CN117133538A - Preparation method of metal powder injection molding sintered rare earth magnet - Google Patents
Preparation method of metal powder injection molding sintered rare earth magnet Download PDFInfo
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- CN117133538A CN117133538A CN202310907338.4A CN202310907338A CN117133538A CN 117133538 A CN117133538 A CN 117133538A CN 202310907338 A CN202310907338 A CN 202310907338A CN 117133538 A CN117133538 A CN 117133538A
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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
- 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
- H01F41/026—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 protecting methods against environmental influences, e.g. oxygen, by surface treatment
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/10—Electroplating with more than one layer of the same or of different metals
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/001—Magnets
-
- 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
- H01F1/0572—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 with a protective layer
-
- 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
-
- 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
Abstract
A preparation method of a metal powder injection molding sintered rare earth magnet belongs to the technical field of rare earth permanent magnet material preparation. And performing functional composite modification on the surface of the rare earth magnet powder by using a barrel plating process, and constructing an oxidation diffusion resisting layer, a degreasing promoting layer, a matrix protection layer and the like to obtain modified rare earth magnet powder. And modifying the adhesive to obtain the modified adhesive. Mixing the modified powder with a modified binder, a coupling agent and the like, granulating, degreasing after injection molding, and sintering to finally prepare the metal powder injection molding sintered rare earth magnet. So that the magnetic property, oxidation resistance and the like of the final product are further improved.
Description
Technical Field
The invention relates to the technical field of rare earth permanent magnet material preparation, in particular to a preparation method of a metal powder injection molding sintered rare earth magnet, which particularly relates to powder surface modification.
Background
Rare earth permanent magnets are widely used in the fields of electronic information, automobile industry, medical appliances, etc. because of their high coercive force, high remanence and high magnetic energy product. With the progress of technology, the market has put higher demands on the size, precision, shape complexity, etc. of magnets. The traditional powder metallurgy technology cannot economically meet the requirements of miniaturization, light weight, precision and the like of products.
The metal powder injection molding (MIM) technology can produce near net shaped products with complex shapes, high dimensional accuracy, and good mechanical strength. According to the MIM process, firstly, alloy powder with finer granularity and a binder material are mixed and refined into a filler suitable for injection molding according to a proportion, then, an injection molding machine is used for high-pressure molding of the mixture, degreasing and binder removal are carried out on molded parts, and finally, a compact magnet is obtained through sintering.
However, the core problem faced in the injection molding process for preparing sintered rare earth magnets (samarium cobalt, neodymium iron boron) is that residual organics in the degreasing process raise the oxygen content and carbon content in the final magnet, resulting in a decrease in magnetic properties. On the one hand, a suitable binder needs to be selected to solve this problem, in particular a binder that is easy to degrease and has a low residual oxygen and carbon content. On the other hand, the rare earth permanent magnetic powder is subjected to surface modification, so that the rare earth permanent magnetic powder can resist the production and preparation environment with high oxygen and high carbon content at high temperature, and the better magnetic performance is maintained.
Patent CN108231310a discloses a preparation method of modified neodymium-iron-boron magnetic powder, modified neodymium-iron-boron magnetic powder and neodymium-iron-boron sintered body. According to the method, the NdFeB magnetic powder is modified by using a silane coupling agent, and a stable coating layer is formed on the surface of the magnetic powder. However, the thickness of the organic coating layer is thin, and the organic coating layer is difficult to withstand a long-time high-temperature environment and is not suitable for a metal powder injection molding process.
Patent CN201910016362.2 discloses a method for preparing sintered neodymium-iron-boron magnet by 3D printing. The method aims to coat a layer of oxygen-free organic film on the surface of the neodymium iron boron magnetic powder to prevent the magnetic powder from being oxidized in the printing process. Although the organic matter film coated on the surface of the magnetic powder can play a role in preventing oxidization in a short time, the organic matter is easy to volatilize and has weak adsorption force with the magnetic powder. In the high-temperature heating process, the organic thin film is easily desorbed from the surface of the magnetic powder, and the oxidation prevention effect is affected.
Patent CN200410017792.X discloses a method for coating a metal layer on the surface of neodymium-iron-boron magnetic powder by using an electrochemical deposition technology. The method reduces metal cations of the electrodeposited solution into metal and deposits the metal on the surface of the magnetic powder, thereby improving the oxidation resistance of the magnetic powder. However, the binding force between the metal layer obtained by electrochemical deposition and the neodymium iron boron matrix is poor, and the expected oxidation resistance effect is difficult to achieve.
CN201110285377.2 discloses a ferrite injection molding granule and a preparation method thereof.
The ferrite injection molding granule with high strength and high temperature resistance is obtained by adding a certain proportion of coupling agent, binder and lubricant into ferrite magnetic powder. However, the method is only used for ferrite injection molding of particles, has a narrow application range and has a large limitation.
CN201910747676.X discloses a material for preparing a high-temperature-resistant injection magnet and a preparation method of the high-temperature-resistant injection magnet. According to the method, neodymium iron boron powder and polytetrafluoroethylene powder are used as main raw materials, and polyphenylene sulfide, a binder and an antioxidant are added, so that the magnet preparation material has good fluidity, and the high-temperature injection molding magnet is ensured to be obtained. However, the impurity atoms are easily introduced into the surface of the magnetic powder through phosphating or coupling modification, so that the magnetic powder performance is reduced.
CN202010060938.8 discloses a method for improving the oxidation corrosion resistance of NdFeB powder and magnets simultaneously. By putting the single metal and NdFeB powder or magnet together into a resistance furnace for heating treatment, a single alloy coating is formed on the surface of the powder or magnet, so that the oxidation resistance of the magnetic powder or magnet is improved. However, the powder obtained by the process has single function, is only used for oxidation prevention, and has limited application range.
Disclosure of Invention
The invention aims to provide a powder surface modification and preparation method of a metal powder injection molding sintered rare earth magnet. The method comprises the following steps: and performing functional composite modification on the surface of the rare earth magnet powder by using a barrel plating process, and constructing an oxidation diffusion resisting layer, a degreasing promoting layer, a matrix protection layer and the like to obtain modified rare earth magnet powder. And modifying the adhesive to obtain the modified adhesive. Mixing the modified powder with a modified binder, a coupling agent and the like, granulating, degreasing after injection molding, and sintering to finally prepare the metal powder injection molding sintered rare earth magnet. So that the product
The invention provides a powder surface modification and preparation method of a metal powder injection molding sintered rare earth magnet, which comprises the following steps:
step (1): performing functional composite modification on the surface of the magnetic powder; and sequentially constructing at least a substrate protective layer, a degreasing promoting layer, an oxidation diffusion resisting layer and other multi-layer functional composite layer structures on the surface of the magnetic powder through barrel plating treatment. Each layer of the multi-layer functional composite layer is a metal simple substance or alloy; the melting point of the metal corresponding to each functionalization layer is gradually reduced from the surface of the magnetic powder outwards;
the preparation method of each layer comprises the following steps: uniformly mixing the rare earth powder corresponding to the previous step (namely corresponding bare rare earth magnet powder or rare earth magnet powder with different functional layers on the surface) with lower melting point metal or alloy adopted by a functional layer to be constructed outside, putting the mixture into a rotatable tubular furnace for barrel plating treatment, pumping the tubular furnace to a vacuum environment, filling argon, setting the rotating speed of the tubular furnace, setting heating temperature and time, and carrying out air cooling on the tubular furnace after heating is finished; forming a metal coating by the mutual contact of the heated lower melting point metal or alloy and the corresponding rare earth powder, and circularly obtaining modified rare earth magnet powder A; the heating temperature enables the lower melting point metal or alloy to at least reach a melting state, and simultaneously enables the functional layer on the surface of the rare earth magnet powder with different functional layers on the surface not to be melted;
step (2): blending and modifying a wax-based binder; mixing 2 or more than 2 wax-based binders according to a certain proportion, heating to 80-100 ℃, and mixing to obtain a modified wax-based binder;
step (3): melting, mixing and granulating the modified rare earth magnet powder A and a modified wax-based binder; adding 1-10 wt.% of wax-based modified binder, 1-10 wt.% of resin-based binder, 0.5-2 wt.% of coupling agent, 0.5-2 wt.% of plasticizer and 80-95 wt.% of modified rare earth magnet powder A into an internal mixer, setting the rotating speed to be 30-80 r/min, mixing at 100-350 ℃ for 5-30 min, taking out to obtain a mixed material B, and crushing into magnet master batch C with the particle size of 1-5 mm;
step (4): a metal injection molded magnet; adding the magnet master batch C obtained in the step (3) into an injection molding machine, setting the injection temperature to be 120-400 ℃, the injection pressure to be 30-100 MPa, and the orientation magnetic field to be 15-20 kOe, and performing injection molding to obtain a metal injection molding blank D;
step (5): degreasing an injection blank; and (3) degreasing the metal injection molding blank D obtained in the step (4), which sequentially comprises solvent degreasing, low-temperature degreasing, high-temperature degreasing and the like.
Step 6): sintering; and (3) rapidly heating the injection blank degreased in the step (5) to 900-1100 ℃ of the sintering temperature of the rare earth permanent magnet, wherein the sintering time is 0.5-3 h, and obtaining the sintered rare earth magnet E.
Further preferably, the rare earth magnet in step (1) may be neodymium iron boron, samarium cobalt or any other rare earth permanent magnet system. Can be melt rapid quenching powder, HDDR-hydrogen explosion powder, rapid hardening powder and powder obtained by any other modes;
the preparation method of the invention, wherein the metal adopted in the functionalized composite layer in the step (1) is selected from one or more of Cu, zn, al, sn, ga, in, mg, bi, sb and the like. Each functional layer selects corresponding metal according to the requirement; further preferably, the substrate protective layer is selected from one or more of Cu, ga, al and the like, and the degreasing promoting layer is selected from one or more of Zn, mg and the like; the oxidation-resistant diffusion layer is one or more selected from Zn, sn, ga, in and the like. The mass ratio of the rare earth powder in the step (1) to the metal adopted by the functional layer to be constructed in the next step (namely the corresponding outer layer) is 1:1-1:5, and the coating thickness of each layer is randomly adjusted within the range of 0.1-100 mu m by adjusting the heating temperature, the heating time and the like of barrel plating; the vacuum environment in the step (1) is 5.0X10 -3 And a vacuum degree of Pa or more. The rotating speed of the tube furnace in the step (1) is 3-8 r/min.
The preparation method comprises the following steps of (1) enabling low-melting-point metal to be in short contact with rare earth powder at a certain temperature, so that a simple substance or alloy coating is formed on the surface of the rare earth powder, and carrying out functional composite modification on the surface of the rare earth magnet powder.
The specific step (1) is to perform functional composite modification on the surface of rare earth magnet powder by using a barrel plating process, and sequentially construct a matrix protection layer, a degreasing promotion layer, an oxidation diffusion resistance layer and the like to obtain modified rare earth magnet powder, wherein the barrel plating coating sequence is as follows: step a) adopting metal harmless to the rare earth magnet powder performance to form a matrix protective layer, and forming an inter-diffusion layer by directly contacting with a matrix to protect the matrix performance from being influenced in the subsequent treatment process; step b) employs a metal having a low boiling point and a melting point lower than that of the metal used in step a) to constitute a degreasing promoting layer outside the base protective layer formed in step a), and promotes efficient degreasing through a gasification process in a thermal degreasing process. And c) forming an oxidation-resistant diffusion layer outside the degreasing promotion layer formed in the step b) by adopting metal with a melting point lower than that of the metal used in the step a) and the step b), and forming a liquid protection layer in the thermal degreasing process to prevent oxidation and diffusion of carbon elements to the magnetic powder matrix.
Further preferably, the wax-based binder in the step (2) is one or more of paraffin wax, polyethylene wax, beeswax and microcrystalline wax, wherein the addition amount of each wax-based binder modification step is 10% -50%;
further preferably, in the step (3), the resin-based binder is one or more of Polyethylene (PE), polyoxymethylene (POM), polypropylene (PP), and Polystyrene (PS);
it is further preferred that the coupling agent in step (3) is one or more of KH550, KH560, KH 570.
It is further preferable that the plasticizer in the step (3) is one or more of sebacate, dibutyl sebacate and dioctyl sebacate.
The preparation method of the invention comprises the following steps: placing the injection molding blank D into a solvent, soaking for 1h, and taking out to perform drying treatment to obtain a solvent degreasing blank; then placing the solvent degreasing blank into a vacuum sintering furnace, heating to 100-700 ℃, wherein the heating rate is 1-10 ℃/min, and preserving the temperature for 3-80h to obtain a low-temperature thermal degreasing blank; and then placing the low-temperature degreasing blank into a vacuum sintering furnace, heating to 700-1000 ℃, keeping the temperature for 1h at a heating rate of 1-10 ℃/min, and obtaining the high-temperature degreasing blank.
Further preferably, the solvent used for degreasing in the step (5) is one or more of acetone, n-heptane, absolute ethyl alcohol, methylene dichloride, chloroform or trichloroethylene.
The invention has the advantages that:
the rare earth magnet powder may be coated with one or more metal layers of different functions including, but not limited to, resistance to high temperature oxidation, enhanced degreasing efficiency, protection of the substrate, etc.
The rare earth magnet powder can be small-particle-size powder with any shape such as spherical, flaky and the like, and has wide application range.
The tube furnace is pumped to a high vacuum environment, so that the rare earth magnet powder and the low-melting-point alloy are prevented from being oxidized in the heating process, and the function of multiple coatings on the surface of the magnetic powder is favorably exerted.
The amount of metal atoms evaporated from the surface layer of the rare earth magnet powder can be effectively controlled by filling a proper amount of argon into the tube furnace, and the thickness of a coating is controlled, so that the rare earth magnet powder still maintains excellent magnetic performance.
The selected low-melting-point metal is in short contact with the rare earth magnet powder at a certain temperature, and a simple substance or alloy coating is formed on the surface of the powder, so that the magnetic powder is effectively protected.
The rotation of the tube furnace can lead the rare earth magnet powder and the low-melting-point alloy to be in real-time dynamic contact, and the full contact of the rare earth magnet powder and the low-melting-point alloy leads the surface of the magnetic powder to form a complete and compact alloy coating.
The alloy coated rare earth magnet powder can effectively enhance the high-temperature oxidation resistance and improve degreasing efficiency, and creates favorable conditions for preparing high-performance metal powder injection molding sintered rare earth magnets.
The modified binder can reduce the viscosity of a melt blending system, increase the fluidity of powder and maintain the shape of a product, and is beneficial to preparing high-performance metal powder injection molding sintered rare earth magnets.
So that the magnetic property, oxidation resistance and the like of the final product are further improved.
Drawings
FIG. 1 is a microstructure of the untreated flaky quench powder and zinc coated quench powder surfaces.
The specific embodiment is as follows:
the invention provides a powder surface modification and preparation method of a metal powder injection molding sintered rare earth magnet by specific examples. The examples are given solely for the purpose of illustration and are not intended to limit the scope of the invention.
Example 1
(1) And (3) carrying out multilayer barrel plating treatment on the flaky neodymium iron boron rapid quenching powder and three metals of Al, zn and Sn in sequence. Firstly uniformly mixing flaky neodymium iron boron powder and Al particles according to the mass ratio of 1:2, then placing the mixture into a rotatable tubular furnace for 620-3 h barrel plating treatment to obtain Al-coated magnetic powder, then uniformly mixing the Al-coated magnetic powder and Zn particles according to the mass ratio of 1:2, placing the mixture into the rotatable tubular furnace for 360-3 h barrel plating treatment to obtain Al-Zn-coated magnetic powder, finally uniformly mixing the Al-Zn-coated magnetic powder and Sn particles according to the mass ratio of 1:2, and placing the mixture into the rotatable tubular furnace for 210-3 h barrel plating treatment to obtain multi-coating powder A1.
Microstructural analysis was performed on the untreated rapid-quench powder and the coating powder using an electron scanning microscope.
FIG. 1 is a microstructure of untreated sheet quench powder and coated powder surfaces. It can be seen from fig. 1 (a) that the untreated quench powder surface is relatively smooth and flat, while the coated powder surface is rough, forming a distinct coating, as shown in fig. 1 (b).
And carrying out a high-temperature oxidation experiment on the untreated powder and the coating powder by using a muffle furnace, wherein the temperature is 200 ℃, the oxidation time is 2 hours, and the weight gain rate of the powder before and after oxidation is calculated. The results showed that the rate of weight gain of the plated powder after oxidation was 0.4% which was much less than 2.9% of the untreated powder, indicating that the plated powder had more excellent resistance to high temperature oxidation than the untreated powder.
The rapid quenching powder with strong high-temperature oxidation resistance is beneficial to the preparation of the high-performance metal injection molding magnet in the next step.
(2) 20wt.% paraffin wax, 40wt.% polyethylene wax and 40wt.% beeswax are uniformly mixed and heated to 80 ℃ to obtain the modified wax-based adhesive.
(3) Adding 4wt.% of modified wax-based binder, 2wt.% of polyethylene resin, 0.5wt.% of sebacate, 0.5wt.% of KH550 and 93wt.% of Nd-Fe-B magnetic powder A1 into an internal mixer, setting the rotating speed to be 60r/min, mixing at 150 ℃ for 10min, taking out to obtain a mixed material B2, and crushing into magnet master batch C2 with the particle size of 1-5 mm;
(4) The magnet master batch C2 was fed into an injection molding machine, the injection temperature was set at 160℃and the injection pressure at 40MPa, and injection molding was performed with an orientation magnetic field of 18kOe, and the injection molded blank D2 was taken out.
(5) Placing the injection molding blank D2 into absolute ethyl alcohol, soaking for 1h, and taking out for drying treatment to obtain a solvent degreasing blank; then placing the solvent degreasing blank into a vacuum sintering furnace, heating to 300 ℃, wherein the heating rate is 5 ℃/min, and preserving heat for 3 hours to obtain a low-temperature thermal degreasing blank; and then placing the low-temperature thermal degreasing blank into a vacuum sintering furnace, heating to 900 ℃, wherein the heating rate is 5 ℃/min, and preserving the temperature for 1h to obtain the high-temperature thermal degreasing blank.
(6) And finally, rapidly heating the degreased blank to 940 ℃ which is the sintering temperature of the rare earth permanent magnet, wherein the sintering time is 2 hours, and obtaining the sintered NdFeB magnet E2.
The magnetic properties, densities, and oxidation weight gain data of the Nd-Fe-B magnet E2 obtained in this example were shown in Table 1.
TABLE 1
Example 2 (comparative):
uniformly mixing Nd-Fe-B quick setting powder and zinc particles according to a mass ratio of 1:5, and then placing the mixture in a rotatable tubular furnace. The vacuum degree of the tube furnace is pumped to 4.5X10 -3 After Pa, argon was introduced at a pressure of 0.05 MPa. The rotational speed of the tube furnace was set to 3r/min. Setting the heating temperature of the tube furnace to 360 ℃ and the heat preservation time to 3 hours. To be added withAfter the heat is finished, the tube furnace is rapidly cooled by using an industrial fan to obtain single-coating magnetic powder A3.
40wt.% of microcrystalline wax and 60wt.% of beeswax are uniformly mixed and heated to 85 ℃ to obtain the modified wax-based adhesive.
8wt.% of modified wax-based binder, 3wt.% of polypropylene, 1wt.% of polyoxymethylene, 1wt.% of dibutyl sebacate, 1wt.% of KH560, 86wt.% of Nd-Fe-B magnetic powder A3 are added into an internal mixer, the rotating speed is set at 80r/min, the mixing temperature is 140 ℃, the mixing time is 10min, the mixing material B3 is taken out, and then the mixture is crushed into magnet master batch C3 with the particle size of 1-5 mm;
the magnet master batch C3 was fed into an injection molding machine, the injection temperature was set at 150℃and the injection pressure at 60MPa, and injection molding was performed with an orientation magnetic field of 18kOe, and the injection molded blank D3 was taken out.
Putting the injection molding blank D3 into absolute ethyl alcohol, soaking for 1h, and taking out for drying treatment; then placing the blank degreased by the solvent into a vacuum sintering furnace, heating to 300 ℃, wherein the heating rate is 5 ℃/min, and preserving heat for 3 hours; and then placing the blank subjected to low-temperature degreasing into a vacuum sintering furnace, heating to 800 ℃, and preserving heat for 1h at a heating rate of 5 ℃/min. And finally, rapidly heating the degreased blank to 1050 ℃ of the sintering temperature of the rare earth permanent magnet, wherein the sintering time is 1h, and obtaining the sintered NdFeB magnet E3.
The magnetic properties, densities, and oxidation weight gain data of the Nd-Fe-B magnet E3 obtained in this example were shown in Table 2.
TABLE 2
Claims (10)
1. The preparation method of the metal powder injection molding sintered rare earth magnet is characterized by comprising the following steps of:
step (1): performing functional composite modification on the surface of the magnetic powder; and sequentially constructing at least a substrate protective layer, a degreasing promoting layer, an oxidation diffusion resisting layer and other multi-layer functional composite layer structures on the surface of the magnetic powder through barrel plating treatment. Each layer of the multi-layer functional composite layer is a metal simple substance or alloy; the melting point of the metal corresponding to each functionalization layer is gradually reduced from the surface of the magnetic powder outwards;
the preparation method of each layer comprises the following steps: uniformly mixing the rare earth powder corresponding to the previous step, namely the corresponding bare rare earth magnet powder or the rare earth magnet powder with different functional layers on the surface, with lower melting point metal or alloy adopted by the functional layer to be constructed on the outer layer, putting the mixture into a rotatable tubular furnace for barrel plating treatment, pumping the tubular furnace to a vacuum environment, filling argon, setting the rotating speed of the tubular furnace, setting heating temperature and time, and carrying out air cooling on the tubular furnace after heating is finished; forming a metal coating by the mutual contact of the heated lower melting point metal or alloy and the corresponding rare earth powder, and circularly obtaining modified rare earth magnet powder A; the heating temperature enables the lower melting point metal or alloy to at least reach a melting state, and simultaneously enables the functional layer on the surface of the rare earth magnet powder with different functional layers on the surface not to be melted;
step (2): blending and modifying a wax-based binder; mixing 2 or more than 2 wax-based binders according to a certain proportion, heating to 80-100 ℃, and mixing to obtain a modified wax-based binder;
step (3): melting, mixing and granulating the modified rare earth magnet powder A and a modified wax-based binder; adding 1-10 wt.% of wax-based modified binder, 1-10 wt.% of resin-based binder, 0.5-2 wt.% of coupling agent, 0.5-2 wt.% of plasticizer and 80-95 wt.% of modified rare earth magnet powder A into an internal mixer, setting the rotating speed to be 30-80 r/min, mixing at 100-350 ℃ for 5-30 min, taking out to obtain a mixed material B, and crushing into magnet master batch C with the particle size of 1-5 mm;
step (4): a metal injection molded magnet; adding the magnet master batch C obtained in the step (3) into an injection molding machine, setting the injection temperature to be 120-400 ℃, the injection pressure to be 30-100 MPa, and the orientation magnetic field to be 15-20 kOe, and performing injection molding to obtain a metal injection molding blank D;
step (5): degreasing an injection blank; degreasing the metal injection molding blank D obtained in the step (4), wherein the degreasing treatment comprises solvent degreasing, low-temperature degreasing and high-temperature degreasing in sequence;
step 6): sintering; and (3) rapidly heating the injection blank degreased in the step (5) to 900-1100 ℃ of the sintering temperature of the rare earth permanent magnet, wherein the sintering time is 0.5-3 h, and obtaining the sintered rare earth magnet E.
2. The method of claim 1 wherein the rare earth magnet of step (1) is selected from the group consisting of neodymium iron boron, samarium cobalt, and any other rare earth permanent magnet system; is melt rapid quenching powder, HDDR-hydrogen explosion powder, rapid hardening powder and powder obtained by any other method.
3. The method of claim 1, wherein the metal used in the functionalized composite layer in step (1) is selected from one or more of Cu, zn, al, sn, ga, in, mg, bi, sb, and each functional layer is selected from a corresponding metal as required.
4. A method according to claim 3, wherein the base protective layer is selected from one or more of Cu, ga, al, etc., and the degreasing promoting layer is selected from one or more of Zn, mg, etc.; the oxidation-resistant diffusion layer is one or more selected from Zn, sn, ga, in and the like.
5. The method according to claim 1, wherein the mass ratio of the rare earth powder in the step (1) to the metal adopted in the next functional layer to be built, namely the corresponding further outer layer, is 1:1-1:5, and the coating thickness of each layer is optionally adjusted within the range of 0.1-100 μm by adjusting the heating temperature, heating time and the like of barrel plating; the vacuum environment in the step (1) is 5.0X10 -3 Vacuum degree above Pa; the rotating speed of the tube furnace in the step (1) is 3-8 r/min.
6. The method of claim 1, wherein the surface of the rare earth magnet powder is subjected to functional composite modification by using a barrel plating process in the specific step (1), a matrix protection layer, a degreasing promotion layer, an oxidation diffusion resistance layer and the like are sequentially constructed, and modified rare earth magnet powder is obtained, and the barrel plating coating sequence is as follows: step a) adopting metal harmless to the rare earth magnet powder performance to form a matrix protective layer, and forming an inter-diffusion layer by directly contacting with a matrix to protect the matrix performance from being influenced in the subsequent treatment process; step b) employs a metal having a low boiling point and a melting point lower than that of the metal used in step a) to constitute a degreasing promoting layer outside the base protective layer formed in step a), and promotes efficient degreasing through a gasification process in a thermal degreasing process. And c) forming an oxidation-resistant diffusion layer outside the degreasing promotion layer formed in the step b) by adopting metal with a melting point lower than that of the metal used in the step a) and the step b), and forming a liquid protection layer in the thermal degreasing process to prevent oxidation and diffusion of carbon elements to the magnetic powder matrix.
7. The method of claim 1, wherein the wax-based binder in step (2) is one or more of paraffin wax, polyethylene wax, beeswax and microcrystalline wax, and wherein the amount of each wax-based binder modification step is 10% to 50%.
8. The method according to claim 1, wherein the resin-based binder in step (3) is one or more of Polyethylene (PE), polyoxymethylene (POM), polypropylene (PP), polystyrene (PS);
the coupling agent in the step (3) is one or more of KH550, KH560 and KH 570;
the plasticizer in the step (3) is one or more of sebacate, dibutyl sebacate and dioctyl sebacate.
9. The method of claim 1, wherein step (5): placing the injection molding blank D into a solvent, soaking for 1h, and taking out to perform drying treatment to obtain a solvent degreasing blank; then placing the solvent degreasing blank into a vacuum sintering furnace, heating to 100-700 ℃, wherein the heating rate is 1-10 ℃/min, and preserving the temperature for 3-80h to obtain a low-temperature thermal degreasing blank; then placing the low-temperature degreasing blank into a vacuum sintering furnace, heating to 700-1000 ℃, keeping the temperature for 1h at a heating rate of 1-10 ℃/min, and obtaining the high-temperature degreasing blank;
the solvent used for degreasing in the step (5) is one or more of acetone, n-heptane, absolute ethyl alcohol, methylene dichloride, chloroform or trichloroethylene.
10. A rare earth magnet prepared according to the method of any one of claims 1 to 9.
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