CN115747611B - 一种辅合金铸片和高剩磁高矫顽力钕铁硼永磁体及制备方法 - Google Patents
一种辅合金铸片和高剩磁高矫顽力钕铁硼永磁体及制备方法 Download PDFInfo
- Publication number
- CN115747611B CN115747611B CN202211255156.5A CN202211255156A CN115747611B CN 115747611 B CN115747611 B CN 115747611B CN 202211255156 A CN202211255156 A CN 202211255156A CN 115747611 B CN115747611 B CN 115747611B
- Authority
- CN
- China
- Prior art keywords
- casting
- auxiliary alloy
- temperature
- alloy
- permanent magnet
- 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.)
- Active
Links
- 239000000956 alloy Substances 0.000 title claims abstract description 137
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 134
- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 title claims description 20
- 238000005266 casting Methods 0.000 claims abstract description 97
- 239000002994 raw material Substances 0.000 claims abstract description 27
- 238000003723 Smelting Methods 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000007670 refining Methods 0.000 claims abstract description 20
- 238000001816 cooling Methods 0.000 claims description 69
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 60
- 239000000843 powder Substances 0.000 claims description 54
- 238000005496 tempering Methods 0.000 claims description 33
- 238000005245 sintering Methods 0.000 claims description 32
- 229910052786 argon Inorganic materials 0.000 claims description 30
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 28
- 239000001257 hydrogen Substances 0.000 claims description 28
- 229910052739 hydrogen Inorganic materials 0.000 claims description 28
- 238000004321 preservation Methods 0.000 claims description 28
- 238000000227 grinding Methods 0.000 claims description 25
- 238000006356 dehydrogenation reaction Methods 0.000 claims description 20
- 239000000314 lubricant Substances 0.000 claims description 20
- 238000011049 filling Methods 0.000 claims description 19
- 238000000465 moulding Methods 0.000 claims description 15
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 13
- 239000002245 particle Substances 0.000 claims description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 9
- 238000010521 absorption reaction Methods 0.000 claims description 9
- 229910052802 copper Inorganic materials 0.000 claims description 9
- 239000010949 copper Substances 0.000 claims description 9
- 229910052779 Neodymium Inorganic materials 0.000 claims description 8
- 238000009826 distribution Methods 0.000 claims description 6
- 230000006698 induction Effects 0.000 claims description 6
- 238000009740 moulding (composite fabrication) Methods 0.000 claims description 5
- 238000010902 jet-milling Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000010936 titanium Substances 0.000 abstract description 21
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 11
- 150000002910 rare earth metals Chemical class 0.000 abstract description 11
- 229910052719 titanium Inorganic materials 0.000 abstract description 10
- 229910052720 vanadium Inorganic materials 0.000 abstract description 9
- 229910052692 Dysprosium Inorganic materials 0.000 abstract description 8
- 229910052771 Terbium Inorganic materials 0.000 abstract description 8
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 abstract description 8
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 abstract description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 5
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 description 23
- 239000007789 gas Substances 0.000 description 11
- 150000002632 lipids Chemical class 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 229910052796 boron Inorganic materials 0.000 description 8
- 230000001276 controlling effect Effects 0.000 description 8
- 238000013461 design Methods 0.000 description 6
- 229910052733 gallium Inorganic materials 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000007712 rapid solidification Methods 0.000 description 5
- 239000003963 antioxidant agent Substances 0.000 description 4
- 230000003078 antioxidant effect Effects 0.000 description 4
- 230000005347 demagnetization Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 3
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 3
- PSGHJMHNCHBIIL-UHFFFAOYSA-N [B].[Fe].[Dy] Chemical compound [B].[Fe].[Dy] PSGHJMHNCHBIIL-UHFFFAOYSA-N 0.000 description 1
- BDGLPDLXSOLKRB-UHFFFAOYSA-N [B].[Fe].[Tb] Chemical compound [B].[Fe].[Tb] BDGLPDLXSOLKRB-UHFFFAOYSA-N 0.000 description 1
- RKLPWYXSIBFAJB-UHFFFAOYSA-N [Nd].[Pr] Chemical compound [Nd].[Pr] RKLPWYXSIBFAJB-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000007306 turnover Effects 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
-
- 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
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
-
- 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
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
-
- 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
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
-
- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
-
- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/16—Both compacting and sintering in successive or repeated steps
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/002—Making metallic powder or suspensions thereof amorphous or microcrystalline
- B22F9/008—Rapid solidification processing
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/023—Hydrogen absorption
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/04—Making ferrous alloys by melting
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
-
- 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
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0573—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes obtained by reduction or by hydrogen decrepitation or embrittlement
-
- 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
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
-
- 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
-
- 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
- H01F41/0273—Imparting anisotropy
-
- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal after-treatment
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/044—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by jet milling
-
- 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
- B22F2201/00—Treatment under specific atmosphere
- B22F2201/20—Use of vacuum
-
- 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
- B22F2202/00—Treatment under specific physical conditions
- B22F2202/05—Use of magnetic field
-
- 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
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/35—Iron
- B22F2301/355—Rare Earth - Fe intermetallic alloys
-
- 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
- B22F2304/00—Physical aspects of the powder
- B22F2304/10—Micron size particles, i.e. above 1 micrometer up to 500 micrometer
-
- 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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
-
- 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
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C2202/00—Physical properties
- C22C2202/02—Magnetic
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Nanotechnology (AREA)
- Hard Magnetic Materials (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
Abstract
本发明提供了一种辅合金铸片和高剩磁高矫顽力钕铁硼永磁体及制备方法,属于永磁体技术领域。本发明中辅合金铸片的制备方法包括以下步骤:提供辅合金原料,按质量分数计,所述辅合金原料的组成包括Pr40~45%,Co1~2%,Ga0.5~1%,B0.6~0.8%,V0.1~0.2%,Ti0.3~0.7%,余量的Fe;将所述辅合金原料进行熔炼,得到熔炼物料;将所述熔炼物料进行速凝铸片,得到辅合金铸片;所述速凝铸片包括依次进行精炼和浇铸。本发明在辅合金铸片中引入钛和钒,并配合特定的速凝铸片工艺,所得辅合金铸片中富含球状微观组织,利用该辅合金铸片能够制备得到无重稀土镝和铽的高性能烧结钕铁硼永磁体。
Description
技术领域
本发明涉及永磁体技术领域,尤其涉及一种辅合金铸片和高剩磁高矫顽力钕铁硼永磁体及制备方法。
背景技术
高性能烧结钕铁硼永磁体在新能源汽车行业及高端消费电子甚至军工行业起到关键核心能量转换作用,高性能烧结钕铁硼永磁体中通常含有重稀土镝或铽,这是因为镝铁硼和铽铁硼的各向异性场高。但重稀土镝或铽价格是镨钕金属的几倍,整个产业链受原材料的高位价格资金周转压力大,因此迫切需要开发无重稀土镝或铽的高性能烧结钕铁硼永磁体。
采用双合金工艺制备烧结钕铁硼永磁体,通过辅合金与主合金配合使用便于在一定程度调控烧结钕铁硼永磁体的微观组织,从而获得性能优异的产品。开发无重稀土镝和铽的高性能烧结钕铁硼永磁体,关键在于辅合金的微观组织的调控,但是目前相关研究较少。
发明内容
本发明的目的在于提供一种辅合金铸片和高剩磁高矫顽力钕铁硼永磁体及制备方法,采用本发明提供的方法制备的辅合金铸片富含球状微观组织,利用该辅合金铸片最终能够制备得到无重稀土镝和铽的高性能烧结钕铁硼永磁体。
为了实现上述发明目的,本发明提供以下技术方案:
本发明提供了一种辅合金铸片的制备方法,包括以下步骤:
提供辅合金原料,按质量分数计,所述辅合金原料的组成包括Pr 40~45%,Co 1~2%,Ga 0.5~1%,B 0.6~0.8%,V 0.1~0.2%,Ti 0.3~0.7%,余量的Fe;
将所述辅合金原料进行熔炼,得到熔炼物料;
将所述熔炼物料进行速凝铸片,得到辅合金铸片;所述速凝铸片包括依次进行精炼和浇铸;所述浇铸的条件包括:浇铸温度为1330~1380℃,铜辊轮转速为60~80rpm;冷却方式为充氩气风冷,冷却时降温速率为7~15℃/min。
优选地,所述熔炼的温度为1390~1430℃,保温时间为3~5min;所述精炼的温度为1460~1510℃,保温时间为2~5min。
优选地,所述精炼与浇铸之间还包括:以3~7℃/min速率降温至浇铸温度,保温5~9min。
本发明提供了上述技术方案所述制备方法制备得到的辅合金铸片,具有球状微观组织,所述球状微观组织的直径为3~15μm。
本发明提供了一种高剩磁高矫顽力钕铁硼永磁体的制备方法,包括以下步骤:
提供主合金铸片,按质量分数计,所述主合金铸片的组成包括M 28.5~29%,Co 1~2%,Ga 0.2~0.5%,Al 0.05~0.15%,B 0.9~0.92%,Ti 0.05~0.15%,余量的Fe,所述M为Pr和Nd;
将所述主合金铸片与上述技术方案所述辅合金铸片依次进行双合金氢破碎、气流磨制粉、取向成型、烧结和回火处理,得到高剩磁高矫顽力钕铁硼永磁体。
优选地,所述辅合金铸片的质量为主合金铸片质量的10~15%;
所述双合金氢破碎包括依次进行吸氢处理、第一脱氢处理和第二脱氢处理;
所述吸氢处理的温度为330~360℃,保温时间为45~60min;
所述第一脱氢处理的温度为435~465℃,保温时间为2~3h;
所述第二脱氢处理的温度为570~590℃,保温时间为6~8h。
优选地,所述气流磨制粉在润滑剂存在条件下进行,所述润滑剂的质量为所述氢破碎后所得粗粉质量的1.5~2‰;所述气流磨制粉的研磨压力为5.9~6.1MPa,出粉速度为130~160kg/h;所述气流磨制粉后所得细粉的d50为2.5~3μm,粒度分布d90/d10为3.47~3.8。
优选地,所述取向成型在磁感应强度为1.8~2.3T且成型压力为3~6MPa的条件下进行;所述取向成型后所得生坯的密度为4.1~4.3g/cm3。
优选地,所述烧结包括依次进行第一烧结和第二烧结;所述第一烧结的条件包括:真空度小于5×10-2Pa,温度为1020~1050℃,保温时间为2~4h;所述第二烧结的条件包括:真空度小于5×10-2Pa,温度为1060~1080℃,保温时间为8~10h;
所述回火处理包括依次进行第一回火处理和第二回火处理;所述第一回火处理的条件包括:真空度小于5Pa,温度为890~920℃,时间为3~5h;所述第二回火处理的条件包括:真空度小于8Pa,温度为490~520℃,时间为5~7h。
本发明提供了上述技术方案所述制备方法制备得到的高剩磁高矫顽力钕铁硼永磁体。
本发明提供了一种辅合金铸片的制备方法,包括以下步骤:提供辅合金原料,按质量分数计,所述辅合金原料的组成包括Pr40~45%,Co 1~2%,Ga 0.5~1%,B 0.6~0.8%,V 0.1~0.2%,Ti 0.3~0.7%,余量的Fe;将所述辅合金原料进行熔炼,得到熔炼物料;将所述熔炼物料进行速凝铸片,得到辅合金铸片;所述速凝铸片包括依次进行精炼和浇铸;所述浇铸的条件包括:浇铸温度为1330~1380℃,铜辊轮转速为60~80rpm;冷却方式为充氩气风冷,冷却时降温速率为7~10℃/min。本发明在辅合金铸片中引入钛和钒,并配合特定的速凝铸片工艺,所得辅合金铸片中富含球状微观组织,利用该辅合金铸片最终能够制备得到无重稀土镝和铽的高性能烧结钕铁硼永磁体。
本发明提供了一种高剩磁高矫顽力钕铁硼永磁体的制备方法,包括以下步骤:提供主合金铸片,按质量分数计,所述主合金铸片的组成包括M 28.5~29%,Co 1~2%,Ga0.2~0.5%,Al 0.05~0.15%,B 0.9~0.92%,Ti 0.05~0.15%,余量的Fe,所述M为Pr和Nd;将所述主合金铸片与上述技术方案所述辅合金铸片依次进行双合金氢破碎、气流磨制粉、取向成型、烧结和回火处理,得到高剩磁高矫顽力钕铁硼永磁体。本发明在辅合金中引入钛和钒,在主合金中引入钛,结合双合金热处理工艺制备得到高剩磁高矫顽力钕铁硼永磁体。具体的,本发明在主合金以及辅合金中引入钛,在烧结钕铁硼制备过程中起到晶粒细化作用;同时在辅合金中引入钒,结合烧结和回火处理工艺,有利于促进富稀土相沿主相晶界处析出,优化富稀土相在烧结钕铁硼永磁体中的均匀分布,最终获得无重稀土镝和铽的高剩磁高矫顽力钕铁硼永磁体,在实施例测试条件下,其剩磁为14.3kGs,矫顽力为17kOe,在满足产业化应用要求的基础上也节约了稀缺稀土资源镝和铽,降低了企业生产成本,促进了稀土资源的平衡利用。此外,本发明提供的方法适于批量化生产,制备得到的产品稳定性好。
附图说明
图1为实施例1制备的辅合金铸片的金相显微镜观察图。
具体实施方式
本发明提供了一种辅合金铸片的制备方法,包括以下步骤:
提供辅合金原料,按质量分数计,所述辅合金原料的组成包括Pr 40~45%,Co 1~2%,Ga 0.5~1%,B 0.6~0.8%,V 0.1~0.2%,Ti 0.3~0.7%,余量的Fe;
将所述辅合金原料进行熔炼,得到熔炼物料;
将所述熔炼物料进行速凝铸片,得到辅合金铸片;所述速凝铸片包括依次进行精炼和浇铸;所述浇铸的条件包括:浇铸温度为1330~1380℃,铜辊轮转速为60~80rpm;冷却方式为充氩气风冷,冷却时降温速率为7~10℃/min。
本发明提供辅合金原料,按质量分数计,所述辅合金原料的组成包括Pr40~45%,Co 1~2%,Ga 0.5~1%,B 0.6~0.8%,V 0.1~0.2%,Ti 0.3~0.7%,余量的Fe;优选包括:Pr41~44%,Co 1.2~1.5%,Ga 0.5~0.8%,B 0.6~0.7%,V 0.15~0.18%,Ti 0.3~0.5%,余量的Fe;具体可以为Pr43%,Co 1.5%,Ga 0.8%,B 0.7%,V 0.15%,Ti0.5%,余量的Fe;或者可以为Pr44%,Co 1.2%,Ga 1%,B 0.8%,V 0.15%,Ti 0.7%,余量的Fe;或者还可以为Pr41%,Co 1.2%,Ga 0.5%,B 0.6%,V 0.18%,Ti 0.3%,余量的Fe。
本发明将所述辅合金原料进行熔炼,得到熔炼物料。在本发明中,所述熔炼的温度优选为1390~1430℃,更优选为1400~1405℃;保温时间优选为3~5min,更优选为3~4min。
得到熔炼物料后,本发明将所述熔炼物料进行速凝铸片,得到辅合金铸片。在本发明中,所述速凝铸片包括依次进行精炼和浇铸。在本发明中,所述精炼的温度优选为1460~1510℃,更优选为1470~1480℃;保温时间优选为2~5min,更优选为2~3min。在本发明中,所述浇铸的条件包括:浇铸温度为1330~1380℃,优选为1340~1360℃,进一步优选为1350~1355℃;铜辊轮转速为60~80rpm,优选为70rpm;冷却方式为充氩气风冷,冷却时降温速率为7~15℃/min,优选为10~15℃/min。本发明优选充氩气风冷至小于40℃,得到辅合金铸片。在本发明中,所述辅合金铸片的厚度优选为0.15~0.25mm。
在本发明中,所述精炼与浇铸之间优选还包括:将精炼后所得精炼物料以3~7℃/min速率降温至浇铸温度,保温5~9min;所述降温的速率优选为5℃/min,所述保温的时间优选为7min。本发明优选将精炼物料以上述速率降温至浇铸温度并保温上述时间的作用是获得成分均匀的物料。
本发明提供了上述技术方案所述制备方法制备得到的辅合金铸片,所述辅合金铸片具有球状微观组织,所述球状微观组织的直径为3~15μm。
本发明提供了一种高剩磁高矫顽力钕铁硼永磁体的制备方法,包括以下步骤:
提供主合金铸片,按质量分数计,所述主合金铸片的组成包括M 28.5~29%,Co 1~2%,Ga 0.2~0.5%,Al 0.05~0.15%,B 0.9~0.92%,Ti 0.05~0.15%,余量的Fe,所述M为Pr和Nd;
将所述主合金铸片与上述技术方案所述辅合金铸片依次进行双合金氢破碎、气流磨制粉、取向成型、烧结和回火处理,得到高剩磁高矫顽力钕铁硼永磁体。
本发明提供主合金铸片,按质量分数计,所述主合金铸片的组成包括M 28.5~29%,Co 1~2%,Ga 0.2~0.5%,Al 0.05~0.15%,B 0.9~0.92%,Ti 0.05~0.15%,余量的Fe;更优选包括:M 28.5~28.8%,Co 1.5~1.8%,Ga 0.3~0.35%,Al 0.08~0.1%,B 0.9~0.91%,Ti 0.01~0.12%,余量的Fe;具体可以为M 28.8%,Co 1.5%,Ga 0.35%,Al 0.1%,B 0.9%,Ti 0.1%,余量的Fe;或者可以为M 28.5%,Co 1.8%,Ga 0.35%,Al0.1%,B 0.9%,Ti 0.12%,余量的Fe;或者还可以为M 29%,Co 1.5%,Ga 0.3%,Al0.1%,B 0.9%,Ti 0.15%,余量的Fe。在本发明中,所述M为Pr和Nd,所述M中Pr与Nd质量比优选为(4~7):(21.8~24.8),更优选为(5~6):(22.5~23.5),具体可以为5.7:23.1、5.8:23、5.7:22.8或5.9:23.1。本发明优选按照主合金铸片的组成配料后进行速凝铸片,得到主合金铸片;所述速凝铸片的条件优选包括:精炼温度优选为1460~1490℃,更优选为1470~1480℃;浇铸温度优选为1390~1420℃,更优选为1405~1420℃;铜辊轮转速优选为40~45rpm,更优选为41~43rpm;冷却方式优选为充氩气风冷,冷却时降温速率优选为7~10℃/min,更优选为8~9℃/min。
得到主合金铸片后,本发明将所述主合金铸片与上述技术方案所述辅合金铸片混合,依次进行双合金氢破碎、气流磨制粉、取向成型、烧结和回火处理,得到高剩磁高矫顽力钕铁硼永磁体。在本发明中,所述辅合金铸片的质量优选为主合金铸片质量的10~15%,更优选为10~12%。下面对各工序进行详细说明。
本发明将所述主合金铸片与辅合金铸片进行双合金氢破碎,得到粗粉。在本发明中,所述双合金氢破碎优选包括依次进行吸氢处理、第一脱氢处理和第二脱氢处理。在本发明中,所述吸氢处理的温度优选为330~360℃,更优选为350~360℃;保温时间优选为45~60min,更优选为55~60min。在本发明中,所述第一脱氢处理的温度优选为435~465℃,更优选为450~460℃;保温时间优选为2~3h,更优选为2.5h。在本发明中,所述第二脱氢处理的温度优选为570~590℃,更优选为580℃;保温时间优选为6~8h,更优选为7h。所述第二脱氢处理后,本发明优选3~7℃/min速率降温至380~420℃,保温25~35min,然后以15~25℃/min降温速率充氩气冷却至室温,得到粗粉;更优选地,本发明将第二脱氢处理后所得物料以5℃/min速率冷却至400℃保温30min,然后以20℃/min降温速率充氩气冷却至室温,得到粗粉。在本发明中,所述粗粉的平均粒径优选为50~100μm,更优选为80μm。在本发明的实施例中,所述双合金氢破碎具体是在氢破炉中进行。
得到粗粉后,本发明将所述粗粉进行气流磨制粉,得到细粉。在本发明中,所述气流磨制粉优选在润滑剂存在条件下进行,所述润滑剂优选为脂类润滑剂;所述润滑剂的质量优选为所述粗粉质量的1.5~2‰,更优选为1.8~2‰。本发明优选将所述粗粉与润滑剂搅拌混合1.5~2.5h,进一步优选为2h,然后进行气流磨制粉。在本发明中,所述气流磨制粉的过程中无需额外添加抗氧化剂。在本发明中,所述气流磨制粉的研磨压力优选为5.9~6.1MPa,更优选为6MPa;出粉速度优选为130~160kg/h,更优选为138~159kg/h,进一步优选为145~150kg/h。在本发明中,所述细粉的d50优选为2.5~3μm,更优选为2.58~2.75μm,进一步优选为2.63~2.68μm;粒度分布d90/d10优选为3.47~3.8,更优选为3.65~3.71。
得到细粉后,本发明将所述细粉进行取向成型,得到生坯。在本发明中,所述取向成型的条件优选包括:磁感应强度优选为1.8~2.3T,更优选为2.12~2.2T;压力优选为3~6MPa,更优选为3.5~5MPa,进一步优选为4~4.5MPa。在本发明中,所述生坯的密度优选为4.1~4.3g/cm3,更优选为4.2~4.25g/cm3,进一步优选为4.21~4.22g/cm3。在本发明的实施例中,具体是在磁场压机中进行所述取向成型。
得到生坯后,本发明将所述生坯进行烧结,得到烧结物料。在本发明中,所述烧结前优选先去除所述生坯中润滑剂;去除所述润滑剂的方式优选为将所述生坯进行加热处理,以使所述润滑剂充分挥发。在本发明中,所述加热处理的温度优选为530~600℃,更优选为570℃;保温时间优选为3~5h,更优选为4h。在本发明中,所述烧结优选包括依次进行第一烧结和第二烧结。在本发明中,所述第一烧结的条件优选包括:真空度优选小于5×10- 2Pa,更优选为5×10-3Pa;温度优选为1020~1050℃,更优选为1030℃;保温时间优选为2~4h,更优选为2h。本发明优选自加热处理所需温度升温至第一烧结所需温度;所述升温的时间优选为5~8h,更优选为6h;所述升温优选为匀速升温。所述第一烧结后,本发明优选自第一烧结所需温度升温至第二烧结所需温度;所述升温的时间优选为20~40min,更优选为30min;所述升温优选为匀速升温。在本发明中,所述第二烧结的条件优选包括:真空度优选小于5×10-2Pa,更优选为5×10-3Pa;温度优选为1060~1080℃,更优选为1065~1070℃;保温时间优选为8~10h,更优选为8h。
得到烧结物料后,本发明将所述烧结物料进行回火处理,得到高剩磁高矫顽力钕铁硼永磁体。在本发明中,所述回火处理优选包括依次进行第一回火处理和第二回火处理。在本发明中,所述第一回火处理的条件优选包括:真空度优选小于5Pa,更优选为3Pa;温度优选为890~920℃,更优选为900~910℃;时间优选为3~5h,更优选为4h。本发明优选自第二烧结的温度经充氩气风冷的方式冷却至第一回火处理所需温度,进行第一回火处理;所述第一回火处理后,优选经充氩气风冷的方式冷却至80~120℃,更优选为100℃,然后升温至第二回火处理所需温度;所述升温的时间优选为3~5h,更优选为3.5h,所述升温优选为匀速升温。在本发明中,所述第二回火处理的条件优选包括:真空度优选小于8Pa,更优选为3Pa;温度优选为490~520℃,更优选为500~510℃;时间优选为5~8h,更优选为6h。所述第二回火处理后,本发明优选经充氩气风冷的方式冷却至小于40℃,得到高剩磁高矫顽力钕铁硼永磁体。
本发明提供了上述技术方案所述制备方法制备得到的高剩磁高矫顽力钕铁硼永磁体。
下面将结合本发明中的实施例,对本发明中的技术方案进行清楚、完整地描述。显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1
根据配方设计成分进行配料,按质量分数计,辅合金原料的组成包括:Pr含量为43%,Co含量为1.5%,Ga含量为0.8%,B含量为0.7%,V含量为0.15%,Ti含量为0.5%,余量的Fe;将所述辅合金原料在1400℃熔炼3min,以10℃/min速率升温至1480℃精炼2min,以5℃/min速率降温至1350℃保温7min,然后进行浇铸,铜辊转速为70rpm,浇铸后充氩气风冷(降温速率为15℃/min)至小于40℃,得到厚度为0.15~0.25mm的辅合金铸片;
根据配方设计成分进行配料,按质量分数计,主合金原料的组成包括:镨钕含量为28.8%(其中,Pr与Nd质量比为5.8:23),Co含量为1.5%,Ga含量为0.35%,Al含量为0.1%,B含量为0.9%,Ti含量为0.1%,余量的Fe;将所述主合金原料进行速凝铸片,得到主合金铸片;所述速凝铸片的条件包括:精炼温度为1470℃;浇铸温度为1405℃;铜辊轮转速为43rpm;冷却方式为充氩气风冷,冷却时降温速率为9℃/min;
将所述主合金铸片与辅合金铸片置于氢破炉中,所述辅合金铸片的质量为主合金铸片质量的10%,采用双合金工艺进行氢破碎,具体是在350℃保温进行吸氢处理60min,在450℃保温进行第一脱氢处理2.5h,之后升温至580℃保温进行第二脱氢处理7h,再以5℃/min速率冷却至400℃保温30min,最后以20℃/min降温速率充氩气冷却至室温(25℃),获得平均粒径为80μm的粗粉;
将所述粗粉与脂类润滑剂搅拌混合2h,所述脂类润滑剂为粗粉质量的1.8‰,将所得混合物料(不额外添加抗氧化剂)进行气流磨制粉,得到细粉;所述气流磨制粉的研磨压力为6MPa,出粉速度为150kg/h;所述细粉的d50为2.68μm,粒度分布d90/d10为3.65;
将所述细粉置于磁场压机中,在磁感应强度为2T且成型压力为4MPa条件下进行取向成型,得到密度为4.2g/cm3的生坯;
将所述生坯在570℃保温4h使得脂类润滑剂充分挥发,控制真空度为5×10-3Pa,匀速升温6h至1030℃,保温进行第一烧结处理2h;然后匀速升温30min至温度为1060℃,保温进行第二烧结处理8h,得到烧结物料;充氩气风冷至910℃,保温进行第一回火处理4h;控制真空度为3Pa,充氩气风冷至100℃,匀速升温3.5h至510℃,保温进行第二回火处理6h,控制真空度为3Pa,充氩气连续风冷至小于40℃,得到高剩磁高矫顽力钕铁硼永磁体。
图1为实施例1制备的辅合金铸片的金相显微镜观察图,结果显示,在金相显微镜下可观察到实施例1制备的辅合金铸片的富含球状微观组织,该球状微观组织的直径为3~15μm。通过扫描电镜观察所述辅合金铸片的成分中富含Pr、Fe、Ga、V及少量的B元素。
按照实施例1的方法重复制备3个高剩磁高矫顽力钕铁硼永磁体样品,并将其在20℃进行圆柱测试,具体测量剩磁(Br)、磁感矫顽力(Hcb)、内禀矫顽力(Hcj)、磁能积((BH)max)、磁体的J退磁曲线上J=0.9Jr时的反向磁场(Hk)、方形度(Hk/Hcj),具体结果如表1所示。由表1可知,采用本发明提供的方法制备的高剩磁高矫顽力钕铁硼永磁体样品经测试后,其剩磁可达到14.3kGs,内禀矫顽力可达到17kOe。而且由表1可知,采用本发明提供的方法制备高剩磁高矫顽力钕铁硼永磁体,产品稳定性好。
表1实施例1中3个高剩磁高矫顽力钕铁硼永磁体样品的性能测试结果
实施例2
根据配方设计成分进行配料,按质量分数计,辅合金原料的组成包括:Pr含量为44%,Co含量为1.2%,Ga含量为1%,B含量为0.8%,V含量为0.15%,Ti含量为0.7%,余量的Fe;将所述辅合金原料在1405℃熔炼3min,以10℃/min速率升温至1480℃精炼2min,以5℃/min速率降温至1355℃保温7min,然后进行浇铸,铜辊转速为70rpm,浇铸后充氩气风冷(降温速率为15℃/min)至小于40℃,得到厚度为0.15~0.25mm的辅合金铸片;
根据配方设计成分进行配料,按质量分数计,主合金原料的组成包括:镨钕含量为28.5%(其中,Pr与Nd质量比为5.7:22.8),Co含量为1.8%,Ga含量为0.35%,Al含量为0.1%,B含量为0.9%,Ti含量为0.12%,余量的Fe;将所述主合金原料进行速凝铸片,得到主合金铸片;所述速凝铸片的条件包括:精炼温度为1470℃;浇铸温度为1405℃;铜辊轮转速为43rpm;冷却方式为充氩气风冷,冷却时降温速率为9℃/min;
将所述主合金铸片与辅合金铸片置于氢破炉中,所述辅合金铸片的质量为主合金铸片质量的10%,采用双合金工艺进行氢破碎,具体是在360℃保温进行吸氢处理60min,在460℃保温进行第一脱氢处理2.5h,之后升温至580℃保温进行第二脱氢处理7h,再以5℃/min速率冷却至400℃保温30min,最后以20℃/min降温速率充氩气冷却至室温(25℃),获得平均粒径为80μm的粗粉;
将所述粗粉与脂类润滑剂搅拌混合2h,所述脂类润滑剂为粗粉质量的2‰,将所得混合物料(不额外添加抗氧化剂)进行气流磨制粉,得到细粉;所述气流磨制粉的研磨压力为6MPa,出粉速度为159kg/h;所述细粉的d50为2.75μm,粒度分布d90/d10为3.71;
将所述细粉置于磁场压机中,在磁感应强度为2.1T且成型压力为5MPa条件下进行取向成型,得到密度为4.21g/cm3的生坯;
将所述生坯在570℃保温4h使得脂类润滑剂充分挥发,控制真空度为5×10-3Pa,匀速升温6h至1030℃,保温进行第一烧结处理2h;然后匀速升温30min至温度为1075℃,保温进行第二烧结处理8h,得到烧结物料;控制真空度为3Pa,充氩气风冷至890℃,保温进行第一回火处理4h;控制真空度为3Pa,充氩气风冷至100℃,匀速升温3.5h至520℃,保温进行第二回火处理6h,控制真空度为3Pa,充氩气连续风冷至小于40℃,得到高剩磁高矫顽力钕铁硼永磁体。
按照实施例2的方法重复制备3个高剩磁高矫顽力钕铁硼永磁体样品,并将其在20℃进行圆柱测试,具体测量剩磁(Br)、磁感矫顽力(Hcb)、内禀矫顽力(Hcj)、磁能积((BH)max)、磁体的J退磁曲线上J=0.9Jr时的反向磁场(Hk)、方形度(Hk/Hcj),具体结果如表2所示。由表2可知,采用本发明提供的方法制备的高剩磁高矫顽力钕铁硼永磁体样品经测试后,其剩磁可达到14.3kGs,内禀矫顽力可达到17kOe。而且由表2可知,采用本发明提供的方法制备高剩磁高矫顽力钕铁硼永磁体,产品稳定性好。
表2实施例2中3个高剩磁高矫顽力钕铁硼永磁体样品的性能测试结果
实施例3
根据配方设计成分进行配料,按质量分数计,辅合金原料的组成包括:Pr含量为41%,Co含量为1.2%,Ga含量为0.5%,B含量为0.6%,V含量为0.18%,Ti含量为0.3%,余量的Fe;将所述辅合金原料在1390℃熔炼3min,以10℃/min速率升温至1470℃精炼2min,以5℃/min速率降温至1340℃保温7min,然后进行浇铸,铜辊转速为70rpm,浇铸后充氩气风冷(降温速率为15℃/min)至小于40℃,得到厚度为0.15~0.25mm的辅合金铸片;
根据配方设计成分进行配料,按质量分数计,主合金原料的组成包括:镨钕含量为29%(其中,Pr与Nd质量比为5.9:23.1),Co含量为1.5%,Ga含量为0.3%,Al含量为0.1%,B含量为0.9%,Ti含量为0.15%,余量的Fe;将所述主合金原料进行速凝铸片,得到主合金铸片;所述速凝铸片的条件包括:精炼温度为1480℃;浇铸温度为1420℃;铜辊轮转速为43rpm;冷却方式为充氩气风冷,冷却时降温速率为9℃/min;
将所述主合金铸片与辅合金铸片置于氢破炉中,所述辅合金铸片的质量为主合金铸片质量的10%,采用双合金工艺进行氢破碎,具体是在350℃保温进行吸氢处理60min,在450℃保温进行第一脱氢处理2.5h,之后升温至580℃保温进行第二脱氢处理7h,再以5℃/min速率冷却至400℃保温30min,最后充氩气冷却至室温(25℃),获得平均粒径为80μm的粗粉;
将所述粗粉与脂类润滑剂搅拌混合2h,所述脂类润滑剂为粗粉质量的1.8‰,将所得混合物料(不额外添加抗氧化剂)进行气流磨制粉,得到细粉;所述气流磨制粉的研磨压力为6MPa,出粉速度为138kg/h;所述细粉的d50为2.58μm,粒度分布d90/d10为3.47;
将所述细粉置于磁场压机中,在磁感应强度为2.2T且成型压力为3.5MPa条件下进行取向成型,得到密度为4.22g/cm3的生坯;
将所述生坯在570℃保温4h使得脂类润滑剂充分挥发,控制真空度为5×10-3Pa,匀速升温6h至1030℃,保温进行第一烧结处理2h;然后匀速升温30min至温度为1060℃,保温进行第二烧结处理8h,得到烧结物料;控制真空度为3Pa,充氩气风冷至900℃,保温进行第一回火处理4h;控制真空度为3Pa,充氩气风冷至100℃,匀速升温3.5h至500℃,保温进行第二回火处理6h,控制真空度为3Pa,充氩气连续风冷至小于40℃,得到高剩磁高矫顽力钕铁硼永磁体。
按照实施例3的方法重复制备3个高剩磁高矫顽力钕铁硼永磁体样品,并将其在20℃进行圆柱测试,具体测量剩磁(Br)、磁感矫顽力(Hcb)、内禀矫顽力(Hcj)、磁能积((BH)max)、磁体的J退磁曲线上J=0.9Jr时的反向磁场(Hk)、方形度(Hk/Hcj),具体结果如表3所示。由表3可知,采用本发明提供的方法制备的高剩磁高矫顽力钕铁硼永磁体样品经测试后,其剩磁可达到14.3kGs,内禀矫顽力可达到17kOe。而且由表3可知,采用本发明提供的方法制备高剩磁高矫顽力钕铁硼永磁体,产品稳定性好。
表3实施例3中3个高剩磁高矫顽力钕铁硼永磁体样品的性能测试结果
以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (9)
1.一种辅合金铸片,具有球状微观组织,所述球状微观组织的直径为3~15μm;所述辅合金铸片的制备方法,包括以下步骤:
提供辅合金原料,按质量分数计,所述辅合金原料的组成包括Pr40~45%,Co 1~2%,Ga 0.5~1%,B 0.6~0.8%,V 0.1~0.2%,Ti 0.3~0.7%,余量的Fe;
将所述辅合金原料进行熔炼,得到熔炼物料;
将所述熔炼物料进行速凝铸片,得到辅合金铸片;所述速凝铸片包括依次进行精炼和浇铸;所述浇铸的条件包括:浇铸温度为1330~1380℃,铜辊轮转速为60~80rpm;冷却方式为充氩气风冷,冷却时降温速率为7~15℃/min。
2.根据权利要求1所述的辅合金铸片,其特征在于,所述熔炼的温度为1390~1430℃,保温时间为3~5min;所述精炼的温度为1460~1510℃,保温时间为2~5min。
3.根据权利要求2所述的辅合金铸片,其特征在于,所述精炼与浇铸之间还包括:以3~7℃/min速率降温至浇铸温度,保温5~9min。
4.一种高剩磁高矫顽力钕铁硼永磁体的制备方法,包括以下步骤:
提供主合金铸片,按质量分数计,所述主合金铸片的组成包括M28.5~29%,Co 1~2%,Ga 0.2~0.5%,Al 0.05~0.15%,B 0.9~0.92%,Ti0.05~0.15%,余量的Fe,所述M为Pr和Nd;
将所述主合金铸片与权利要求1~3任一项所述辅合金铸片依次进行双合金氢破碎、气流磨制粉、取向成型、烧结和回火处理,得到高剩磁高矫顽力钕铁硼永磁体。
5.根据权利要求4所述的制备方法,其特征在于,所述辅合金铸片的质量为主合金铸片质量的10~15%;
所述双合金氢破碎包括依次进行吸氢处理、第一脱氢处理和第二脱氢处理;
所述吸氢处理的温度为330~360℃,保温时间为45~60min;
所述第一脱氢处理的温度为435~465℃,保温时间为2~3h;
所述第二脱氢处理的温度为570~590℃,保温时间为6~8h。
6.根据权利要求4或5所述的制备方法,其特征在于,所述气流磨制粉在润滑剂存在条件下进行,所述润滑剂的质量为所述氢破碎后所得粗粉质量的1.5~2‰;所述气流磨制粉的研磨压力为5.9~6.1MPa,出粉速度为130~160kg/h;所述气流磨制粉后所得细粉的d50为2.5~3μm,粒度分布d90/d10为3.47~3.8。
7.根据权利要求4所述的制备方法,其特征在于,所述取向成型在磁感应强度为1.8~2.3T且成型压力为3~6MPa的条件下进行;所述取向成型后所得生坯的密度为4.1~4.3g/cm3。
8.根据权利要求4所述的制备方法,其特征在于,所述烧结包括依次进行第一烧结和第二烧结;所述第一烧结的条件包括:真空度小于5×10-2Pa,温度为1020~1050℃,保温时间为2~4h;所述第二烧结的条件包括:真空度小于5×10-2Pa,温度为1060~1080℃,保温时间为8~10h;
所述回火处理包括依次进行第一回火处理和第二回火处理;所述第一回火处理的条件包括:真空度小于5Pa,温度为890~920℃,时间为3~5h;所述第二回火处理的条件包括:真空度小于8Pa,温度为490~520℃,时间为5~7h。
9.权利要求4~8任一项所述制备方法制备得到的高剩磁高矫顽力钕铁硼永磁体。
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202211255156.5A CN115747611B (zh) | 2022-10-13 | 2022-10-13 | 一种辅合金铸片和高剩磁高矫顽力钕铁硼永磁体及制备方法 |
JP2022212387A JP7471389B1 (ja) | 2022-10-13 | 2022-12-28 | 補助合金鋳片及び高残留磁気・高保磁力のネオジム-鉄-ホウ素永久磁石並びに製造方法 |
EP22217234.8A EP4354471A1 (en) | 2022-10-13 | 2022-12-29 | Auxiliary alloy casting piece, high-remanence and high-coercive force ndfeb permanent magnet, and preparation methods thereof |
US18/091,899 US20240127993A1 (en) | 2022-10-13 | 2022-12-30 | AUXILIARY ALLOY CASTING PIECE, HIGH-REMANENCE AND HIGH-COERCIVE FORCE NdFeB PERMANENT MAGNET, AND PREPARATION METHODS THEREOF |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202211255156.5A CN115747611B (zh) | 2022-10-13 | 2022-10-13 | 一种辅合金铸片和高剩磁高矫顽力钕铁硼永磁体及制备方法 |
Publications (2)
Publication Number | Publication Date |
---|---|
CN115747611A CN115747611A (zh) | 2023-03-07 |
CN115747611B true CN115747611B (zh) | 2023-10-20 |
Family
ID=85017841
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202211255156.5A Active CN115747611B (zh) | 2022-10-13 | 2022-10-13 | 一种辅合金铸片和高剩磁高矫顽力钕铁硼永磁体及制备方法 |
Country Status (4)
Country | Link |
---|---|
US (1) | US20240127993A1 (zh) |
EP (1) | EP4354471A1 (zh) |
JP (1) | JP7471389B1 (zh) |
CN (1) | CN115747611B (zh) |
Citations (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103426624A (zh) * | 2013-08-14 | 2013-12-04 | 林建强 | 钕铁硼永磁体的制备方法 |
CN105741995A (zh) * | 2016-04-27 | 2016-07-06 | 宁波耐力誉磁业科技有限公司 | 一种高性能烧结钕铁硼永磁体及其制备方法 |
CN108766753A (zh) * | 2018-05-11 | 2018-11-06 | 包头稀土研究院 | 高磁能积高矫顽力烧结钕铁硼磁体的制备方法 |
CN109102976A (zh) * | 2018-08-10 | 2018-12-28 | 浙江东阳东磁稀土有限公司 | 一种提高稀土钕铁硼磁性能的方法 |
CN110289161A (zh) * | 2019-07-16 | 2019-09-27 | 宁德市星宇科技有限公司 | 一种低稀土含量的钕铁硼磁体的制备方法 |
CN110853856A (zh) * | 2019-11-22 | 2020-02-28 | 安泰科技股份有限公司 | 一种高矫顽力含铈磁体及其制备方法 |
CN112509775A (zh) * | 2020-12-15 | 2021-03-16 | 烟台首钢磁性材料股份有限公司 | 一种低量添加重稀土的钕铁硼磁体及其制备方法 |
WO2021223436A1 (zh) * | 2020-05-08 | 2021-11-11 | 中国科学院宁波材料技术与工程研究所 | 一种高性能钕铁硼永磁材料及其制备方法 |
CN113838622A (zh) * | 2021-09-26 | 2021-12-24 | 太原理工大学 | 一种高矫顽力烧结钕铁硼磁体及其制备方法 |
Family Cites Families (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP6119548B2 (ja) * | 2012-10-17 | 2017-04-26 | 信越化学工業株式会社 | 希土類焼結磁石の製造方法 |
JP2015122395A (ja) | 2013-12-24 | 2015-07-02 | 日立金属株式会社 | R−t−b系焼結磁石の製造方法 |
JP6414740B2 (ja) | 2014-10-27 | 2018-10-31 | 日立金属株式会社 | R−t−b系焼結磁石の製造方法 |
CN104575906B (zh) | 2014-12-11 | 2017-05-24 | 赣州市东磁稀土有限公司 | 一种高性能低成本稀土永磁材料及其制备方法 |
CN106328331B (zh) * | 2015-06-16 | 2019-02-26 | 有研稀土新材料股份有限公司 | 烧结钕铁硼磁体用辅助合金铸片及其制备方法 |
JP6508571B2 (ja) | 2015-06-30 | 2019-05-08 | 日立金属株式会社 | R−t−b系焼結磁石の製造方法およびr−t−b系焼結磁石 |
CN106601407B (zh) * | 2017-01-23 | 2019-06-07 | 包头市神头稀土科技发展有限公司 | 提高钕铁硼磁体矫顽力的方法 |
CN107610865A (zh) * | 2017-10-16 | 2018-01-19 | 包头稀土研究院 | 钕铁硼永磁材料的制备方法 |
CN111009369B (zh) | 2019-10-29 | 2021-08-27 | 厦门钨业股份有限公司 | 一种稀土永磁材料及其制备方法和应用 |
CN113223807B (zh) * | 2021-05-31 | 2022-08-19 | 包头金山磁材有限公司 | 一种钕铁硼永磁体及其制备方法和应用 |
-
2022
- 2022-10-13 CN CN202211255156.5A patent/CN115747611B/zh active Active
- 2022-12-28 JP JP2022212387A patent/JP7471389B1/ja active Active
- 2022-12-29 EP EP22217234.8A patent/EP4354471A1/en active Pending
- 2022-12-30 US US18/091,899 patent/US20240127993A1/en active Pending
Patent Citations (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103426624A (zh) * | 2013-08-14 | 2013-12-04 | 林建强 | 钕铁硼永磁体的制备方法 |
CN105741995A (zh) * | 2016-04-27 | 2016-07-06 | 宁波耐力誉磁业科技有限公司 | 一种高性能烧结钕铁硼永磁体及其制备方法 |
CN108766753A (zh) * | 2018-05-11 | 2018-11-06 | 包头稀土研究院 | 高磁能积高矫顽力烧结钕铁硼磁体的制备方法 |
CN109102976A (zh) * | 2018-08-10 | 2018-12-28 | 浙江东阳东磁稀土有限公司 | 一种提高稀土钕铁硼磁性能的方法 |
CN110289161A (zh) * | 2019-07-16 | 2019-09-27 | 宁德市星宇科技有限公司 | 一种低稀土含量的钕铁硼磁体的制备方法 |
CN110853856A (zh) * | 2019-11-22 | 2020-02-28 | 安泰科技股份有限公司 | 一种高矫顽力含铈磁体及其制备方法 |
WO2021223436A1 (zh) * | 2020-05-08 | 2021-11-11 | 中国科学院宁波材料技术与工程研究所 | 一种高性能钕铁硼永磁材料及其制备方法 |
CN112509775A (zh) * | 2020-12-15 | 2021-03-16 | 烟台首钢磁性材料股份有限公司 | 一种低量添加重稀土的钕铁硼磁体及其制备方法 |
CN113838622A (zh) * | 2021-09-26 | 2021-12-24 | 太原理工大学 | 一种高矫顽力烧结钕铁硼磁体及其制备方法 |
Non-Patent Citations (2)
Title |
---|
周寿增,董清飞著.《超强永磁体 稀土铁系永磁材料》.北京:冶金工业出版社,1999,第308-309页. * |
黄小卫,李红卫主编.《中国稀土》.北京:冶金工业出版社,2015,(第第1版版),第85-86段. * |
Also Published As
Publication number | Publication date |
---|---|
CN115747611A (zh) | 2023-03-07 |
JP7471389B1 (ja) | 2024-04-19 |
US20240127993A1 (en) | 2024-04-18 |
JP2024059059A (ja) | 2024-04-30 |
EP4354471A1 (en) | 2024-04-17 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
WO2021249159A1 (zh) | 重稀土合金、钕铁硼永磁材料、原料和制备方法 | |
CN109448946B (zh) | 一种各向异性SmCo/MnBi复合磁体及其制备方法 | |
CN111223627B (zh) | 钕铁硼磁体材料、原料组合物、制备方法、应用 | |
CN110957090B (zh) | 一种钐钴1:5型永磁材料及其制备方法 | |
CN108154986B (zh) | 一种含y高丰度稀土永磁体及其制备方法 | |
CN108231312A (zh) | 一种基于混合稀土制备的永磁合金及其制备方法 | |
EP3667685A1 (en) | Heat-resistant neodymium iron boron magnet and preparation method therefor | |
CN106128677A (zh) | 一种钕铁硼磁体的多段烧结方法 | |
CN112750587A (zh) | 高性能烧结钐钴磁体的制备方法 | |
CN111261355B (zh) | 钕铁硼磁体材料、原料组合物、制备方法、应用 | |
CN106328331B (zh) | 烧结钕铁硼磁体用辅助合金铸片及其制备方法 | |
US20210280344A1 (en) | Method for preparing NdFeB magnet powder | |
CN112582123B (zh) | 低温度系数高使用温度烧结钐钴磁体的制备方法 | |
CN112420306A (zh) | 一种高性能的烧结钕铁硼磁环及其制备方法 | |
WO2023035490A1 (zh) | 一种含La的R-T-B稀土永磁体 | |
WO2023280259A1 (zh) | 一种耐腐蚀、高性能钕铁硼烧结磁体及其制备方法和用途 | |
CN115747611B (zh) | 一种辅合金铸片和高剩磁高矫顽力钕铁硼永磁体及制备方法 | |
CN113871120B (zh) | 一种混合稀土永磁材料及其制备方法 | |
CN113921218B (zh) | 一种高剩磁钕铁硼磁体及其制备方法和应用 | |
CN108597707A (zh) | 一种含Ce烧结磁体及制备方法 | |
CN113539600A (zh) | 一种高磁能积和高矫顽力的含Dy稀土永磁体及制备方法 | |
CN111462974B (zh) | 一种高性能双主相复合稀土永磁体材料及其制备方法 | |
CN111968850B (zh) | 一种放电等离子烧结制备高矫顽力钕铁硼永磁材料的方法 | |
CN111145997B (zh) | 一种提高矫顽力的n30型烧结混合稀土合金的磁性材料的制备方法 | |
CN115662773A (zh) | 一种高密度无铽烧结钕铁硼永磁体及其制备方法 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |