US3558372A - Method of making permanent magnet material powders - Google Patents

Method of making permanent magnet material powders Download PDF

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Publication number
US3558372A
US3558372A US701840*A US3558372DA US3558372A US 3558372 A US3558372 A US 3558372A US 3558372D A US3558372D A US 3558372DA US 3558372 A US3558372 A US 3558372A
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US
United States
Prior art keywords
acid
powder
permanent magnet
coercive force
materials
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
Application number
US701840*A
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English (en)
Inventor
Joseph J Becker
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
General Electric Co
Original Assignee
General Electric Co
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Filing date
Publication date
Application filed by General Electric Co filed Critical General Electric Co
Application granted granted Critical
Publication of US3558372A publication Critical patent/US3558372A/en
Anticipated expiration legal-status Critical
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Classifications

    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23FNON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F3/00Brightening metals by chemical means
    • C23F3/04Heavy metals
    • C23F3/06Heavy metals with acidic solutions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14Treatment of metallic powder
    • B22F1/145Chemical treatment, e.g. passivation or decarburisation
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C19/00Alloys based on nickel or cobalt
    • C22C19/07Alloys based on nickel or cobalt based on cobalt
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/06Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys in the form of particles, e.g. powder

Definitions

  • the present invention relates generally to the art of making permanent magnets and is more particularly concerned with new magnetic material powders having unique characteristics and with a novel method for producing these powders.
  • the detrimental eiTects of grinding upon the magnetic characteristics of the cobalt-rare earth materials can be eliminated and the coercive force of mechanically-reduced materials of this kind can be enhanced to a surprising extent.
  • the method of this invention centers in the key step of chemically smoothing the surfaces of finely-divided, ground, magnetic material. This step is carried out with an acid mixture in a contact period of from a few seconds to 30 minutes during which time the individual powder particles preferably are not substantially reduced in size but their sharp edges and points are rounded and smoothed by acid attack.
  • This invention thus centers in the concept of subjecting these ground materials to a chemical treatment to eliminate the degrading effects of the grinding upon their magnetic properties.
  • the invention is also based upon my discoveries that such treatment can result in surprisingly large increases in coercive force of these cobalt-rare earth materials, and that this result can be obtained without incurring a significant product yield penalty or other substantial dis advantage.
  • the chemical treatment is carried out according to this invention by contacting cobalt-rare earth magnetic material with a suitable acid solution, the material in powder form preferably being immersed in the acid solution for the required period of contact time and then promptly removed and rinsed free from that solution in order to arrest the acid attack.
  • Time and temperature are interrelated factors in this method, I have found, however, that practical operating ranges of these variables are so broad that the necessity for precise control of the method can readily be avoided. Thus, except for threshold or marginal conditions of time and temperature, the operating conditions or a combination of these conditions is not critical to the success or failure of the method in terms of the products obtained.
  • the acid mixture will be at rooom temperature but it may be at any temperature at which the acid mixture is a liquid.
  • the period of immersion or contact may likewise be anywhere from one or two seconds to 30 minutes, my present preference being about 30 seconds. Prolonged acid contact may lead to significantly diminishing magnet material yields, particularly if the treating solution temperature is substantially above room temperature.
  • the mechanical or manipulative limitation which generally is the important one. Acid solutions I prefer for this process act rapidly enough that momentary contact is sufficient to insure consistently good results and it remains only to device means enabling immersion and removal of the powder materials at the rate desired in a batchwise or a continuous chemical treatment operation. In any event a second or two would appear to be a reasonable immersion contact period and five to 10 seconds would be an easier goal to reach in production operations.
  • cobalt-rare earth magnet material of particle size in the range between 250 mesh and +325 mesh (U.S. standard screen sizes).
  • Materials of this kind may, however, be treated according to this invention with the foregoing results when the particles are twice as large, but the maximum coercive force obtainable is lower because of the fact that particle size is generally inversely proportional to coercive force.
  • Much finer particles may likewise be treated in accordance with this method but at the cost of smaller product yields because of the relatively larger proportion of each particle dissolved in the acid attack.
  • Acid A Three parts nitric acid One part sulfuric acid One part orthophosphoric acid Five parts glacial acetic acid One part nitric acid One part sulfuric acid One part orthophosphoric acid Five parts glacial acetic acid 200 grams chromic oxide grams nitric acid 10 grams sodium sulfate Water to one liter volume. 4 Microns.
  • Co Y was prepared by arc-melting cobalt and yttrium together under an argon atmosphere and then casting the melt to form an ingot.
  • a piece of the resulting very brittle ingot weighing about one half gram was ground with mortar and pestle and the resulting powder was screened and the fraction passing a 250 mesh screen and return on a 325 mesh screen was selected for test.
  • the remainder of the -250 +325 mesh powder fraction was placed in a dish with ml. of a mixture of 3 parts nitric acid, one part sulfuric acid, one part orthophosphoric acid and five parts glacial acetic acid.
  • the acid mixture was at C., and the powder was permitted to remain in the acid mixture for seconds whereupon the powder was removed from the acid mixture and rinsed with water and with acetone and permitted to dry in air.
  • This sample was then mounted inparaffin and tested as described above with the result that the coercive force was found to be 3340 oersteds, as stated in the third entry of Table I.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Power Engineering (AREA)
  • Hard Magnetic Materials (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
US701840*A 1968-01-31 1968-01-31 Method of making permanent magnet material powders Expired - Lifetime US3558372A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US70184068A 1968-01-31 1968-01-31

Publications (1)

Publication Number Publication Date
US3558372A true US3558372A (en) 1971-01-26

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US701840*A Expired - Lifetime US3558372A (en) 1968-01-31 1968-01-31 Method of making permanent magnet material powders

Country Status (7)

Country Link
US (1) US3558372A (en])
BE (1) BE726341A (en])
DE (1) DE1901056A1 (en])
ES (1) ES362575A1 (en])
FR (1) FR2001038A1 (en])
GB (1) GB1210332A (en])
NL (1) NL6900668A (en])

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3699487A (en) * 1970-11-07 1972-10-17 Nix Elektro Physik Hans Magnet for use in magnetic thickness gauges
US3900749A (en) * 1974-04-02 1975-08-19 Hmw Industries Permanent magnet generator
US5186765A (en) * 1989-07-31 1993-02-16 Kabushiki Kaisha Toshiba Cold accumulating material and method of manufacturing the same
US20030201031A1 (en) * 2002-04-29 2003-10-30 Electron Energy Corporation Method of improving toughness of sintered RE-Fe-B-type, rare earth permanent magnets
US20030201035A1 (en) * 2002-04-29 2003-10-30 Electron Energy Corporation Modified sintered RE-Fe-B-type, rare earth permanent magnets with improved toughness
US20060005898A1 (en) * 2004-06-30 2006-01-12 Shiqiang Liu Anisotropic nanocomposite rare earth permanent magnets and method of making
US20060054245A1 (en) * 2003-12-31 2006-03-16 Shiqiang Liu Nanocomposite permanent magnets

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3699487A (en) * 1970-11-07 1972-10-17 Nix Elektro Physik Hans Magnet for use in magnetic thickness gauges
US3900749A (en) * 1974-04-02 1975-08-19 Hmw Industries Permanent magnet generator
US5186765A (en) * 1989-07-31 1993-02-16 Kabushiki Kaisha Toshiba Cold accumulating material and method of manufacturing the same
US5449416A (en) * 1989-07-31 1995-09-12 Kabushiki Kaisha Toshiba Cold accumulating material and method of manufacturing the same
US20030201031A1 (en) * 2002-04-29 2003-10-30 Electron Energy Corporation Method of improving toughness of sintered RE-Fe-B-type, rare earth permanent magnets
US20030201035A1 (en) * 2002-04-29 2003-10-30 Electron Energy Corporation Modified sintered RE-Fe-B-type, rare earth permanent magnets with improved toughness
US20050081960A1 (en) * 2002-04-29 2005-04-21 Shiqiang Liu Method of improving toughness of sintered RE-Fe-B-type, rare earth permanent magnets
US6966953B2 (en) 2002-04-29 2005-11-22 University Of Dayton Modified sintered RE-Fe-B-type, rare earth permanent magnets with improved toughness
US6994755B2 (en) 2002-04-29 2006-02-07 University Of Dayton Method of improving toughness of sintered RE-Fe-B-type, rare earth permanent magnets
US20060054245A1 (en) * 2003-12-31 2006-03-16 Shiqiang Liu Nanocomposite permanent magnets
US20060005898A1 (en) * 2004-06-30 2006-01-12 Shiqiang Liu Anisotropic nanocomposite rare earth permanent magnets and method of making

Also Published As

Publication number Publication date
ES362575A1 (es) 1970-11-01
BE726341A (en]) 1969-05-29
DE1901056A1 (de) 1969-08-28
FR2001038A1 (en]) 1969-09-19
GB1210332A (en) 1970-10-28
NL6900668A (en]) 1969-08-04

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