A true JPS6389608A (en) | 1988-04-20 |
Family
ID=16991456
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61235801A Pending JPS6389608A (en) | 1986-10-03 | 1986-10-03 | Production of rare earth magnet alloy powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6389608A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0547525A (en) * | 1991-08-09 | 1993-02-26 | Sankyo Seiki Mfg Co Ltd | Rare earth bonded magnet |
| CN108994308A (en) * | 2018-08-06 | 2018-12-14 | 金川集团股份有限公司 | A kind of preparation method of low-apparent-density atomization nickel powder |
-
1986
- 1986-10-03 JP JP61235801A patent/JPS6389608A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0547525A (en) * | 1991-08-09 | 1993-02-26 | Sankyo Seiki Mfg Co Ltd | Rare earth bonded magnet |
| CN108994308A (en) * | 2018-08-06 | 2018-12-14 | 金川集团股份有限公司 | A kind of preparation method of low-apparent-density atomization nickel powder |
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