CN116936213A - Sm-Fe-Ti/Nd-Fe-B-containing composite bonded magnet and preparation method thereof - Google Patents
Sm-Fe-Ti/Nd-Fe-B-containing composite bonded magnet and preparation method thereof Download PDFInfo
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- CN116936213A CN116936213A CN202210315706.1A CN202210315706A CN116936213A CN 116936213 A CN116936213 A CN 116936213A CN 202210315706 A CN202210315706 A CN 202210315706A CN 116936213 A CN116936213 A CN 116936213A
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- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 48
- 229910002593 Fe-Ti Inorganic materials 0.000 title claims abstract description 37
- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000006247 magnetic powder Substances 0.000 claims abstract description 76
- 239000011230 binding agent Substances 0.000 claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 49
- 238000003723 Smelting Methods 0.000 claims description 38
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 26
- 239000002994 raw material Substances 0.000 claims description 21
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical group CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 18
- 239000003822 epoxy resin Substances 0.000 claims description 16
- 229920000647 polyepoxide Polymers 0.000 claims description 16
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 15
- 229910052802 copper Inorganic materials 0.000 claims description 15
- 239000010949 copper Substances 0.000 claims description 15
- 238000007873 sieving Methods 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 14
- 238000010791 quenching Methods 0.000 claims description 14
- 230000000171 quenching effect Effects 0.000 claims description 14
- 229910052786 argon Inorganic materials 0.000 claims description 13
- 239000002245 particle Substances 0.000 claims description 13
- 229910045601 alloy Inorganic materials 0.000 claims description 8
- 239000000956 alloy Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000011812 mixed powder Substances 0.000 claims description 8
- 239000010453 quartz Substances 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 239000011261 inert gas Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 229910052772 Samarium Inorganic materials 0.000 claims description 5
- 238000000748 compression moulding Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 238000005498 polishing Methods 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 239000000853 adhesive Substances 0.000 claims description 2
- 230000001070 adhesive effect Effects 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 230000006698 induction Effects 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical group [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 claims description 2
- 238000007711 solidification Methods 0.000 claims description 2
- 230000008023 solidification Effects 0.000 claims description 2
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 22
- 150000002910 rare earth metals Chemical class 0.000 abstract description 17
- 229910052692 Dysprosium Inorganic materials 0.000 abstract description 3
- 238000013329 compounding Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 11
- 230000006835 compression Effects 0.000 description 6
- 238000007906 compression Methods 0.000 description 6
- 229910000859 α-Fe Inorganic materials 0.000 description 5
- 239000000843 powder Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 238000007664 blowing Methods 0.000 description 2
- 230000005347 demagnetization Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
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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
- H01F1/0558—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together bonded together
-
- 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
- H01F1/0578—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 bonded together
-
- 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
- H01F1/059—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and Va elements, e.g. Sm2Fe17N2
- H01F1/0593—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and Va elements, e.g. Sm2Fe17N2 of tetragonal ThMn12-structure
-
- 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
Abstract
The application discloses a composite bonded magnet containing Sm-Fe-Ti/Nd-Fe-B and a preparation method thereof. The composite bonding magnet containing Sm-Fe-Ti/Nd-Fe-B is composed of a main phase of ThMn 12 Sm-Fe-Ti based magnetic powder with crystalline phase and Nd as main phase 2 Fe 14 The B is formed by compounding Nd-Fe-B base magnetic powder and a binder, wherein the content of the Sm-Fe-Ti base magnetic powder is 10-90 wt%, the content of the binder is 1-5 wt%, and the content of the Nd-Fe-B base magnetic powder is 10-90 wt%. The composite bonded magnet prepared by the application has compact structure, has higher magnetic performance of Nd-Fe-B rare earth permanent magnet and has ThMn 12 The rare earth permanent magnet has good temperature stability, and does not use expensive heavy rare earth elements such as Dy, tb and the likeThe element greatly reduces the production cost of the magnet and is suitable for industrial mass production.
Description
Technical Field
The application belongs to the technical field of bonded magnet preparation, and particularly relates to a composite bonded magnet containing Sm-Fe-Ti/Nd-Fe-B and a preparation method thereof.
Background
The Nd-Fe-B rare earth permanent magnet has excellent magnetic performance and is the most widely used permanent magnet material at present. Along with the development of modern technological life, nd-Fe-B rare earth permanent magnet becomes one of key raw materials of high and new technologies such as electric automobiles, direct-drive wind generators, magnetomechanical technologies, consumer electronics and the like. In order to meet the requirement of the industry field on the higher temperature stability of the magnet, heavy rare earth elements such as Dy, tb and the like are required to be added into the Nd-Fe-B rare earth permanent magnet. However, the price of the heavy rare earth element is high, so that the price of the Nd-Fe-B rare earth permanent magnet also rises sharply. Therefore, development of a novel magnet having a lower price and better temperature stability is urgently required. While ThMn 12 The rare earth permanent magnet has been studied more because of its advantages of high iron content, no use of heavy rare earth elements, good temperature stability, and intrinsic properties comparable to Nd-Fe-B. However, thMn 12 There are also many problems in the preparation of rare earth permanent magnets. First, it is difficult to mix ThMn 12 The rare earth permanent magnet has good intrinsic performance, is converted into extrinsic performance with use value, and has a relatively low coercive force although the anisotropic field is relatively large, and the coercive force is lower than 15% of the anisotropic field; secondly, thMn 12 The rare earth permanent magnet is difficult to prepare compact bulk magnets, and in sintering and hot-press thermal deformation processes, due to the higher vapor pressure of Sm and ThMn 12 Rare earth permanent magnets have no non-magnetic grain boundary phase that can isolate the primary phase grains, so it is difficult to produce dense magnets by both methods. Therefore, how to fully utilize ThMn 12 Rare earth permanent magnets are currently a concern.
Disclosure of Invention
In order to solve the defects and the shortcomings of the prior art, the application aims to provide a composite bonded magnet containing Sm-Fe-Ti/Nd-Fe-B.
Another object of the present application is to provide a method for preparing the above composite bonded magnet.
The application aims at realizing the following technical scheme:
a composite bonded magnet containing Sm-Fe-Ti/Nd-Fe-B is prepared from ThMn as main phase 12 Sm-Fe-Ti based magnetic powder with crystalline phase and Nd as main phase 2 Fe 14 The composite type magnetic powder comprises Nd-Fe-B base magnetic powder of B and a binder, wherein the content of the Sm-Fe-Ti base magnetic powder is 10-90 wt%, the content of the binder is 1-5 wt%, and the content of the Nd-Fe-B base magnetic powder is 10-90 wt%.
Preferably, the component of the Sm-Fe-Ti magnetic powder is Sm x A y Fe 11-z M z Sm is samarium element, A is one of Zr, nd, la, ce, Y elements, fe is iron element, M is one or more of Ti, V, nb, al, ga elements, wherein x is more than 0.4 and less than 1.6,0 and y is more than 0.8, and z is more than 0 and less than 1.5.
A preparation method of a composite bonded magnet containing Sm-Fe-Ti/Nd-Fe-B comprises the following preparation steps:
(1) Preparing Sm according to atomic ratio x A y Fe 11-z M z Raw materials of each element;
(2) Smelting under the protection of inert gas to obtain cast ingots with uniform components;
(3) Mechanically polishing the cast ingot obtained in the step (2), removing a surface oxide layer, and then smelting and rapidly quenching to obtain a strip with uniform components;
(4) Carrying out heat treatment on the strip obtained in the step (3) under the protection of inert gas, and then grinding and sieving the strip to obtain magnetic powder;
(5) Sieving Nd-Fe-B based magnetic powder, mechanically mixing Sm-Fe-Ti based magnetic powder with proper particle size and Nd-Fe-B based magnetic powder with proper particle size, adding the mixed magnetic powder into an organic solvent containing a binder, stirring at room temperature until the organic solvent volatilizes, and drying to obtain mixed powder;
(6) And placing the mixed powder into a die, and performing compression molding and solidification in a pressure device at room temperature.
In the step (1), the raw materials of each element need to be mechanically polished before being configured, so as to remove the surface oxide layer and other impurities.
In the step (2), the inert gas is argon with the purity more than or equal to 99.99 percent.
In the step (2), the smelting mode is one of arc smelting and induction smelting, the smelting process is that each smelting is carried out for 1min, so as to ensure that the Sm volatilization amount in the smelting process is 35 wt%, the furnace is opened for sample turning after the smelting is finished, the smelting is repeated for 3 times,
in the step (3), the smelting and rapid quenching process comprises the following steps: mechanically crushing the polished cast ingot into uniform small cast ingots, then placing the small cast ingots into a quartz tube with an opening small hole of 0.5mm at the lower end, enabling the height of the tube opening to be 2-5mm away from a copper roller, melting the small cast ingots to a molten state under the protection of argon with the purity of more than or equal to 99.99%, and spraying the molten alloy onto the copper roller after the rotating speed of the water-cooled copper roller reaches 30-50m/s to obtain a rapid quenching strip with the thickness of 0.2-0.5 mm.
In the step (4), the temperature of the heat treatment is 800-1000 ℃, and the time of the heat treatment is 5-10min.
In the step (5), the mechanical mixing time of the Sm-Fe-Ti-based magnetic powder and the Nd-Fe-B-based magnetic powder is 20-60 min.
In the step (5), the particle sizes of the Sm-Fe-Ti based magnetic powder and the Nd-Fe-B based magnetic powder are 75-150 mu m.
In the step (5), the adhesive is one of E44 epoxy resin, E51 epoxy resin, F44 epoxy resin and AFG-90H epoxy resin, and the organic solvent is acetone.
In the step (5), the mass ratio of the mixed magnetic powder to the binder is 100:3.
In the step (5), the drying temperature is 80-120 ℃ and the drying time is 0.5-2h.
In the step (6), the pressing pressure is 800-2000MPa, the pressing time is 10-120s, and the pressure device is a hydraulic press.
In the step (6), the curing temperature is 80-200 ℃, and the curing time is 0.5-2h.
Compared with the prior art, the application has the following advantages:
(1) By taking the main phase as ThMn 12 Sm-Fe-Ti magnetic powder with crystal phase and Nd as main phase 2 Fe 14 B Nd-Fe-B magnetic powder is compounded, and the obtained isotropic bonded magnet is combined with ThMn 12 The rare earth permanent magnet and the Nd-Fe-B rare earth permanent magnet have the advantages of higher magnetic performance of the Nd-Fe-B rare earth permanent magnet and ThMn 12 The rare earth permanent magnet has good temperature stability.
(2) Sm-Fe-Ti magnetic powder with the particle size of 75-150 mu m and Nd-Fe-B magnetic powder are mixed, and a bonding process is adopted, so that the bonded magnet obtained by pressing is more compact.
(3) Compared with the Nd-Fe-B bonded magnet widely used at present, due to ThMn 12 The rare earth permanent magnet has high iron content, does not use heavy rare earth elements such as Dy, tb and the like, greatly reduces the production cost of the magnet, and is suitable for industrial mass production.
(4) Compared with the other bonding magnet ferrite widely used at present, the composite bonding magnet has higher magnetic performance, and can fill the gap of magnetic performance between ferrite and Nd-Fe-B bonding magnet.
Drawings
FIG. 1 is a graph showing demagnetization curves of example 1, example 2, comparative example 1, and comparative example 2, in which an external magnetic field is applied at room temperature; wherein, the abscissa is the external magnetic field H, and the ordinate is the magnetic polarization intensity J;
FIG. 2 is a graph showing demagnetization curves of example 1, example 2, comparative example 1, and comparative example 2 when an external magnetic field is applied at 100 ℃.
Detailed Description
The present application will be described in further detail with reference to examples, but embodiments of the present application are not limited thereto. The raw materials related to the application can be directly purchased from the market. For process parameters not specifically noted, reference may be made to conventional techniques.
Example 1
This example produces Sm as the nominal composition 0.8 Zr 0.2 Fe 11 Magnetic powder of Ti and Nd with commercial brand number of MQP-B + 2 Fe 13 The composite bonded magnet of the CoB magnetic powder comprises the following raw materials in parts by weight: sm (Sm) 0.8 Zr 0.2 Fe 11 20 parts of Ti magnetic powder, nd 2 Fe 13 80 parts of CoB magnetic powder and 3 parts of E44 epoxy resin.
The preparation method of the composite bonded magnet comprises the following specific steps:
(1) The components Sm are in atomic ratio 0.8 Zr 0.2 Fe 11 Ti configurationRaw material Sm, zr, fe, ti is ready for use, and the raw material needs to be mechanically polished to remove a surface oxide layer before being configured;
(2) Placing the raw materials in the step (1) into a crucible, wherein Sm is required to be placed at the lowest layer, arc smelting is carried out under the protection of argon with the purity of 99.99%, each time of smelting is carried out for 1min, so as to ensure that the Sm volatile amount in the smelting process is constant, and after the smelting is finished, turning over the furnace, and repeatedly smelting for 3 times to obtain cast ingots with uniform components;
(3) Mechanically polishing the cast ingot obtained in the step (2) to remove a surface oxide layer, mechanically crushing the cast ingot into uniform small cast ingots, then placing the small cast ingots into a quartz tube with an opening small hole of 0.5mm at the lower end, enabling the nozzle to be 2-5mm away from a copper roller, melting the small cast ingots to a molten state under the protection of argon with the purity of more than or equal to 99.99%, and spraying the molten alloy onto the copper roller after the rotating speed of the water-cooled copper roller reaches 30-50m/s to obtain a rapid quenching strip with the thickness of 0.2-0.5 mm;
(4) Putting the rapid quenching strip obtained in the step (3) into a quartz tube, introducing argon with the purity of 99.99%, and performing tube sealing treatment; then placing into a muffle furnace, and heat-treating at 800-1000deg.C for 5-10min. Grinding the heat-treated strip with aluminum oxide mortar, sieving, and sieving Sm with particle diameter of 75-150 μm 0.8 Zr 0.2 Fe 11 Ti magnetic powder;
(5) For Nd with commercial brand number of MQP-B +) 2 Fe 13 Sieving CoB magnetic powder, and sieving Nd with particle size of 75-150 μm 2 Fe 13 CoB magnetic powder;
(6) Weighing Sm in the step (4) according to the weight ratio of 20:80 0.8 Zr 0.2 Fe 11 Ti magnetic powder and Nd in step (5) 2 Fe 13 And (3) placing CoB magnetic powder in a sample tube, and mechanically mixing for 20min to ensure that the two magnetic powder are uniformly mixed. Adding the uniformly mixed magnetic powder into acetone containing E44 epoxy resin, uniformly stirring at room temperature until the acetone volatilizes, and drying in a blowing drying oven at 80 ℃ for 0.5h to obtain mixed powder;
(7) And (3) placing the mixed powder obtained in the step (6) into a hard alloy die with the diameter of 11.5mm, and performing compression molding in a hydraulic press at room temperature, wherein the compression pressure is 1200MPa, and the compression time is 30s. Placing the pressed magnet into a blast drying oven for curing, wherein the curing temperature is 160 ℃ and the curing time is 1.5h;
the room temperature magnetic properties of the prepared composite bonded magnet are shown in fig. 1 and table 1, and the high temperature resistance is shown in fig. 2 and table 2.
Wherein the coercivity temperature coefficientWherein H is cj (T) and H cj (T 0 ) Respectively at temperatures T and T 0 Coercive force at the time, T is 100 ℃, T 0 Is 25 ℃.
Example 2
Unlike example 1, this example changes Sm 0.8 Zr 0.2 Fe 11 Ti magnetic powder and Nd 2 Fe 13 Proportion of CoB magnetic powder. The embodiment consists of the following raw materials in parts by weight: sm (Sm) 0.8 Zr 0.2 Fe 11 60 parts of Ti magnetic powder and Nd with commercial brand number of MQP-B+ 2 Fe 13 40 parts of CoB magnetic powder and 3 parts of E44 epoxy resin.
The preparation method of the composite bonded magnet comprises the following specific steps:
(1) The components Sm are in atomic ratio 0.8 Zr 0.2 Fe 11 Preparing a raw material Sm, zr, fe, ti for standby, wherein the raw material needs to be mechanically polished to remove a surface oxide layer before preparing;
(2) Placing the raw materials in the step (1) into a crucible, wherein Sm is required to be placed at the lowest layer, arc smelting is carried out under the protection of argon with the purity of 99.99%, each smelting time is 1min, so as to ensure that the Sm volatile amount in the smelting process is constant, and after the smelting is finished, turning over the furnace, and repeatedly smelting for 3 times to obtain cast ingots with uniform components.
(3) Mechanically polishing the cast ingot obtained in the step (2) to remove a surface oxide layer, mechanically crushing the cast ingot into uniform small cast ingots, then placing the small cast ingots into a quartz tube with an opening small hole of 0.5mm at the lower end, enabling the tube opening to be 2-5mm away from the copper roller, carrying out smelting and rapid quenching under the protection of argon with the purity of more than or equal to 99.99%, and spraying the molten alloy onto the copper roller after the rotating speed of the water-cooled copper roller reaches 30-50m/s to obtain a rapid quenching strip with the thickness of 0.2-0.5 mm;
(4) And (3) putting the quick quenching strip obtained in the step (3) into a quartz tube, introducing argon with the purity of 99.99%, performing tube sealing treatment, then putting into a muffle furnace, and performing heat treatment for 5-10min at 800-1000 ℃. Grinding the heat-treated strip with aluminum oxide mortar, sieving, and sieving Sm with particle diameter of 75-150 μm 0.8 Zr 0.2 Fe 11 Ti magnetic powder;
(5) For Nd with commercial brand number of MQP-B +) 2 Fe 13 Sieving CoB magnetic powder, and sieving Nd with particle size of 75-150 μm 2 Fe 13 CoB magnetic powder;
(6) Weighing Sm in the step (4) according to the weight ratio of 60:40 0.8 Zr 0.2 Fe 11 Ti magnetic powder and Nd in step (5) 2 Fe 13 And (3) placing CoB magnetic powder in a sample tube, and mechanically mixing for 20min to ensure that the two magnetic powder are uniformly mixed. Adding the uniformly mixed magnetic powder into acetone containing E44 epoxy resin, uniformly stirring at room temperature until the acetone volatilizes, and drying in a blowing drying oven at 80 ℃ for 0.5h to obtain mixed powder;
(7) And (3) placing the mixed powder obtained in the step (6) into a hard alloy die with the diameter of 11.5mm, and performing compression molding in a hydraulic press at room temperature, wherein the compression pressure is 1200MPa, and the compression time is 30s. Placing the pressed magnet into a blast drying oven for curing, wherein the curing temperature is 160 ℃ and the curing time is 1.5h;
the room temperature magnetic properties of the prepared composite bonded magnet are shown in fig. 1 and table 1, and the high temperature resistance is shown in fig. 2 and table 2.
Comparative example 1
Unlike example 1 and example 2, this comparative example uses Sm alone 0.8 Zr 0.2 Fe 11 The Ti magnetic powder is prepared from the following raw materials in parts by weight: sm (Sm) 0.8 Zr 0.2 Fe 11 100 parts of Ti magnetic powder and 3 parts of E44 epoxy resin.
The preparation method of the composite bonded magnet comprises the following specific steps:
(1) The components Sm are in atomic ratio 0.8 Zr 0.2 Fe 11 Preparing raw materials Sm, zr and F by Tie. Ti is reserved, and the raw materials need to be mechanically polished before being configured to remove the surface oxide layer;
(2) Placing the raw materials in the step (1) into a crucible, wherein Sm is required to be placed at the lowest layer, arc smelting is carried out under the protection of argon with the purity of 99.99%, each time of smelting is carried out for 1min, so as to ensure that the Sm volatile amount in the smelting process is constant, and after the smelting is finished, turning over the furnace, and repeatedly smelting for 3 times to obtain cast ingots with uniform components;
(3) Mechanically polishing the cast ingot obtained in the step (2) to remove a surface oxide layer, mechanically crushing the cast ingot into uniform small cast ingots, then placing the small cast ingots into a quartz tube with an opening small hole of 0.5mm at the lower end, enabling the tube opening to be 2-5mm away from the copper roller, carrying out smelting and rapid quenching under the protection of argon with the purity of more than or equal to 99.99%, and spraying the molten alloy onto the copper roller after the rotating speed of the water-cooled copper roller reaches 30-50m/s to obtain a rapid quenching strip with the thickness of 0.2-0.5 mm;
(4) And (3) putting the quick quenching strip obtained in the step (3) into a quartz tube, introducing argon with the purity of 99.99%, performing tube sealing treatment, then putting into a muffle furnace, and performing heat treatment for 5-10min at 800-1000 ℃. Grinding the heat-treated strip with aluminum oxide mortar, sieving, and sieving Sm with particle diameter of 75-150 μm 0.8 Zr 0.2 Fe 11 Ti magnetic powder;
(5) The Sm obtained in the step (4) is subjected to a reaction 0.8 Zr 0.2 Fe 11 Adding Ti magnetic powder into acetone containing E44 epoxy resin, stirring uniformly at room temperature until the acetone volatilizes, and drying in a blast drying oven at 80 ℃ for 0.5h to obtain dried powder;
(6) Placing the powder obtained in the step (5) into a hard alloy die with the diameter of 11.5mm, and performing compression molding in a hydraulic press at room temperature, wherein the compression pressure is 1200MPa, and the compression time is 30s. Placing the pressed magnet into a blast drying oven for curing, wherein the curing temperature is 160 ℃ and the curing time is 1.5h;
the room temperature magnetic properties of the prepared bonded magnet are shown in fig. 1 and table 1, and the high temperature resistance is shown in fig. 2 and table 2.
Comparative example 2
Unlike comparative example 1, this comparative example uses only Nd with the commercial designation MQP-B + 2 Fe 13 The CoB magnetic powder comprises the following raw materials in parts by weight: nd 2 Fe 13 100 parts of CoB magnetic powder and 3 parts of E44 epoxy resin.
The preparation method of the composite bonded magnet comprises the following steps:
(1) Sieving with a screen to obtain Nd with particle size of 75-150 μm 2 Fe 13 Adding the screened magnetic powder into acetone containing E44 epoxy resin, uniformly stirring at room temperature until the acetone volatilizes, and drying in a blast drying oven at 80 ℃ for 0.5h to obtain dried powder;
(6) The powder obtained in step (1) was placed in a cemented carbide mold having a diameter of 11.5mm, and was press-molded at room temperature under a pressure of 1200MPa for a dwell time of 30s. Placing the pressed magnet into a blast drying oven for curing, wherein the curing temperature is 160 ℃ and the curing time is 1.5h;
table 1 magnetic properties at room temperature comparison
Magnetic properties: the measurement is carried out according to GB-T3217-2013 permanent magnet (hard magnetic) material magnetism test method.
TABLE 2 comparison of magnetic energy product decline
As can be seen from examples and comparative examples, nd was added 2 Fe 13 The magnetic property of the Sm-Fe-Ti/Nd-Fe-B composite bonding magnet of the CoB magnetic powder is superior to that of Sm only 0.8 Zr 0.2 Fe 11 A bonded magnet prepared from Ti magnetic powder. In example 2, sm was added 0.8 Zr 0.2 Fe 11 Sm-Fe-Ti/Nd-Fe-B composite bonding magnet of Ti magnetic powderThe coercive force temperature coefficient of the body is larger than that of Nd alone 2 Fe 13 Bonded magnets made of CoB magnetic powder and having a magnetic energy product reduced by a percentage less than Nd alone 2 Fe 13 The bonded magnet prepared from CoB magnetic powder shows that the temperature stability is good. Compared with the Nd-Fe-B bonded magnet widely used at present, the Sm-Fe-Ti/Nd-Fe-B composite bonded magnet has lower raw material price and Sm 0.8 Zr 0.2 Fe 11 The raw material price of each element of Ti is Nd only 2 Fe 13 7% of CoB, sm is added 0.8 Zr 0.2 Fe 11 The raw material price of example 1 of the Ti magnetic powder was reduced by 19% compared with comparative example 2, but the magnetic properties were not greatly reduced; and the magnetic energy product of the ferrite of the other bonding magnet widely used at present is only 0.8-13kJ/m 3 Whereas the magnetic energy product of example 1 of the present application was 64kJ/m 3 The bonded magnet of the present application is superior to ferrite, and thus can fill the market gap between ferrite and Nd-Fe-B bonded magnet.
The above examples are preferred embodiments of the present application, but the embodiments of the present application are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present application should be made in the equivalent manner, and the embodiments are included in the protection scope of the present application.
Claims (9)
1. A composite bonded magnet containing Sm-Fe-Ti/Nd-Fe-B is characterized in that: from the main phase of ThMn 12 Sm-Fe-Ti based magnetic powder with crystalline phase and Nd as main phase 2 Fe 14 The composite type magnetic powder comprises Nd-Fe-B base magnetic powder of B and a binder, wherein the content of the Sm-Fe-Ti base magnetic powder is 10-90 wt%, the content of the binder is 1-5 wt%, and the content of the Nd-Fe-B base magnetic powder is 10-90 wt%;
the component composition of the Sm-Fe-Ti-based magnetic powder is Sm x A y Fe 11-z M z Sm is samarium element, A is one of Zr, nd, la, ce, Y elements, fe is iron element, M is one or more of Ti, V, nb, al, ga elements, wherein x is more than 0.4 and less than 1.6,0 and y is more than 0.8, and z is more than 0 and less than 1.5.
2. The Sm-Fe-Ti/Nd-Fe-B containing composite bonded magnet according to claim 1, wherein: the content of the Sm-Fe-Ti-based magnetic powder is 20-60 wt%, the content of the binder is 3 wt%, and the content of the Nd-Fe-B-based magnetic powder is 40-80 wt%.
3. A preparation method of a composite bonded magnet containing Sm-Fe-Ti/Nd-Fe-B is characterized by comprising the following steps: the preparation method comprises the following preparation steps:
(1) Preparing Sm according to atomic ratio x A y Fe 11-z M z Raw materials of each element;
(2) Smelting under the protection of inert gas to obtain cast ingots with uniform components;
(3) Mechanically polishing the cast ingot obtained in the step (2), removing a surface oxide layer, and then smelting and rapidly quenching to obtain a strip with uniform components;
(4) Carrying out heat treatment on the strip obtained in the step (3) under the protection of inert gas, and then grinding and sieving the strip to obtain magnetic powder;
(5) Sieving Nd-Fe-B based magnetic powder, mechanically mixing Sm-Fe-Ti based magnetic powder with proper particle size and Nd-Fe-B based magnetic powder with proper particle size, adding the mixed magnetic powder into an organic solvent containing a binder, uniformly stirring at room temperature until the organic solvent volatilizes, and drying to obtain mixed powder;
(6) And placing the mixed powder into a die, and performing compression molding and solidification in a pressure device at room temperature.
4. A method for producing a Sm-Fe-Ti/Nd-Fe-B containing composite bonded magnet according to claim 3, characterized in that:
in the step (1), the raw materials of each element need to be mechanically polished before being configured, so as to remove the surface oxide layer and other impurities.
5. A method for producing a Sm-Fe-Ti/Nd-Fe-B containing composite bonded magnet according to claim 3, characterized in that:
in the step (2), the inert gas is argon with the purity more than or equal to 99.99 percent;
in the step (2), the smelting mode is one of arc smelting and induction smelting, the smelting process is that each smelting is carried out for 1min, the furnace is opened for turning after the smelting is completed, and the smelting is repeated for 3 times.
6. A method for producing a Sm-Fe-Ti/Nd-Fe-B containing composite bonded magnet according to claim 3, characterized in that:
in the step (3), the smelting and rapid quenching process comprises the following steps: mechanically crushing the polished cast ingot into uniform small cast ingots, then placing the small cast ingots into a quartz tube with an opening small hole of 0.5mm at the lower end, enabling the height of the tube opening to be 2-5mm away from a copper roller, melting the small cast ingots to a molten state under the protection of argon with the purity of more than or equal to 99.99%, and spraying the molten alloy onto the copper roller after the rotating speed of the water-cooled copper roller reaches 30-50m/s to obtain a rapid quenching strip with the thickness of 0.2-0.5 mm.
7. A method for producing a Sm-Fe-Ti/Nd-Fe-B containing composite bonded magnet according to claim 3, characterized in that:
in the step (4), the temperature of the heat treatment is 800-1000 ℃, and the time of the heat treatment is 5-10min.
8. A method for producing a Sm-Fe-Ti/Nd-Fe-B containing composite bonded magnet according to claim 3, characterized in that:
in the step (5), the mechanical mixing time of the Sm-Fe-Ti-based magnetic powder and the Nd-Fe-B-based magnetic powder is 20-60 min;
in the step (5), the particle sizes of the Sm-Fe-Ti based magnetic powder and the Nd-Fe-B based magnetic powder are 75-150 mu m;
in the step (5), the adhesive is one of E44 epoxy resin, E51 epoxy resin, F44 epoxy resin and AFG-90H epoxy resin, and the organic solvent is acetone;
in the step (5), the mass part ratio of the mixed magnetic powder to the binder is 100:3;
in the step (5), the drying temperature is 80-120 ℃ and the drying time is 0.5-2h.
9. A method for preparing a composite bonded magnet containing Sm-Fe-Ti/Nd-Fe-B as set forth in claim 3, characterized in that:
in the step (6), the pressing pressure is 800-2000MPa, the pressing time is 10-120s, and the pressure device is a hydraulic press;
in the step (6), the curing temperature is 80-200 ℃, and the curing time is 0.5-2h.
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