CN111799081B - Preparation method of functional film on surface of neodymium iron boron permanent magnet - Google Patents
Preparation method of functional film on surface of neodymium iron boron permanent magnet Download PDFInfo
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- CN111799081B CN111799081B CN202010603072.0A CN202010603072A CN111799081B CN 111799081 B CN111799081 B CN 111799081B CN 202010603072 A CN202010603072 A CN 202010603072A CN 111799081 B CN111799081 B CN 111799081B
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- 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
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- 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
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- C23C4/134—Plasma spraying
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Abstract
The invention discloses a preparation method of a functional film layer on the surface of a neodymium iron boron permanent magnet, which comprises the following steps: s1: deoiling, pickling and washing the neodymium iron boron permanent magnet; s2: uniformly stirring and mixing the Ni-MOFs material, the nano copper powder, the sodium dodecyl sulfate, the deionized water and the normal hexane, adding the modified epoxy resin and the fluorine-containing silane coupling agent, stirring, and then spraying and granulating; s3: carrying out vacuum plasma spraying operation on the neodymium iron boron permanent magnet to obtain a neodymium iron boron permanent magnet bottom layer; s4: preparing a graft modified epoxy resin/organic silicon polymer interpenetrating network polymer; s5: and (3) coating the interpenetrating network polymer on the bottom layer, and curing at high temperature to form a functional film layer on the surface of the neodymium iron boron permanent magnet. The functional film layer on the surface of the neodymium iron boron permanent magnet prepared by the invention not only has excellent protection performance such as humidity and heat resistance, corrosion resistance, scratch resistance and the like, but also has excellent mechanical properties such as strong bonding force, strong toughness and the like, thereby prolonging the service life of the sintered neodymium iron boron magnet.
Description
Technical Field
The invention relates to the technical field of neodymium iron boron, in particular to a preparation method of a functional film layer on the surface of a neodymium iron boron permanent magnet.
Background
The sintered Nd-Fe-B permanent magnet has excellent characteristics and performance price, and is widely applied to various industries such as computers, motors, electric vehicles, instruments, magnetic transmission bearings, high-fidelity speakers, nuclear magnetic resonance imaging instruments, aerospace and aviation and the like. The sintered neodymium iron boron has large surface porosity and is easy to oxidize and corrode, a protective functional film layer is usually formed on the surface of the sintered neodymium iron boron by surface treatment, and the protective functional film layer on the surface can be realized by methods such as metal plating, chemical plating, organic matter coating, physical vapor deposition and the like. The method for electroplating the metal coating has the advantages of low requirement on equipment, simpler process conditions, high film forming speed, low cost and the like, but has the problems of high metal consumption cost, influence of heavy metal pollution on the ecological environment and the like; compared with electroplating, the chemical plating can obtain a thin plating layer, a plating layer with low magnetism and high protection, the size of a plated workpiece can be diversified, but the problems that the chemical plating solution is difficult to maintain, H2 is continuously generated in the plating process, the brittleness of the plating layer is increased, the plating layer is easy to crack in the later use process and the like exist; the organic coating is mainly made of epoxy resin, and can be realized by methods such as spin coating, brush coating, spray coating, electrostatic powder spray coating, cathode electrophoresis and the like, but the organic coating of the epoxy resin has the defects of poor moisture and heat resistance, poor toughness and other various performances, and particularly a sintered neodymium-iron-boron magnet working in a high-humidity and high-heat environment has short service life and cannot meet the long-term operation requirement. The functional film layer on the surface of the neodymium iron boron prepared by the existing method has more defects and cannot meet the long-term operation requirement under severe environment.
In view of this, it is urgently needed to provide a method for preparing a functional film on the surface of a neodymium iron boron permanent magnet, so that the prepared functional film not only has the properties of humidity and heat resistance, corrosion resistance and wear resistance, but also has strong bonding force with a substrate, and can meet the long-term operation requirement in a more severe environment.
Disclosure of Invention
In view of the defects of the prior art, the invention provides a preparation method of a surface functional film layer of a neodymium iron boron permanent magnet, which aims to solve the problems of low humidity resistance, corrosion resistance, wear resistance and the like and poor toughness of the surface functional film layer of the prior neodymium iron boron permanent magnet, so that a neodymium iron boron surface protective layer has good protective performance and mechanical performance, and the service life of the neodymium iron boron permanent magnet in a severe environment is prolonged.
In order to achieve the above purposes, the technical scheme adopted by the invention is as follows:
a preparation method of a functional film layer on the surface of a neodymium iron boron permanent magnet comprises the following steps:
s1: ultrasonically cleaning and degreasing the neodymium iron boron permanent magnet, and then sequentially carrying out acid washing and water washing treatment to obtain a pretreated neodymium iron boron permanent magnet;
s2: weighing 10-30 parts by weight of Ni-MOFs material, 0.5-0.8 part by weight of nano copper powder, 1.4-1.8 parts by weight of sodium dodecyl sulfate, 30-50 parts by weight of deionized water and 45-55 parts by weight of n-hexane, uniformly stirring and mixing, then adding 60-80 parts by weight of modified epoxy resin and 0.1-0.3 part by weight of fluorine-containing silane coupling agent, stirring at high speed, and carrying out spray granulation to obtain particles with the particle size of 0.1-0.5 mu m;
s3: placing the neodymium iron boron permanent magnet processed in the step S1 in a vacuum chamber, and performing plasma spraying operation under the protection of inert gas, so that the particles obtained in the step S2 are uniformly sprayed on the surface of the neodymium iron boron permanent magnet processed in the step S1, and a neodymium iron boron permanent magnet bottom layer is obtained;
s4: weighing 30-45 parts of epoxy resin and 20-30 parts of dimethyl diphenyl polysiloxane, dissolving in 100 parts of toluene, stirring and heating to 100-150 ℃, dropwise adding 1-10 parts of ammonium persulfate aqueous solution and mixed solution formed by combining acrylic acid and phenyl trichlorosilane, reacting for 3-6 hours after dropwise adding for 0.5-1 hour, then adding 0.1-1 part of hexafluorobisphenol A diacrylate for graft modification reaction, and continuing to react for 1-3 hours to obtain a graft modified epoxy resin/organic silicon polymer interpenetrating network polymer;
s5: and (4) applying the graft modified epoxy resin/organic silicon polymer interpenetrating network polymer obtained in the step (S4) on the neodymium iron boron permanent magnet bottom layer obtained in the step (S3), and curing at high temperature to form the neodymium iron boron permanent magnet surface functional film layer.
In the preparation process of the bottom layer, the organic metal frame Ni-MOFs material arranged in a regular structure is used as a carrier, and under the action of high-temperature plasma, metal copper and nickel are uniformly coated on the surface of the neodymium iron boron permanent magnet at the same time, so that the corrosion resistance and the wear resistance of the neodymium iron boron permanent magnet are improved; because the porosity of copper is lower than that of nickel, and the copper is non-magnetic metal, the magnetic shielding of the magnet is smaller than that of nickel, and the copper replaces part of nickel, the magnetic performance loss of the magnet caused by the magnetic shielding of a nickel layer is reduced, the metal copper can permeate into the pores on the surface of the magnet, and the corrosion resistance of the magnet is further improved; in addition, a plurality of primary amine functional groups on the multidentate organic ligand in the Ni-MOFs material are beneficial to reacting with the modified epoxy resin to form a compact network structure, and meanwhile, the bonding force with a magnet can be improved, and the service life of the surface functional film layer under a severe condition is prolonged.
Preferably, the ultrasonic power of the ultrasonic cleaning is 1500-3000W, and the ultrasonic frequency is 30-40 KHz.
Preferably, the pickling solution for pickling consists of 1-5 wt% of hydrochloric acid solution and thiourea, wherein the thiourea accounts for 0.5-1.5 wt% of the total mass of the pickling solution.
Preferably, the preparation method of the Ni-MOFs material comprises the following steps: dissolving 0.05-0.1 mol/L of organic carboxylic acid MOF ligand shown in a chemical formula I and 0.15-0.3 mol/L of nickel nitrate in 1L of dimethylformamide, condensing and refluxing for 6-18 h at 120-150 ℃, cooling to room temperature, filtering, repeatedly washing with acetone, and drying to obtain the Ni-MOFs material,
preferably, the modified epoxy resin is an aliphatic and/or aromatic epoxy resin. The modified epoxy resin has a toughening effect, and provides the impact resistance of the functional film layer on the surface of the neodymium iron boron permanent magnet.
Preferably, the fluorine-containing silane coupling agent is at least one of heptadecafluorotrimethoxysilane, heptadecafluorotriethoxysilane, tridecafluoryltrimethoxysilane, tridecafluoryltriethoxysilane, dodecafluorotrimethoxysilane and dodecafluorotriethoxysilane. The fluorine-containing silane coupling agent is beneficial to improving the hydrophobicity of the functional film on the surface of the neodymium iron boron permanent magnet and reducing the permeation of water molecules in the film in the environment, thereby being beneficial to improving the humidity resistance of the functional film on the surface of the neodymium iron boron permanent magnet.
Preferably, the vacuum chamber has a vacuum degree of 50 to 100Pa and a temperature of 150 to 200 ℃.
Preferably, the curing temperature of the high-temperature curing is 130-180 ℃, and the curing time is 1-10 h.
Preferably, the thickness of neodymium iron boron permanent magnet bottom is 5 ~ 15 um.
Preferably, the thickness of the functional film layer on the surface of the neodymium iron boron permanent magnet is 20-30 um.
The graft modified epoxy resin/organic silicon polymer interpenetrating network polymer coated on the bottom layer has excellent binding force with the substrate layer, improves the peeling resistance of the film layer and has better integrity; the interpenetrating network polymer is formed by the grafting modification of the epoxy resin and the organic silicon polymer, so that the protective layer has the excellent characteristics of the epoxy resin and the organic silicon polymer, and has excellent mechanical properties, corrosion resistance, scratch resistance, humidity resistance and the like.
The invention has the beneficial effects that:
the substrate layer, the neodymium iron boron permanent magnet and the surface protective layer of the functional film layer on the surface of the neodymium iron boron permanent magnet prepared by the invention have stronger bonding performance; in general, through the preparation of the composite film layer, the performances of corrosion resistance, wear resistance, weather resistance, humidity resistance and the like of the surface of the neodymium iron boron permanent magnet are improved, and the service life of the neodymium iron boron permanent magnet under a severe condition is prolonged.
Detailed Description
The following description is presented to disclose the invention so as to enable any person skilled in the art to practice the invention. The preferred embodiments in the following description are given by way of example only, and other obvious variations will occur to those skilled in the art.
Example 1
The preparation method of the functional film layer on the surface of the neodymium iron boron permanent magnet comprises the following steps:
s1: ultrasonically cleaning and degreasing the neodymium iron boron permanent magnet, and then sequentially carrying out acid washing and water washing treatment to obtain a pretreated neodymium iron boron permanent magnet; the ultrasonic power of the ultrasonic cleaning is 2000W, and the ultrasonic frequency is 35 KHz; the pickling solution for pickling consists of 3 wt% of hydrochloric acid solution and thiourea, wherein the thiourea accounts for 1wt% of the total mass of the pickling solution;
s2: weighing 20 parts of Ni-MOFs material, 0.6 part of nano copper powder, 1.6 parts of sodium dodecyl sulfate, 40 parts of deionized water and 50 parts of n-hexane according to parts by weight, stirring and mixing uniformly, then adding 70 parts of aliphatic epoxy resin and 0.2 part of heptadecafluorosilane trimethoxy silane, stirring at a high speed, and carrying out spray granulation to obtain particles with the particle size of 0.3 mu m; the aliphatic epoxy resin is aliphatic glycidyl ether epoxy resin, and has an epoxy equivalent of 460 and a viscosity of 9000 cps;
s3: placing the neodymium iron boron permanent magnet processed in the step S1 into a vacuum chamber, wherein the vacuum degree of the vacuum chamber is 70Pa, the temperature of the vacuum chamber is 180 ℃, and performing plasma spraying operation under the protection of inert gas to uniformly spray the particles obtained in the step S2 on the surface of the neodymium iron boron permanent magnet processed in the step S1 to obtain a neodymium iron boron permanent magnet bottom layer; the thickness of the bottom layer of the neodymium iron boron permanent magnet is 10 um;
s4: weighing 37 parts of epoxy resin and 25 parts of dimethyl diphenyl polysiloxane, dissolving in 100 parts of toluene, stirring, heating to 120 ℃, dropwise adding 5 parts of ammonium persulfate aqueous solution and a mixed solution composed of acrylic acid and phenyl trichlorosilane, completing dropwise adding within 0.5h, reacting for 3h, then adding 0.5 part of hexafluorobisphenol A diacrylate for graft modification reaction, and continuing to react for 2h to obtain a graft modified epoxy resin/organic silicon polymer interpenetrating network polymer;
s5: coating the graft modified epoxy resin/organic silicon polymer interpenetrating network polymer obtained in the step S4 on the neodymium iron boron permanent magnet bottom layer obtained in the step S3, and after high-temperature curing, the curing temperature of the high-temperature curing is 150 ℃, and the curing time is 5 hours, so that a functional film layer on the surface of the neodymium iron boron permanent magnet is formed; the thickness of neodymium iron boron permanent magnet surface function rete is 25 um.
The preparation method of the Ni-MOFs material comprises the following steps: dissolving 0.07mol/L of organic carboxylic acid MOF ligand shown in a chemical formula I and 0.21mol/L of nickel nitrate in 1L of dimethylformamide, condensing and refluxing for 12h at 130 ℃, cooling to room temperature, filtering, repeatedly washing with acetone, and drying to obtain the Ni-MOFs material,
example 2
The preparation method of the functional film layer on the surface of the neodymium iron boron permanent magnet comprises the following steps:
s1: ultrasonically cleaning and degreasing the neodymium iron boron permanent magnet, and then sequentially carrying out acid washing and water washing treatment to obtain a pretreated neodymium iron boron permanent magnet; the ultrasonic power of the ultrasonic cleaning is 1500W, and the ultrasonic frequency is 30 KHz; the pickling solution for pickling consists of 1wt% of hydrochloric acid solution and thiourea, wherein the thiourea accounts for 0.5wt% of the total mass of the pickling solution;
s2: weighing 10 parts of Ni-MOFs material, 0.5 part of nano copper powder, 1.4 parts of sodium dodecyl sulfate, 30 parts of deionized water and 45 parts of n-hexane according to parts by weight, stirring and mixing uniformly, then adding 60 parts of aliphatic epoxy resin and 0.1 part of dodeca-fluoroalkyl trimethoxy silane, stirring at a high speed, and performing spray granulation to obtain particles with the particle size of 0.1 mu m; the aliphatic epoxy resin is aliphatic glycidyl ether epoxy resin, and the epoxy equivalent is 470, and the viscosity is 10500 cps;
s3: placing the neodymium iron boron permanent magnet processed in the step S1 in a vacuum chamber, wherein the vacuum degree of the vacuum chamber is 100Pa, the temperature of the vacuum chamber is 150 ℃, and performing plasma spraying operation under the protection of inert gas to uniformly spray the particles obtained in the step S2 on the surface of the neodymium iron boron permanent magnet processed in the step S1 to obtain a neodymium iron boron permanent magnet bottom layer; the thickness of the bottom layer of the neodymium iron boron permanent magnet is 5 um;
s4: weighing 30 parts of epoxy resin and 20 parts of dimethyl diphenyl polysiloxane, dissolving in 100 parts of toluene, stirring, heating to 100 ℃, dropwise adding 1 part of ammonium persulfate aqueous solution and a mixed solution composed of acrylic acid and phenyl trichlorosilane, completing dropwise adding for 1h, reacting for 3h, then adding 1 part of hexafluorobisphenol A diacrylate, carrying out graft modification reaction, and continuing to react for 1h to obtain a graft modified epoxy resin/organic silicon polymer interpenetrating network polymer;
s5: coating the graft modified epoxy resin/organic silicon polymer interpenetrating network polymer obtained in the step S4 on the neodymium iron boron permanent magnet bottom layer obtained in the step S3, and after high-temperature curing, wherein the curing temperature of the high-temperature curing is 130 ℃, and the curing time is 10 hours, so that a functional film layer on the surface of the neodymium iron boron permanent magnet is formed; the thickness of neodymium iron boron permanent magnet surface function rete is 20 um.
The preparation method of the Ni-MOFs material comprises the following steps: dissolving 0.05mol/L of organic carboxylic acid MOF ligand shown in a chemical formula I and 0.15mol/L of nickel nitrate in 1L of dimethylformamide, condensing and refluxing for 18h at 120 ℃, cooling to room temperature, filtering, repeatedly washing with acetone, and drying to obtain the Ni-MOFs material,
example 3
The preparation method of the functional film layer on the surface of the neodymium iron boron permanent magnet comprises the following steps:
s1: ultrasonically cleaning and degreasing the neodymium iron boron permanent magnet, and then sequentially carrying out acid washing and water washing treatment to obtain a pretreated neodymium iron boron permanent magnet; the ultrasonic power of the ultrasonic cleaning is 3000W, and the ultrasonic frequency is 40 KHz; the pickling solution for pickling consists of 5wt% of hydrochloric acid solution and thiourea, wherein the thiourea accounts for 1.5wt% of the total mass of the pickling solution;
s2: weighing 30 parts of Ni-MOFs material, 0.8 part of nano copper powder, 1.8 parts of sodium dodecyl sulfate, 50 parts of deionized water and 55 parts of n-hexane according to parts by weight, stirring and mixing uniformly, then adding 80 parts of aromatic epoxy resin and 0.3 part of tridecyl-trimethoxy silane, stirring at a high speed, and carrying out spray granulation to obtain particles with the particle size of 0.5 mu m; the aromatic epoxy resin is polyphenol type glycidyl ether epoxy resin, and has an epoxy equivalent of 440 and a viscosity of 8500 cps;
s3: placing the neodymium iron boron permanent magnet processed in the step S1 in a vacuum chamber, wherein the vacuum degree of the vacuum chamber is 50Pa, the temperature of the vacuum chamber is 200 ℃, and performing plasma spraying operation under the protection of inert gas to uniformly spray the particles obtained in the step S2 on the surface of the neodymium iron boron permanent magnet processed in the step S1 to obtain a neodymium iron boron permanent magnet bottom layer; the thickness of the bottom layer of the neodymium iron boron permanent magnet is 15 um;
s4: weighing 45 parts of epoxy resin and 30 parts of dimethyl diphenyl polysiloxane, dissolving in 100 parts of toluene, stirring, heating to 150 ℃, dropwise adding 10 parts of ammonium persulfate aqueous solution and mixed solution formed by combining acrylic acid and phenyl trichlorosilane, completing dropwise adding for 1h, reacting for 3h, then adding 1 part of hexafluorobisphenol A diacrylate, carrying out graft modification reaction, and continuing to react for 3h to obtain a graft modified epoxy resin/organic silicon polymer interpenetrating network polymer;
s5: coating the graft modified epoxy resin/organic silicon polymer interpenetrating network polymer obtained in the step S4 on the neodymium iron boron permanent magnet bottom layer obtained in the step S3, and after high-temperature curing, wherein the curing temperature of the high-temperature curing is 180 ℃, and the curing time is 10 hours, so that a functional film layer on the surface of the neodymium iron boron permanent magnet is formed; the thickness of neodymium iron boron permanent magnet surface function rete is 30 um.
The preparation method of the Ni-MOFs material comprises the following steps: dissolving 0.1mol/L of organic carboxylic acid MOF ligand shown in a chemical formula I and 0.3mol/L of nickel nitrate in 1L of dimethylformamide, condensing and refluxing for 18h at 150 ℃, cooling to room temperature, filtering, repeatedly washing with acetone, and drying to obtain the Ni-MOFs material,
comparative example 1
The preparation method of the functional film layer on the surface of the neodymium iron boron permanent magnet is basically similar to that of the embodiment 1, and the main difference is that the Ni-MOFs material is not adopted in the preparation process of the substrate.
Comparative example 2
The preparation method of the surface functional film layer of the neodymium iron boron permanent magnet in the comparative example is basically similar to that in example 1, and mainly differs in that the surface functional film layer does not comprise a substrate layer and only comprises one protective layer.
Comparative example 3
The preparation method of the surface functional film layer of the neodymium iron boron permanent magnet in the comparative example is basically similar to that in example 1, and mainly differs in that the surface functional film layer does not comprise a protective layer and only comprises a substrate layer.
The neodymium iron boron permanent magnet surface functional film layers prepared in the embodiments 1-3 and the comparative examples 1-3 are subjected to performance tests, and the performance results are shown in the table 1:
and (3) testing the adhesive force: the adhesion performance of the surface functional film layer is judged by performing an adhesion test according to GB 9286-1998.
And (3) corrosion resistance testing: testing the salt spray corrosion resistance of a sample by using an SH-90 type salt spray corrosion test box according to GB/T2423.17-1993; the test environment temperature is (35 +/-2) DEG C, the time of occurrence of rust is taken as the evaluation standard of the corrosion resistance of the functional film layer on the surface of the neodymium iron boron, and the evaluation standard is counted in hours.
And (3) wear resistance test: according to GB/T1768-1979, after grinding 200 circles by a grinding wheel under a weight of 250g, the weight loss of the surface functional film layer is tested, so as to judge the wear resistance of the film layer.
Impact resistance test: the test was performed according to GB 1732-93.
And (3) testing the moist heat resistance: and (3) soaking the neodymium iron boron materials prepared by the preparation methods of the embodiments 1-3 and the comparative examples 1-3 in hot water at 80 ℃ for cooking for 68 hours, taking out and drying, observing the appearance of the functional film layer on the surface of the neodymium iron boron permanent magnet, and testing the change condition of the adhesive force of the neodymium iron boron permanent magnet to judge the heat resistance of the neodymium iron boron permanent magnet.
TABLE 1
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed.
Claims (9)
1. A preparation method of a functional film layer on the surface of a neodymium iron boron permanent magnet is characterized by comprising the following steps:
s1: ultrasonically cleaning and degreasing the neodymium iron boron permanent magnet, and then sequentially carrying out acid washing and water washing treatment to obtain a pretreated neodymium iron boron permanent magnet;
s2: weighing 10-30 parts by weight of Ni-MOFs material, 0.5-0.8 part by weight of nano copper powder, 1.4-1.8 parts by weight of sodium dodecyl sulfate, 30-50 parts by weight of deionized water and 45-55 parts by weight of n-hexane, uniformly stirring and mixing, then adding 60-80 parts by weight of modified epoxy resin and 0.1-0.3 part by weight of fluorine-containing silane coupling agent, stirring at high speed, and carrying out spray granulation to obtain particles with the particle size of 0.1-0.5 mu m;
s3: placing the neodymium iron boron permanent magnet processed in the step S1 in a vacuum chamber, and performing plasma spraying operation under the protection of inert gas, so that the particles obtained in the step S2 are uniformly sprayed on the surface of the neodymium iron boron permanent magnet processed in the step S1, and a neodymium iron boron permanent magnet bottom layer is obtained;
s4: weighing 30-45 parts of epoxy resin and 20-30 parts of dimethyl diphenyl polysiloxane, dissolving in 100 parts of toluene, stirring and heating to 100-150 ℃, dropwise adding 1-10 parts of ammonium persulfate aqueous solution and mixed solution formed by combining acrylic acid and phenyl trichlorosilane, reacting for 3-6 hours after dropwise adding for 0.5-1 hour, then adding 0.1-1 part of hexafluorobisphenol A diacrylate for graft modification reaction, and continuing to react for 1-3 hours to obtain a graft modified epoxy resin/organic silicon polymer interpenetrating network polymer;
s5: coating the graft modified epoxy resin/organic silicon polymer interpenetrating network polymer obtained in the step S4 on the neodymium iron boron permanent magnet bottom layer obtained in the step S3, and forming a functional film layer on the surface of the neodymium iron boron permanent magnet after high-temperature curing;
the preparation method of the Ni-MOFs material comprises the following steps: dissolving 0.05-0.1 mol/L of organic carboxylic acid MOF ligand shown in a chemical formula I and 0.15-0.3 mol/L of nickel nitrate in 1L of dimethylformamide, condensing and refluxing for 6-18 h at 120-150 ℃, cooling to room temperature, filtering, repeatedly washing with acetone, and drying to obtain the Ni-MOFs material,
2. the method for preparing the functional film on the surface of the neodymium-iron-boron permanent magnet according to claim 1, wherein the ultrasonic power of the ultrasonic cleaning is 1500-3000W, and the ultrasonic frequency is 30-40 KHz.
3. The method for preparing the functional film on the surface of the neodymium-iron-boron permanent magnet according to claim 1, wherein the pickling solution for pickling consists of 1-5 wt% of hydrochloric acid solution and thiourea, and the thiourea accounts for 0.5-1.5 wt% of the total mass of the pickling solution.
4. The method for preparing the functional film layer on the surface of the neodymium-iron-boron permanent magnet according to claim 1, wherein the modified epoxy resin is aliphatic and/or aromatic epoxy resin.
5. The method for preparing the functional film on the surface of the neodymium-iron-boron permanent magnet according to claim 1, wherein the fluorine-containing silane coupling agent is at least one of heptadecafluoro-alkyl trimethoxy silane, heptadecafluoro-alkyl triethoxy silane, tridecyl-alkyl trimethoxy silane, tridecyl-alkyl triethoxy silane, dodecafluoro-alkyl trimethoxy silane and dodecafluoro-alkyl triethoxy silane.
6. The method for preparing the functional film layer on the surface of the neodymium-iron-boron permanent magnet according to claim 1, wherein the vacuum chamber has a vacuum degree of 50-100 Pa and a temperature of 150-200 ℃.
7. The method for preparing the functional film on the surface of the neodymium-iron-boron permanent magnet according to claim 1, wherein the curing temperature of the high-temperature curing is 130-180 ℃, and the curing time is 1-10 hours.
8. The method for preparing the functional film on the surface of the neodymium-iron-boron permanent magnet according to claim 1, wherein the thickness of the bottom layer of the neodymium-iron-boron permanent magnet is 5-15 um.
9. The method for preparing the functional film on the surface of the neodymium iron boron permanent magnet according to claim 1, wherein the thickness of the functional film on the surface of the neodymium iron boron permanent magnet is 20-30 um.
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