CN116825462B - Vehicle-mounted Gao Wen-iron-boron-resistant permanent magnet and preparation method thereof - Google Patents
Vehicle-mounted Gao Wen-iron-boron-resistant permanent magnet and preparation method thereof Download PDFInfo
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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
- H01F1/057—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
- H01F1/0576—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 pressed, e.g. hot working
-
- 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
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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
- H01F41/0266—Moulding; Pressing
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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
- H01F41/0293—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 diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
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- Engineering & Computer Science (AREA)
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- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The invention belongs to the field of magnetic materials, and particularly relates to a vehicle-mounted Gao Wen-iron-boron-resistant permanent magnet and a preparation method thereof, wherein the preparation method comprises the following steps: 1) Uniformly mixing matrix phase magnetic powder, R phase magnetic powder, B phase magnetic powder, a linking material and a wetting agent, placing the mixture in a mould for orientation and carrying out low-temperature hot-press molding to obtain a rough blank; 2) And performing cold deformation processing on the rough blank after low-temperature primary sintering, controlling the processing deformation amount of the rough blank, and sequentially performing high-temperature sintering and tempering treatment to obtain the vehicle-mounted Gao Wen-iron-boron-resistant permanent magnet. The invention realizes effective optimization of the performance of the permanent magnet material through component and structure adjustment, has better temperature resistance, and simultaneously improves the mechanical property and thermal shock resistance of the permanent magnet material, so that the permanent magnet material has very excellent use effect when being used for vehicles.
Description
Technical Field
The invention belongs to the field of magnetic materials, and particularly relates to a vehicle-mounted Gao Wen-iron-boron-resistant permanent magnet and a preparation method thereof.
Background
Neodymium iron boron magnets are the most widely used permanent magnet materials and the most mature manufacturing process at present, and are also called hard magnet materials, which are materials capable of keeping constant magnetism after being magnetized. It finds application in various fields by virtue of its excellent magnetic properties.
With the development of new energy automobile fields in China in recent years, different demands are also made on the performance of the NdFeB permanent magnets. In new energy automobiles, the permanent magnet material has wide application, namely the most common application is a starting motor part, and in starting motor structures such as a driving motor and a power-assisted steering motor of the automobile, the weight and the volume of the automobile can be obviously reduced by adopting the permanent magnet motor, so that the permanent magnet material is a key for realizing light weight and miniaturization of the existing new energy automobiles.
However, the existing permanent magnets have obvious use defects when used in vehicle. For example, the magnetic performance of the conventional NdFeB permanent magnet is only 82-85% under the working temperature condition of about 100 ℃, and the magnetic performance is further severely reduced when the temperature is increased to 180 ℃ and 260 ℃. Meanwhile, the permanent magnet is cracked and damaged and loses weight and fails due to the high-frequency vibration of the motor and the thermal shock environment generated by the cold circulation in the new energy vehicle. It can be seen that the existing neodymium iron boron magnet generally does not have excellent temperature resistance. In order to solve the problem, technicians continuously develop the high-resistance Wen iron boron magnetic steel. For example, the common dysprosium-series and/or terbium-series Gao Wen-series permanent magnets are used as permanent magnet materials which are successfully developed relatively early and have good service performance, and can keep good magnetic performance under the working condition of higher temperature, but the permanent magnets are high in cost due to the fact that higher dysprosium and/or terbium content is needed, and the permanent magnets are easy to crack and damage and lose efficacy under the thermal shock condition and the high-frequency shock condition. In this regard, the development of the low dysprosium Gao Wen iron boron permanent magnet is realized by the technical personnel through research and development, and the permanent magnet has a certain thermal shock resistance, but the mechanical property of the permanent magnet is found to have obvious defects in the actual use process, such as the permanent magnet is easy to damage and lose efficacy under the near 100Hz high-frequency vibration condition.
Disclosure of Invention
The invention aims to provide a vehicle-mounted Gao Wen-resistant iron-boron permanent magnet and a preparation method thereof.
The invention aims at: the high temperature resistance of the neodymium iron boron permanent magnet can be effectively improved, the neodymium iron boron permanent magnet can be suitable for a high-frequency environment in vehicle-mounted use, and the neodymium iron boron permanent magnet can be effectively suitable for the use of a starting motor part of a new energy vehicle.
In order to achieve the above object, the present invention adopts the following scheme.
A method for preparing a vehicle-mounted Gao Wen-iron-boron permanent magnet,
the preparation method comprises the following steps:
1) Uniformly mixing matrix phase magnetic powder, R phase magnetic powder, B phase magnetic powder, a linking material and a wetting agent, placing the mixture in a mould for orientation and carrying out low-temperature hot-press molding to obtain a rough blank;
2) And performing cold deformation processing on the rough blank after low-temperature primary sintering, controlling the processing deformation amount of the rough blank, and sequentially performing high-temperature sintering and tempering treatment to obtain the vehicle-mounted Gao Wen-iron-boron-resistant permanent magnet.
Further, the method comprises the steps of,
the composition of the matrix phase magnetic powder in the step 1) comprises the following components:
13 to 15at% of PrNd, 6 to 6.5at% of B and the balance of Fe;
the praseodymium-neodymium alloy, boron and iron are weighed according to the ingredients, and then are mixed for smelting and crushing to prepare 100-120 mesh matrix phase magnetic powder.
Further, the method comprises the steps of,
the component composition of the R-phase magnetic powder in the step 1) comprises:
12-16at% of NdCu, 6-8at% of Nd, 2-3at% of Dy, 1.5-2.5at% of Ni, 0.5-1.0at% of Tb and the balance of Fe;
according to the components, the ingredients are weighed, mixed, smelted and crushed to prepare R-phase magnetic powder with 20-35 meshes.
Further, the method comprises the steps of,
the component composition of the B-phase magnetic powder in the step 1) comprises:
nd 0.5-2.0 at%, B35-45 at% and Fe for the rest;
according to the components, the ingredients are weighed, mixed, smelted and crushed to prepare the B-phase magnetic powder with the mesh number of 2000-8000 meshes.
Further, the method comprises the steps of,
the usage mass ratio of the matrix phase magnetic powder, the R phase magnetic powder and the B phase magnetic powder is 100: (12-22): (5-8).
Further, the method comprises the steps of,
the linking material is metal aluminum powder;
the wetting agent is organic silicone oil, and methyl silicone oil is usually selected;
the consumption of the linking material is 1-3wt% of the matrix phase magnetic powder;
the dosage of the wetting agent is 5-8wt% of the matrix phase magnetic powder.
Further, the method comprises the steps of,
the orientation process in the step 1) controls the strength of an orientation magnetic field to be 1.3-1.6 and T, and the orientation time is 25-30 min;
the low-temperature hot pressing process in the step 1) is carried out under the vacuum condition, the control temperature is 80-95 ℃, the hot pressing pressure is 15-25 MPa, and the pressure maintaining time is 25-35 min.
Further, the method comprises the steps of,
step 2), controlling the temperature in the low-temperature primary sintering process to be 360-380 ℃ and the sintering time to be 1-2 h;
and 2) controlling the deformation amount of the cold working deformation to be 12-15%.
Further, the method comprises the steps of,
step 2), sintering at the high temperature in a non-nitrogen protective atmosphere or a vacuum atmosphere, wherein the sintering temperature is 1050-1150 ℃ and the sintering time is 2-4 h;
and 2) tempering, wherein the tempering control swing temperature is 560-620 ℃ and the tempering time is 5-7 h.
A vehicle-mounted Gao Wen-iron-boron-resistant permanent magnet.
The preparation method of the vehicle-mounted Gao Wen-resistant iron-boron permanent magnet is complete as follows:
1) Weighing praseodymium-neodymium alloy, boron and iron according to the proportion of PrNd 13-15 at%, B6-6.5 at% and the balance of Fe, mixing, carrying out vacuum smelting and ball milling at 1520-1560 ℃, preparing R2Fe14B matrix phase magnetic powder of 100-120 meshes, weighing neodymium, neodymium copper alloy, dysprosium, terbium, nickel and iron according to the proportion of NdCu 12-16 at%, nd 6-8 at%, dy 2-3 at%, ni 1.5-2.5 at%, tb 0.5-1.0 at% and the balance of Fe, mixing, carrying out vacuum smelting and ball milling at 1720-1760 ℃, preparing R2TM 8R phase magnetic powder of 20-35 meshes, weighing neodymium, iron and boron according to the proportion of Nd 0.5-2.0 at%, B35-45 at% and the balance of Fe, mixing, carrying out vacuum smelting at 1520-1560 ℃, hydrogen crushing and ball milling, and preparing RB4TM 8B phase magnetic powder of 2000-8000 meshes;
2) Taking matrix phase magnetic powder, R phase magnetic powder and B phase magnetic powder according to the mass ratio of 100: (12-22): mixing the components in the ratio of (5-8), adding 1-3wt% of metal aluminum powder of the matrix phase magnetic powder and 5-8wt% of dimethyl silicone oil of the matrix phase magnetic powder, uniformly mixing, placing the mixture in a die to orient for 25-30 min under the condition of 1.3-1.6T, and hot-pressing for 25-35 min under the condition of 15-25 MPa at the low temperature of 80-95 ℃ to obtain a rough blank;
3) And (3) performing primary sintering at the low temperature of 360-380 ℃ for 1-2 hours, performing cold deformation processing, controlling the processing deformation amount to be 12-15%, then sintering at the high temperature of 1050-1150 ℃ in a vacuum atmosphere for 2-4 hours, and tempering at the temperature of 560-620 ℃ for 5-7 hours to obtain the vehicle-mounted Gao Wen-resistant iron-boron permanent magnet.
In the process, the invention adopts the multiphase magnetic powder composite sintering process which is emerging in recent years for research. The multiphase magnetic powder composite sintering process generally adopts two-phase magnetic powder for matching, one is used as a main phase, the other is used as an auxiliary phase, the mechanical property and the special property of the permanent magnet are enhanced through the auxiliary phase, and the main phase is used as a main magnetic phase to form stable magnetism. However, the existing multi-phase magnetic powder composite sintering process is basically only suitable for the sintering treatment of the dual-phase magnetic powder, but is not suitable for the mixed use of more multi-phase magnetic powder. The main reasons are that excessive phase components are difficult to homogenize, and the problems of unstable magnetic property, unstable mechanical property and the like are easy to generate, and because different phase materials have different inherent magnetism, in-phase agglomeration and uneven distribution are easy to generate in the mixing process. But the invention adopts three-phase magnetic powder matching, and firstly solves the problem of difficult mixing of multiphase magnetic powder. In order to solve the problem, the technical scheme of the invention adopts coarser matrix phase magnetic powder and R phase magnetic powder, so that the problem of the agglomeration of the prior magnetism can be avoided to a certain extent, and meanwhile, ultrafine B phase magnetic powder is added. The matrix phase magnetic powder and the R phase magnetic powder are main components which are mutually matched to generate magnetism, the matrix phase magnetic powder can generate more effective magnetic phases in the sintering process, the R phase magnetic powder has a magnetic phase structure, and the B phase magnetic powder adopts superfine powder for adding so as to realize three-phase dispersion. The B-phase magnetic powder has weak initial magnetism, basically has no obvious magnetism before orientation molding, has good dispersivity, is easy to uniformly disperse between the matrix phase magnetic powder and the R-phase magnetic powder with larger particles, is used as an interface to separate the matrix phase magnetic powder and the R-phase magnetic powder so as to improve the dispersion uniformity, and meanwhile, the B-phase magnetic powder can generate good pinning effect, and the coarse-grain magnet generates polycrystal mode crystallization so as to ensure the dispersion uniformity of the matrix phase magnetic powder and the R-phase magnetic powder and realize processing refinement. In order to match with the processing refining effect, the invention also adopts cold processing deformation after primary burning.
Cold working deformation is a common way of working alloys and parts of permanent magnets. The method generally adopts a large pressure of 60MPa or more to form at least 60% of large deformation supercritical cold working deformation, and even adopts super strong pressure of hundreds of megapascals to carry out the super large deformation supercritical cold working deformation with the deformation reaching 95%, and aims to realize phagocytosis coarsening and growth of crystal grains and then crush and refine again so as to obtain better mechanical properties. However, for the multiphase magnetic powder composite magnetic powder, the adoption of supercritical cold working deformation cannot generate good beneficial effects, even the phenomenon of ingredient enrichment is more serious possibly caused by the engulfment and coarsening growth of crystal grains, and the density of the permanent magnet is too high, so that the problem that the permanent magnet is easy to crack or even differentiate under the thermal shock condition due to uneven ingredients, high density and the difference of the swelling and shrinking of part of the ingredients is caused. The invention adopts coarse matrix phase magnetic powder, R phase magnetic powder and superfine B phase magnetic powder to match, and adopts about 30MPa pressure to carry out near critical cold deformation processing, because the matrix phase magnetic powder and R phase magnetic powder have larger particles, the internal swallowing and coarsening growth process is not easy to overgrow, the B phase magnetic powder gradually increases coarsely and becomes larger, and because of the crushing property and pinning effect, the coarse crystal structures of the matrix phase magnetic powder and R phase magnetic powder reaching critical deformation are easily damaged in cold deformation processing, so that the B phase magnetic powder can be further crushed and diffused into the original matrix phase magnetic powder and R phase magnetic powder, secondary homogenization and grain refinement are realized, the effect that the coarse crystal refinement can be realized only by supercritical processing deformation is realized, the optimization of the mechanical property of the permanent magnet can be realized under the condition of small amount of deformation processing, and the compactness of the magnet is correspondingly slightly reduced, so that the harm of thermal shock to the permanent magnet is reduced.
In addition, the invention adopts special R-phase magnetic powder, lubricant and linking material for matching in order to realize the optimization of the high temperature resistance of the permanent magnet. The R-phase-rich magnetic powder adopts the scheme of matching low-content dysprosium with low-content terbium to replace the dysprosium component which is required to be at least 7.2at% for the traditional Gao Wen-iron-boron-resistant permanent magnet, reduces the consumption of high-value rare earth, saves the cost to a certain extent, and has lower actual dysprosium content and terbium content in the whole permanent magnet material, but can generate good high-temperature resistance. The high dysprosium component is required to be adopted in the traditional high dysprosium neodymium iron boron magnet because of the single-phase composition characteristic and the dysprosium diffusion characteristic, dysprosium is directly doped in the permanent magnet material and diffused, the diffusion trend of the dysprosium is led to form deep enrichment and cannot be uniformly dispersed in the permanent magnet material, and in order to ensure effective dispersion of the dysprosium, each part of the integral permanent magnet material can be ensured to reach a certain dysprosium content, namely, a back diffusion region can also be ensured to have a certain dysprosium content. However, the invention adopts a multiphase composite technology to match with B-phase magnetic powder dispersion and cold working deformation, so that R-phase magnetic powder can be uniformly dispersed firstly, and then is limited by interface action in the treatment process, so that dysprosium diffusion distance is limited, and each part can be ensured to contain dispersed dysprosium. Terbium is added to reduce the temperature sensitivity of the permanent magnet material. Compared with dysprosium, the addition of terbium can not improve the magnetic performance of the permanent magnet material, but can improve the coercive force of the permanent magnet to a certain extent, because the anisotropic field of the intermetallic table formed by terbium, TM (transition metal) and boron is much larger than that of the intermetallic table formed by dysprosium, TM and boron, and meanwhile, the anisotropic field can promote the formation of the diamagnetic domain nucleation field of magnetocrystalline, so that the sensitivity of the magnet to temperature is weakened, and the temperature resistance of the permanent magnet is improved.
In addition, the invention also adopts organic silicone oil as a lubricant and metal aluminum powder as a linking material. The organic silicone oil is decomposed to form silicon dioxide in the heat treatment process and is matched with the metal aluminum powder to form a glassy continuous belt, the glassy continuous belt can form the limit on magnetic crystals and magnetic domains, the stability of the magnetic crystals and the magnetic domains under the high-temperature condition is improved, a barrier belt is formed, the formation of the barrier belt further inhibits the enrichment and diffusion trend of dysprosium, and the problems of component segregation and the like are avoided.
The invention has the advantages that: the invention realizes effective optimization of the performance of the permanent magnet material through component and structure adjustment, has better temperature resistance, and simultaneously improves the mechanical property and thermal shock resistance of the permanent magnet material, so that the permanent magnet material has very excellent use effect when being used for vehicles.
Detailed Description
The present invention will be described in further detail with reference to specific examples. Those of ordinary skill in the art will be able to implement the invention based on these descriptions. In addition, the embodiments of the present invention referred to in the following description are typically only some, but not all, embodiments of the present invention. Therefore, all other embodiments, which can be made by one of ordinary skill in the art without undue burden, are intended to be within the scope of the present invention, based on the embodiments of the present invention.
The raw materials used in the examples of the present invention are all commercially available or available to those skilled in the art unless specifically stated otherwise; the methods used in the examples of the present invention are those known to those skilled in the art unless specifically stated otherwise.
Example 1
A vehicle-mounted Gao Wen-iron-boron-resistant permanent magnet is prepared by the following method:
1) Weighing praseodymium-neodymium alloy, boron and iron according to the proportion of PrNd 14at%, B6 at% and the balance of Fe, mixing, carrying out vacuum melting and ball milling at 1550 ℃, respectively sieving with 100-120 meshes to obtain 100-120 meshes of R2Fe14B matrix phase magnetic powder, weighing neodymium, neodymium-copper alloy, dysprosium, terbium, nickel and iron according to the proportion of NdCu 13.5at%, nd 7at%, dy 2.5at%, ni 2at%, tb 0.8at% and the balance of Fe, mixing, carrying out vacuum melting and ball milling at 1750 ℃ to obtain 20-35 meshes of R2TM 8R phase magnetic powder, respectively sieving with 20-35 meshes of Nd 1.0at%, B40 at%, and the balance of Fe, weighing neodymium, iron and boron, mixing, carrying out vacuum melting, hydrogen crushing and ball milling at 1550 ℃ according to the proportion of Nd 1.0at%, and 8000 meshes of Fe, and respectively sieving with 6000-8000 meshes to obtain RB4TM6B phase magnetic powder with 6000-8000 meshes;
2) Taking matrix phase magnetic powder, R phase magnetic powder and B phase magnetic powder according to the mass ratio of 100:17:6, adding 2wt% of metal aluminum powder of the matrix phase magnetic powder and 6wt% of dimethyl silicone oil of the matrix phase magnetic powder, uniformly mixing, placing in a mould, orienting for 30min under the condition of 1.3T, and hot-pressing for 30min under the condition of 20MPa at the low temperature of 85 ℃ to obtain a rough blank;
3) And (3) performing low-temperature primary sintering on the rough blank at 380 ℃ for 1.5 hours, performing cold deformation processing at 30MPa, controlling the processing deformation amount to be 13%, then placing the rough blank in a vacuum atmosphere, performing high-temperature sintering at 1100 ℃ for 3 hours, and performing tempering treatment at 600 ℃ for 6 hours to obtain the vehicle-mounted Gao Wen-iron-boron permanent magnet.
And performing characterization test on the performance of the prepared vehicle-mounted Gao Wen-iron-boron permanent magnet.
The frequency vibration weightlessness rate is that the sample is placed on a 200Hz ultrahigh frequency vibration testing machine, then a thermal vibration test is carried out, the vibration test is continuously carried out for 12 hours, the sample mass before and after the measurement is carried out, and the weightlessness rate is calculated so as to verify the anti-vibration performance of the sample. In addition, a thermal shock test is carried out on the sample, the sample is quickly heated to 200 ℃ and kept warm for ten minutes, then the temperature is quickly reduced to less than or equal to 15 ℃ within 10 seconds in a water cooling mode, and after 300 times of quick temperature rise and reduction cycles are repeatedly carried out, the quality change of the sample is characterized, the macroscopic surface morphology of the sample is observed, the surface of the sample prepared by the method has no cracks and cracks, the volume has no obvious change, the quality change rate is less than 0.5%, and the permanent magnet prepared by the method has very excellent thermal shock resistance.
Example 2
A vehicle-mounted Gao Wen-iron-boron-resistant permanent magnet is prepared by the following method:
1) Weighing praseodymium-neodymium alloy, boron and iron according to the proportion of PrNd 13at%, B6 at% and the balance of Fe, mixing, carrying out vacuum melting and ball milling at 1550 ℃, respectively sieving with 100-120 meshes to obtain 100-120 meshes of R2Fe14B matrix phase magnetic powder, weighing neodymium, neodymium-copper alloy, dysprosium, terbium, nickel and iron according to the proportion of NdCu 12at%, nd 6at%, dy 3at%, ni 2.5at%, tb 0.5at% and the balance of Fe, mixing, carrying out vacuum melting and ball milling at 1750 ℃, respectively sieving with 20-35 meshes to obtain 20-35 meshes of R2TM 8R phase magnetic powder, weighing neodymium, iron and boron according to the proportion of Nd 0.5at%, B45 at% and the balance of Fe, mixing, carrying out vacuum melting at 1550 ℃, hydrogen crushing and ball milling, respectively sieving with 6000 meshes and 8000 meshes to obtain 6000-8000 meshes of RB4TM6B phase magnetic powder;
2) Taking matrix phase magnetic powder, R phase magnetic powder and B phase magnetic powder according to the mass ratio of 100:12:5, adding 1wt% of metal aluminum powder of the matrix phase magnetic powder and 5wt% of dimethyl silicone oil of the matrix phase magnetic powder, uniformly mixing, placing in a mould, orienting for 30min under the condition of 1.3T, and hot-pressing for 30min under the condition of 20MPa at the low temperature of 80 ℃ to obtain a rough blank;
3) And (3) performing low-temperature primary sintering on the rough blank at 380 ℃ for 1.5 hours, performing cold deformation processing at 30MPa, controlling the processing deformation amount to be 12%, then placing the rough blank in a vacuum atmosphere, performing high-temperature sintering at 1100 ℃ for 3 hours, and performing tempering treatment at 600 ℃ for 6 hours to obtain the vehicle-mounted Gao Wen-iron-boron permanent magnet.
And performing characterization test on the performance of the prepared vehicle-mounted Gao Wen-iron-boron permanent magnet.
| Test temperature | Br(T) | Hcj(kA/m) | Frequency vibration weight loss ratio (%) |
| 20℃ | 1.17 | 1.82×10 3 | ＜0.1 |
| 100℃ | 1.16 | 1.76×10 3 | ＜0.1 |
| 150℃ | 1.15 | 1.67×10 3 | ＜0.1 |
| 180℃ | 1.14 | 1.50×10 3 | ＜0.1 |
| 260℃ | 1.10 | 1.22×10 3 | 0.3 |
The frequency vibration weightlessness rate is that the sample is placed on a 200Hz ultrahigh frequency vibration testing machine, then a thermal vibration test is carried out, the vibration test is continuously carried out for 12 hours, the sample mass before and after the measurement is carried out, and the weightlessness rate is calculated so as to verify the anti-vibration performance of the sample. In addition, a thermal shock test is carried out on the sample, the sample is quickly heated to 200 ℃ and kept warm for ten minutes, then the temperature is quickly reduced to less than or equal to 15 ℃ within 10 seconds in a water cooling mode, and after 300 times of quick temperature rise and reduction cycles are repeatedly carried out, the quality change of the sample is characterized, the macroscopic surface morphology of the sample is observed, the surface of the sample prepared by the method has no cracks and cracks, the volume has no obvious change, the quality change rate is less than 0.5%, and the permanent magnet prepared by the method has very excellent thermal shock resistance.
Example 3
A vehicle-mounted Gao Wen-iron-boron-resistant permanent magnet is prepared by the following method:
1) Weighing praseodymium-neodymium alloy, boron and iron according to the proportion of PrNd 15at%, B6.5 at% and the balance of Fe, mixing, carrying out vacuum melting and ball milling at 1550 ℃, respectively sieving with 100-120 meshes to obtain 100-120 meshes of R2Fe14B matrix phase magnetic powder, weighing neodymium, neodymium-copper alloy, dysprosium, terbium, nickel and iron according to the proportion of NdCu 16at%, nd 8at%, dy 2at%, ni 1.5at%, tb 1.0at% and the balance of Fe, mixing, carrying out vacuum melting and ball milling at 1750 ℃, respectively sieving with 20-35 meshes to obtain 20-35 meshes of R2TM 8R phase magnetic powder, weighing neodymium, iron and boron according to the proportion of Nd 2.0at%, B35 at% and the balance of Fe, mixing, carrying out vacuum melting, hydrogen crushing and ball milling at 1550 ℃, and respectively sieving with 6000 meshes and 8000 meshes to obtain 6000-8000 meshes of RB4TM6B phase magnetic powder;
2) Taking matrix phase magnetic powder, R phase magnetic powder and B phase magnetic powder according to the mass ratio of 100:22:8, adding 3wt% of metal aluminum powder of the matrix phase magnetic powder and 8wt% of dimethyl silicone oil of the matrix phase magnetic powder, uniformly mixing, placing in a mould, orienting for 30min under the condition of 1.3T, and hot-pressing for 35min under the condition of 15MPa at the low temperature of 95 ℃ to obtain a rough blank;
3) And (3) performing low-temperature primary sintering on the rough blank at 380 ℃ for 1.5 hours, performing cold deformation processing at 30MPa, controlling the processing deformation amount to be 15%, then placing the rough blank in a vacuum atmosphere, performing high-temperature sintering at 1100 ℃ for 3 hours, and performing tempering treatment at 600 ℃ for 6 hours to obtain the vehicle-mounted Gao Wen-iron-boron permanent magnet.
And performing characterization test on the performance of the prepared vehicle-mounted Gao Wen-iron-boron permanent magnet.
The frequency vibration weightlessness rate is that the sample is placed on a 200Hz ultrahigh frequency vibration testing machine, then a thermal vibration test is carried out, the vibration test is continuously carried out for 12 hours, the sample mass before and after the measurement is carried out, and the weightlessness rate is calculated so as to verify the anti-vibration performance of the sample. In addition, a thermal shock test is carried out on the sample, the sample is quickly heated to 200 ℃ and kept warm for ten minutes, then the temperature is quickly reduced to less than or equal to 15 ℃ within 10 seconds in a water cooling mode, and after 300 times of quick temperature rise and reduction cycles are repeatedly carried out, the quality change of the sample is characterized, the macroscopic surface morphology of the sample is observed, the surface of the sample prepared by the method has no cracks and cracks, the volume has no obvious change, the quality change rate is less than 0.5%, and the permanent magnet prepared by the method has very excellent thermal shock resistance.
Example 4
A vehicle-mounted Gao Wen-iron-boron-resistant permanent magnet is prepared by the following method:
1) Weighing praseodymium-neodymium alloy, boron and iron according to the proportion of PrNd 14at%, B6 at% and the balance of Fe, mixing, carrying out vacuum melting and ball milling at 1550 ℃, respectively sieving with 100-120 meshes to obtain 100-120 meshes of R2Fe14B matrix phase magnetic powder, weighing neodymium, neodymium-copper alloy, dysprosium, terbium, nickel and iron according to the proportion of NdCu 13.5at%, nd 7at%, dy 2.5at%, ni 2at%, tb 0.8at% and the balance of Fe, mixing, carrying out vacuum melting and ball milling at 1750 ℃ to obtain 20-35 meshes of R2TM 8R phase magnetic powder, respectively sieving with 20-35 meshes of Nd 1.0at%, B40 at%, and the balance of Fe, weighing neodymium, iron and boron, mixing, carrying out vacuum melting, hydrogen crushing and ball milling at 1550 ℃ according to the proportion of Nd 1.0at%, and 8000 meshes of Fe, and respectively sieving with 6000-8000 meshes to obtain RB4TM6B phase magnetic powder with 6000-8000 meshes;
2) Taking matrix phase magnetic powder, R phase magnetic powder and B phase magnetic powder according to the mass ratio of 100:17:8, adding 2wt% of metal aluminum powder of the matrix phase magnetic powder and 8wt% of dimethyl silicone oil of the matrix phase magnetic powder, uniformly mixing, placing in a mould, orienting for 30min under the condition of 1.3T, and hot-pressing for 30min under the condition of 20MPa at the low temperature of 85 ℃ to obtain a rough blank;
3) And (3) performing low-temperature primary sintering on the rough blank at 380 ℃ for 1.5 hours, performing cold deformation processing at 30MPa, controlling the processing deformation amount to be 13%, then placing the rough blank in a vacuum atmosphere, performing high-temperature sintering at 1100 ℃ for 3 hours, and performing tempering treatment at 600 ℃ for 6 hours to obtain the vehicle-mounted Gao Wen-iron-boron permanent magnet.
And performing characterization test on the performance of the prepared vehicle-mounted Gao Wen-iron-boron permanent magnet.
| Test temperature | Br(T) | Hcj(kA/m) | Frequency vibration weight loss ratio (%) |
| 20℃ | 1.19 | 1.91×10 3 | ＜0.1 |
| 100℃ | 1.18 | 1.85×10 3 | ＜0.1 |
| 150℃ | 1.16 | 1.75×10 3 | ＜0.1 |
| 180℃ | 1.15 | 1.55×10 3 | ＜0.1 |
| 260℃ | 1.10 | 1.29×10 3 | 0.1 |
The frequency vibration weightlessness rate is that the sample is placed on a 200Hz ultrahigh frequency vibration testing machine, then a thermal vibration test is carried out, the vibration test is continuously carried out for 12 hours, the sample mass before and after the measurement is carried out, and the weightlessness rate is calculated so as to verify the anti-vibration performance of the sample. In addition, a thermal shock test is carried out on the sample, the sample is quickly heated to 200 ℃ and kept warm for ten minutes, then the temperature is quickly reduced to less than or equal to 15 ℃ within 10 seconds in a water cooling mode, and after 300 times of quick temperature rise and reduction cycles are repeatedly carried out, the quality change of the sample is characterized, the macroscopic surface morphology of the sample is observed, the surface of the sample prepared by the method has no cracks and cracks, the volume has no obvious change, the quality change rate is less than 0.5%, and the permanent magnet prepared by the method has very excellent thermal shock resistance.
From the preparation process and the characterization results of the embodiments 1 to 4, it can be seen that the permanent magnet material prepared by the method has good magnetic properties and heat resistance, can keep excellent properties at high temperature, can still have higher magnetic property retention rate at 260 ℃, has small influence on the permanent magnet properties due to vibration conditions and thermal shock conditions, and has very good dynamic heat resistance, and after a thermal shock test, the permanent magnet material has no cracking, cracking and other conditions, has no obvious change in volume, and is uniform in internal components and free from local thermal expansion deformation.
Comparative example 1
The specific preparation process of the vehicle-mounted Gao Wen-iron-boron permanent magnet is the same as that of the embodiment 1, and the specific preparation process is as follows:
the prepared R2Fe14B matrix phase magnetic powder is crushed to 6000-8000 meshes, and the prepared R2TM 8R phase magnetic powder is crushed to 6000-8000 meshes to replace the coarse-grain magnetic powder used in the original example 1.
And performing characterization test on the performance of the prepared permanent magnet.
The frequency vibration weightlessness rate is that the sample is placed on a 200Hz ultrahigh frequency vibration testing machine, then a thermal vibration test is carried out, the vibration test is continuously carried out for 12 hours, the sample mass before and after the measurement is carried out, and the weightlessness rate is calculated so as to verify the anti-vibration performance of the sample. In addition, a thermal shock test is carried out on the sample, the sample is rapidly heated to 200 ℃ and kept warm for ten minutes, the temperature is rapidly reduced to less than or equal to 15 ℃ within 10 seconds in a water cooling mode, and after 300 rapid temperature rise and reduction cycles are repeatedly carried out, the quality change of the sample is characterized, the macroscopic surface morphology of the sample is observed, and the prepared sample has no cracks and cracks on the surface, no obvious change in volume, but the quality change rate reaches 2.9%. It can be seen that the sample prepared in this example shows a very significant decrease in the anti-vibration and anti-thermal shock properties, particularly in the anti-vibration properties, which are mass loss at low temperature, although the magnetic properties are superior to those of the sample prepared in example 1 at 180 ℃ due to the refinement of the magnetic powder. When the device is suitable for vehicle-mounted use, the working environment is often accompanied by normal frequency vibration of 80-100 Hz, and in partial special working scenes, higher frequency vibration can exist, so that the service life of the device is limited. Loss is generated under the action of long-term vibration, the magnetic performance of the permanent magnet is gradually reduced along with the occurrence of the loss, and the service life of the permanent magnet is far lower than that of the permanent magnet prepared in the embodiment 1 of the invention.
Comparative example 2
The specific preparation process of the vehicle-mounted Gao Wen-iron-boron permanent magnet is the same as that of the embodiment 1, and the specific preparation process is as follows:
and B phase magnetic powder is not added.
And performing characterization test on the performance of the prepared permanent magnet.
| Test temperature | Br(T) | Hcj(kA/m) | Frequency vibration weight loss ratio (%) |
| 20℃ | 1.21 | 1.98×10 3 | 1.9 |
| 100℃ | 1.16 | 1.39×10 3 | 2.7 |
| 150℃ | 1.12 | 1.21×10 3 | 3.6 |
| 180℃ | 1.09 | 1.11×10 3 | 4.1 |
| 260℃ | 0.97 | 1.02×10 3 | 4.4 |
The frequency vibration weightlessness rate is that the sample is placed on a 200Hz ultrahigh frequency vibration testing machine, then a thermal vibration test is carried out, the vibration test is continuously carried out for 12 hours, the sample mass before and after the measurement is carried out, and the weightlessness rate is calculated so as to verify the anti-vibration performance of the sample. In addition, a thermal shock test is carried out on the sample, the sample is rapidly heated to 200 ℃ and kept warm for ten minutes, then is rapidly cooled to less than or equal to 15 ℃ in 10 seconds by a water cooling mode, and after 300 rapid heating and cooling cycles are repeatedly carried out, the quality change of the sample is represented, the macroscopic surface morphology of the sample is observed, and the prepared sample has microcracks on the surface, no obvious cracking phenomenon exists, no obvious change in volume exists, and the quality change rate reaches 2.6%. Therefore, the addition of the B-phase magnetic powder has important effect and significance for improving the heat resistance and the frequency vibration resistance of the permanent magnet. Similarly, another set of experiments was performed simultaneously with the sample preparation of this set. The other group of test concrete preparation process is the same as that of the example 1, but the cold working deformation amount reaches 60%, namely, the conventional supercritical processing treatment is carried out, the obtained sample is further weakened in the aspect of thermal shock resistance, very obvious local expansion deformation occurs in the thermal shock test process, the mass change rate is as high as 4.1%, and a certain crack can be observed macroscopically. The B-phase magnetic powder and cold working deformation are key to realizing the strengthening of the mechanical property and the thermal shock resistance of the permanent magnet, and the permanent magnet has excellent frequency shock resistance and thermal shock resistance under the combined action of the B-phase magnetic powder and the cold working deformation.
Comparative example 3
The specific preparation process of the vehicle-mounted Gao Wen-iron-boron permanent magnet is the same as that of the embodiment 1, and the specific preparation process is as follows:
the conventional phenol formaldehyde type phenolic resin is dissolved in acetone with the mass being 2 times that of the phenolic resin to be matched with a wetting agent to replace dimethyl silicone oil.
And performing characterization test on the performance of the prepared permanent magnet.
| Test temperature | Br(T) | Hcj(kA/m) | Frequency vibration weight loss ratio (%) |
| 20℃ | 1.18 | 1.88×10 3 | ＜0.1 |
| 100℃ | 1.17 | 1.55×10 3 | ＜0.1 |
| 150℃ | 1.13 | 1.39×10 3 | ＜0.1 |
| 180℃ | 1.07 | 1.20×10 3 | 0.1 |
| 260℃ | 0.96 | 1.03×10 3 | 0.3 |
The frequency vibration weightlessness rate is that the sample is placed on a 200Hz ultrahigh frequency vibration testing machine, then a thermal vibration test is carried out, the vibration test is continuously carried out for 12 hours, the sample mass before and after the measurement is carried out, and the weightlessness rate is calculated so as to verify the anti-vibration performance of the sample. In addition, a thermal shock test is carried out on the sample, the sample is rapidly heated to 200 ℃ and kept warm for ten minutes, the temperature is rapidly reduced to less than or equal to 15 ℃ within 10 seconds in a water cooling mode, and after 300 rapid temperature rise and reduction cycles are repeatedly carried out, the quality change of the sample is represented, the macroscopic surface morphology of the sample is observed, the surface of the sample prepared by the method has no crack and cracking phenomenon, no obvious volume expansion exists, and the mass change rate after thermal shock reaches 1.9%. It can be seen that the wetting agent of the present invention has the effect of strengthening the performance of the permanent magnet in addition to the effect of wetting the particles. The simple replacement of the wetting agent leads to the ineffective formation of the barrier band, which produces obvious reduction in high temperature resistance and thermal shock resistance, but the mechanical properties are reserved to a certain extent. It can be seen that a suitable lubricant can form an effective bond with the metallic aluminum as a binder to produce a significant strengthening effect on the performance of the permanent magnet.
Claims (6)
1. A preparation method of a vehicle-mounted Gao Wen-iron-boron permanent magnet is characterized in that,
the preparation method comprises the following steps:
1) Uniformly mixing matrix phase magnetic powder, R phase magnetic powder, B phase magnetic powder, a linking material and a wetting agent, placing the mixture in a mould for orientation and carrying out low-temperature hot-press molding to obtain a rough blank;
2) Performing cold deformation processing on the rough blank after low-temperature primary sintering, controlling the processing deformation amount of the rough blank, and sequentially performing high-temperature sintering and tempering treatment to obtain the vehicle-mounted Gao Wen iron boron permanent magnet;
the composition of the matrix phase magnetic powder in the step 1) comprises the following components:
PrNd 13-15 at%, B6-6.5 at%, and Fe in balance;
weighing praseodymium-neodymium alloy, boron and iron according to the ingredients, mixing, smelting and crushing to prepare 100-120 mesh matrix phase magnetic powder;
the component composition of the R-phase magnetic powder in the step 1) comprises:
12-16 at% of NdCu, 6-8 at% of Nd, 2-3 at% of Dy, 1.5-2.5 at% of Ni, 0.5-1.0 at% of Tb and the balance of Fe;
weighing neodymium, neodymium copper alloy, dysprosium, terbium, nickel and iron according to the components, mixing, smelting and crushing to prepare R-phase magnetic powder with 20-35 meshes;
the component composition of the B-phase magnetic powder in the step 1) comprises:
nd 0.5-2.0 at%, B35-45 at%, and Fe in balance;
weighing neodymium, iron and boron according to the ingredients, mixing, smelting and crushing to prepare B-phase magnetic powder with the mesh number of 2000-8000 meshes;
the linking material is metal aluminum powder;
the wetting agent is dimethyl silicone oil;
the consumption of the linking material is 1-3 wt% of the base phase magnetic powder;
the dosage of the wetting agent is 5-8 wt% of the matrix phase magnetic powder.
2. The method for preparing the vehicle-mounted Gao Wen-Fe-B permanent magnet according to claim 1, wherein the method comprises the following steps of,
the usage mass ratio of the matrix phase magnetic powder, the R phase magnetic powder and the B phase magnetic powder is 100: (12-22): (5-8).
3. The method for preparing the vehicle-mounted Gao Wen-Fe-B permanent magnet according to claim 1, wherein the method comprises the following steps of,
the orientation process in the step 1) controls the strength of an orientation magnetic field to be 1.3-1.6 and T, and the orientation time is 25-30 min;
the low-temperature hot pressing process in the step 1) is carried out under the vacuum condition, the control temperature is 80-95 ℃, the hot pressing pressure is 15-25 MPa, and the pressure maintaining time is 25-35 min.
4. The method for preparing the vehicle-mounted Gao Wen-Fe-B permanent magnet according to claim 1, wherein the method comprises the following steps of,
step 2), the control temperature of the low-temperature primary sintering process is 360-380 ℃, and the sintering time is 1-2 h;
and 2) controlling the deformation amount of the cold deformation processing to be 12-15%.
5. The method for preparing the vehicle-mounted Gao Wen-Fe-B permanent magnet according to claim 1, wherein the method comprises the following steps of,
step 2) the high-temperature sintering is carried out in a nitrogen protection atmosphere or a vacuum atmosphere, the sintering temperature is 1050-1150 ℃, and the sintering time is 2-4 h;
and 2) tempering, wherein the tempering temperature is controlled to be 560-620 ℃ and the tempering time is 5-7 h.
6. A vehicle-mounted Gao Wen-resistant permanent magnet produced by the method of any one of claims 1 to 5.
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| CN202311038049.1A CN116825462B (en) | 2023-08-17 | 2023-08-17 | Vehicle-mounted Gao Wen-iron-boron-resistant permanent magnet and preparation method thereof |
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| CN202311038049.1A CN116825462B (en) | 2023-08-17 | 2023-08-17 | Vehicle-mounted Gao Wen-iron-boron-resistant permanent magnet and preparation method thereof |
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| CN110895985A (en) * | 2019-11-06 | 2020-03-20 | 包头稀土研究院 | Mixed rare earth sintered neodymium-iron-boron permanent magnet and preparation method thereof |
| CN113948263A (en) * | 2021-10-08 | 2022-01-18 | 宁波市合美达新材料有限公司 | Neodymium iron boron material and preparation method thereof |
| CN115036089A (en) * | 2022-07-07 | 2022-09-09 | 宁波迈泰克磁材科技有限公司 | High-temperature-resistant neodymium-iron-boron magnetic steel for vehicle-mounted main motor and preparation method thereof |
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| US5114502A (en) * | 1989-06-13 | 1992-05-19 | Sps Technologies, Inc. | Magnetic materials and process for producing the same |
| CN104681268A (en) * | 2013-11-28 | 2015-06-03 | 湖南稀土金属材料研究院 | Processing method for improving coercive force of sintered neodymium-iron-boron magnet |
| CN109786097A (en) * | 2018-12-26 | 2019-05-21 | 湖北永磁磁材科技有限公司 | A kind of preparation method of driving motor dedicated high performance Nd-Fe-B permanent magnet |
| CN110895985A (en) * | 2019-11-06 | 2020-03-20 | 包头稀土研究院 | Mixed rare earth sintered neodymium-iron-boron permanent magnet and preparation method thereof |
| CN113948263A (en) * | 2021-10-08 | 2022-01-18 | 宁波市合美达新材料有限公司 | Neodymium iron boron material and preparation method thereof |
| CN115036089A (en) * | 2022-07-07 | 2022-09-09 | 宁波迈泰克磁材科技有限公司 | High-temperature-resistant neodymium-iron-boron magnetic steel for vehicle-mounted main motor and preparation method thereof |
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