PREPARATION METHOD OF RING-SHAPED SINTERED ND-FE-B MAGNET AND ITS MOULDING DIE

Abstract

The disclosure provides a preparation method, which comprises: providing a moulding die for a ring-shaped sintered Nd—Fe—B magnet; placing a Nd—Fe—B magnetic powder into the mould cavity of the moulding die in a loosely packed state, the loosely packed height of the Nd—Fe—B magnetic powder is L;

placing a flexible cylindrical core into the loosely packed Nd—Fe—B magnetic powder at a L/2 position, wherein an axial direction of the flexible cylindrical core is horizontal and parallel to the direction of a magnetic field in the mould cavity;

applying a vertical pressure to the Nd—Fe—B magnetic powder to obtain a ring-shaped green block assembly with the flexible cylindrical core embedded;

after encapsulating and isolating the ring-shaped green block assembly, applying an isostatic pressure to the ring-shaped green block assembly;

sintering the ring-shaped green block assembly to obtain a ring-shaped sintered blank;

thermally aging, grinding and slicing the ring-shaped sintered blank.

Claims

1. A method for preparing a ring-shaped sintered Nd—Fe—B magnet, comprising the following steps: step a) providing a moulding die for a ring-shaped sintered Nd—Fe—B magnet including a main block, an upper indenter, a lower indenter, and a mould cavity, the main block including two opposite non-magnetically conductive side plates and two opposite magnetic side plates; in the space formed between the two non-magnetic side plates and the two magnetic side plates, there is provided the lower indenter and the upper indenter, wherein the lower indenter is at the bottom of the space, the upper indenter is at the top of the space, and the mould cavity is located between the upper and lower indenters; step b) placing a Nd—Fe—B magnetic powder into the mould cavity of the moulding die in a loosely packed state, the loosely packed height of the Nd—Fe—B magnetic powder is L; step c) placing a flexible cylindrical core into the loosely packed Nd—Fe—B magnetic powder at a L/2 position, wherein an axial direction of the flexible cylindrical core is horizontal and parallel to the direction of a magnetic field in the mould cavity; step d) applying a vertical pressure to the Nd—Fe—B magnetic powder to obtain a ring-shaped green block assembly with the flexible cylindrical core embedded therein; step e) after encapsulating and isolating the ring-shaped green block assembly, applying an isostatic pressure to the ring-shaped green block assembly; step f) sintering the ring-shaped green block assembly to obtain a ring-shaped sintered blank; and step g) thermally aging, grinding and slicing the ring-shaped sintered blank to obtain the ring-shaped sintered Nd—Fe—B magnet.

2. The preparation method according to claim 1, wherein the flexible cylindrical core is formed from powders of alumina and/or zirconia, which are bonded with an organic adhesive.

3. The preparation method according to claim 1, wherein a weight content of the powders of alumina and/or zirconia in the flexible cylindrical core is 50wt. %-90 wt. % of the total weight of the flexible cylindrical core.

4. The preparation method according to claim 2, wherein the organic adhesive is a polyethylene glycol.

5. The preparation method according to claim 1, wherein the flexible cylindrical core has a diameter of 2 mm<R<5 mm and a length W which is equal to the mould cavity width.

6. Use of a flexible cylindrical core formed from powders of alumina and/or zirconia, which are bonded with an organic adhesive, for preparing a ring-shaped sintered Nd—Fe—B magnet.

7. Use of the flexible cylindrical core according to claim 6, wherein a weight content of the powders of alumina and/or zirconia in the flexible cylindrical core is 50 wt. %-90 wt. % of the total weight of the flexible cylindrical core.

8. Use of the flexible cylindrical core according to claim 6, wherein the organic adhesive is a polyethylene glycol.

9. A moulding die for a ring-shaped sintered Nd—Fe—B magnet including a main block, an upper indenter, a lower indenter, and a mould cavity, the main block including two opposite non-magnetically conductive side plates and two opposite magnetic side plates; in the space formed between the two non-magnetic side plates and the two magnetic side plates, there is provided the lower indenter and the upper indenter, wherein the lower indenter is at the bottom of the space, the upper indenter is at the top of the space, and the mould cavity is located between the upper and lower indenters; a Nd—Fe—B magnetic powder placed into the mould cavity of the moulding die in a loosely packed state, the loosely packed height of the Nd—Fe—B magnetic powder is L; and a flexible cylindrical core placed into the loosely packed Nd—Fe—B magnetic powder at a L/2 position, wherein an axial direction of the flexible cylindrical core is horizontal and parallel to the direction of a magnetic field in the mould cavity.

10. The preparation method according to claim 3, wherein the organic adhesive is a polyethylene glycol.

11. Use of the flexible cylindrical core according to claim 7, wherein the organic adhesive is a polyethylene glycol.

Description

DESCRIPTION OF THE DRAWINGS

[0072] FIG. 1 is a first schematic cross-sectional view on a moulding device during the inventive preparation process.

[0073] FIG. 2 is a second schematic cross-sectional view on the moulding device during the inventive preparation process.

DETAILED DESCRIPTION OF THE DISCLOSURE

[0074] Reference will now be made in detail to embodiments, examples of which are illustrated in the accompanying drawings. Effects and features of the exemplary embodiments, and implementation methods thereof will be described with reference to the accompanying drawings. In the drawings, like reference numerals denote like elements, and redundant descriptions are omitted. The present disclosure, however, may be embodied in various different forms, and should not be construed as being limited to only the illustrated embodiments herein. Rather, these embodiments are provided as examples so that this disclosure will be thorough and complete, and will fully convey the aspects and features of the present disclosure to those skilled in the art.

[0075] A Nd—Fe—B magnet (also known as NIB or Neo magnet) is the most widely used type of rare-earth magnet. It is a permanent magnet made from an alloy of neodymium, iron, and boron to form the Nd2Fe14B tetragonal crystalline structure as a main phase. Besides, the microstructure of Nd—Fe—B magnets includes usually a Nd-rich phase. The alloy may include further elements in addition to or partly substituting neodymium and iron, which is however not important for the present disclosure far as the microstructure includes the main phase and the Nd-rich phase. In other words, a Nd—Fe—B magnet at presently understood covers all such alloy compositions. Because of different manufacturing processes, Nd—Fe—B magnets are divided into two subcategories, namely sintered Nd—Fe—B magnets and bonded Nd—Fe—B magnets. Conventional manufacturing processes for both subcategories usually include the sub-step of preparing Nd—Fe—B powders from Nd—Fe—B alloy flakes obtained by a strip casting process. The presently presented process refers to sintered Nd—Fe—B magnets.

[0076] The composition of the Nd—Fe—B powder may refer to the commercially available general-purpose sintered Nd—Fe—B grades. For example, its basic composition can be set to Re.sub.aT(1-abc)B.sub.bM.sub.c, where RE is a rare earth element selected from at least one of Pr, Nd, Dy, Tb, Ho, and Gd, T is at least one of Fe or Co, B is element B, M is at least one of Al, Cu, Ga, Ti, Zr, Nb, Mo, and V, and a, b, and c may be 27 wt. %≤a≤wt.33%, 0.85 wt. %≤b≤1.3 wt. %, and c≤5 wt. %.

[0077] Commercially available or freshly produced alloy powders could be used for the inventive process of preparing ring-shaped sintered Nd—Fe—B magnets. Specifically, Nd—Fe—B alloy flakes may be produced by a strip casting process, then subjected to a hydrogen embrittlement process and jet milling for preparing the desired Nd—Fe—B magnet powders. The strip casting process, the hydrogen embrittlement process, and the jet milling process are currently well-known technologies.

[0078] For forming a sintered Nd—Fe—B magnet, the powder is generally moulded at first time in a moulding die under pressure and parallel magnetic field conditions, and the moulded block is moulded for a second time under liquid isostatic pressing conditions, followed by vacuum sintering in a vacuum sintering furnace for densification. Afterwards, heat aging treatment is performed in a heat treatment furnace to obtain a blank.

[0079] The preparation method of a ring-shaped sintered Nd—Fe—B magnet further includes—after obtaining the sintered block—processing different steps of grinding and slicing using conventional machine equipment.

[0080] The moulding die for the ring-shaped (or annular) sintered Nd—Fe—B magnet of the present disclosure comprises a flexible cylindrical core. The flexible cylindrical core may be formed of a commercially available powder material, specifically alumina powder, zirconia powder or mixtures thereof. An average particle size (D50) of the powder material is preferably in the range of 0.5 to 2 mm. Further, the cylindrical core includes an organic adhesive as plasticiser and binder. Organic adhesives acting as plasticiser and binder for ceramic moulding compounds are well-known in the art. The organic adhesive preferably has sufficient strength to stabilise the core up to a temperature of at least 100° C., which will simplify the production process and handling of the core. Preferably, a thermally induced decomposition of the organic adhesive should start at a temperature of 150° C. to 350° C. The organic adhesive for adhering the powder material may be a commercially available adhesive. Specifically, the organic adhesive may be a polyethylene glycol, such as PEG-600. The organic adhesive is preferably added to the above-mentioned powder material in form of particles, such as PEG particles.

[0081] The reason why in particular polyethylene glycol may be used in the production of the flexible cylindrical core is that polyethylene glycol is a highly viscous, water-soluble organic material, and its viscosity can be used to prepare a high-viscosity glue. After forming a semi-solid mixture with the powder, the bonding is firm, the moisture content is low, and the deformation during drying is also small.

[0082] A weight content of alumina, zirconia or mixtures thereof in the flexible cylindrical core is preferably between 50wt. %-90wt. % of the total weight of the flexible cylindrical core. The remaining content is preferably the organic adhesive. Impurities and additives should preferably be less than 1 wt. %. When the content is less than 50wt. %, the fluidity of the mixture for forming the flexible cylindrical core is too high and accurate forming and stability of the flexible cylindrical core may deteriorate. Further, decomposition of the core during the sintering of the magnet may be too fast resulting in an increased crack rate. When the content is higher than 90wt. %, the bonding is not strong enough and easy to loosen.

[0083] During moulding, the flexible cylindrical core is placed in the Nd—Fe—B powder in a horizontal direction, and the depth of the insertion is at half of the loose height of the powder.

[0084] The magnetic field in the mould cavity during moulding is horizontal. When the flexible cylindrical core is embedded in the green block under the pressure of the forming press, the position of the core is at the center of the green block.

[0085] When the green block shrinks during the sintering process, its radial proportion decreases, but the arc shape remains basically unchanged.

[0086] The method where the cylindrical core is at one-half of the loose mounting height can be optimized by the following steps. For example, the powder feeding process is divided into two equal weight proportions. After the powder is given for the first time, the core is placed into the powder, and then the second part of the powder is added.

[0087] Alternatively, an auxiliary positioning plate can be used to first put the core and positioning plate into the cavity, and then add all the powder into the cavity. When the powder is loosely packed, the positioning plate will be pulled out from the mould cavity.

[0088] The flexible cylindrical core will play a role in reducing the incidence of cracks: due to the sintering, the core is inside the Nd—Fe—B green block and enters the furnace together with the sintered green block.

[0089] During a low-temperature stage of vacuum heating and sintering (for example, 400° C. or below) at the beginning of the sintering process step, heat will be transferred to the inside of the Nd—Fe—B green block through the core, so that the inner arc surface of the Nd—Fe—B green block also heats up at the same time, reducing the temperature difference between the inner arc surface and the outer arc surface, thereby reducing the difference in shrinkage and, as a consequence, avoiding cracks.

[0090] At the same time, because the flexible cylindrical core is a bonded hybrid structure, and its strength is lower than that of the sintered green block, the organic adhesive, in particular polyethylene glycol, begins to decompose when the temperature further rises.

[0091] Under the dual effects of its own heating and the shrinkage of the green block wrapped around it, the organic material (such as polyethylene glycol) inside the green block is degassed and discharged, and the flexible cylindrical core begins to soften and shrink.

[0092] Since the sintering of Nd—Fe—B at low temperature is mainly liquid phase sintering, and the porosity is large, the shrinkage rate of the green block is relatively large, but the softening and shrinking process of the flexible cylindrical core coincides with the liquid phase sintering stage, which can be reduced to a certain extent. The shrinkage of the fit inner ring can continuously transfer heat, make the inside and outside of the green block heat evenly, and reduce the proportion of sintering cracks.

[0093] When the temperature continues to rise (for example, between 400° C. and 800° C.), the polyethylene glycol of the flexible cylindrical core has gradually completely decomposed and volatilized completely, and the flexible cylindrical core completely loses its support and collapses into powder.

[0094] Most of the shrinkage process of the toroidal magnet has also been completed. In the second stage of liquid phase sintering, the shrinkage rate is reduced, the density increase rate is reduced, and sintering cracks will no longer occur.

[0095] The moulding die for an annular sintered Nd—Fe—B magnet will be set into a moulding device. Pressing equipment of the moulding device may include, for example, a hydraulic press. A magnetic field power supply will apply a magnetic field during the pressing, specifically a magnetic field of 1.5 to 2.0 Tesla. The pressing direction is up and down pressing and the magnetic field direction is set to a horizontal direction.

[0096] In order to illustrate the beneficial effects of the present disclosure in improving the qualification rate of sintered products, a quality factor rate is calculated by using the ratio of the number of crack-free annular blanks after sintering and the number of forming green blanks into the furnace.

[0097] In order to facilitate the description of the beneficial effects of the present disclosure in improving the material utilization rate, the weight ratio of the product processed by the internal grinder to the powder feed weight ratio before forming is used to calculate the material utilization rate.

EXAMPLE 1

[0098] 40 g of alumina powder and 20 g of a polyethylene glycol (PEG-600, colloidal solution) are mix evenly and placed in a cylinder. In a rubber mould, isostatic pressure moulding is performed at 200 MPa and the pressed blank is dried at 120° C. for 2 h to prepare a flexible cylindrical core.

[0099] The diameter R1 of the flexible cylindrical core is 4 mm, and the length W1 is 50 mm.

[0100] In the loosely packed state, 86 g of Nd—Fe—B powder is filled into the moulding die, and the loose packed height L1 of the poured powder is 30 mm.

[0101] The flexible cylindrical core is embedded into the powder in a horizontal manner so that the height direction position is at L1/2, i.e. 15 mm.

[0102] The indenter of the moulding die is closed and under a magnetic field of 1.5 Tesla the powder and the core are integrally formed. After demoulding, an annular green block assembly is obtained.

[0103] After encapsulating the annular green block assembly, the density is increase by applying 200 MPa by water isostatic pressure.

[0104] The green block assembly is sintered and densified in a vacuum furnace at a sintering temperature of 1030° C. and a sintering time of 10 hours to obtain a round ring sintered blank.

[0105] Aging treatment of the blank in an aging furnace is performed to obtain a semi-finished product.

[0106] The end face, outer arc surface, and inner arc surface of the semi-finished product is grinded blank on a surface grinder and the grinding depth is 0.5 mm.

[0107] The semi-finished blank is sliced along its axial direction on an inner circular slicer to obtain a circular ring machine processed product, i.e. a ring-shaped sintered Nd—Fe—B magnet.

EXAMPLE 2

[0108] 40 g of alumina powder and 36 g of a polyethylene glycol (PEG-600, colloidal solution) are mix evenly and placed in a cylinder. In a rubber mould, isostatic pressure moulding is performed at 200 MPa and the pressed blank is dried at 120° C. for 2 h to prepare a flexible cylindrical core.

[0109] The diameter R1 of the flexible cylindrical core is 5 mm, and the length W1 is 50 mm.

[0110] In the loosely packed state, 86 g of Nd—Fe—B powder is filled into the moulding die, and the loose packed height L1 of the poured powder is 31 mm.

[0111] The flexible cylindrical core is embedded into the powder in a horizontal manner so that the height direction position is at L1/2, i.e. 15.5 mm.

[0112] The indenter of the moulding die is closed and under a magnetic field of 1.5 Tesla the powder and the core are integrally formed. After demoulding, an annular green block assembly is obtained.

[0113] After encapsulating the annular green block assembly, the density is increase by applying 200 MPa by water isostatic pressure.

[0114] The green block assembly is sintered and densified in a vacuum furnace at a sintering temperature of 1030° C. and a sintering time of 10 hours to obtain a round ring sintered blank.

[0115] Aging treatment of the blank in an aging furnace is performed to obtain a semi-finished product.

[0116] The end face, outer arc surface, and inner arc surface of the semi-finished product is grinded blank on a surface grinder and the grinding depth is 0.5 mm.

[0117] The semi-finished blank is sliced along its axial direction on an inner circular slicer to obtain a circular ring machine processed product, i.e. a ring-shaped sintered Nd—Fe—B magnet.

COMPARATIVE EXAMPLE 1

[0118] A cylindrical core made of stainless steel is prepared. The diameter R1 of the cylindrical core is 5 mm and the length W1 is 50 mm.

[0119] The radius R1 of the flexible cylindrical core is 4 mm, and the length W1 is 50 mm.

[0120] In the loosely packed state, 86 g of Nd—Fe—B powder is filled into the moulding die, and the loose packed height L1 of the poured powder is 30 mm.

[0121] The flexible cylindrical core is embedded into the powder in a horizontal manner so that the height direction position is at L1/2, i.e. 15 mm.

[0122] The indenter of the moulding die is closed and under a magnetic field of 1.5 Tesla the powder and the core are integrally formed. After demoulding, an annular green block assembly is obtained.

[0123] After encapsulating the annular green block assembly, the density is increase by applying 200 MPa by water isostatic pressure and then the stainless steel core is taken out.

[0124] The green block assembly is sintered and densified in a vacuum furnace at a sintering temperature of 1030° C. and a sintering time of 10 hours to obtain a round ring sintered blank.

[0125] Aging treatment of the blank in an aging furnace is performed to obtain a semi-finished product.

[0126] The end face, outer arc surface, and inner arc surface of the semi-finished product is grinded blank on a surface grinder and the grinding depth is 0.5 mm.

[0127] The semi-finished blank is sliced along its axial direction on an inner circular slicer to obtain a circular ring machine processed product, i.e. a ring-shaped sintered Nd—Fe—B magnet.

[0128] During the continuous production of multiple annular sintered blanks, it was found that in the process of removing the stainless steel core, it is easy to cause the inner wall of the annular green blank to fall off, resulting in a material drop off from the inside surface of the annular sintered blank after sintering.

COMPARATIVE EXAMPLE 2

[0129] 45 g of alumina powder and 60 g of polyethylene glycol (PEG-600, colloidal solution) are mix and stir evenly, in a cylindrical rubber mould, isostatically pressed at 200 Mpa, and dried for 2 h at 120° C.

[0130] A diameter R1 of the flexible cylindrical core is 6 mm and the length W1 is 50 mm. The diameter of the flexible cylindrical core in this comparative example is larger than this application.

[0131] In the loosely packed state, pour 86 g of powder is filled into the forming mould and the loose packed height of the poured powder is L1=35 mm.

[0132] The flexible cylindrical core is embedded into the powder in a horizontal manner so that the height direction position is at L1/2.

[0133] The indenter of the moulding die is closed and under a magnetic field of 1.5 Tesla the powder and the core are integrally formed. After demoulding, an annular green block assembly is obtained.

[0134] After encapsulating the annular green block assembly, the density is increase by applying 200 MPa by water isostatic pressure.

[0135] The green block assembly is sintered and densified in a vacuum furnace at a sintering temperature of 1030° C. and a sintering time of 10 hours to obtain a round ring sintered blank.

[0136] The subsequent machining process is the same as in Example 1.

COMPARATIVE EXAMPLE 3

[0137] In the loosely packed state, pour 118 g of Nd—Fe—B powder is added into the forming mould, but no core is used inside the mould during moulding.

[0138] The indenter is closed and the powder is moulded under the condition of a magnetic field of 1.5 Tesla. After demoulding, a cylindrical green block is obtained.

[0139] After packaging the cylindrical green block, the density is increased under 200 Mpa water isostatic pressure.

[0140] The green block is sintered and densified in a vacuum furnace at a sintering temperature of 1030° C. and a sintering time of 10 hours to obtain a cylindrical sintered blank.

[0141] Grinding the end face and the outer arc surface of the sintered blank on a surface grinder is done with a grinding volume of 0.5 mm.

[0142] The inner round hole is processed with a drilling knife on the blank after the outer arc surface is exposed to shine.

[0143] The subsequent machining process is the same as in Example 1.

[0144] In the production process of Comparative Example 3, drilling the round hole takes a long time and at the same time, there is a lot of material waste.

COMPARATIVE EXAMPLE 4

[0145] In the loosely packed state, pour 86 g of Nd—Fe—B powder is filled into the forming mould with a loose packed height of L1=35 mm.

[0146] A cylindrical core made of aluminum with a diameter of 5 mm is set into the loose powder horizontally so that the aluminum core is at L1/2.

[0147] The indenter is closed and the powder is moulded under the condition of a magnetic field of 1.5 Tesla. After demoulding, a cylindrical green block is obtained.

[0148] After packaging the cylindrical green block, the density is increased under 200 Mpa water isostatic pressure.

[0149] The green block is sintered and densified in a vacuum furnace at a sintering temperature of 1030° C. and a sintering time of 10 hours to obtain a cylindrical sintered blank.

[0150] After the end of the sintering step, it is observed that because of the presence of aluminum inside the sintered blank at this time, during the sintering process, the aluminum melts and fuses with the inner arc surface of the sintered blank. The appearance and structure of the magnet are severely damaged and cannot he put into subsequent production. Therefore, the material utilization rate cannot be determined.

COMPARATIVE EXAMPLE 5

[0151] In the loosely packed state, pour 86 g of Nd—Fe—B powder is filled into the forming mould with a loose packed height of L1=35 mm.

[0152] A cylindrical core made of ceramic material with a diameter of 5 mm is set into the loose powder horizontally so that the aluminum core is at L1/2.

[0153] The indenter is closed and the powder is moulded under the condition of a magnetic field of 1.5 Tesla. After demoulding, a cylindrical green block is obtained, which contains a ceramic core.

[0154] After packaging the cylindrical green block, the density is increased under 200 Mpa water isostatic pressure.

[0155] The green block containing the ceramic core is sintered and densified in a vacuum furnace at a sintering temperature of 1030° C. and a sintering time of 10 hours to obtain a cylindrical sintered blank.

[0156] After the sintering step, the appearance of the blank was observed, and it was found that because of the high hardness inside, the ceramic core that could not shrink with the green block caused the green block to be completely cracked after sintering and could not be put into subsequent production. No statistics on material utilization rate could be determined.

[0157] In Table 1, the blank qualification rate and material utilization rate of each example and comparative example is summarized.

TABLE-US-00001 TABLE 1 Statistic table of blank qualification rate and material utilization rate Weight after Qualified Powder weight internal grinding Material rate of category core (g) (g) utilization sintering blocks Example 1 Soft core with  86 73 85% 98% R = 4 mm Example 2 Soft core with  86 70 81% 96% R = 5 mm Comparative stainless steel  86 66 77% 50% example 2 Comparative Soft core with  86 71 83% 70% example 2 R = 6 mm Comparative No core 118 71 60% 99% example 3 Comparative Aluminum  86 With out maching —  0% example 4 core-do not take out Comparative Ceramic-do not  86 With out maching —  0% example 5 take out

Analysis of the Results:

[0158] It can be seen from the comparison that the qualified rate as well as the material utilization rate of Examples 1 and 2 is high.

[0159] Comparative Example 3 did not use any form of core, and the weight was significantly higher when feeding powder, but the material utilization rate was not high. Although the pass rate was high, it was because all magnetic powder was used.

[0160] Therefore, the annular Nd—Fe—B magnet produced by the process method and device of the present disclosure can significantly improve the material utilization rate and the blank sintering pass rate.