CN1184724A - Method for preparing powder of raw material for making permanent magnet - Google Patents

Method for preparing powder of raw material for making permanent magnet Download PDF

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Publication number
CN1184724A
CN1184724A CN97120487A CN97120487A CN1184724A CN 1184724 A CN1184724 A CN 1184724A CN 97120487 A CN97120487 A CN 97120487A CN 97120487 A CN97120487 A CN 97120487A CN 1184724 A CN1184724 A CN 1184724A
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CN
China
Prior art keywords
powder
permanent magnet
raw material
magnetic properties
iron powder
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.)
Granted
Application number
CN97120487A
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Chinese (zh)
Other versions
CN1104984C (en
Inventor
关根重信
佐藤广治
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Sanei Kasei Co Ltd
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Sanei Kasei Co Ltd
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Application filed by Sanei Kasei Co Ltd filed Critical Sanei Kasei Co Ltd
Publication of CN1184724A publication Critical patent/CN1184724A/en
Application granted granted Critical
Publication of CN1104984C publication Critical patent/CN1104984C/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • 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
    • H01F1/047Alloys characterised by their composition
    • 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
    • H01F1/047Alloys characterised by their composition
    • H01F1/053Alloys characterised by their composition containing rare earth metals
    • 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
    • H01F1/047Alloys characterised by their composition
    • H01F1/053Alloys characterised by their composition containing rare earth metals
    • H01F1/0536Alloys characterised by their composition containing rare earth metals sintered
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H01F41/0293Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F7/00Magnets
    • H01F7/02Permanent magnets [PM]

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Hard Magnetic Materials (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)

Abstract

PROBLEM TO BE SOLVED: To provide a method for manufacturing raw material powder for a permanent magnet which is easily manufactured and excellent in magnetic characteristics. SOLUTION: In this method for manufacturing raw material powder, after acicular iron powder is compression molded under presence of a magnetic field, the compression molded material is burned in a non-oxidizing gas atmosphere at 800-1000 DEG C., and then the obtained burned material is pulverized and mixed with fine powder of magnetic characteristics improving component, and the mixture is burned at 500-600 DEG C. while it is made to flow by argon gas, hydrogen gas or nitrogen gas.

Description

The preparation method of raw material powder for permanent magnet
Technical field that the present invention belongs to
The present invention relates to the preparation method of the raw material powder for permanent magnet of magnetic properties excellence.
Prior art
Permanent magnet has been obtained surprising progress, and especially rare earth-iron-boron based permanent magnet as the magnet that excellent magnetic properties is arranged, is subjected to liking of people.Special public clear 61-34242 communique discloses a kind of sintered magnet of magnetic anisotropy, and its composition is terres rares (R) 8~30% (atom), boron (B) 2~28% (atom), iron (Fe) 65~82% (atom) (comprising that a part is replaced by Co and/or Ni).Following opinion is also disclosed, the existence that promptly can allow industry manufacturings such as composition beyond above-mentioned such as Cu, Co, S, P, Ca, Mg, O, Si, Al to go up unavoidable impurities, and in three elements system basic composition FeBR, can also usually improve coercive force by one or more yuan that add among Al, Ti, V, Cr, Mn, Ni, Zn, Zr, Nb, Mo, Ta, W, Sn, Bi, the Sb.Having obtained Maximum Energy Product (BH) max in an embodiment is the above excellent like this permanent magnet of 35MGOe.When material powder prepared, preparation earlier contained the casting alloy of mentioned component, with Mechanical Method casting alloy is ground into powder then, thereby needs Crashing Costs.And the different such problems of each batch performance are arranged.
In addition, a kind of permanent magnet primitive powder has also been proposed, promptly in hydrogen stream, add in the acicular iron powder that thermal reduction obtains at 300~600 ℃ in FeOOH (α-goethite) acicular crystal, add, spread magnetic characteristic improvement compositions such as neodymium rare earth metals such as (Nd), boron, cobalt, but because initiation material FeOOH (α-goethite) is that length-width ratio is the acicular crystal about 5: 1~10: 1, thereby the length-width ratio of resulting acicular iron powder is difficult to be shaped under the situation that is used for the binding magnet purposes also more than 5: 1.
The problem that invention will solve
The purpose of this invention is to provide be easy to prepare, the preparation method of the raw material powder for permanent magnet of magnetic properties excellence.
In order to solve the means of problem
The preparation method of the raw material powder for permanent magnet that the present invention relates to, it is characterized in that acicular iron powder is after magnetic field exists lower compression to be shaped, the compression molding thing in the non-oxidizing gas atmosphere 800 ℃~1000 ℃ roastings, resulting calcining matter is pulverized, attritive powder with magnetic properties improvement composition mixes again, mixture forms fluidised form by argon gas, hydrogen or nitrogen, simultaneously 500~600 ℃ of roastings.
The present invention does not relate to the selection of the magnetic properties improvement composition that adds in the ferrous components, and be based on following neodoxy, promptly use the initiation material of acicular iron powder as ferrous components, then this acicular iron powder is carried out particular procedure, make it to add magnetic properties improvement composition, even thereby form identical, the raw material powder for permanent magnet of the magnetic properties that also can improve.
The working of an invention form
Acicular iron powder obtains by making FeOOH (α-goethite) acicular crystal carry out hydrogen reduction 300~600 ℃ of heating in atmosphere of hydrogen, be length below 10 μ m, width is at its powder of about 1/10~1/5.The acicular iron powder that uses among the present invention also can contain magnetic characteristic improvement compositions such as cobalt.
Such acicular iron powder, if in the presence of the magnetic field with the acicular iron powder compression molding after, make the compression molding thing in the non-oxidizing gas atmosphere in 800 ℃~1000 ℃ roastings, then the acicular iron powder in the compression molding thing is understood fusion and is become cubic.Resulting calcining matter is pulverized, and the attritive powder with magnetic properties improvement composition mixes again.As magnetic properties improvement composition, can be any principal component, but especially good be the such rare earth metal of neodymium, praseodymium, or the combination of rare earth metal and boron.Replace boron, or with boron, also can add at least a in silicon, chromium, titanium, manganese, copper, nickel, the vanadium.
The iron powder of roasting, pulverizing and magnetic properties improvement mixture of ingredients form fluidised form by argon gas, hydrogen or nitrogen, simultaneously 500~600 ℃ of roastings.The magnetic properties improvement composition that adds is diffused in the top layer of iron powder, thereby has improved magnetic properties.
The magnetic properties improvement composition that adds is fine as far as possible powder, spread to help quickening, but the Mechanical Method pulverizing is limited.Form fluidised gas as being used for,, then can make hydrogen adsorption in such rare earth metal of neodymium, praseodymium etc. if use hydrogen at first.Then, if use argon gas or nitrogen as fluidizing gas, the hydrogen of absorption is discharged, at this moment, disintegration phenomenon can take place in the metal that has adsorbed hydrogen.Utilize this phenomenon, repeat to use hydrogen earlier, use argon gas or nitrogen process then, make magnetic properties improvement composition become subparticle, can quicken its diffusion to the iron powder top layer by the hydrogen disintegration as fluidizing gas.
Can make sintered magnet or binding magnet with well-established law according to the raw material powder for permanent magnet that the present invention obtains.
Below specify formation of the present invention and effect with embodiment, but the invention is not restricted to the following example.
Embodiment 1
The about 2 μ m of average length that α-goethite (goethite) acicular crystal obtains with hydrogen reducing, length are than about 10: 1 acicular iron powder, in the presence of the magnetic field of 10KOe, with 3t/cm 2The pressure compression molding after, in argon atmosphere 900 ℃ of roastings.Acicular iron powder fusion and become cubic.The calcining matter that obtains is pulverized, again with as neodymium metal attritive powder, boron attritive powder and the cobalt attritive powder of magnetic properties improvement composition with final Nd8% (weight), B5% (weight), Co10% (weight), all the other are that the ratio of iron powder is mixed, mixture forms fluidised form with argon gas, 500 ℃ of roastings 20 hours, prepared raw material powder for permanent magnet simultaneously.This material powder in the magnetic field of 10KOe with 3t/cm 2Pressure forming, in a vacuum 1000 ℃ keep 1 hour sintering after, carry out Ageing Treatment (ageing), obtain permanent magnet.Measure Maximum Energy Product BHmax, relict flux density Br and the coercive force iHc of this permanent magnet, the results are shown in Table 1.
Comparative example 1
The raw material acicular iron powder is shaped in the state lower compression that does not have magnetic field, with embodiment 1 the same carrying out, has prepared raw material powder for permanent magnet in addition.From this material powder,, obtain permanent magnet with embodiment 1 the same carrying out.Measure Maximum Energy Product BHmax, relict flux density Br and the coercive force iHc of this permanent magnet, the results are shown in Table 1.
Table 1
????Br ??(gauss) ????iHc ????(Oe) ????BHmax ????(MgOe)
Embodiment ???15664 ????9572 ?????55.7
Comparative example 1 ???8709 ????1094 ?????16.4
From the contrast of table 1 illustrated embodiment 1 and comparative example 1 as can be seen, even form identical, the present invention of the use iron powder that roasting becomes after making the acicular iron powder compression molding under the existence of magnetic field, with make the acicular iron powder compression molding under the state that does not have magnetic field to exist after the situation of roasting compare, magnetic properties also is significantly increased.

Claims (2)

1, the preparation method of raw material powder for permanent magnet, it is characterized in that acicular iron powder is after magnetic field exists lower compression to be shaped, the compression molding thing in the non-oxidizing gas atmosphere 800 ℃~1000 ℃ roastings, the calcining matter that obtains is pulverized, and mix with the attritive powder of magnetic properties improvement composition, mixture forms fluidised form with argon gas, hydrogen or nitrogen, simultaneously 500~600 ℃ of roastings.
2, the preparation method of the described raw material powder for permanent magnet of claim 1, wherein magnetic properties improvement composition is a rare earth metal.
CN97120487A 1996-10-24 1997-10-21 Method for preparing powder of raw material for making permanent magnet Expired - Fee Related CN1104984C (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP281930/96 1996-10-24
JP281930/1996 1996-10-24
JP8281930A JPH10125517A (en) 1996-10-24 1996-10-24 Manufacture of raw material powder for permanent magnet

Publications (2)

Publication Number Publication Date
CN1184724A true CN1184724A (en) 1998-06-17
CN1104984C CN1104984C (en) 2003-04-09

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CN97120487A Expired - Fee Related CN1104984C (en) 1996-10-24 1997-10-21 Method for preparing powder of raw material for making permanent magnet

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JP (1) JPH10125517A (en)
KR (1) KR19980032050A (en)
CN (1) CN1104984C (en)
TW (1) TW345666B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101190457B (en) * 2006-12-01 2013-06-19 M·J·鲁特纳 Process for making iron powder or microalloyed steel powder from iron oxide powder by oxidation and reduction

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105057097B (en) * 2015-09-16 2017-03-22 重庆市九瑞粉末冶金有限责任公司 Waterfall type separation device for magnetic iron powder particles

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101190457B (en) * 2006-12-01 2013-06-19 M·J·鲁特纳 Process for making iron powder or microalloyed steel powder from iron oxide powder by oxidation and reduction

Also Published As

Publication number Publication date
JPH10125517A (en) 1998-05-15
CN1104984C (en) 2003-04-09
KR19980032050A (en) 1998-07-25
TW345666B (en) 1998-11-21

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