METHOD FOR PRODUCING MAGNETS

Abstract: A method for producing magnets from powdered magnetic alloy. The method comprises aligning a particle charge of magnet alloy within a container, which aligning may be achieved by use of a pulsating magnetic field; and consolidating the charge after alignment to a density in excess of 95% of theoretical density as by cold or hot isostatic pressing, or a combination thereof.

Description: METHOD FOR PRODUCING MAGNETS This invention relates to a method for producing magnets with improved remanence. It is conventional practice to produce magnets from powdered magnetic alloys, including rare earth cobalt magnets, by compacting as by die pressing a charge of aligned or oriented fine powder of a magnetic alloy of the desired magnet composition. Thereafter, the compacted charge is heat treated at temperatures of the order of 1093 to 11430C (2000 to 20900F). It is known that by increasing the density in the production of magnets of this type from particle charges of the magnetic material that remanence can be improved. Conventionally, density is increased by raising the sinterfngtemperature after die pressing; however, this results in a corresponding lowering of coercive force. It is accordingly an object of the present invention to provide a method for producing from powdered magnetic alloy magnets with increased density, and thus improved remanence, without resorting to higher sintering temperatures that serve to lower coercive force. Another object of the invention is in the production of magnets to provide for improved alignment or orientation to achieve higher remanence values. The present invention provides a method for producing magnets with improved remanence by consolidating a particle charge of a magnet alloy to form a magnet article, characterised in that said method comprises applying a magnetic field to said particle charge within a container to magnetically align said particles, said magnetic field being applied as at least one pulse with each said pulse having a duration not exceeding one second and a power level of at least 50,000 oersted (39789 ampere turns per centimetre) and thereafter consolidating said particle charge to a final density. The present invention also provides a method for producing magnets with improved remanence by consolidating a particle charge of a magnet alloy to form a magnet article, characterised in that said method comprises applying a magnetic field to said particle charge to magnetically align said particles, and thereafter hot isostatically pressing said particles to consolidate the same to full density. ft has been determined broadly in accordance with the invention that improved remanence is a function of both the degree of alignment of the individual magnetic dipoles (powder particles) and density (the number of dipoles that are present in a given volume of the body of the magnet material). Accordingly, in the broader aspects of the invention it has been discovered that if one subjects a particle charge of magnet alloy, which may be one or more transition elements, e.g. nickel, cobalt, iron, chromium, manganese, copper, zirconium and titanium, in combination with at least one rare earth element, e.g. samarium, to a temperature that is below the full density sintering temperature but above the temperature necessary to produce a close-pore structure and then subjects the material while at this temperature to isostatic compacting, increased density and thus improved remanence is achieved while maintaining good coercive force. Coercive force is maintained by maintaining the temperature below the full density sintering temperature. Additionally, remanence is improved by aligning or orienting the material by the use of a pulsating magnetic field within a container. The container may be a collapsible container within which the material can thereafter be isostatically compacted. The pulsating magnetic field should have a pulse duration not exceeding one second per pulse and each pulse typically will be of the order of 15 millisecond. At least one pulse and preferably two pulses at a power level of at least 50,000 Oe (39789 ampere turns per centimetre) is suitable for the purpose. After magnetic alignment of the particles, the particles may be compacted to an intermediate density by additional pulsing. Conventionally, highly oriented SmCo5 magnets have been produced by the use of superconducting solenoids to generate the high-intensity magnetic fields. These superconducting solenoids must be operated at cryogenic temperatures (-268 C (-4500F))to pass the high-density current necessary to generate these high-intensity magnetic fields In the practice of the invention, however, the required highintensity magnetic fields are preferably produced by discharging an assemblage of capacitors, e.g. four hundred to one thousand capacitors, thereby eliminating the need for superconducting solenoids. The container may be a rubber bag and preferably after alignment the bag is evacuated in the presence of a constant DC field which serves to maintain alignment. Alternatively, the particles of magnet material may be aligned within a preformed container, which will be collapsible and of a material such as stainless steel. The step of subjecting the aligned material to a steady DC field in an evacuated container has been found to "lock in" the alignment and thus ensure improved remanence. Consolidation of the particles may be effected in any suitable manner, eg., by die pressing plus sintering, by cold isostatic compactions plus sintering or by hot isostatic pressing. The following constitutes specific examples with respect to the practice of. the invention as described above and demonstrate its utility: Example 1: SmCo5 powder was oriented in a die cavity with an applied magnetic field and pressed, the applied field and the pressing direction being normal to each other. The pressed powder after sintering and post sintering had the properties as set forth in Table I. The sintered magnet was loosely wrapped with stainless steel foil (not pressure tight; for handling convenience only) and as-hot-isostatically pressed (HIPed) at 954 0C (17500F). The as-HIPed magnet had the properties as set forth in Table I. The HIPed magnet was reheat treated at 910 C (16700F) for three hours and quenched. The magnetic properties after HIPing and heat treatment are set forth in Table I. TABLE I Hr Hc Hci BHmax Hk (G) (Oe) (Oe) MGOe Oe Pgm/Cm3 Die Pressed and Sintered 8,900 8,600 15,100 19. 8 12,400 8.07 After HIP 9,400 9,100 11,500 22.1 10,000 8.53 Heat Treatment after HIP 9,400 9,200 > 20,000 22.1 15,800 Example 2: Another magnet prepared according to the same procedures prescribed as -in Example 1 had the properties set forth in Table II. TABLE II Br Hc Hci BHmax Hk 3 G Oe Oe MGOe Oe pgm/Cm G MGOe Die Pressed and Sintered 9,000 8,400 14,000 19.0 9,400 .8.07 After HIP 9,400 8,800 10,600 21.1 9,200 8.53 Example 3: Another magnet of SinCo5 from a batch other than in Examples 1 and 2 was prepared as described in Example 1. The properties are recorded in Table III. TABLE III Br Hc Hci BHmax Hk G Oe ¯ Oe MGOe Oe Die Pressed and Sintered 9,200 8,800 > 20,000 21.0 9,400 After HIP 9,600 4,600 7,600 13.2 2,200 Heat Treatment after HIP 9,600 9,400 > 20,000 22.5 9,600 It may be seen from the magnetic property data that remanence is improved by hot isostatic pressing after conventional aligning and cold pressing. Further improvement is achieved with respect to coercive force when after hotisostatic pressing the magnet is subjected to post sintering heat treatment. The deterioration of the coercive force after HIPing is believed to be due to phase separation. Example 4: Using the powder from the same batch as in Example 3, a magnet was made by sintering SmCo5 powder that was previously oriented and cold isostatically pressed. The magnet had the properties set forth in Table IV. TABLE IV Br Hc Hci BHmax Hk 3 G Oe Oe MgOe Oe Egm/Cm Cold Isostatically Pressed and Sintered 9,700 9,000 17,700 23.5 9,600 8.31 After HIP 9,800 6,000 7,000 22.0 5,200 8.49 Heat Treatment After HIP 9,800 9,200 > 20,000 24.0 12,400 With the magnet alloy of Example 4 the theoretical maximum density is 8.6 gm/Cm3. The specific magnet had a density of 8.31 gm/Cm3 before hot isostatic pressing and the density increase after hot isostatic pressing was only about 2%, which accounts for the small improvement in remanence reported in the example. It is anticipated that if the theoretical maximum density had been achieved during hot isostatic pressing about a 3% increase in remanence would result. Example 5: SmCo5 alloy was loaded into a stainless container and hydrogen admitted into the container, The pressure was built up to 30 atmospheres; hydrogen absorption by the alloy results in a disintegration of the alloy to about 80 mesh powder. The dehydrided powder was jet milled to about 4 P particle size. The fine powder was loaded into a rubber bag of 19.05mm (3/4") diameter and the bag was contained in a stainless or plastics sheath. The bag was then pressurized and the powder oriented by placing the rubber bag along with the sheath inside a coil-, and pulsing the coil,-at least three times, with enough power to generate 60,000 Oe (47746 ampere turns per centimetre) within the coil. The oriented powder was then placed in a steady DC field of 10 kOe and the bag evacuated to lock the alignment. The evacuated bag containing the powder was then placed in an isostatic press chamber and compressed with a pressure up to 7040 Kg/cm2 (100,000 psi). The green compact was subsequently sintered between 1000-12000C and post sinter aged between 870-9300C. The magnets prepared from these four batches of powder in the manner described above had the properties set forth in Table V, which Table also shows magnetic properties of conventional commercial magnets. TABLE V Br Hc Hci BHmax Hk G Oe Oe MGOe Oe Batch # I 10,000 9,600 11,800 24 8,600 BatchiII 10,200 10,200 18,000 26 14,800 Batch+#III 10,600 9,800 17,000 28 10,400 Batch + IV 10,200 9,600 15,300 25 10,800 Commercial ) 8,800 8,600 15,000 19 10,000 Magnets ) 9,200 8,800 20,000 21 10,000 Example 6: Powder of SmCos was loaded in a rubber bag and oriented in the poles of an electromagnet in a field of 25 kOe. The oriented powder was then evacuated maintaining the steady DC field. The evacuated bag containing the oriented powder was isostatically pressed followed by sintering and heat treatment. The magnet had the following properties as shown in Table VI, c TABLE VI Br Hc Hci BHmax G Oe Oe MGOe Magnet Prepared Without a Pulsating d.c. Field 8,900 6,400 7,200 19.0 Example 7: A fourth batch of SmCo5 was processed into magnets by procedures as described in Example 1 except for a change in the compaction method. The powder contained in the bag after alignment was initially compactcd inside the bag by placing the bag towards the end of the coil and employing the field gradient present in the coil during pulsing to bring forth an initial compaction to an intermediate density by additional pulsing. The oriented compacted powder placed in a steady DC field was evacuated, isostatically pressed and sintered. The sintered sample was of uniform diameter and had a flat top and bottom contrary to the samples prepared without the field gradient packing which had a pyramidal top. The magnetic properties of the sintered magnet prepared as per this example are shown in Table VII. TABLE VII Br Hc Hci BHmax: . Hk G Oe Oe MGOe Oe 1O,000 9,800 > 20,000 25.0 13,000 Example 8: A rectangular preform which has the dimensions of a die cavity was loaded with powder and the powder was oriented in a pulse coil. The oriented powder in the preform was transferred to a die press and placed between the upper and lower punches. After all the powder had transferred into the die cavity the powder was pressed between the upper and lower punches under the application of a DC field. The die pressed part was sintered and post sintered. The magnet prepared in this manner had the following properties set forth on Table VIII. Example 9: From the same batch of powder one magnet was pressed by directly feeding the powder into the die cavity, applying the DC field, and pressing. The properties of these two magnets are set forth in Table VIII. TABLE VIII Br Hc Hci BHmax Hk G Oe Oe MGOe Oe Premagnetized powder in a preform before transferring into the die cavity 9,750 8,700 810,000 23.7 8,800 Direct location of powder in the die cavity 8,800 7,400 t10,000 19.0 6,000 It may be seen from the data reported in Examples 5 to 9 that aligning by the use of a pulsating magnetic field in accordance with the practice of the invention, as opposed to the conventional practice of aligning by the use of a steadystate magnetic field, resulted in improvement in remanence and energy product.

Claims: CLAIMS 1. A method for producing magnets with improved remanence by consolidating a particle charge of a magnet alloy to form a magnet article, characterised in that said method comprises applying a magnetic field to said particle charge within a container to magnetically align said particles, said magnetic field being applied as at least one pulse with each said pulse having a duration not exceeding one second and a power level of at least 50,000 oersted (39789 ampere turns per centimetre) and thereafter consolidating said particle charge to a final density. 2. The method of claim 1, characterised in that said particles are loaded into a collapsible container for magnetic alignment and subsequent consolidation. 3. The method of claim 2, characterised in that said container is a rubber bag. 4. The method of claim 1, 2 or 3 characterised in that said container is preformed to the desired shape of the particle charge after consolidation. > r 5. The method of 1any one of claims 1 to 4,' characterised in that said container is evacuated in the presence of a DC electric field after alignment of said particles. 6. The method of any one of the preceding claims, characterised in that said magnet alloy comprises at least one transition element and at least one rare earth element. 7. The method of claim 6, characterised in that at least one of said transition elements is cobalt. 8. The method of claim 6 or 7, characterised in that at least one of said rare earth elements is samarium. 9. The method of any one of the preceding claims, characterised in that after magnetic alignment bf said particles, said particles are compacted to an intermediate density by additional pulsing. 10. The method of any one of the preceding claims, characterised in that consolidation is by die pressing plus sintering. 11. The method of any one of the preceding claims 1 to 9, characterised in that consolidation is by cold isostatic compaction plus sintering. 12. A method for producing magnets with improved remanence by consolidating a particle charge of a magnet alloy to form a magnet article, characterised in that said method comprises applying a magnetic field to said particle charge to magnetically align said particles, and thereafter hot isostatically pressing said particles to consolidate the same to full density. 13. The method of claim 12, characterised in that prior to hot isostatic pressing said particle charge is heated to a temperature below the full density sintering temperature thereof but above the temperature necessary to render the particle charge substantially gas-impervious. 14. The method of claim 12 or 13, characterised in that said magnet alloy comprises at least one transition element and at least one rare earth element. 15. The method of claim 14, characterised in that at least one of said transition elements is cobalt. 16. The method of claim 14 or 15, characterised in that at least one of said rare earth elements is samarium. 17. The method of any one of claims 12 to 16, characterised in that the aligned charge is given preliminary room temperature densification by die pressing or cold isostatic compaction before heating or final densification.

Inventors: NARASIMHAN, KALATUR SABDAM VANGIPURAM LAKSHMI, PREUSCH, CHARLES DANIEL
Applicants: CRUCIBLE MATERIALS CORPORATION
Application year: 1982
Main classification: H01F1
IPC codes: H01F1, H01F13, H01F41