US3558372A - Method of making permanent magnet material powders - Google Patents
Method of making permanent magnet material powders Download PDFInfo
- 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
- Authority
- 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
Links
- 239000000843 powder Substances 0.000 title description 24
- 239000000463 material Substances 0.000 title description 22
- 238000004519 manufacturing process Methods 0.000 title description 4
- 239000002245 particle Substances 0.000 abstract description 13
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 9
- 150000001875 compounds Chemical class 0.000 abstract description 6
- 229910000765 intermetallic Inorganic materials 0.000 abstract description 3
- 239000002253 acid Substances 0.000 description 24
- 238000000034 method Methods 0.000 description 18
- 239000000203 mixture Substances 0.000 description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 239000000126 substance Substances 0.000 description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 5
- 238000000227 grinding Methods 0.000 description 5
- 229910017604 nitric acid Inorganic materials 0.000 description 5
- 229960000583 acetic acid Drugs 0.000 description 4
- 239000012362 glacial acetic acid Substances 0.000 description 4
- 239000000696 magnetic material Substances 0.000 description 4
- 235000011007 phosphoric acid Nutrition 0.000 description 4
- 229910052684 Cerium Inorganic materials 0.000 description 3
- 229910001122 Mischmetal Inorganic materials 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 3
- 239000010419 fine particle Substances 0.000 description 3
- 238000007654 immersion Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000009499 grossing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- 241001480079 Corymbia calophylla Species 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 230000003467 diminishing effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 238000010951 particle size reduction Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 150000002910 rare earth metals Chemical group 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23F—NON-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
- C23F3/00—Brightening metals by chemical means
- C23F3/04—Heavy metals
- C23F3/06—Heavy metals with acidic solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/07—Alloys based on nickel or cobalt based on cobalt
-
- 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
- H01F1/06—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 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.
Landscapes
- 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)
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 |
Family
ID=24818894
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
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)
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 |
-
1968
- 1968-01-31 US US701840*A patent/US3558372A/en not_active Expired - Lifetime
- 1968-12-31 BE BE726341D patent/BE726341A/xx unknown
-
1969
- 1969-01-03 GB GB579/69A patent/GB1210332A/en not_active Expired
- 1969-01-10 DE DE19691901056 patent/DE1901056A1/de active Pending
- 1969-01-15 NL NL6900668A patent/NL6900668A/xx unknown
- 1969-01-16 ES ES362575A patent/ES362575A1/es not_active Expired
- 1969-01-30 FR FR6901903A patent/FR2001038A1/fr not_active Withdrawn
Cited By (11)
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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