CN113496816A - Production method of samarium-cobalt-based permanent magnet block and samarium-cobalt-based permanent magnet block - Google Patents
Production method of samarium-cobalt-based permanent magnet block and samarium-cobalt-based permanent magnet block Download PDFInfo
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- 229910000938 samarium–cobalt magnet Inorganic materials 0.000 title claims abstract description 77
- KPLQYGBQNPPQGA-UHFFFAOYSA-N cobalt samarium Chemical compound [Co].[Sm] KPLQYGBQNPPQGA-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 29
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000000843 powder Substances 0.000 claims abstract description 43
- 239000011812 mixed powder Substances 0.000 claims abstract description 40
- 239000002994 raw material Substances 0.000 claims abstract description 39
- 238000000034 method Methods 0.000 claims abstract description 35
- 229910052742 iron Inorganic materials 0.000 claims abstract description 21
- 238000002425 crystallisation Methods 0.000 claims abstract description 19
- 230000008025 crystallization Effects 0.000 claims abstract description 19
- 238000000280 densification Methods 0.000 claims abstract description 19
- 239000011159 matrix material Substances 0.000 claims abstract description 15
- 238000000498 ball milling Methods 0.000 claims abstract description 8
- 230000001360 synchronised effect Effects 0.000 claims abstract description 4
- 238000003825 pressing Methods 0.000 claims description 80
- 238000004321 preservation Methods 0.000 claims description 40
- 230000008569 process Effects 0.000 claims description 16
- 230000006835 compression Effects 0.000 claims description 10
- 238000007906 compression Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 6
- 239000010941 cobalt Substances 0.000 claims description 4
- 229910017052 cobalt Inorganic materials 0.000 claims description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 4
- 238000012360 testing method Methods 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 description 10
- 230000009286 beneficial effect Effects 0.000 description 9
- 229910045601 alloy Inorganic materials 0.000 description 6
- 239000000956 alloy Substances 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 6
- 238000007731 hot pressing Methods 0.000 description 6
- 238000000227 grinding Methods 0.000 description 5
- 239000000696 magnetic material Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000006247 magnetic powder Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 4
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000000713 high-energy ball milling Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 229910052756 noble gas Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910000531 Co alloy Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 1
- QVYYOKWPCQYKEY-UHFFFAOYSA-N [Fe].[Co] Chemical compound [Fe].[Co] QVYYOKWPCQYKEY-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 230000005347 demagnetization Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 229910001172 neodymium magnet Inorganic materials 0.000 description 1
- 229910052754 neon Inorganic materials 0.000 description 1
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 150000002835 noble gases Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus 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
- H01F41/02—Apparatus 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
- H01F41/0253—Apparatus 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
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- 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
- H01F1/0555—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together
- H01F1/0556—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together pressed
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus 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
- H01F41/02—Apparatus 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
- H01F41/0253—Apparatus 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
- H01F41/0266—Moulding; Pressing
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F7/00—Magnets
- H01F7/02—Permanent magnets [PM]
- H01F7/0205—Magnetic circuits with PM in general
- H01F7/021—Construction of PM
-
- H—ELECTRICITY
- H02—GENERATION; CONVERSION OR DISTRIBUTION OF ELECTRIC POWER
- H02K—DYNAMO-ELECTRIC MACHINES
- H02K1/00—Details of the magnetic circuit
- H02K1/02—Details of the magnetic circuit characterised by the magnetic material
-
- H—ELECTRICITY
- H02—GENERATION; CONVERSION OR DISTRIBUTION OF ELECTRIC POWER
- H02K—DYNAMO-ELECTRIC MACHINES
- H02K1/00—Details of the magnetic circuit
- H02K1/06—Details of the magnetic circuit characterised by the shape, form or construction
-
- H—ELECTRICITY
- H02—GENERATION; CONVERSION OR DISTRIBUTION OF ELECTRIC POWER
- H02K—DYNAMO-ELECTRIC MACHINES
- H02K15/00—Methods or apparatus specially adapted for manufacturing, assembling, maintaining or repairing of dynamo-electric machines
- H02K15/02—Methods or apparatus specially adapted for manufacturing, assembling, maintaining or repairing of dynamo-electric machines of stator or rotor bodies
- H02K15/03—Methods or apparatus specially adapted for manufacturing, assembling, maintaining or repairing of dynamo-electric machines of stator or rotor bodies having permanent magnets
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Powder Metallurgy (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The invention discloses a production method of a samarium cobalt-based permanent magnet block and the samarium cobalt-based permanent magnet block. The method comprises the following steps: (1) performing ball milling on first mixed powder containing samarium-cobalt-based hard magnetic raw material powder and iron-based soft magnetic raw material powder to obtain second mixed powder containing an amorphous hard magnetic phase and a nano soft magnetic grain phase; the second mixed powder takes an amorphous hard magnetic phase as a matrix, and a nano-scale soft magnetic grain phase is distributed in the matrix; (2) the second mixed powder is formed into a green body, and then a pressure field and a thermal field are applied to the green body such that crystallization of at least a portion of the amorphous hard magnetic phase is synchronized with densification of at least a portion of the green body. The permanent magnet block obtained by the method has higher density and maximum magnetic energy product.
Description
Technical Field
The invention relates to a production method of a samarium-cobalt-based permanent magnet block and the samarium-cobalt-based permanent magnet block, in particular to a production method of an isotropic samarium-cobalt-based permanent magnet block and the samarium-cobalt-based permanent magnet block.
Background
The isotropic rare earth permanent magnet has the advantages of low rare earth content, short preparation period, high magnetic consistency, near-net shaping, capability of magnetizing to form any even number of inner circle magnetic poles and outer circle magnetic poles and the like, thereby being widely applied to the manufacture of precise motors and micro-special motors such as servo motors, direct current motors, brushless motors, starting motors and the like. At present, most of isotropic block magnets are neodymium-iron-boron type magnets subjected to Nd2Fe14The influence of the Curie temperature (nearly 310 ℃) of the B phase is that the use temperature is lower, mostly below 150 ℃, and the magnetic performance of the B phase is sharply reduced or even disappears due to the high-temperature use at the temperature higher than 240 ℃, especially higher than 300 ℃, so that the high-temperature use has great challenges. The samarium cobalt-based permanent magnet has a higher Curie temperature of 720-920 ℃, so that the samarium cobalt-based permanent magnet can be applied at a high temperature of more than 300 ℃, and has an obvious high-temperature use advantage. However, the maximum energy product of isotropic samarium cobalt-based permanent magnets is low due to the problems of excessive grain growth during high temperature fabrication (above 700 ℃) and difficulty in densification of the magnets at low temperatures.
CN104078175A discloses a preparation method of samarium cobalt based nanocrystalline permanent magnet material. Smelting the raw materials under the protection of inert gas to obtain samarium-cobalt-based alloy; mechanically crushing samarium-cobalt-based alloy into samarium-cobalt-based alloy coarse powder; milling samarium cobalt-based alloy coarse powder and iron powder by using a high-energy ball mill to obtain nano composite magnetic powder; and annealing the nanocrystalline composite magnetic powder under a vacuum condition. The method adds the organic ball grinding agent during ball milling, so that the magnetic powder is easy to oxidize during annealing, and the remanence and the magnetic energy product of the magnetic powder are lower. In addition, the method does not carry out high-pressure pressing when the magnetic measurement sample is prepared by adopting a pulsed magnetic field orientation method, so that the density of the permanent magnet is not high, and the magnetic performance of the permanent magnet is lower.
CN108335900A discloses a method for preparing SmCo7A method of a/Co composite permanent magnet. Physically mixing the crushed metals Sm and Co, and carrying out ball milling on the mixed metals in an inert atmosphere to obtain amorphous structure powder; and under the protection of inert gas, the amorphous structure powder is subjected to pressure sintering, the sintering temperature is 650-850 ℃, the sintering pressure is 1GPa, and the maximum magnetic energy product is only about 5 MGOe. The maximum magnetic energy product of the composite permanent magnet obtained by the method is low, a strong high-pressure condition of 1GPa is required in the high-temperature preparation process at 700-850 ℃, and the requirement on a pressing die is extremely high.
Disclosure of Invention
In view of this, the invention provides a method for producing a samarium cobalt-based permanent magnet block, which has a low preparation temperature, and the prepared samarium cobalt-based permanent magnet block has high density and maximum energy product. Further, the permanent magnet blocks obtained by the production method have larger size. Furthermore, the production method of the invention has lower pressing pressure, avoids harsh mold structure design and complex mold material selection, and is beneficial to industrial production.
In another aspect, the present invention provides a samarium cobalt based permanent magnet block having isotropy, higher density and maximum energy product, and larger size.
The technical purpose is achieved through the following technical scheme.
In one aspect, the invention provides a method for producing samarium cobalt-based permanent magnet blocks, which comprises the following steps:
(1) performing ball milling on first mixed powder containing samarium-cobalt-based hard magnetic raw material powder and iron-based soft magnetic raw material powder to obtain second mixed powder containing an amorphous hard magnetic phase and a nano soft magnetic grain phase; the second mixed powder takes an amorphous hard magnetic phase as a matrix, and a nano-scale soft magnetic grain phase is distributed in the matrix;
(2) the second mixed powder is formed into a green body, and then a pressure field and a thermal field are applied to the green body such that crystallization of at least a portion of the amorphous hard magnetic phase is synchronized with densification of at least a portion of the green body.
According to the production method of the present invention, preferably, a crystallization process of a part of the amorphized hard magnetic phase and a part of a densification process of the green compact are performed simultaneously.
According to the production method of the present invention, preferably, the crystallization process of the entire amorphized hard magnetic phase and the entire densification process of the green compact are performed simultaneously.
According to the production method of the present invention, preferably, at least a part of the crystallization process of the amorphized hard magnetic phase and at least a part of the densification process of the green body are carried out under the combined action of the pressure field and the thermal force field.
According to the production method of the present invention, preferably, the manner of applying the pressure field and the thermal force field to the green body is selected from one of the following manners:
(1) synchronously raising the pressure and the temperature to the highest pressure and the highest pressure temperature, and then carrying out heat preservation and pressure maintaining;
(2) synchronously raising the pressure and the temperature, reaching the highest pressing pressure, and then carrying out heat preservation and pressure maintaining after reaching the highest pressing temperature;
(3) synchronously raising the pressure and the temperature, reaching the highest pressing temperature, and then carrying out heat preservation and pressure maintaining after reaching the highest pressing pressure;
(4) raising the temperature to a preset temperature, synchronously raising the pressure and the temperature to the highest pressure and the highest pressure, and then carrying out heat preservation and pressure maintaining;
(5) raising the temperature to a preset temperature, then raising the pressure and the temperature synchronously, reaching the highest pressing temperature, and then carrying out heat preservation and pressure maintaining after reaching the highest pressing pressure;
(6) raising the temperature to a preset temperature, and then raising the pressure and the temperature synchronously, wherein the highest pressing pressure is reached, and then the temperature is kept and the pressure is maintained after the highest pressing temperature is reached;
(7) raising the temperature to a preset temperature, raising the pressure to the highest pressure at the preset temperature, raising the temperature to the highest pressure, and then carrying out heat preservation and pressure maintaining;
(8) raising the pressure to a preset pressure, and then synchronously raising the pressure and the temperature to a highest pressure and a highest pressure temperature, and then carrying out heat preservation and pressure maintaining;
(9) raising the pressure to a preset pressure, raising the pressure and the temperature synchronously, reaching the highest pressing temperature, and then preserving heat and pressure after reaching the highest pressing pressure;
(10) raising the pressure to a preset pressure, then raising the pressure and the temperature synchronously, reaching the highest pressing pressure, and then carrying out heat preservation and pressure maintaining after reaching the highest pressing temperature;
(11) raising the pressure to a preset pressure, raising the temperature to the highest pressing temperature under the preset pressure, raising the pressure to the highest pressing pressure, and then carrying out heat preservation and pressure maintaining;
wherein the preset temperature is lower than the highest pressing temperature, and the preset pressure is lower than the highest pressing pressure.
According to the production method provided by the invention, preferably, the maximum pressing temperature is 420-600 ℃, the maximum pressing pressure is 800-2000MPa, the preset temperature is 250-410 ℃, the preset pressure is 300-700 MPa, and the heat preservation and pressure maintaining time is 1-60 min.
According to the production method of the present invention, preferably, the manner of applying the pressure field and the thermal force field to the green body is selected from one of the following manners:
(A) synchronously raising the pressure and the temperature, and carrying out heat preservation and pressure maintaining for 1-60 min after the preset temperature of 250-410 ℃ reaches the maximum compression pressure of 800-2000MPa and then the maximum compression temperature of 420-600 ℃;
(B) and raising the temperature to a preset temperature of 250-410 ℃, synchronously raising the pressure and the temperature to a maximum compression pressure of 800-2000MPa and a maximum compression temperature of 420-600 ℃, and then carrying out heat preservation and pressure maintaining for 1-60 min.
According to the production method of the present invention, preferably, the samarium cobalt-based hard magnetic raw material powder has SmCoxThe composition of the representation,x represents the atomic ratio of Co to Sm, and x is more than or equal to 1.5 and less than or equal to 12; the size of the cobalt-based hard magnetic material powder is 5-200 microns;
the iron-based soft magnetic raw material powder has Fe100-yCoyThe composition is expressed, y represents the atomic percent of Co, and y is more than or equal to 0 and less than 100; the size of the iron-based soft magnetic raw material powder is 1-50 microns.
According to the production method of the invention, preferably, the weight ratio of the samarium cobalt-based hard magnetic raw material powder to the iron-based soft magnetic raw material powder is 1.5-9.
On the other hand, the samarium-cobalt-based permanent magnet block prepared by the method has isotropy, the diameter of the samarium-cobalt-based permanent magnet block is larger than 10mm, the height of the samarium-cobalt-based permanent magnet block is larger than 2.5mm, the density is larger than 98%, and the maximum magnetic energy product is 18-23 MGOe;
wherein the density represents the percentage of the measured density of the permanent magnet blocks to the theoretical density; the actually measured density is measured by adopting an Archimedes drainage method; for samarium cobalt-based permanent magnet blocks with the height less than 5mm, the maximum energy product is measured by a vibration sample magnetometer at room temperature in a maximum magnetic field of 2.1T, the permanent magnet block for testing is firstly cut, and then magnetizing treatment is carried out under a pulse magnetic field of 7-8T; for samarium-cobalt-based permanent magnet blocks with the height of more than or equal to 5mm, the maximum magnetic energy product is measured by adopting a pulsed magnetic field measuring instrument under the maximum magnetic field of 8T.
In the production method, the crystallization process of the amorphous hard magnetic phase and the densification process of the green body are synchronously carried out under the action of the pressure field and the thermal force field, so that the isotropic samarium-cobalt-based permanent magnet block with higher density and maximum energy product is obtained under the condition of lower temperature. Further, the permanent magnet blocks of the present invention have a large size. According to the preferred technical scheme, the pressing pressure is lower, the harsh mold structure design and the complex mold material selection are avoided, and the industrial production is facilitated.
Drawings
Fig. 1 is an XRD spectrum of samarium cobalt based permanent magnet blocks of example 1, example 2 and comparative example 1.
Detailed Description
The present invention will be further described with reference to the following specific examples, but the scope of the present invention is not limited thereto.
In the present invention, pressure means absolute pressure, i.e., pressure directly acting on the surface of a container or object.
The inert gas includes nitrogen or a noble gas. Examples of noble gases include, but are not limited to, helium, neon, argon.
The density represents the percentage of the measured density of the permanent magnet blocks relative to the theoretical density. The test methods are described in detail below.
The residual magnetism is a value of magnetic flux density corresponding to a place where the magnetic field intensity is zero on the saturation hysteresis line, and the unit is Tesla (T) or Gaussian (Gs).
The magnetic energy product is the product of the magnetic flux density (B) and the corresponding magnetic field strength (H) at any point on the demagnetization curve. Its maximum value is the "maximum energy product" in gauss oersted (GOe).
The room temperature may be referred to as normal temperature or ordinary temperature, and is about 16 to 35 ℃.
An anaerobic environment is one that is free of oxygen or contains only a small amount of oxygen.
In the present invention, the preset temperature is lower than the maximum pressing temperature, and the preset pressure is lower than the maximum pressing pressure.
< production method >
The production method of the samarium cobalt-based permanent magnet block comprises the following steps: (1) mixing a hard magnetic raw material and a soft magnetic raw material; (2) and (4) crystallizing and densifying. The method adopts a method of simultaneously raising temperature and pressure to synchronously carry out the crystallization process and the densification process, thereby improving the density and the maximum energy product of the samarium-cobalt-based permanent magnet block. If the temperature is firstly raised to the highest temperature and then the pressure is raised, the magnet presents the process of crystallization first and densification later, so that the regulation and control of the pressure on the amorphous crystallization process are basically lost, and the maximum energy product of the obtained permanent magnet block is lower.
The samarium cobalt-based permanent magnet block obtained by the method has isotropy. The diameter of the samarium-cobalt-based permanent magnet block is larger than 10mm, and the height of the samarium-cobalt-based permanent magnet block is larger than 2.5 mm; preferably, the height is greater than 3.3 mm; more preferably, the height is greater than 6 mm. The density of the samarium cobalt-based permanent magnet block is more than 98 percent; preferably, greater than 98.5%; more preferably, greater than 99%. The maximum magnetic energy product of the samarium-cobalt-based permanent magnet block is 18-23 MGOe; preferably 20 to 23 MGOe; more preferably 21 to 23 MGOe.
As will be explained in detail below.
< step of mixing hard magnetic Material and Soft magnetic Material >
Performing ball milling on first mixed powder containing samarium-cobalt-based hard magnetic raw material powder and iron-based soft magnetic raw material powder to obtain second mixed powder containing an amorphous hard magnetic phase and a nano soft magnetic grain phase; the second mixed powder takes an amorphous hard magnetic phase as a matrix, and a nanometer soft magnetic grain phase is distributed in the matrix. Preferably, a first mixed powder composed of a samarium cobalt-based hard magnetic raw material powder and an iron-based soft magnetic raw material powder is ball-milled to obtain a second mixed powder containing an amorphized hard magnetic phase and a nano-scale soft magnetic grain phase.
In the present invention, the samarium cobalt-based hard magnetic raw material powder may have a composition represented by the formula (1):
SmCox (1)
wherein x represents the atomic ratio of Co to Sm, and x is more than or equal to 1.5 and less than or equal to 12; preferably, 3. ltoreq. x.ltoreq.7.
Examples of samarium cobalt-based hard magnetic feedstock powders of the present invention include, but are not limited to, SmCo2、SmCo3、Sm2Co7、SmCo5、SmCo7、SmCo12. Preferably SmCo5. The average particle size of the cobalt-based hard magnetic material is 5-200 microns, preferably 10-180 microns, and more preferably 50-150 microns. This is beneficial to improving the maximum magnetic energy product of the permanent magnet block.
In the present invention, the iron-based soft magnetic raw material powder may have a composition as shown in formula (2):
Fe100-yCoy
wherein y represents the atomic percent of Co, and y is more than or equal to 0 and less than 100.
The iron-based soft magnetic raw material powder of the present invention may be an iron powder or an iron-cobalt alloy powder, and is preferably an iron powder. The average particle size of the iron-based soft magnetic material can be 1-50 micrometers, preferably 2-30 micrometers, and more preferably 5-10 micrometers. This is beneficial to improving the maximum magnetic energy product of the permanent magnet block.
In the invention, the weight ratio of the samarium cobalt-based hard magnetic raw material powder to the iron-based soft magnetic raw material powder can be 1.5-9; preferably 1.9 to 5.7; more preferably 2.3 to 4. This is beneficial to improving the maximum magnetic energy product of the permanent magnet block.
The equipment used for ball milling in the invention can be a vibration ball mill and a planetary ball mill. In certain embodiments of the invention, the equipment used for ball milling is a Spex-8000D three-dimensional vibration ball mill, the mass ratio of the grinding balls to the first mixed powder is (15-30): 1, and the grinding time is 3-10 h. Thus, the iron-based soft magnetic raw material is beneficial to being subjected to nano-size transformation, and nano-scale soft magnetic grains are more uniformly distributed in the amorphous hard magnetic phase matrix, so that the maximum magnetic energy and the density of the permanent magnetic block are improved.
< step of crystallization and densification >
The second mixed powder is formed into a green body, and then a pressure field and a thermal field are applied to the green body such that crystallization of at least a portion of the amorphous hard magnetic phase is synchronized with densification of at least a portion of the green body. In certain embodiments of the present invention, the crystallization of a portion of the amorphized hard magnetic phase is performed simultaneously with a portion of the densification of the green body. In other embodiments of the present invention, the crystallization process of the entire amorphized hard magnetic phase and the entire densification process of the green body are performed simultaneously. In still other embodiments of the present invention, the crystallization of at least a portion of the amorphized hard magnetic phase and at least a portion of the densification of the green body are performed in the co-action of a pressure field and a thermal field.
In the present invention, the second mixed powder may be formed into a green body by means of pressing. The pressing pressure can be 100-800 MPa; preferably 300-700 MPa; more preferably 400 to 600 MPa. In certain embodiments of the invention, the second mixed powder is placed in a compaction die; and applying 300-800 MPa pressure to the pressing die in an oxygen-free environment at the temperature of 0-450 ℃ to form a green body. The oxygen-free environment may be provided by a glove box filled with an inert gas or by a hot press. The pressing temperature is preferably 10-50 ℃; more preferably 16 to 35 ℃. This is beneficial to improving the maximum magnetic energy product of the permanent magnet block. In the present invention, the pressing die may be pressed by a hydraulic press or a tablet press. The compacting die may be coated with a release agent to facilitate separation of the permanent magnet blocks from the compacting die. The release agent can be selected from one or more of molybdenum disulfide, boron nitride and graphite.
In the present invention, the manner of applying the pressure field and the thermal force field to the green body may be selected from one of the following manners:
(1) synchronously raising the pressure and the temperature to the highest pressure and the highest pressure temperature, and then carrying out heat preservation and pressure maintaining;
(2) synchronously raising the pressure and the temperature, reaching the highest pressing pressure, and then carrying out heat preservation and pressure maintaining after reaching the highest pressing temperature; preferably, the preset temperature is reached when the maximum compression pressure is reached;
(3) synchronously raising the pressure and the temperature, reaching the highest pressing temperature, and then carrying out heat preservation and pressure maintaining after reaching the highest pressing pressure; preferably, the preforming pressure is reached when the maximum pressing temperature is reached;
(4) raising the temperature to a preset temperature, synchronously raising the pressure and the temperature to the highest pressure and the highest pressure, and then carrying out heat preservation and pressure maintaining;
(5) raising the temperature to a preset temperature, then raising the pressure and the temperature synchronously, reaching the highest pressing temperature, and then carrying out heat preservation and pressure maintaining after reaching the highest pressing pressure;
(6) raising the temperature to a preset temperature, and then raising the pressure and the temperature synchronously, wherein the highest pressing pressure is reached, and then the temperature is kept and the pressure is maintained after the highest pressing temperature is reached;
(7) raising the temperature to a preset temperature, raising the pressure to the highest pressure at the preset temperature, raising the temperature to the highest pressure, and then carrying out heat preservation and pressure maintaining;
(8) raising the pressure to a preset pressure, and then synchronously raising the pressure and the temperature to a highest pressure and a highest pressure temperature, and then carrying out heat preservation and pressure maintaining;
(9) raising the pressure to a preset pressure, raising the pressure and the temperature synchronously, reaching the highest pressing temperature, and then preserving heat and pressure after reaching the highest pressing pressure;
(10) raising the pressure to a preset pressure, then raising the pressure and the temperature synchronously, reaching the highest pressing pressure, and then carrying out heat preservation and pressure maintaining after reaching the highest pressing temperature;
(11) and raising the pressure to a preset pressure, raising the temperature to the highest pressing temperature under the preset pressure, raising the pressure to the highest pressing pressure, and then carrying out heat preservation and pressure maintaining.
In the manner of applying the pressure field and the thermal field to the green body, the maximum pressing temperature can be 420-600 ℃; preferably 450-550 ℃; more preferably 470 to 540 ℃. The maximum pressure can be 800-; preferably 1300-2000 MPa; more preferably 1500-. The preset temperature can be 250-410 ℃; preferably 300-400 ℃; more preferably 330 to 400 ℃. The preset pressure can be 300-700 MPa; preferably 350-700 MPa; more preferably 400 to 700 MPa. The heat preservation and pressure maintaining time can be 1-60 min; preferably 5-40 min; more preferably 10 to 30 min. Thus being beneficial to improving the density and the maximum magnetic energy product of the permanent magnet block body.
In some embodiments, the pressure and the temperature are synchronously increased, and the heat preservation and pressure maintaining are carried out for 1-60 min after the preset temperature of 250-410 ℃ reaches the maximum pressure of 800-2000MPa and then reaches the maximum pressure of 420-600 ℃. The maximum pressure can be 800-; preferably 1300-2000 MPa; more preferably 1500-. The preset temperature can be 250-410 ℃; preferably 300-400 ℃; more preferably 330 to 400 ℃. The maximum pressing temperature can be 420-600 ℃; preferably 450-550 ℃; more preferably 470 to 530 ℃. The heat preservation and pressure maintaining time can be 1-60 min; preferably 5-30 min; more preferably 10 to 15 min. Thus being beneficial to improving the maximum magnetic energy and the density of the permanent magnet block.
In other embodiments, the temperature is increased to a preset temperature of 250-410 ℃, then the pressure and the temperature are synchronously increased to the maximum compression pressure of 800-2000MPa and the maximum compression temperature of 420-600 ℃, and then the heat preservation and pressure maintaining are carried out for 1-60 min. The preset temperature can be 250-410 ℃; preferably 300-400 ℃; more preferably 330 to 400 ℃. The maximum compression pressure can be 800-2000 MPa; preferably 1300-2000 MPa; more preferably 1500 to 2000 MPa. The maximum pressing temperature can be 420-600 ℃; preferably 450-550 ℃; more preferably 470 to 530 ℃. The heat preservation and pressure maintaining time can be 1-60 min; preferably 5-40 min; more preferably 10 to 30 min. Thus being beneficial to improving the maximum magnetic energy and the density of the permanent magnet block.
< samarium cobalt-based permanent magnet bulk >
The samarium cobalt-based permanent magnet block body is prepared by the method. The samarium cobalt based permanent magnet block has isotropy. The diameter of the samarium-cobalt-based permanent magnet block is larger than 10mm, and the height of the samarium-cobalt-based permanent magnet block is larger than 2.5 mm; preferably, the height is greater than 3.3 mm; more preferably, the height is greater than 6 mm. The density of the samarium cobalt-based permanent magnet block is more than 98 percent; preferably, greater than 98.5%; more preferably, greater than 99%. The maximum magnetic energy product of the samarium-cobalt-based permanent magnet block is 18-23 MGOe; preferably 20 to 23 MGOe; more preferably 21 to 23 MGOe.
The samarium cobalt based permanent magnet blocks obtained in the following examples and comparative examples are described below:
density: the density is measured density/theoretical density multiplied by 100 percent;
the actually measured density is measured by an Archimedes drainage method.
Remanence Br and maximum energy product (BH)max: for a magnet with the height less than 5mm, the maximum energy product is measured by a vibration sample magnetometer (lakeshore 7410) at room temperature at the maximum magnetic field of 2.1T, and the permanent magnet blocks obtained by pressing before the test are cut into small blocks and are magnetized under the pulse magnetic field of 7-8T; for the magnet with the height being more than or equal to 5mm, the maximum magnetic energy product is measured by adopting a pulse magnetic field measuring instrument under the maximum magnetic field of 8T.
Comparative example 1
(1) Sieving samarium cobalt-based hard magnetic raw material powder (SmCo) with 100 mesh sieve5About 150 microns) and 1500 mesh sieved iron-based soft magnetic raw material powder (Fe, about 10 microns) were uniformly mixed to obtain a first mixed powder(the weight ratio of the samarium cobalt-based hard magnetic raw material powder to the iron-based soft magnetic raw material powder in the first mixed powder was 3.0). Placing the first mixed powder in a Spex-8000D three-dimensional vibration ball mill (the mass ratio of grinding balls to the first mixed powder is 20:1) under the protection of inert gas for high-energy ball milling for 3 hours to obtain second mixed powder containing an amorphous hard magnetic phase and a nanometer soft magnetic crystal particle phase; the second mixed powder takes an amorphous hard magnetic phase as a matrix, and a nanometer soft magnetic grain phase is distributed in the matrix.
(2) Placing the second mixed powder in a pressing die coated with a molybdenum disulfide release agent in a glove box filled with inert gas; at room temperature, a press of 500MPa was applied to the press dies by a tablet press to form a green body.
(3) Placing the green body and the corresponding pressing mold in a hot pressing furnace, and vacuumizing the hot pressing furnace to 1 × 10-3And Pa, raising the temperature to the highest pressing temperature of 500 ℃, and then raising the pressure to the highest pressing pressure of 2000MPa for heat preservation and pressure maintenance for 13min to obtain the samarium-cobalt-based permanent magnet block. The density is 98.9 percent, the remanence Br is 11.3kGs, and the maximum energy product (BH)max17.0MGOe, and the size of the permanent magnet block is phi 10 multiplied by 3 mm.
Examples 1 to 3
(1) Sieving samarium cobalt-based hard magnetic raw material powder (SmCo) with 100 mesh sieve5About 150 microns) and 1500 mesh sieved iron-based soft magnetic raw material powder (Fe, about 10 microns) were uniformly mixed to obtain a first mixed powder (the weight ratio of the samarium cobalt-based hard magnetic raw material powder to the iron-based soft magnetic raw material powder in the first mixed powder was 3.0). And (3) placing the first mixed powder in a Spex-8000D three-dimensional vibration ball mill under the protection of inert gas for high-energy ball milling for 3h to obtain second mixed powder containing an amorphous hard magnetic phase and a nano soft magnetic crystal particle phase. The second mixed powder takes an amorphous hard magnetic phase as a matrix, and a nano-scale soft magnetic grain phase is distributed in the matrix.
(2) Placing the second mixed powder in a WC hard alloy pressing die coated with a molybdenum disulfide release agent in a glove box filled with inert gas; and applying 500MPa pressure to the pressing die through a hydraulic press at room temperature to form a green body.
(3) Mixing the green bodyAnd placing the corresponding pressing mould in a hot-pressing furnace, and vacuumizing the hot-pressing furnace to 1 × 10-3Pa, synchronously raising the pressure and the temperature, reaching the highest pressing pressure when reaching the preset temperature, then continuing to raise the temperature to reach the highest pressing temperature of 500 ℃ and carrying out heat preservation and pressure maintenance for 13min to obtain the samarium-cobalt-based permanent magnet block. See table 1 for specific parameters and table 2 for properties of samarium cobalt based permanent magnet blocks.
As can be seen from FIG. 1, comparing examples 1-2 with comparative example 1, the hard magnetic phase of the samarium cobalt-based permanent magnet bulk is Sm in a manner that crystallization and densification are simultaneously performed2Co17The phase is mainly changed into SmCo3The phase is dominant, and the content of the soft magnetic phase is obviously increased. This demonstrates the effectiveness of the treatment regime for magnet microstructure and magnet performance control.
TABLE 1
TABLE 2
Examples 4 to 11
(1) Sieving samarium cobalt-based hard magnetic raw material powder (SmCo) with 100 mesh sieve5About 150 microns) and 1500 mesh sieved iron-based soft magnetic raw material powder (Fe, about 10 microns) were uniformly mixed to obtain a first mixed powder. And (3) placing the first mixed powder in a Spex-8000D three-dimensional vibration ball mill (the mass ratio of the grinding balls to the first mixed powder is 25:1) under the protection of inert gas for high-energy ball milling for 3 hours to obtain second mixed powder containing an amorphous hard magnetic phase and a nanometer soft magnetic crystal particle phase. The second mixed powder takes an amorphous hard magnetic phase as a matrix, and a nano-scale soft magnetic grain phase is distributed in the matrix.
(2) Placing the second mixed powder in a WC hard alloy pressing die coated with a molybdenum disulfide release agent in a glove box filled with inert gas; and applying a pressure of 600MPa to the pressing die through a hydraulic press at room temperature to form a green body.
(3) Placing the green body and the corresponding pressing mold in a hot pressing furnace, and vacuumizing the hot pressing furnace to 1 × 10-3And Pa, raising the temperature to a preset temperature, and then synchronously raising the pressure and the temperature to the highest pressing pressure and the highest pressing temperature and then carrying out heat preservation and pressure maintaining to obtain the samarium-cobalt-based permanent magnet block. See table 3 for specific parameters and table 4 for properties of samarium cobalt based permanent magnet blocks.
TABLE 3
TABLE 4
The present invention is not limited to the above-described embodiments, and any variations, modifications, and substitutions which may occur to those skilled in the art may be made without departing from the spirit of the invention.
Claims (10)
1. A production method of a samarium cobalt-based permanent magnet block is characterized by comprising the following steps:
(1) performing ball milling on first mixed powder containing samarium-cobalt-based hard magnetic raw material powder and iron-based soft magnetic raw material powder to obtain second mixed powder containing an amorphous hard magnetic phase and a nano soft magnetic grain phase; the second mixed powder takes an amorphous hard magnetic phase as a matrix, and a nano-scale soft magnetic grain phase is distributed in the matrix;
(2) the second mixed powder is formed into a green body, and then a pressure field and a thermal field are applied to the green body such that crystallization of at least a portion of the amorphous hard magnetic phase is synchronized with densification of at least a portion of the green body.
2. The production method as claimed in claim 1, wherein the crystallization of a part of the amorphized hard magnetic phase and a part of the densification of the green body are carried out simultaneously.
3. The production method according to claim 1, wherein the crystallization process of the entire amorphized hard magnetic phase and the entire densification process of the green body are performed simultaneously.
4. The method of claim 1, wherein at least a portion of the crystallization of the amorphized hard magnetic phase and at least a portion of the densification of the green body are performed in combination in a pressure field and a thermal field.
5. The method of claim 1, wherein the green body is subjected to the pressure field and the thermal field in a manner selected from one of the following manners:
(1) synchronously raising the pressure and the temperature to the highest pressure and the highest pressure temperature, and then carrying out heat preservation and pressure maintaining;
(2) synchronously raising the pressure and the temperature, reaching the highest pressing pressure, and then carrying out heat preservation and pressure maintaining after reaching the highest pressing temperature;
(3) synchronously raising the pressure and the temperature, reaching the highest pressing temperature, and then carrying out heat preservation and pressure maintaining after reaching the highest pressing pressure;
(4) raising the temperature to a preset temperature, synchronously raising the pressure and the temperature to the highest pressure and the highest pressure, and then carrying out heat preservation and pressure maintaining;
(5) raising the temperature to a preset temperature, then raising the pressure and the temperature synchronously, reaching the highest pressing temperature, and then carrying out heat preservation and pressure maintaining after reaching the highest pressing pressure;
(6) raising the temperature to a preset temperature, and then raising the pressure and the temperature synchronously, wherein the highest pressing pressure is reached, and then the temperature is kept and the pressure is maintained after the highest pressing temperature is reached;
(7) raising the temperature to a preset temperature, raising the pressure to the highest pressure at the preset temperature, raising the temperature to the highest pressure, and then carrying out heat preservation and pressure maintaining;
(8) raising the pressure to a preset pressure, and then synchronously raising the pressure and the temperature to a highest pressure and a highest pressure temperature, and then carrying out heat preservation and pressure maintaining;
(9) raising the pressure to a preset pressure, raising the pressure and the temperature synchronously, reaching the highest pressing temperature, and then preserving heat and pressure after reaching the highest pressing pressure;
(10) raising the pressure to a preset pressure, then raising the pressure and the temperature synchronously, reaching the highest pressing pressure, and then carrying out heat preservation and pressure maintaining after reaching the highest pressing temperature;
(11) raising the pressure to a preset pressure, raising the temperature to the highest pressing temperature under the preset pressure, raising the pressure to the highest pressing pressure, and then carrying out heat preservation and pressure maintaining;
wherein the preset temperature is lower than the highest pressing temperature, and the preset pressure is lower than the highest pressing pressure.
6. The production method according to claim 5, wherein the maximum pressing temperature is 420 to 600 ℃, the maximum pressing pressure is 800 to 2000MPa, the preset temperature is 250 to 410 ℃, the preset pressure is 300 to 700MPa, and the holding time is 1 to 60 min.
7. The method of claim 1, wherein the green body is subjected to the pressure field and the thermal field in a manner selected from one of the following manners:
(A) synchronously raising the pressure and the temperature, reaching the maximum pressure of 800-2000MPa at the preset temperature of 250-410 ℃, and then carrying out heat preservation and pressure maintaining for 1-60 min after reaching the maximum pressure temperature of 420-600 ℃;
(B) and raising the temperature to a preset temperature of 250-410 ℃, synchronously raising the pressure and the temperature to a maximum compression pressure of 800-2000MPa and a maximum compression temperature of 420-600 ℃, and then carrying out heat preservation and pressure maintaining for 1-60 min.
8. The production method according to claim 1, characterized in that:
the cobalt-based hard magnetic samarium cobalt powder has SmCoxThe composition represented by (1.5) x is not less than 12; the size of the cobalt-based hard magnetic raw material powder is 5-200 microns；
The iron-based soft magnetic raw material powder has Fe100-yCoyThe composition represented by (A) and (B), y represents the atomic percent of Co, and 0. ltoreq. y<100, respectively; the size of the iron-based soft magnetic raw material powder is 1-50 microns.
9. The production method of claim 1, the weight ratio of samarium cobalt based hard magnetic raw material powder to iron based soft magnetic raw material powder being 1.5 to 9.
10. The samarium cobalt-based permanent magnet block obtained by the production method according to any one of claims 1 to 9, wherein the samarium cobalt-based permanent magnet block has isotropy, the diameter of the samarium cobalt-based permanent magnet block is more than 10mm, the height of the samarium cobalt-based permanent magnet block is more than 2.5mm, the density is more than 98%, and the maximum magnetic energy product is 18 to 23 MGOe;
wherein the density represents the percentage of the measured density of the permanent magnet block body relative to the theoretical density; the actually measured density is measured by adopting an Archimedes drainage method; for samarium cobalt-based permanent magnet blocks with the height less than 5mm, the maximum energy product is measured by a vibration sample magnetometer at room temperature in a maximum magnetic field of 2.1T, the permanent magnet block for testing is firstly cut, and then magnetizing treatment is carried out under a pulse magnetic field of 7-8T; for samarium-cobalt-based permanent magnet blocks with the height of more than or equal to 5mm, the maximum magnetic energy product is measured by adopting a pulsed magnetic field measuring instrument under the maximum magnetic field of 8T.
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