CN116072414A - Preparation method of anisotropic bonded magnet with high orientation degree - Google Patents
Preparation method of anisotropic bonded magnet with high orientation degree Download PDFInfo
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- CN116072414A CN116072414A CN202310168969.9A CN202310168969A CN116072414A CN 116072414 A CN116072414 A CN 116072414A CN 202310168969 A CN202310168969 A CN 202310168969A CN 116072414 A CN116072414 A CN 116072414A
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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
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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
- H01F41/0273—Imparting anisotropy
Abstract
A preparation method of an anisotropic bonded magnet with high orientation degree belongs to the technical field of magnetic material preparation. The preparation method comprises the following steps: firstly, the adhesive is dissolved in a solvent to form a uniform and stable solution, and then the anisotropic magnetic powder with the pretreated surface is added into the solution. And then placing the magnetic powder/binder solution into a ball milling tank for ball milling and refining, so that the magnetic powder can be uniformly dispersed in the solution, and better calendaring orientation anisotropy is obtained. Finally, adding an extractant while carrying out vacuum suction filtration on the suspension after ball milling, separating out magnetic powder/binder composites to obtain pre-oriented precipitates, crushing and sieving the precipitates, and then carrying out calendaring molding. When the calendaring molding is performed, the pre-oriented magnetic powder/binder composite is further mechanically oriented, thereby preparing the anisotropic bonded magnet with a higher degree of orientation.
Description
Technical Field
The invention relates to the technical field of magnetic material preparation, in particular to a preparation method of a flexible anisotropic bonded magnet with high orientation degree.
Background
The flexible anisotropic bonded magnet is an anisotropic composite permanent magnet material prepared by uniformly mixing high-performance anisotropic permanent magnet powder with a binder (resin) and other additives according to a certain proportion and then adopting a calendaring molding method. The flexible anisotropic bonding permanent magnet material has high magnetic performance and mechanical performance, and is easy to process into flexible bonding magnetic plates, magnetic strips, magnetic rings and other devices with complex shapes, thereby meeting various different requirements.
The high-performance bonded magnet commonly used in the market at present is a bonded NdFeB magnet. Wherein the magnetic energy product of the isotropically bonded NdFeB magnetic powder is usually 12-18MGOe, and the magnetic energy product of the isotropically bonded NdFeB magnetic powder prepared from the isotropically bonded NdFeB magnetic powder is usually 8-12MGOe, and the magnetic energy product ratio of the magnetic powder to the magnetic powder is about 67%. The magnetic energy product of the anisotropic bonded NdFeB magnetic powder is usually 30-40MGOe, and the maximum magnetic energy product of the anisotropic bonded NdFeB magnetic powder prepared from the anisotropic bonded NdFeB magnetic powder can reach 20MGOe, and the magnetic energy product ratio of the magnetic powder to the magnetic powder is about 50%. By comparing the magnetic energy product ratio of the anisotropic bonded magnet to the isotropic bonded magnet, it was found that the anisotropic bonded magnet was less than 10-20% of the isotropic bonded magnet, mainly because each particle of the anisotropic bonded magnet could not achieve a sufficiently high orientation when the anisotropic bonded magnet was used to prepare a magnet, and thus high magnetic properties could not be achieved, whereas the isotropic bonded magnet had no orientation problem. It can be seen that increasing the degree of orientation of the magnet, and thus its magnetic properties, is an important solution to the current increase in magnetic properties of anisotropic bonded magnets.
In CN200610089368.5 patent document, there is described a magnetically oriented anisotropic rolled bonded magnet and a method for producing the same, that is, the method comprising granulating a material, and then magnetically orienting and rolling the granulated material on a magnetic calender. The main innovation point of the method is that an electromagnet is added into a roller of a traditional calender so as to generate an orientation magnetic field, so that materials are oriented under the action of the magnetic field when passing through the roller, and an anisotropic magnet is generated, but the required external orientation magnetic field strength is very high due to the very high coercive force of NdFeB magnetic powder, and the high-strength external electromagnetic field is difficult to realize for calendaring equipment. At the same time, the method of applying a magnetic field in the calender rolls is not ideal in orientation.
Publication No. CN101800106 describes a method for preparing a high-orientation flexible anisotropic bonded magnet by using a two-step temperature-tracing magnetic field orientation process separated from a calendaring process and a temperature-tracing magnetic field orientation process, wherein the calendaring flexible bonded magnet is heated at a certain temperature for a certain time and then immediately placed in a magnetic field for temperature-tracing magnetic field orientation to obtain the high-orientation flexible anisotropic bonded magnet. However, when the magnet is subjected to temperature magnetic field orientation, magnetic powder particles rotate to cause damage to the surface flatness of the magnet, so that the oriented magnet is subjected to secondary flattening rolling, and the orientation degree of the magnet is damaged by secondary rolling, so that the magnetic performance of the magnet is affected.
Therefore, there is an urgent need to develop a process for obtaining a highly oriented anisotropic bonded magnet without applying a high-energy magnetic field for orientation during or after calender molding, and a flexible anisotropic bonded magnet with high degree of orientation, which is excellent in production performance and simple in process, is desired.
Disclosure of Invention
The invention provides the preparation method of the anisotropic bonded magnet which can obtain high orientation without applying high-energy magnetic field for orientation in the calendaring process or after molding, avoids complex and tedious production process flow with high energy consumption caused by high-energy magnetic field orientation, and fully exerts the advantages of simple and continuous production of the calendaring process.
The invention aims at realizing the following steps:
step (1) preparation of a magnetic powder/binder suspension:
the binder is added to the solution and stirred at a suitable temperature so that the binder is completely dissolved in the solution, and then the surface-pretreated anisotropic magnetic powder is added to the solution.
The adhesive is a high polymer material, and the component of the adhesive is any one of polyurethane elastomer (TPU), ethylene-vinyl acetate copolymer (EVA), styrene-ethylene-butylene-styrene block copolymer (SEBS) and Chlorinated Polyethylene (CPE).
Wherein the addition proportion of the binder is 1-20% of the mass of the magnetic powder.
Wherein the solution is a benign solvent corresponding to the selected binder, and when the binder resin is TPU, the solution is preferably N, N-dimethylformamide; when the binder resin is EVA, the solution is preferably toluene; when the binder resin is SEBS, the solution is preferably tetrahydrofuran; when the binder resin is CPE, the solution is preferably xylene.
In the preparation method of the magnetic powder/binder suspension, the magnetic powder/binder suspension is preferably stirred for 6-8 hours at 80 ℃ so that the binder can be fully dissolved in the solution.
Wherein the anisotropic magnetic powder is preferably rolled anisotropic magnetic powder or mixed magnetic powder of the rolled anisotropic magnetic powder and the anisotropic magnetic powder A; the rolled anisotropic magnetic powder A is selected from rolled anisotropic Nd-Fe-B magnetic powder and rolled anisotropic Sm-Co magnetic powder, and the anisotropic magnetic powder A is selected from anisotropic Sm-Fe-N magnetic powder and anisotropic Nd-Fe-N magnetic powder; when the mixed magnetic powder is selected, the anisotropic Sm-Fe-N, nd-Fe-N magnetic powder accounts for 1-20wt% of the rolled anisotropic magnetic powder.
Wherein the surface pretreatment steps are as follows: dissolving a surface pretreatment agent in an acetone solution, and then adding magnetic powder and stirring to achieve uniform distribution; next, the mixture is dried under a vacuum drying oven to remove the solvent, and finally the magnetic powder with the pretreated surface is obtained, wherein in the surface treatment process, a part of groups of the coupling agent molecules react with hydroxyl groups on the surface of the magnetic powder to form chemical bonds; then, when the magnetic powder and the binder act at a later stage, the other part of groups react with the binder to form physical entanglement, and the magnetic powder and the binder are organically combined to increase the binding force between the two.
Wherein the surface pretreatment agent is preferably one or a mixture of two of a silane coupling agent and a titanate coupling agent, and the mass of the surface pretreatment agent is 0.5-1.0wt% of the magnetic powder.
And (2) ball milling of the magnetic powder/binder suspension:
and (3) placing the magnetic powder/binder suspension obtained in the step (1) into a ball milling tank for ball milling refinement treatment.
The ball milling method comprises the following specific steps: in order to avoid oxidation of magnetic powder in the ball milling process, a magnetic powder/binder suspension is added into a ball milling tank in a vacuum glove box, ball milling medium is agate beads or zirconia beads, the ball milling medium is taken out of the vacuum glove box after sealing, ball milling is carried out for 1-6H, and the diameter-thickness ratio (D/H) of the magnetic powder after ball milling is 3.0-4.0.
Preparation of the pre-oriented precipitate in step (3):
and (3) carrying out vacuum suction filtration on the suspension after ball milling in the step (2), and simultaneously adding the extraction liquid ethanol into the suspension at constant speed, wherein the extraction liquid ethanol has good intersolubility with a solution and poor intersolubility with the magnetic powder/binder compound or even is mutually insoluble, so that the magnetic powder/binder compound is separated out to obtain a precipitate. Filtering the obtained precipitate with ethanol for 4-6 times, and vacuum filtering; then placing the precipitate obtained by extraction into a vacuum drying oven for drying to obtain a pre-oriented precipitate; the specific orientation principle is shown in figure 1, when vacuum filtration is carried out, the magnetic powder particles gradually drop under the action of pressure difference and gravity, and layered stacking is shown on the surface of the filter membrane to form pre-orientation, as shown in figure 2.
Wherein, the vacuum filtration of the suspension is carried out, and a microporous filter membrane with the pore diameter of 0.22 μm is preferably adopted;
wherein the vacuum drying temperature is 40-80 ℃.
And (4) calendaring and molding the anisotropic bonded magnet:
crushing and sieving the precipitate obtained after drying in the step (3), and then uniformly stirring and mixing the crushed particles with one or more of a plasticizer and a lubricant as a processing aid, and then carrying out calendaring molding to obtain the magnetic flux sheet with the thickness of 0.1-4 mm.
Wherein the mass of the processing aid is 0.1-5% of the mass of the magnetic powder/binder mixture.
Compared with the prior art, the invention has the greatest characteristics that: (1) the magnetic powder in the solution is thinned in the ball milling process, the magnetic powder can be uniformly dispersed in the solution, and better rolling orientation anisotropy is obtained; (2) the magnetic powder/binder mixture prepared by vacuum suction filtration avoids the risk of reduced magnetic performance caused by oxidation of the magnetic powder in conventional mixing granulation; (3) the magnetic powder is pre-oriented in the vacuum filtration process, and then the pre-oriented magnetic powder/binder compound is further mechanically oriented in the calendaring process, so that the orientation effect is effectively improved, and the magnetic property is greatly improved.
Drawings
FIG. 1 is an orientation schematic diagram of vacuum filtration;
FIG. 2 is a view of a surface layered tiling to form a pre-orientation.
Detailed Description
Comparative example 1
In this example, the anisotropic NdFeB magnetic powder was 95 parts, the binder TPU was 4 parts, and the processing aid stearic acid was 1 part. The anisotropic NdFeB magnetic powder is firstly subjected to ball milling treatment for 2 hours, and the magnetic powder after ball milling is subjected to surface treatment by a silane coupling agent KH550, wherein the mass of the surface treatment agent is 0.5wt% of the magnetic powder. Mixing and granulating the surface-treated NdFeB magnetic powder, a binding agent TPU and a processing aid stearic acid by using an internal mixer, wherein the mixing temperature is 150-170 ℃, and then carrying out calendaring molding to obtain a product with the thickness of 0.1-4mm, wherein the calendaring molding temperature is 150-170 ℃. The properties of the resulting magnet are shown in the following table.
Table 1:
| DOA(％) | B r (kG) | H cj (kOe) | (BH) max (MGOe) |
| 61％ | 5.63 | 14.88 | 6.88 |
wherein, the liquid crystal display device comprises a liquid crystal display device,
DOA in the table represents the degree of orientation of the magnet;
b in Table r Representing the remanence of the magnet;
h in the table cj Represents the intrinsic coercivity of the magnet;
in the table (BH) max Representing the maximum magnetic energy product of the magnet;
example 1
In this example, the anisotropic NdFeB magnetic powder after surface treatment with the silane coupling agent KH550 was used in an amount of 95 parts, the binder TPU was 4 parts, and the processing aid stearic acid was 1 part, wherein the mass of the surface treatment agent was 0.5wt% of the magnetic powder. First, 4 parts of the dried TPU was dissolved in dimethylformamide, stirred at 80℃for 4 hours, and then 95 parts of a calendaring-oriented anisotropic NdFeB magnetic powder was added to the TPU solution. The NdFeB/TPU dispersion was then continuously ball milled for 2 hours and the NdFeB magnetic powder was refined and uniformly distributed in the TPU solution. And (3) carrying out vacuum suction filtration on the ball-milled mixed solution, simultaneously adding ethanol as an extracting solution into the suspension at constant speed, wherein pre-oriented NdFeB/TPU precipitate appears, carrying out multiple times of filtration and suction filtration on the obtained precipitate by using ethanol, and then drying the precipitate in a vacuum drying oven at 60 ℃ until the quality is not changed. Crushing the dried precipitate, sieving with 5 mesh standard sieve, and calendaring to obtain product with thickness of 0.1-4mm at 150-170deg.C. The properties of the resulting magnet are shown in the following table. As can be seen from the comparison of example 1 and comparative example 1, the magnet subjected to the pre-orientation treatment had an orientation degree improved by 33% and a magnetic energy product improved by 53% as compared with the magnet not subjected to the pre-orientation treatment.
Table 2:
| DOA(％) | B r (kG) | H cj (kOe) | (BH) max (MGOe) |
| 81％ | 7.00 | 14.87 | 10.52 |
comparative example 2
In this example, 95 parts of anisotropic magnetic powder, 4 parts of binder TPU, and 1 part of processing aid stearic acid were used, wherein the anisotropic magnetic powder comprises 93 parts of a mixed magnetic powder of a calendared anisotropic NdFeB magnetic powder and 2 parts of an anisotropic SmFeN magnetic powder. The NdFeN/SmFeN magnetic powder is firstly subjected to ball milling treatment for 1h, and the ball milled magnetic powder is subjected to surface treatment by a silane coupling agent KH550, wherein the mass of the surface treatment agent is 0.5wt% of the magnetic powder. Mixing the surface-treated NdFeN/SmFeN mixed magnetic powder, a binder TPU and a processing aid stearic acid by an internal mixer, granulating at 60-80 ℃, and then carrying out calendaring molding to obtain a product with the thickness of 0.1-4mm, wherein the calendaring molding temperature is 60-80 ℃. The properties of the resulting magnet are shown in the following table.
Table 3:
| DOA(％) | B r (kG) | H cj (kOe) | (BH) max (MGOe) |
| 67％ | 5.77 | 14.70 | 7.28 |
example 2
In this example, the adopted anisotropic composite magnetic powder after surface treatment was 95 parts, the binder CPE was 4 parts, and the processing aid stearic acid was 1 part, wherein the anisotropic magnetic powder comprised 93 parts of a mixed magnetic powder of a calendared oriented anisotropic NdFeB magnetic powder and 2 parts of an anisotropic SmFeN magnetic powder, wherein the mass of the surface treatment agent was 0.5wt% of the magnetic powder. First, 4 parts of CPE was dissolved in xylene, stirred at 80℃for 6 hours, and then 95 parts of the surface-treated anisotropic composite magnetic powder was added to the CPE solution. The NdFeN/SmFeN/CPE dispersion was then ball milled continuously for 1h, and the magnetic powder was refined and uniformly distributed in the CPE solution. And (3) carrying out vacuum suction filtration on the ball-milled mixed solution, simultaneously adding ethanol as an extraction solution into the suspension at constant speed, wherein pre-oriented NdFeN/SmFeN/CPE precipitates appear, carrying out multiple times of filtration and suction filtration on the obtained precipitates by using ethanol, and then drying the precipitates in a vacuum drying oven at 60 ℃ until the quality is unchanged. Crushing the dried precipitate, sieving with 5 mesh standard sieve, and calendaring to obtain product with thickness of 0.1-4mm at 60-80deg.C. The properties of the resulting magnet are shown in the following table. As can be seen from the comparison of example 2 and comparative example 2, the magnet subjected to the pre-orientation treatment has an orientation degree increased by 28% and a magnetic energy product increased by 74% as compared with the magnet not subjected to the pre-orientation treatment.
Table 4:
| DOA(％) | B r (kG) | H cj (kOe) | (BH) max (MGOe) |
| 86％ | 7.77 | 14.71 | 12.70 |
the above description is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions easily come within the technical scope of the present invention by those skilled in the art should be included in the scope of the present invention. Therefore, the protection scope of the present invention should be subject to the protection scope of the claims.
Claims (8)
1. The preparation method of the anisotropic bonded magnet with high orientation degree is characterized by comprising the following steps of:
step (1) preparation of a magnetic powder/binder suspension:
adding the binder into the solution, stirring at a proper temperature to enable the binder to be completely dissolved in the solution, and then adding the anisotropic magnetic powder subjected to surface pretreatment into the solution;
the adhesive is a high polymer material, and the component of the adhesive is any one of polyurethane elastomer (TPU), ethylene-vinyl acetate copolymer (EVA), styrene-ethylene-butylene-styrene block copolymer (SEBS) and Chlorinated Polyethylene (CPE);
and (2) ball milling of the magnetic powder/binder suspension:
and (3) placing the magnetic powder/binder suspension obtained in the step (1) into a ball milling tank for ball milling refinement treatment.
The ball milling method comprises the following specific steps: in order to avoid oxidation of magnetic powder in the ball milling process, adding a magnetic powder/binder suspension into a ball milling tank in a vacuum glove box, taking out the ball milling medium which is agate beads or zirconia beads from the vacuum glove box after sealing cover, and carrying out ball milling for 1-6H, wherein the diameter-thickness ratio (D/H) of the magnetic powder after ball milling is 3.0-4.0;
preparation of the pre-oriented precipitate in step (3):
and (3) carrying out vacuum suction filtration on the suspension after ball milling in the step (2), and simultaneously adding the extraction liquid ethanol into the suspension at constant speed, wherein the extraction liquid ethanol has good intersolubility with a solution and poor intersolubility with the magnetic powder/binder compound or even is mutually insoluble, so that the magnetic powder/binder compound is separated out to obtain a precipitate. Filtering the obtained precipitate with ethanol for 4-6 times, and vacuum filtering; then placing the precipitate obtained by extraction into a vacuum drying oven for drying to obtain a pre-oriented precipitate; when vacuum filtration is carried out, under the action of pressure difference and gravity, magnetic powder particles gradually drop, and layered stacking is shown on the surface of a filter membrane to form pre-orientation;
and (4) calendaring and molding the anisotropic bonded magnet:
crushing and sieving the precipitate obtained after drying in the step (3), and then uniformly stirring and mixing the crushed particles with one or more of a plasticizer, a lubricant and the like as a processing aid, and then carrying out calendaring molding to obtain the magnetic flux sheet with the thickness of 0.1-4 mm.
2. The method for producing a highly oriented anisotropic bonded magnet according to claim 1, wherein the binder in step (1) is added in an amount of 1 to 20% by mass of the magnetic powder.
3. The method for producing an anisotropic bonded magnet having a high degree of orientation according to claim 1, wherein the solution in step (1) is a benign solvent corresponding to the selected binder, and when the binder resin is TPU, the solution is preferably N, N-dimethylformamide; when the binder resin is EVA, the solution is preferably toluene; when the binder resin is SEBS, the solution is preferably tetrahydrofuran; when the binder resin is CPE, the solution is preferably xylene;
in the preparation method of the magnetic powder/binder suspension, the magnetic powder/binder suspension is stirred for 6-8 hours at 80 ℃ so that the binder can be fully dissolved in the solution.
4. The method for producing a high-orientation anisotropic bonded magnet according to claim 1, wherein the anisotropic magnetic powder in step (1) is preferably a rolled anisotropic magnetic powder or a mixed magnetic powder of a rolled anisotropic magnetic powder and an anisotropic magnetic powder a; the rolled anisotropic magnetic powder A is selected from rolled anisotropic Nd-Fe-B magnetic powder and rolled anisotropic Sm-Co magnetic powder, and the anisotropic magnetic powder A is selected from anisotropic Sm-Fe-N magnetic powder and anisotropic Nd-Fe-N magnetic powder; when the mixed magnetic powder is selected, the anisotropic Sm-Fe-N, nd-Fe-N magnetic powder accounts for 1-20wt% of the rolled anisotropic magnetic powder.
5. The method for preparing an anisotropic bonded magnet with high degree of orientation according to claim 1, wherein the surface pretreatment step of step (1) is as follows: dissolving a surface pretreatment agent in an acetone solution, and then adding magnetic powder and stirring to achieve uniform distribution; next, the mixture is dried under a vacuum drying oven to remove the solvent, and finally the magnetic powder with the pretreated surface is obtained, wherein in the surface treatment process, a part of groups of the coupling agent molecules react with hydroxyl groups on the surface of the magnetic powder to form chemical bonds; then, when the magnetic powder and the binder act at the later stage, the other part of groups react with the binder to form physical entanglement, and the magnetic powder and the binder are organically combined to increase the binding force between the two;
the surface pretreatment agent is preferably one or a mixture of two of a silane coupling agent and a titanate coupling agent, and the mass of the surface pretreatment agent is 0.5-1.0wt% of the magnetic powder.
6. The method for producing an anisotropic bonded magnet with high degree of orientation according to claim 1, wherein, in the step (3), vacuum filtration of the suspension is performed using a microporous filter membrane with a pore size of 0.22 μm;
wherein the vacuum drying temperature is 40-80 ℃.
7. The method of producing a highly oriented anisotropic bonded magnet according to claim 1, wherein the processing aid in step (4) is 0.1 to 5% by mass of the magnetic powder/binder mixture.
8. An anisotropic bonded magnet of high degree of orientation prepared according to the method of any one of claims 1 to 7.
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