阅读说明：本技术 一种叠片稀土永磁器件的制造方法 (Method for manufacturing laminated rare earth permanent magnet device ) 是由 段永利 邓文宇 齐丽君 张毅 孙昊天 于 2020-12-10 设计创作，主要内容包括：本发明公开了一种叠片稀土永磁器件的制造方法,包括：制备稀土永磁体；将两片以上的稀土永磁体沿稀土永磁体的磁场取向方向层叠排列；通过相邻两片稀土永磁体间涂覆的胶体粘接使其联结成叠片稀土永磁器件。在所述的叠片稀土永磁器件中,相邻两片稀土永磁体之间存在间隔膜层,且间隔膜层的厚度在300μm以下。所述的制造方法中包括在稀土永磁体预制件表面附着含有Tb元素的粉末或膜层的步骤,并对表面附着有粉末或膜层的稀土永磁体预制件进行真空热处理制成稀土永磁体。本发明采用叠片的结构形式制造渗铽效果优异的超厚磁体,同时还可以减小电机工作时在永磁器件内部产生的涡流损耗。(The invention discloses a method for manufacturing a laminated rare earth permanent magnet device, which comprises the following steps: preparing a rare earth permanent magnet; more than two pieces of rare earth permanent magnets are arranged in a laminated manner along the orientation direction of the magnetic field of the rare earth permanent magnets; the two adjacent rare earth permanent magnets are bonded by the colloid coated between the two adjacent rare earth permanent magnets to form the laminated rare earth permanent magnet device. In the laminated rare earth permanent magnet device, an interlayer membrane layer is arranged between two adjacent rare earth permanent magnets, and the thickness of the interlayer membrane layer is less than 300 mu m. The manufacturing method comprises the steps of attaching powder or a film layer containing Tb on the surface of the rare earth permanent magnet prefabricated member, and carrying out vacuum heat treatment on the rare earth permanent magnet prefabricated member with the powder or the film layer attached on the surface to manufacture the rare earth permanent magnet. The invention adopts the laminated structure form to manufacture the ultra-thick magnet with excellent terbium infiltration effect, and can reduce the eddy current loss generated in the permanent magnet device when the motor works.)

1. A method for manufacturing a laminated rare earth permanent magnet device comprises the following steps: (1) preparing a rare earth permanent magnet material raw material containing rare earth into a sintering blank, and preparing the sintering blank into a rare earth permanent magnet, wherein the thickness of the rare earth permanent magnet is less than 5 mm; (2) more than two pieces of rare earth permanent magnets are arranged in a laminated manner along the orientation direction of the magnetic field of the rare earth permanent magnets; (3) the two adjacent rare earth permanent magnets are bonded by the colloid coated between the two adjacent rare earth permanent magnets to be connected into a laminated rare earth permanent magnet device; in the laminated rare earth permanent magnet device, an interlayer membrane layer is arranged between two adjacent rare earth permanent magnets, and the thickness of the interlayer membrane layer is less than 300 mu m.

2. The method of claim 1, wherein the method comprises the steps of: the laminated rare earth permanent magnet device is tile-shaped or cuboid.

3. The method of claim 1, wherein the method comprises the steps of: after the rare earth permanent magnets are bonded by the adhesive bonding, the method further comprises a step of machining or surface treatment of the bonded body.

4. The method of claim 1, wherein the method comprises the steps of: the thickness of the interlayer membrane layer is less than 100 μm; the thickness of the rare earth permanent magnet is less than 3 mm.

5. The method of claim 1, wherein the method comprises the steps of: the step (1) comprises: preparing alloy raw materials comprising pure iron, ferroboron and rare earth into alloy sheets by a vacuum rapid hardening process; preparing alloy powder from an alloy sheet by a hydrogen crushing process and airflow milling; under the protection of nitrogen gas making magnetic field forming of alloy powder, the density of pressed compact is 4.1-4.8g/cm³(ii) a Carrying out vacuum sintering on the pressed compact formed by the magnetic field to prepare a sintered blank, wherein the density of the sintered blank is 7.3-7.7g/cm³。

6. The method of claim 5, wherein the method comprises the following steps: the alloy powder obtained by the airflow milling powder comprises ultrafine powder with the granularity less than 1 mu m and common powder with the granularity more than 1 mu m, and the nitrogen content and the heavy rare earth element content in the ultrafine powder are higher than those in the common powder; after the ultrafine powder and the common powder are uniformly mixed, the ultrafine powder is wrapped around the common powder.

7. The method of claim 5, wherein the method comprises the following steps: the step (1) further comprises: and (3) preparing a sintered blank through a vacuum sintering process, and then machining the sintered blank to prepare the rare earth permanent magnet.

8. The method of claim 5, wherein the method comprises the following steps: the method comprises the steps of preparing a sintered blank through a vacuum sintering process, machining the sintered blank to prepare a rare earth permanent magnet prefabricated part, attaching powder or a film layer containing Tb on the surface of the rare earth permanent magnet prefabricated part, and performing vacuum heat treatment on the rare earth permanent magnet prefabricated part with the powder or the film layer attached to the surface to prepare the rare earth permanent magnet.

9. The method of claim 8, wherein the method comprises the steps of: the adhesion of the powder containing Tb on the surface of the rare earth permanent magnet prefabricated member is completed by adopting a pressure immersion method.

10. The method of claim 8, wherein the method comprises the steps of: the film layer containing Tb is attached to the surface of the rare earth permanent magnet prefabricated member by adopting at least one method selected from sputtering, evaporation and spraying.

11. The method of claim 1, wherein the method comprises the steps of: the manufacturing method further comprises a step of preparing an interlayer membrane layer on the surface of the rare earth permanent magnet, wherein the step of forming the interlayer membrane layer on the surface of the rare earth permanent magnet through at least one method selected from coating, electrophoresis, phosphorization, chemical conversion, anodic oxidation, chemical deposition and the like.

12. The method of claim 1, wherein the method comprises the steps of: the average grain size of the rare earth permanent magnet is within the range of 3-13 mu m, the rare earth permanent magnet contains N, Al, Tb, Pr, Nd, Ga and Cu elements, and the content is as follows: n is more than or equal to 0.03 weight percent and less than or equal to 0.09 weight percent; al is more than or equal to 0.1 weight percent and less than or equal to 0.6 weight percent; tb is more than or equal to 0.05wt% and less than or equal to 2.9 wt%; pr is more than or equal to 3 weight percent and less than or equal to 14 weight percent; nd is more than or equal to 13wt% and less than or equal to 28 wt%; ga is more than or equal to 0.09wt% and less than or equal to 0.19 wt%; cu is more than or equal to 0.08 weight percent and less than or equal to 0.24 weight percent.

Technical Field

The invention belongs to the field of rare earth permanent magnet, and particularly relates to a laminated rare earth permanent magnet device and a manufacturing method thereof.

Background

The Nd-Fe-B rare earth permanent magnet is a basic electronic component and an electric appliance element widely used in the world at present, and is widely applied to computers, mobile phones, televisions, automobiles, motors, toys, audios, automation equipment, nuclear magnetic resonance imaging and the like. With the requirements of energy conservation and low-carbon economy, the neodymium-iron-boron rare earth permanent magnet is applied to the fields of energy-saving household appliances, hybrid electric vehicles, wind power generation and the like.

In 1983, M.sgawaa et al firstly prepared sintered Nd-Fe-B rare earth permanent magnet by powder metallurgy method and confirmed that Nd exists in the rare earth permanent magnet₂Fe₁₄Phase B and grain boundary phase, U.S. Pat. No. 4, 5,645,651 issued in 1997 discloses the metallographic structure of R-Fe-Co-B; the emergence of neodymium iron boron rare earth permanent magnet marks the birth of the third generation rare earth permanent magnet material; with the application of neodymium iron boron, extensive research on neodymium iron boron has been carried out, and up to now, a neodymium iron boron rare earth permanent magnet with the maximum energy product (BH) max of 52MGOe can be produced in batches, and it has been found that the coercive force Hcj of the magnet can be improved from 12KOe to 30KOe and the use temperature can be improved from 80 ℃ to 180 ℃ by replacing light rare earth elements Pr and Nd with heavy rare earth elements Dy, Tb and Ho. With the use of neodymium iron boron rare earth permanent magnets in wind power generation, automobiles, servo motors, energy-saving motors and electronic devices, the use amount of heavy rare earth element Dy is more and more, and because Dy is a scarce heavy rare earth resource, the world reserves are rare, and the heavy rare earth permanent magnets are only produced in ion mines in the south of China at present; the reduction of the consumption of Dy is very important for protecting scarce resources and reducing the cost of the Nd-Fe-B rare earth permanent magnet.

In order to improve the magnetic performance of the neodymium iron boron rare earth permanent magnet material and reduce the use amount of heavy rare earth materials such as Dy and Tb, a great deal of research work is carried out on neodymium iron boron practitioners represented by Japanese enterprises. It is believed that the chemical patent US7488393, CN100565719C discloses a method for manufacturing a high-performance R-Fe-B permanent magnet, in which Dy, Tb-containing oxygen/fluoride is attached to the surface of a sintered ndfeb magnet, and then Dy, Tb in the powder is infiltrated into the magnet by diffusion heat treatment. Hitachi metal also discloses a method of manufacturing a sintered magnet by forming a Dy or Tb-containing film on the surface of the magnet by evaporation and adhesion, and then subjecting the magnet to diffusion heat treatment to cause Dy or Tb to penetrate into the magnet, in US8182619 and US 8206516. Researchers in China also carry out similar research on the magnet dysprosium terbium penetration technology.

Although the technology of diffusing dysprosium terbium into the magnet can improve the coercive force of the sintered neodymium iron boron permanent magnet to a certain degree and improve the heat resistance of the magnet, the depth of the dysprosium terbium into the magnet is limited, so that the thickness of a rare earth permanent magnet device applicable to the technology is limited to a certain extent, and the requirements of application fields such as servo motors, electric automobile motors and the like with higher requirements on the magnetic flux density of the permanent magnet device are difficult to meet. In addition, in a permanent magnet motor with high power, as the volume of a permanent magnet device in a rotor becomes larger, large eddy current loss is generated in the permanent magnet device, the loss causes high temperature rise, and in an extreme case, the permanent magnet device may be demagnetized, so that the performance of the motor is reduced.

Disclosure of Invention

In order to overcome the defects of the prior art, the invention provides a laminated rare earth permanent magnet device and a manufacturing method thereof.

A laminated rare earth permanent magnet device is formed by laminating more than two rare earth permanent magnets, wherein the rare earth permanent magnets are bonded and connected through colloid, an interlayer membrane layer is arranged between every two adjacent rare earth permanent magnets, the thickness of the interlayer membrane layer is less than 300 mu m, and the thickness of the rare earth permanent magnet is less than 5 mm; the rare earth permanent magnet consists of a main phase and a grain boundary phase, wherein the main phase has R₂T₁₄The structure B, the grain boundary phase is distributed around the main phase, and the grain boundary phase contains rare earth elements Pr and Nd; the rare earth permanent magnet contains at least 2 of rare earth elements La, Ce, Pr, Nd, Dy and Tb. The stacking arrangement direction of the rare earth permanent magnets is consistent with the orientation direction of the magnetic field of the rare earth permanent magnets. More preferably, the thickness of the spacing film layer is less than or equal to 100 μm; the thickness of the rare earth permanent magnet is less than 3 mm.

The laminated rare earth permanent magnet device is tile-shaped or cuboid.

In a preferred embodiment, the spacing film layer is mainly composed of at least one selected from the group consisting of an epoxy resin layer, a Dacromet layer, a chemical conversion layer, a phosphate layer, an oxide layer, a coating film layer and an insulating paint layer. The spacer film layer is insulating.

After the rare earth permanent magnets are bonded by the adhesive bonding, the method further comprises a step of machining or surface treatment of the bonded body.

The method comprises the steps of adhering powder or a film layer containing Tb on the surface of a rare earth permanent magnet prefabricated part and carrying out vacuum heat treatment on the rare earth permanent magnet prefabricated part with the powder or the film layer adhered on the surface.

The average grain size of the rare earth permanent magnet is within the range of 3-13 mu m, the rare earth permanent magnet also contains N, Al, Tb, Pr, Nd, Ga and Cu elements, and the contents are as follows: n is more than or equal to 0.03 weight percent and less than or equal to 0.09 weight percent; al is more than or equal to 0.1 weight percent and less than or equal to 0.6 weight percent; tb is more than or equal to 0.05wt% and less than or equal to 2.9 wt%; pr is more than or equal to 3 weight percent and less than or equal to 14 weight percent; nd is more than or equal to 13wt% and less than or equal to 28 wt%; ga is more than or equal to 0.09wt% and less than or equal to 0.19 wt%; cu is more than or equal to 0.08 weight percent and less than or equal to 0.24 weight percent. Preferably, the rare earth permanent magnet also contains at least one selected from La and Ce, and the total content of La and Ce is in the range of 2-19 wt%.

A method for manufacturing a laminated rare earth permanent magnet device comprises the following steps: (1) preparing a rare earth permanent magnet material raw material containing rare earth into a sintering blank, and preparing the sintering blank into a rare earth permanent magnet, wherein the thickness of the rare earth permanent magnet is less than 5 mm; (2) more than two pieces of rare earth permanent magnets are arranged in a laminated manner along the orientation direction of the magnetic field of the rare earth permanent magnets; (3) the two adjacent rare earth permanent magnets are bonded by the colloid coated between the two adjacent rare earth permanent magnets to be connected into a laminated rare earth permanent magnet device; in the laminated rare earth permanent magnet device, an interlayer membrane layer is arranged between two adjacent rare earth permanent magnets, and the thickness of the interlayer membrane layer is less than 300 mu m. Preferably, the thickness of the spacing film layer is less than 100 μm; the thickness of the rare earth permanent magnet is less than 3 mm.

The laminated rare earth permanent magnet device is tile-shaped or cuboid.

The method comprises a step of joining 2 or more rare earth permanent magnets by adhesive bonding and then machining or surface-treating the joined body.

The step (1) comprises: preparing alloy raw materials comprising pure iron, ferroboron and rare earth into alloy sheets by a vacuum rapid hardening process; preparing alloy powder from an alloy sheet by a hydrogen crushing process and airflow milling; under the protection of nitrogen gas making magnetic field forming of alloy powder, the density of pressed compact is 4.1-4.8g/cm³(ii) a Carrying out vacuum sintering on the pressed compact formed by the magnetic field to prepare a sintered blank, wherein the density of the sintered blank is 7.3-7.7g/cm³. The alloy powder obtained by the airflow milling powder comprises ultrafine powder with the granularity less than 1 mu m and common powder with the granularity more than 1 mu m, and the nitrogen content and the heavy rare earth element content in the ultrafine powder are higher than those in the common powder; after the ultrafine powder and the common powder are uniformly mixed, the ultrafine powder is wrapped around the common powder.

The step (1) further comprises: and (3) preparing a sintered blank through a vacuum sintering process, and then machining the sintered blank to prepare the rare earth permanent magnet.

The step (1) further comprises: the method comprises the steps of preparing a sintered blank through a vacuum sintering process, machining the sintered blank to prepare a rare earth permanent magnet prefabricated part, attaching powder or a film layer containing Tb on the surface of the rare earth permanent magnet prefabricated part, and performing vacuum heat treatment on the rare earth permanent magnet prefabricated part with the powder or the film layer attached to the surface to prepare the rare earth permanent magnet.

In one embodiment of the present invention, the attachment of the powder containing Tb element to the surface of the rare earth permanent magnet preform is performed by a pressure immersion method.

In another embodiment of the invention, the film layer containing Tb is attached on the surface of the rare earth permanent magnet prefabricated member by at least one method selected from sputtering, evaporation and spraying.

The manufacturing method also comprises a step of preparing an interlayer membrane layer on the surface of the rare earth permanent magnet, wherein the step can be to form an insulating interlayer membrane layer on the surface of the rare earth permanent magnet by one of the methods selected from coating, electrophoresis, phosphorization, chemical conversion, anodic oxidation, chemical deposition and the like, and also can realize the formation of the interlayer membrane layer on the surface of the rare earth permanent magnet by coating adhesive colloid between two adjacent rare earth permanent magnets.

The manufacturing method also comprises the steps of pressurizing and shaping the combination body coated with the adhesive colloid between two adjacent rare earth permanent magnets and curing the adhesive colloid.

The invention has the advantages of

The technical scheme of the invention breaks through the limitation of the heavy rare earth grain boundary diffusion technology on manufacturing super-thick magnet products, adopts the structural form of lamination to manufacture the super-thick magnet with excellent terbium permeation effect, enables the heavy rare earth grain boundary diffusion technology to be competent for the production and the manufacture of low heavy rare earth sintered neodymium iron boron rare earth permanent magnet device products with the thickness of more than 10mm, obviously improves the heat resistance of the magnet, and enables the magnet to meet the requirements of application fields of servo motors, electric automobile motors and the like with higher requirements on the magnetic performance of the permanent magnet devices.

In addition, the spacing film layer between the rare earth permanent magnets forming the laminated rare earth permanent magnet device is beneficial to separating and reducing eddy current loss generated in the permanent magnet device when the motor works, the problem of heating and demagnetization of the permanent magnet device generated by the eddy current loss is solved, the stability and the reliability of the permanent magnet device of the permanent magnet motor are improved, and the stable work of the high-power permanent magnet motor is ensured.