JPH05308011A - Method of manufacturing rare-earth magnetic minute powder - Google Patents
Method of manufacturing rare-earth magnetic minute powderInfo
- Publication number
- JPH05308011A JPH05308011A JP3084283A JP8428391A JPH05308011A JP H05308011 A JPH05308011 A JP H05308011A JP 3084283 A JP3084283 A JP 3084283A JP 8428391 A JP8428391 A JP 8428391A JP H05308011 A JPH05308011 A JP H05308011A
- Authority
- JP
- Japan
- Prior art keywords
- aqueous solution
- boron
- rare
- reducing agent
- hydroride
- 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
- 239000000843 powder Substances 0.000 title claims abstract description 17
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 16
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 5
- 239000007864 aqueous solution Substances 0.000 claims abstract description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 11
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 10
- RJTANRZEWTUVMA-UHFFFAOYSA-N boron;n-methylmethanamine Chemical compound [B].CNC RJTANRZEWTUVMA-UHFFFAOYSA-N 0.000 claims abstract description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 5
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims abstract description 5
- 229910052742 iron Inorganic materials 0.000 claims abstract description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract 4
- 239000010941 cobalt Substances 0.000 claims abstract 2
- 229910017052 cobalt Inorganic materials 0.000 claims abstract 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract 2
- 229910052759 nickel Inorganic materials 0.000 claims abstract 2
- 229910052700 potassium Inorganic materials 0.000 claims description 7
- 239000011591 potassium Substances 0.000 claims description 7
- 239000012279 sodium borohydride Substances 0.000 claims description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 abstract description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 abstract description 4
- 239000011521 glass Substances 0.000 abstract description 4
- 229910001172 neodymium magnet Inorganic materials 0.000 abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 239000012153 distilled water Substances 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- XSDQTOBWRPYKKA-UHFFFAOYSA-N amiloride Chemical compound NC(=N)NC(=O)C1=NC(Cl)=C(N)N=C1N XSDQTOBWRPYKKA-UHFFFAOYSA-N 0.000 abstract 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 abstract 3
- 229910052796 boron Inorganic materials 0.000 abstract 3
- 229910017544 NdCl3 Inorganic materials 0.000 abstract 1
- MOOAHMCRPCTRLV-UHFFFAOYSA-N boron sodium Chemical compound [B].[Na] MOOAHMCRPCTRLV-UHFFFAOYSA-N 0.000 abstract 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 abstract 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 abstract 1
- ATINCSYRHURBSP-UHFFFAOYSA-K neodymium(iii) chloride Chemical compound Cl[Nd](Cl)Cl ATINCSYRHURBSP-UHFFFAOYSA-K 0.000 abstract 1
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 150000003839 salts Chemical class 0.000 abstract 1
- 239000002244 precipitate Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 239000004033 plastic Substances 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 238000010791 quenching Methods 0.000 description 3
- 230000000171 quenching effect Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229910000521 B alloy Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0573—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes obtained by reduction or by hydrogen decrepitation or embrittlement
Landscapes
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Hard Magnetic Materials (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、プラスチック磁石等に
利用される希土類磁石微粉末の作製法に関するものであ
る。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing fine powders of rare earth magnets used for plastic magnets and the like.
【０００２】[0002]
【従来の技術】従来、鉄族三員元素−希土類元素−ホウ
素合金の希土類磁石微粉末を作製する方法としては、母
合金のインゴットをつくり粉砕するか、液体急冷法によ
りリボンをつくり粉砕することが知られている。2. Description of the Related Art Conventionally, as a method for producing a fine powder of a rare earth magnet of an iron group three-member element-rare earth element-boron alloy, an ingot of a mother alloy is produced and pulverized, or a ribbon is produced and pulverized by a liquid quenching method. It has been known.
【０００３】[0003]
【発明が解決しようとする課題】インゴットをつくり粉
砕したり、液体急冷法によりリボンをつくり粉砕し、希
土類磁石微粉末を作製するには、大きな炉、液体急冷装
置、粉砕装置などの高価な装置、高エネルギー、複雑な
行程を必要とするためコスト高になるという課題があっ
た。An expensive device such as a large furnace, a liquid quenching device, or a crushing device is used to produce rare earth magnet fine powder by making and crushing an ingot or making a ribbon by a liquid quenching method. However, there is a problem that the cost is high because it requires high energy and complicated process.
【０００４】[0004]
【問題を解決するための手段】水素化ホウ素カリウムま
たは水素化ホウ素ナトリウム等の還元剤とジメチルアミ
ンボランの還元剤を含む水溶液に、鉄族三員元素の塩化
物または硫酸塩と希土類元素の塩化物または硫酸塩の水
溶液を加えるというきわめて簡単な方法により希土類磁
石微粉末を作製できるため、従来の方法より容易にしか
も低コストになる。[Means for Solving the Problem] An aqueous solution containing a reducing agent such as potassium borohydride or sodium borohydride and a reducing agent for dimethylamine borane is added to a chloride of an iron group three-member element or a sulfate and a rare earth element chloride. Since the rare earth magnet fine powder can be produced by an extremely simple method of adding a substance or an aqueous solution of sulfate, the method is easier and less expensive than the conventional method.
【０００５】[0005]
【作用】ＭＳＯ4 とＲＣｌ3 の水溶液を強い還元剤であ
る水素化ホウ素カリウムで還元した場合次の反応が考え
られる。 （化１） 2MSO4+KBH4+2H2O → 2M+2H2+2H2SO4+KBO2--(1) 4MSO4+2KBH4 → 2M2B+K2SO4+4H2 --(2) 2RCl3+KBH4+2H2O → 2R+H2+6HCl+KBO2 --(3) 4RCl3+3KBH4 → R4B3+14KCl+6H2 --(4) M: 鉄族三員元素 R:希土類元素 これらの還元反応は、急激に起こり０．１μｍ程度の微
細なＲ−Ｍ−Ｂ粉末を析出させる。次に、析出した微細
な粉末は、自己触媒的な働きをし、弱い還元剤であるジ
メチルアミンボランにより表面にＲ−Ｍ−Ｂを析出させ
粒成長して行く。プラスチックスに磁石粉末を分散させ
つくるプラスチック磁石では、保磁力等から考えて、１
μｍ前後の粉末になるよう還元剤の量を調整することが
望ましい。When the aqueous solution of MSO 4 and RCl 3 is reduced with potassium borohydride which is a strong reducing agent, the following reaction is considered. (Formula 1) 2MSO 4 + KBH 4 + 2H 2 O → 2M + 2H 2 + 2H 2 SO 4 + KBO 2 - (1) 4MSO 4 + 2KBH 4 → 2M 2 B + K2SO 4 + 4H 2 - (2 ) 2RCl 3 + KBH 4 + 2H 2 O → 2R + H 2 + 6HCl + KBO 2- (3) 4RCl 3 + 3KBH 4 → R 4 B 3 + 14KCl + 6H 2- (4) M: Iron group 3 Member element R: Rare earth element These reduction reactions occur rapidly and precipitate fine R-M-B powder of about 0.1 μm. Next, the fine powder deposited acts as an autocatalyst, and R-M-B is deposited on the surface by dimethylamine borane, which is a weak reducing agent, to grow grains. Considering the coercive force and other factors, plastic magnets made by dispersing magnet powder in plastics
It is desirable to adjust the amount of the reducing agent so that the powder has a particle size of about μm.
【０００６】[0006]
【実施例】以下実施例により本発明を説明する。 − Ｎｄ−Ｆｅ−Ｂ微粉末の作製 − ＦｅＳＯ4 とＮｄＣｌ3 およびジメチルアミンボランを
含む水溶液に水素化ホウ素カリウム水溶液に滴下した
後、１０分間放置し、Ｎｄ−Ｆｅ−Ｂ微粉末を析出させ
た。析出物は、ガラス・フィルターで濾過し蒸留水洗、
メタノール洗、アセトン洗を行った後、ガラス・フィル
ターごと真空乾燥を行った。EXAMPLES The present invention will be described below with reference to examples. -Preparation of Nd-Fe-B fine powder-Nd-Fe-B fine powder was deposited by dropping an aqueous solution containing FeSO 4 , NdCl 3 and dimethylamine borane into a potassium borohydride aqueous solution and then leaving it for 10 minutes. . The precipitate is filtered with a glass filter, washed with distilled water,
After washing with methanol and washing with acetone, vacuum drying was performed together with the glass filter.
【０００７】なお、析出物のＦｅとＮｄの組成比は溶液
の組成比にほぼ一致する。還元剤の濃度、液温、放置時
間は、目的とする析出物のＢ濃度および粒径により調整
すればよい。ただし、水素化ホウ素カリウムの量は（化
１）の式から化学量論的に計算される反応終結量の半分
以下に抑えることが望ましい。 （１）ＦｅＳＯ4 、ＮｄＣｌ3 およびジメチルアミンボ
ランを含む水溶液 容器にモル比８７．５：１２．５のＦｅＳＯ4 とＮｄＣ
ｌ3 を合計０．０２ｍｏｌ入れ、さらに０．１ｍｏｌの
ジメチルアミンボランを入れ、水１００ミリリットルを
加えた。この溶液を７０℃で加熱した。 （２）水素化ホウ素カリウム水溶液 容器に０．０１ｍｏｌの水素化ホウ素カリウムと、水２
０ミリリットルを加えた。 （３） 析出物 析出物の粒径を走査型電子顕微鏡で観察した結果、粒径
が１μｍ前後で大きさがかなりそろったＮｄ−Ｆｅ−Ｂ
が析出していることがわかった。この粉末を使用して製
作した磁石で得られた磁気特性はＢｓ＝１２００Ｇ、ｉ
Ｈｃ＝１．５ｋＯｅであった。The composition ratio of Fe and Nd in the precipitate substantially matches the composition ratio of the solution. The concentration of the reducing agent, the liquid temperature, and the standing time may be adjusted according to the B concentration and particle size of the target precipitate. However, it is desirable that the amount of potassium borohydride be suppressed to half or less of the reaction termination amount stoichiometrically calculated from the formula (Formula 1). (1) Aqueous solution containing FeSO 4 , NdCl 3 and dimethylamine borane In a container, FeSO 4 and NdC having a molar ratio of 87.5: 12.5 were used.
The l 3 placed total 0.02 mol, further put dimethylamine borane 0.1 mol, was added 100 ml of water. The solution was heated at 70 ° C. (2) Potassium borohydride aqueous solution 0.01 mol of potassium borohydride and water 2
0 ml was added. (3) Precipitate As a result of observing the grain size of the deposit with a scanning electron microscope, Nd-Fe-B having a grain size of about 1 μm and having a substantially uniform size.
Was found to have precipitated. The magnetic characteristics obtained with the magnet manufactured using this powder are Bs = 1200G, i
Hc = 1.5 kOe.
【０００８】[0008]
【発明の効果】以上実施例でも述べたように本発明は、
インゴットやリボン材を粉砕することなしに容易に希土
類磁石微粉末を作製することのできる工業的にも優れた
ものである。As described in the above embodiments, the present invention is
This is an industrially excellent product in which the rare earth magnet fine powder can be easily produced without crushing the ingot or the ribbon material.
Claims (1)
素ナトリウム等の還元剤とジメチルアミンボランの還元
剤を含む水溶液に、鉄族三員元素（鉄、コバルト、ニッ
ケル）の塩化物または硫酸塩と希土類元素の塩化物また
は硫酸塩を加えることにより希土類磁石微粉末つくるこ
とを特徴とした希土類磁石微粉末の作製法。1. An aqueous solution containing a reducing agent such as potassium borohydride or sodium borohydride and a reducing agent for dimethylamine borane, and a chloride or sulfate of an iron group three-member element (iron, cobalt, nickel) and a rare earth. A method for producing a fine powder of a rare earth magnet, which is characterized in that a fine powder of a rare earth magnet is produced by adding a chloride or a sulfate of an element.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3084283A JPH05308011A (en) | 1991-04-16 | 1991-04-16 | Method of manufacturing rare-earth magnetic minute powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3084283A JPH05308011A (en) | 1991-04-16 | 1991-04-16 | Method of manufacturing rare-earth magnetic minute powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH05308011A true JPH05308011A (en) | 1993-11-19 |
Family
ID=13826137
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3084283A Pending JPH05308011A (en) | 1991-04-16 | 1991-04-16 | Method of manufacturing rare-earth magnetic minute powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH05308011A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013204067A (en) * | 2012-03-27 | 2013-10-07 | Nec Tokin Corp | Powder and spherical particle combination and method for producing them, mixed powder of powder and spherical particle combination, magnetic paste containing the mixed powder, and inductor and magnetic core material using the magnetic paste |
| CN108987015A (en) * | 2018-06-28 | 2018-12-11 | 宁波招宝磁业有限公司 | A kind of preparation method of high-performance neodymium-iron-boron magnet |
-
1991
- 1991-04-16 JP JP3084283A patent/JPH05308011A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013204067A (en) * | 2012-03-27 | 2013-10-07 | Nec Tokin Corp | Powder and spherical particle combination and method for producing them, mixed powder of powder and spherical particle combination, magnetic paste containing the mixed powder, and inductor and magnetic core material using the magnetic paste |
| CN108987015A (en) * | 2018-06-28 | 2018-12-11 | 宁波招宝磁业有限公司 | A kind of preparation method of high-performance neodymium-iron-boron magnet |
| CN108987015B (en) * | 2018-06-28 | 2020-06-30 | 宁波招宝磁业有限公司 | Preparation method of high-performance neodymium iron boron magnet |
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