CN111441017A - Method for preparing anticorrosive coating on surface of neodymium iron boron magnet - Google Patents

Method for preparing anticorrosive coating on surface of neodymium iron boron magnet Download PDF

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CN111441017A
CN111441017A CN202010336589.8A CN202010336589A CN111441017A CN 111441017 A CN111441017 A CN 111441017A CN 202010336589 A CN202010336589 A CN 202010336589A CN 111441017 A CN111441017 A CN 111441017A
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boron magnet
evaporation
coating
neodymium
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程俊峰
林建强
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Ningbo Zhaobao Magnet Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/34—Nitrides
    • C23C16/345—Silicon nitride
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
    • 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
    • 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

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  • Physics & Mathematics (AREA)
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Abstract

The invention discloses a method for preparing an anticorrosive coating on the surface of a neodymium iron boron magnet, which comprises the following steps: 1) surface pretreatment: cleaning the surface of the magnet and drying; 2) surface cleaning: vacuumizing, heating to 100 ℃, introducing argon, applying negative bias to the cavity, and carrying out plasma cleaning on the sample; 3) surface evaporation: vacuumizing, heating to 200-300 ℃, introducing auxiliary gas, generating plasma by glow discharge, bombarding a metal target, performing vacuum evaporation, and performing evaporation plating on the surface of the neodymium iron boron magnet to form a composite coating; the auxiliary gas comprises a first component, a second component and a third component, wherein the first component is silazane, the second component is one or two of nitrogen and ammonia, and the third component is argon and helium; 4) and after the evaporation is finished, continuously vacuumizing until the temperature of the vacuum chamber is reduced to be below 100 ℃, and closing the equipment. The invention adopts vacuum thermal evaporation to generate the inorganic nano-particle-metal composite film, so that the corrosion resistance of the surface of the neodymium iron boron magnet is improved.

Description

Method for preparing anticorrosive coating on surface of neodymium iron boron magnet
Technical Field
The invention relates to a neodymium iron boron magnet coating, in particular to a method for preparing an anti-corrosion coating on the surface of a neodymium iron boron magnet.
Background
As an important rare earth application material, the neodymium iron boron rare earth permanent magnet material is closely related to the life of people. The magnetic material has extremely high magnetic energy and coercive force, and is widely applied to various motors with excellent performance. However, the inherent corrosion resistance of the permanent magnet material of neodymium iron boron rare earth is not enough due to the multi-phase structure of neodymium iron boron and the difference of chemical characteristics among phases, once the crystal boundary Nd-rich phase is corroded and dissolved, the bonding medium among the main phase crystal grains in the magnet disappears, so that the main phase crystal grains fall off, and in severe cases, the magnet is pulverized and failed. Therefore, how to effectively improve the corrosion resistance of the neodymium iron boron becomes the key of application expansion.
At present, the conventional methods for improving the corrosion resistance of neodymium iron boron mainly comprise two main types, namely an alloying method and an external protective coating method. The corrosion resistance of the magnet itself is improved to some extent by the alloying method, but the method increases the production cost of the magnet and significantly reduces the magnetic performance of the magnet. Therefore, the industry generally adopts a method of adding a protective coating on the surface of the magnet to thoroughly solve the defect of poor corrosion resistance of the magnet. The surface protective coating method is to coat a compact and flawless coating on the surface of the magnet to prevent the magnet from contacting with water, oxygen, corrosive solution and other substances in the environment, thereby improving the corrosion resistance of the magnet. Methods for providing a protective layer on the surface of the neodymium-iron-boron include electroplating, electroless plating, organic coating, and Physical Vapor Deposition (PVD) plating. The PVD method comprises vacuum evaporation plating, magnetron sputtering coating, arc ion plating and the like. At present, Physical Vapor Deposition (PVD), which is one of modern surface treatment technologies, is gradually applied to the field of surface protection treatment of neodymium iron boron rare earth permanent magnet materials. The metal film deposited on the surface of the neodymium iron boron rare earth permanent magnet material by adopting the technology has the characteristics of stability, strong binding force of a plating layer/matrix, high density and the like, and has stronger anti-corrosion capability in cold and hot alternating environments. The technology can solve the problem of environmental pollution caused in the electroplating process, and is considered as a new direction for the protection development of the neodymium iron boron rare earth permanent magnet.
The vacuum thermal evaporation plating technology is a process of placing a workpiece to be plated in a high vacuum chamber, heating an evaporation boat at the bottom of the vacuum chamber to vaporize or sublimate evaporation materials, and finally condensing the evaporation boat on the surface of a base piece to form a film. The technology has the advantages of simple process, high coating deposition rate, obvious effect and the like. Because Al has lower potential and can generate a compact protective oxide film Al at a proper temperature2O3In addition, the deposition rate of vacuum plating Al is high, so that Al is one of the preferred metal protective coatings for vacuum plating of Nd-Fe-B rare earth permanent magnet materials. In recent years, researchers have prepared an Al thin film on the surface of a sintered neodymium-iron-boron magnet by means of vacuum thermal evaporation. Zhangpengjie et al [ chinese surface engineering, 2016, 29 (4): p49 ~ 58.]The research shows that the Al film is evaporated on the surface of the sintered neodymium iron boron in vacuum, but the bonding force between the obtained Al film and the substrate is low, the formed columnar crystal structure is easy to become a corrosive medium permeation channel, and the process has a certain environmental pollution problem.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for preparing an anticorrosive coating on the surface of a neodymium iron boron magnet.
The technical scheme adopted by the invention for solving the technical problem is as follows: a method for preparing an anticorrosive coating on the surface of a neodymium-iron-boron magnet comprises the following steps:
1) surface pretreatment: cleaning the surface of the semi-finished neodymium iron boron magnet, removing pollutants and then drying;
2) surface cleaning: vacuumizing, heating to 100 ℃, introducing argon, applying negative bias to the cavity, and carrying out plasma cleaning on the sample;
3) surface evaporation, namely vacuumizing, heating to 200-300 ℃, introducing auxiliary gas, and controlling the vacuum degree to be 1 × 10-2～10×10-2Pa, generating plasma by glow discharge, bombarding a metal target material, performing vacuum evaporation for 10-60 minutes, and performing evaporation on the surface of the neodymium iron boron magnet to form a composite coating; the composite coating is an inorganic nano-particle-metal coating;the auxiliary gas comprises a first component, a second component and a third component, wherein the first component is silazane, the second component is one or two of nitrogen and ammonia, and the third component is argon and helium;
4) and after the evaporation is finished, continuously vacuumizing until the temperature of the vacuum chamber is reduced to be below 100 ℃, and closing the equipment.
Furthermore, in the auxiliary gas, the volume ratio of the sum of the first component and the second component to the third component is 1: 9-1: 1.
Further, the metal in the composite coating is one or a combination of more of aluminum, chromium, titanium, nickel, zinc, copper and tin.
Further, the inorganic nanoparticles in the composite coating are silicon nitride, which is a reaction product of the first component and the second component in the auxiliary gas.
Further, the silazane is a combination of one or more of hexamethyldisilazane, bis (tert-butylamino) silane, bis (diethylamino) silane, bis (isopropylamino) silane, tris (dimethylamino) silane.
Further, the thickness of the composite coating is 0.1-20 μm.
Chemical Vapor Deposition (CVD) is a process of generating solid deposits by reacting gaseous or Vapor substances at a gas or gas-solid interface.
In plasma, substances are changed from gas state to plasma state, and are enriched with electrons, ions, excited state atoms, molecules and free radicals, which are very active, and many reaction systems which are difficult to carry out become easy to carry out under the plasma condition. The plasma enhanced chemical vapor deposition is: in chemical vapor deposition, a gas is excited to generate low-temperature plasma, and the chemical activity of a reaction substance is enhanced, so that the epitaxy is performed. The preparation method of semiconductor film material and other material film is characterized by that it utilizes glow discharge to make ionization in the deposition chamber, then makes chemical reaction deposition on the substrate. And carrying out plasma enhancement on the silicon-containing gas and the nitrogen-containing gas to prepare silicon nitride nano particles, and depositing to obtain the silicon nitride inorganic film.
In the silicon nitride deposition process, inert gas is added into the discharge of silicon-containing gas and nitrogen-containing gas to improve the physical or chemical properties of the deposited film. The inert gas participates in the discharge to form a large amount of excited state and metastable state atoms, and the atoms emit ultraviolet light to promote the dehydration reaction of the growing film to form a denser film.
The ion plating is based on vacuum evaporation plating, a device which makes inert gas generate glow discharge so as to generate plasma is added into the equipment, the plasma in an electric field ionizes evaporated atoms in the atmosphere of the plasma, and the substrate is bombarded and plated by the plasma evaporated material and inert gas ions. The ion plating combines glow discharge, plasma technology and vacuum evaporation coating technology, and has the advantages of high deposition speed, strong film adhesion, good diffraction, wide range of platable materials and the like.
Therefore, in the process of preparing the surface coating of the neodymium iron boron magnet, the addition of the inert gas can improve the physical and chemical properties of the inorganic deposition film on one hand, and can play a role of ion plating on the other hand, so that the silicon nitride nanoparticles and the metal are co-deposited on the surface of the neodymium iron boron magnet to form an inorganic-metal composite film, and the corrosion resistance is improved.
The invention has the beneficial effects that: compared with the prior art, the Ru iron boron magnet surface anticorrosive coating provided by the invention has the following advantages:
(1) the compactness and the flatness of the deposited film are obviously improved by adopting the plasma assistance, and the columnar crystal structure of the PVD-Al film is inhibited, so that the corrosion resistance is better;
(2) the nanometer silicon nitride particles generated by vacuum thermal evaporation can be co-deposited on the surface of neodymium iron boron with metal to form an inorganic nanometer particle-metal composite film, and the inorganic nanometer particle-metal composite film has better corrosion resistance than a pure metal coating film, because the silicon nitride inorganic nanometer particles can be embedded on defect corrosion matrix metal serving as an inert substance obstacle, the microstructure of a metal coating is improved, and the corrosion resistance of the coating is improved. Meanwhile, the codeposition of the inorganic nano particles also prevents corrosion points on the interface from being generated, accelerates the passivation process of the matrix metal and obviously improves the corrosion resistance of the neodymium iron boron magnet.
Drawings
FIG. 1 is an SEM image of the surface topography of the product obtained in example 1.
FIG. 2 is a SEM image of the cross-sectional morphology of the product obtained in example 1.
FIG. 3 is an SEM image of the surface morphology of the product obtained in comparative example 1.
FIG. 4 is a SEM image of the cross-sectional morphology of the product obtained in comparative example 1.
Detailed Description
The invention is further illustrated by the following specific examples. These examples are intended to illustrate the invention and are not intended to limit the scope of the invention.
A method for preparing an anti-corrosion coating on the surface of a neodymium iron boron magnet, comprising the following steps:
1) surface pretreatment: cleaning the surface of a semi-finished neodymium iron boron magnet, specifically, uniformly mixing 80-mesh glass beads and brown corundum in a weight ratio of 3: 1 to obtain a sand blasting abrasive, and blasting sand by using compressed air of 0.3Mpa until the surface is bright; putting the sand-blasted sample into alcohol for ultrasonic cleaning for 20min, and drying for later use;
2) surface cleaning: vacuumizing, heating to 100 ℃, introducing argon, applying negative bias to the cavity, and performing surface cleaning and activation treatment on the sample by adopting argon plasma under vacuum; in the step, the surface of the neodymium iron boron permanent magnet is activated by adopting an ion source, so that the potential energy of the surface of the neodymium iron boron permanent magnet can be improved by 1 order of magnitude, the energy barrier required by the combination of the subsequent coating and the surface of the neodymium iron boron permanent magnet is reduced, the combination of the subsequent coating is facilitated, the firmness of the coating is improved, surface impurities and oxides are removed, and the combination force of the coating and a substrate is improved;
3) surface evaporation, namely vacuumizing, heating to 200-300 ℃, introducing auxiliary gas, and controlling the vacuum degree to be 1 × 10-2～10×10-2Pa, glow discharge to generate plasma to bombard the metal targetThe method comprises the steps of carrying out vacuum evaporation on a neodymium iron boron magnet for 10-60 minutes, and carrying out evaporation on the surface of the neodymium iron boron magnet to form a composite coating, wherein the composite coating is an inorganic nanoparticle-metal coating, the auxiliary gas comprises a first component, a second component and a third component, the first component is silazane, the second component is one or two of nitrogen and ammonia, the third component is argon and helium, and in the surface vacuum evaporation step, the evaporation pressure is 1 × 10-2Pa, the corrosion resistance of the aluminum protective coating is best, and the corrosion resistance of the aluminum protective coating on the surface of the neodymium iron boron is further improved after the auxiliary gas ion bombardment is added, however, the corrosion resistance is 1 × 10-2Pa, the gas molecules in the furnace are too few, which makes the glow discharge difficult to occur, metal atoms can not be ionized, and the effect of ion-assisted bombardment can not be achieved, the gas pressure is too high (higher than 10 × 10)-2Pa), the deposition efficiency was low and the effect was poor, and therefore, 1 × 10 was used-2～10×10-2pa, the power of the ion source is 3 kW-20 kW.
4) And after the evaporation is finished, continuously vacuumizing until the temperature of the vacuum chamber is reduced to be below 100 ℃, and closing the equipment.
In the auxiliary gas, the volume ratio of the sum of the first component and the second component to the third component is 1: 9-1: 1. The metal in the composite coating is one or a combination of more of aluminum, chromium, titanium, nickel, zinc, copper and tin. The inorganic nanoparticles in the composite coating are silicon nitride, which is a reaction product of a first component and a second component in an auxiliary gas. The silazane is a combination of one or more of hexamethyldisilazane, bis (tert-butylamino) silane, bis (diethylamino) silane, bis (isopropylamino) silane, tris (dimethylamino) silane. The thickness of the composite coating is 0.1-20 mu m.
Example 1
A method for preparing an anti-corrosion coating on the surface of a neodymium iron boron magnet, comprising the following steps:
step 1), surface pretreatment: the 80-mesh glass beads and brown corundum are uniformly mixed according to the weight ratio of 3: 1 to be used as a sand blasting abrasive, and the sand is blasted by using the pressure of 0.3Mpa until the surface is bright. And (4) putting the sand-blasted sample into alcohol for ultrasonic cleaning for 20min, and drying for later use.
Step 2), surface cleaning: vacuumizing to the vacuum degree of 10-1Pa, heating to 100 ℃, introducing argon until the vacuum degree is 1Pa, applying negative bias voltage of 800V to the cavity, and carrying out plasma cleaning on the sample for 3 minutes;
step 3), surface evaporation, namely vacuumizing, heating to 200 ℃, introducing an auxiliary gas (hexamethyldisilazane/nitrogen/argon) 2/2/6 (volume ratio), and controlling the vacuum degree to be 6 × 10-2Pa, generating plasma by glow discharge, bombarding an aluminum metal target, carrying out vacuum evaporation on metal aluminum for 30 minutes, and carrying out evaporation on the surface of the neodymium iron boron magnet to form a composite coating;
and 4) after the evaporation is finished, continuously vacuumizing until the temperature of the vacuum chamber is reduced to be below 100 ℃, and closing the equipment.
Example 2
In step 3), the auxiliary gas used was hexamethyldisilazane/ammonia gas/argon (volume ratio) 1/2/6, and the rest of the conditions were the same as in example 1.
Example 3
In the step 3), the auxiliary gas adopted is bis (diethylamino) silane/nitrogen/helium (volume ratio) 2/3/5, the temperature is raised to 300 ℃, and the vacuum degree is 10 × 10-2Pa, vacuum evaporating the metal nickel for 60 minutes. The remaining conditions were the same as in example 1.
Example 4
In the step 3), the adopted auxiliary gas is hexamethyldisilazane/nitrogen/helium (volume ratio) of 0.5/0.5/9, the temperature is raised to 200 ℃, and the vacuum degree is 8 × 10-2Pa, vacuum evaporating the metal aluminum for 40 minutes. The remaining conditions were the same as in example 1.
Comparative example 1
Compared with the embodiment 1, the metal aluminum is directly vacuumized and evaporated in the step 3) without auxiliary gas plasma formation.
Comparative example 2
Compared with the embodiment 1, argon is introduced into the step 3) for plasma formation, and aluminum metal is evaporated in a vacuum-assisted manner.
In the above examples 1-4 and comparative examples 1-2, the adopted semi-finished ndfeb magnets were all of 45H, 20mm × 5mm 355 mm × 1.5.5 mm which were chamfered and polished after the mechanical processing, and in addition, the obtained ndfeb magnets were subjected to salt spray tests, respectively, and the insulation and magnetic property changes of the ndfeb magnets before and after the salt spray test were tested to detect the damage of the plating layer, wherein the salt spray test standard adopted the GB 6458-86 standard.
Salt spray resistance time (h) Coating bonding force (MPa)
Example 1 1010 42.5
Example 2 980 41.3
Example 3 650 38.9
Example 4 710 40.1
Comparative example 1 58 29.8
Comparative example 2 112 30.7
Base body 10 -
The above embodiments are only for illustrating the invention and are not to be construed as limiting the invention, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention, therefore, all equivalent technical solutions also belong to the scope of the invention, and the scope of the invention is defined by the claims.

Claims (6)

1. A method for preparing an anticorrosive coating on the surface of a neodymium-iron-boron magnet is characterized by comprising the following steps: the method comprises the following steps:
1) surface pretreatment: cleaning the surface of the semi-finished neodymium iron boron magnet, removing pollutants and then drying;
2) surface cleaning: vacuumizing, heating to 100 ℃, introducing argon, applying negative bias to the cavity, and carrying out plasma cleaning on the sample;
3) surface evaporation, namely vacuumizing, heating to 200-300 ℃, introducing auxiliary gas, and controlling the vacuum degree to be 1 × 10-2～10×10-2Pa, generating plasma by glow discharge, bombarding a metal target material, performing vacuum evaporation for 10-60 minutes, and performing evaporation on the surface of the neodymium iron boron magnet to form a composite coating; the composite coating is an inorganic nano-particle-metal coating; the auxiliary gas comprises a first component, a second component and a third component, wherein the first component is silazane, the second component is one or two of nitrogen and ammonia, and the third component is argon and helium;
4) and after the evaporation is finished, continuously vacuumizing until the temperature of the vacuum chamber is reduced to be below 100 ℃, and closing the equipment.
2. The method for preparing the surface anticorrosive coating of the neodymium-iron-boron magnet according to claim 1, characterized by comprising the following steps: in the auxiliary gas, the volume ratio of the sum of the first component and the second component to the third component is 1: 9-1: 1.
3. The method for preparing the surface anticorrosive coating of the neodymium-iron-boron magnet according to claim 1, characterized by comprising the following steps: the metal in the composite coating is one or a combination of more of aluminum, chromium, titanium, nickel, zinc, copper and tin.
4. The method for preparing the surface anticorrosive coating of the neodymium-iron-boron magnet according to claim 1, characterized by comprising the following steps: the inorganic nanoparticles in the composite coating are silicon nitride, which is a reaction product of a first component and a second component in an auxiliary gas.
5. The method for preparing the surface anticorrosive coating of the neodymium-iron-boron magnet according to claim 1, characterized by comprising the following steps: the silazane is a combination of one or more of hexamethyldisilazane, bis (tert-butylamino) silane, bis (diethylamino) silane, bis (isopropylamino) silane, tris (dimethylamino) silane.
6. The method for preparing the surface anticorrosive coating of the neodymium-iron-boron magnet according to claim 1, characterized by comprising the following steps: the thickness of the composite coating is 0.1-20 mu m.
CN202010336589.8A 2020-04-24 2020-04-24 Method for preparing anticorrosive coating on surface of neodymium iron boron magnet Withdrawn CN111441017A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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CN112768169A (en) * 2020-12-30 2021-05-07 包头天和磁材科技股份有限公司 Preform, method for producing the same, method for producing corrosion-resistant magnet, and use of the same
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CN114574806A (en) * 2022-03-02 2022-06-03 浙江大学 Rare earth permanent magnet material surface corrosion-resistant coating and preparation method thereof
CN114622170A (en) * 2022-03-16 2022-06-14 宁波招宝磁业有限公司 Preparation method of surface anticorrosive coating of neodymium iron boron

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JP7232302B2 (en) 2020-11-13 2023-03-02 コマディール・エス アー Anti-corrosion protection for portable watch magnets, especially neodymium-iron-boron magnets
US12012651B2 (en) * 2020-11-13 2024-06-18 Comadur Sa Corrosion-inhibiting protection for watch magnets, in particular neodymium-iron-boron magnets
CN114481076B (en) * 2020-11-13 2024-04-12 柯马杜股份有限公司 Corrosion protection for watch magnets, particularly neodymium-iron-boron magnets
KR102536438B1 (en) * 2020-11-13 2023-05-26 코마도 쏘시에떼 아노님 Corrosion-inhibiting protection for watch magnets, in particular neodymium-iron-boron magnets
CN114481076A (en) * 2020-11-13 2022-05-13 柯马杜股份有限公司 Corrosion protection for watch magnets, in particular neodymium-iron-boron magnets
US20220154327A1 (en) * 2020-11-13 2022-05-19 Comadur Sa Corrosion-inhibiting protection for watch magnets, in particular neodymium-iron-boron magnets
KR20220065674A (en) * 2020-11-13 2022-05-20 코마도 쏘시에떼 아노님 Corrosion-inhibiting protection for watch magnets, in particular neodymium-iron-boron magnets
JP2022078952A (en) * 2020-11-13 2022-05-25 コマディール・エス アー Anti-corrosion protection for portable timepiece magnets, in particular neodymium-iron-boron magnets
CN112725751B (en) * 2020-12-16 2022-03-25 太原理工大学 Preparation method of surface protective coating of ultrathin neodymium-iron-boron permanent magnet
CN112725751A (en) * 2020-12-16 2021-04-30 太原理工大学 Preparation method of surface protective coating of ultrathin neodymium-iron-boron permanent magnet
CN112768169A (en) * 2020-12-30 2021-05-07 包头天和磁材科技股份有限公司 Preform, method for producing the same, method for producing corrosion-resistant magnet, and use of the same
CN112992521A (en) * 2021-03-09 2021-06-18 合肥工业大学 Preparation method of low-weight-loss sintered NdFeB magnet
CN114574806A (en) * 2022-03-02 2022-06-03 浙江大学 Rare earth permanent magnet material surface corrosion-resistant coating and preparation method thereof
CN114622170A (en) * 2022-03-16 2022-06-14 宁波招宝磁业有限公司 Preparation method of surface anticorrosive coating of neodymium iron boron

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Application publication date: 20200724