CN114717511B - Preparation method of Al film on surface of sintered NdFeB magnet - Google Patents
Preparation method of Al film on surface of sintered NdFeB magnet Download PDFInfo
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- CN114717511B CN114717511B CN202210332039.8A CN202210332039A CN114717511B CN 114717511 B CN114717511 B CN 114717511B CN 202210332039 A CN202210332039 A CN 202210332039A CN 114717511 B CN114717511 B CN 114717511B
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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
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
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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
- C23C14/06—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
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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
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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
- C23C24/00—Coating starting from inorganic powder
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
- C23C24/10—Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
- C23C24/103—Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
- C23C24/106—Coating with metal alloys or metal elements only
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention belongs to the field of surface protection of rare earth permanent magnet materials, in particular to a preparation method of an Al film on the surface of a sintered neodymium iron boron magnet, which comprises the steps of firstly pretreating the sintered neodymium iron boron magnet by adopting a laser cleaning method, blowing dirt away from the surface of the magnet in time by adopting an inert gas, then depositing a layer of Al film on the pretreated surface of the magnet by adopting a vacuum evaporation method, finally treating the Al film by adopting a laser remelting technology, finally preparing the Al film with high binding force, high densification and high corrosion resistance on the surface of the magnet, effectively removing various pollutants adsorbed on the surface of the magnet, blowing the dirt cleaned by laser away from the surface of the magnet in time by adopting the inert gas, avoiding secondary pollution and oxidation on the clean surface, realizing metallurgical bonding between the Al film and a matrix by adopting the laser remelting, changing the columnar structure of the Al film, obviously improving the density of the Al film, and greatly improving the corrosion resistance of the Al film.
Description
Technical Field
The invention belongs to the field of surface protection of rare earth permanent magnet materials, and particularly relates to a preparation method of an Al film on the surface of a sintered NdFeB magnet.
Background
Since the advent of 1983, sintered neodymium-iron-boron magnets have greatly promoted the rapid development of permanent magnet materials and related fields by virtue of their excellent comprehensive magnetic properties and abundant resource reserves. However, the sintered neodymium-iron-boron magnet prepared by adopting the powder metallurgy process has a multiphase structure, the potential difference between phases is larger, particularly the electrochemical activity of a grain boundary rare earth-rich phase is highest, corrosion is very easy to occur in an electrochemical environment, a small amount of grain boundary rare earth-rich phase is taken as an anode to bear a large amount of current density, the corrosion characteristics of a large cathode and a small anode are formed, adhesion medium is lost between crystal grains due to corrosion of the grain boundary rare earth-rich phase, the crystal grains connected with each other are formed into isolated particles, and finally pulverization of the magnet is caused, so that the expansion of the application field of the magnet is severely limited. Therefore, it is an urgent problem to improve the corrosion resistance of sintered neodymium iron boron magnets.
At present, an alloying element method and a surface protection method are mainly adopted to improve the corrosion resistance of the sintered NdFeB magnet. The alloy element method is to add trace elements such as Cu, al, co and the like to improve the corrosion resistance of the magnet when the alloy is prepared, but the method can reduce the magnetic performance of the magnet to a certain extent and can not fundamentally solve the problem of poor corrosion resistance of the magnet. The surface protection method is characterized in that on the basis of not affecting the magnetic performance of the neodymium-iron-boron magnet, a layer of coating/plating layer with corrosion resistance is coated on the surface of the neodymium-iron-boron substrate, so that the contact between an external corrosion medium and the substrate is isolated, and the poor corrosion resistance of the sintered neodymium-iron-boron magnet can be obviously improved.
Common surface protection methods for sintered NdFeB magnets include electroplating, electroless plating, cathodic electrophoresis, spraying, physical vapor deposition, and the like. Among them, physical vapor deposition is an environment-friendly surface protection technology, and attention is paid to the fact that vacuum evaporation Al film has been applied to surface protection of sintered NdFeB magnets. However, the prepared Al film has poor binding force with the neodymium iron boron matrix, the Al film grows in a columnar crystal structure, obvious gaps are formed among crystals to penetrate through the film, the gaps become quick corrosion channels for outside corrosion solution to permeate to the matrix, and finally, the corrosion of the Al film on the surface of the magnet is caused to lose the protective effect.
The publication No. CN105671503B is a preparation method of a high corrosion resistant composite coating on the surface of a sintered NdFeB magnet, a Zn film and a vacuum evaporation Al film are sequentially deposited on the surface of the magnet in an alternating magnetron sputtering mode, and the columnar crystal structure of the Al film is broken through the deposited Zn film, so that a rapid corrosion channel for a corrosive solution to permeate to a substrate is blocked, and the corrosion resistance of the Al film is improved. Chinese patent CN201911230623.7 discloses a sintered NdFeB magnet surface densified Al coating and a method for preparing the same, wherein the surface of the sintered NdFeB magnet is evaporated by ball milling, so as to achieve densification of the Al coating, close gaps between columnar crystals of Al in the evaporation process, and improve corrosion resistance and surface hardness of the evaporated Al coating.
Based on the teaching of the patent disclosure about improving the density of the vacuum evaporation Al film, the invention adopts the laser remelting technology to process the vacuum evaporation Al film on the surface of the sintered NdFeB magnet, thereby obtaining the high-binding force and high-densification Al film.
Therefore, the invention provides a preparation method of an Al film on the surface of a sintered NdFeB magnet.
Disclosure of Invention
In order to overcome the deficiencies of the prior art, at least one technical problem presented in the background art is solved.
The technical scheme adopted for solving the technical problems is as follows: the invention discloses a preparation method of an Al film on the surface of a sintered NdFeB magnet, which comprises the following steps:
s1: magnet pretreatment: carrying out surface pretreatment on the sintered NdFeB magnet by adopting a laser cleaning method, and blowing dirt away from the surface of the magnet in time by using inert gas;
s2: preparing a vacuum evaporation Al film: depositing a layer of Al film on the surface of the pretreated magnet by adopting a vacuum evaporation process in a vacuum evaporation device;
s3: laser remelting treatment: and the laser remelting technology is adopted to carry out modification treatment on the Al film deposited on the surface of the magnet, so that the density of the Al film and the binding force between the Al film and the matrix are improved.
Preferably, the pre-treatment of the magnet in S1 is performed by a laser cleaning method to pre-treat the surface of the sintered neodymium iron boron magnet so as to remove greasy dirt and oxide skin on the surface of the magnet, and the technological parameters of the laser cleaning include: the laser power is 100-2500W, the laser beam wavelength is 1064nm, the pulse width is 50-300 ns, the laser scanning speed is 5-150 mm/s, and the laser incident angle is 20-90 degrees; and S1, preprocessing the magnet, namely blowing dirt cleaned by the laser away from the surface of the magnet in time by using inert gas to avoid secondary pollution and oxidation of the cleaning surface, wherein the inert gas is one of argon and helium.
Preferably, the preparation of the S2 vacuum evaporation Al film adopts a vacuum evaporation process to deposit a layer of Al film on the surface of the pretreated magnet, and the process parameters of the vacuum evaporation include that the vacuum degree is 1 multiplied by 10 -3 ～5×10 -3 Pa, the evaporation current is 2000-2900A, and the vacuum evaporation time is 50-80 min.
Preferably, the S3 laser remelting treatment is carried out, and a laser remelting technology is adopted to carry out modification treatment on the Al film deposited on the surface of the magnet, so that the density of the Al film and the binding force between the Al film and a matrix are improved; the technological parameters of the laser remelting comprise: the laser power is 1000-3000W, the scanning speed is 5-15 mm/s, the spot size is 2-5 mm, the lap joint coefficient is 5% -20%, and inert gas is filled as shielding gas, wherein the inert gas is one of argon gas and helium gas.
Preferably, the vacuum evaporation device comprises a shell, a crucible and an adjusting clamp; the crucible is fixedly connected to the position, close to the bottom surface of the shell, inside the shell, and the inside of the crucible is used for placing the evaporation material; an adjusting clamp is arranged in the shell at the top of the crucible; the adjusting clamp comprises a push rod, a motor and a rotating pressing block; the inner side surface of the shell is provided with first hydraulic grooves, and the number of the first hydraulic grooves is four; push rods are slidably connected inside the four first hydraulic grooves; wherein motors are fixedly connected inside any two adjacent push rods; the surfaces of the four push rods are respectively and rotatably connected with a rotary pressing block; during operation, through the inside hydraulic pressure of two relative first hydraulic tanks of control, the push rod can drive to correspond and rotate the briquetting extrusion sintered neodymium iron boron magnet, fix sintered neodymium iron boron magnet, then correspond the motor through the control and rotate, the motor can drive and correspond and rotate the briquetting and rotate, rotate the briquetting and can drive sintered neodymium iron boron magnet and rotate, make four wherein faces of sintered neodymium iron boron magnet, adjust gradually to the decurrent direction, be convenient for carry out the vacuum evaporation to these four faces of sintered neodymium iron boron magnet, accomplish behind the vacuum evaporation of these four faces, derive first hydraulic tank through control two other push rods, two push rods can drive and correspond the briquetting and extrude fixed sintered neodymium iron boron magnet, adduction original two push rods, the motor is controlled to rotate this moment, the motor can drive and rotate the briquetting, make sintered neodymium iron boron magnet rotate, control does not switch over to decurrent two surfaces, the surface of vacuum evaporation has realized carrying out the complete evaporation to the processing to sintered neodymium iron boron magnet.
Preferably, the inner surface of the shell is provided with second hydraulic grooves at the top and bottom positions of the adjusting clamp; a sealing plate is slidably connected inside the second hydraulic groove; the top surface of the sealing plate positioned at the bottom is provided with air inlets which are uniformly arranged; the bottom surface of the sealing plate positioned at the top part is provided with uniformly arranged air outlets; during operation, through setting up two shrouding, derive through two shrouding of control and correspond and obtain the second hydraulic pressure groove, two shrouding can make the sintered neodymium iron boron magnetism body be in the space of totally sealing, then control inlet port air inlet goes into cooling gas, cooling gas can be through sintered neodymium iron boron magnetism body surface to derive through the venthole, realized the cooling to sintered neodymium iron boron magnetism body, when follow-up change is to the clamp of sintered neodymium iron boron magnetism body, avoid producing the damage to the Al film that has vacuum evaporation.
Preferably, the inside of the air outlet holes are all in sliding connection with a control block; springs are fixedly connected to the tops of the control blocks; during operation, through setting up the control block, and the control block receives the pretension pressure of spring, when because the inside of shell is in vacuum state, the control block can carry out automatic shutoff to the venthole under the initial state, along with the continuous import gas of inlet port, the pressure between two shrouding increases, and then the control block slides and extrudees the spring for it is automatic to open to go out the gas pocket, has guaranteed that a large amount of cooling gas stops around sintering neodymium iron boron magnetism body, realizes quick cooling.
Preferably, the cooling grooves are formed in the positions, close to the air outlet holes, of the inner part of the sealing plate, and the cooling grooves are externally connected with a cooling air source through a pipeline; the inside of the cooling groove is slidably connected with an elastic plate, and the elastic plates are fixedly connected with the bottom surfaces of the corresponding control blocks; elastic sheets are fixedly connected between the elastic plates and the bottom surfaces of the corresponding cooling grooves; inclined holes are formed in the positions, close to the air outlet holes, of the surface of the sealing plate; the bottom opening positions of the air outlet holes are fixedly connected with a first heating plate; the bottom surfaces of the control blocks are fixedly connected with a second heating plate; during operation, through setting up elastic plate and elastic sheet, when the control piece upwards moves, the control piece can extrude the spring, can stimulate simultaneously and correspond the elastic plate, make the elastic plate export correspond the cooling tank, because the inside external cooling air supply that has of cooling tank, make the elastic plate of export be in cooling state, after the pressure between two shrouding risees, the inside of gas can be led into the venthole through the inclined hole to adsorb the solid particle in the gas through the elastic plate, realize the preliminary purification to exhaust gas, the cotton complete purification exhaust gas of final rethread simultaneously, accomplish the cooling back to sintered neodymium iron boron magnet, the control piece resets, under the effect of elastic sheet, the elastic plate is retrieved into corresponding cooling tank, and the in-process of retrieving, the adsorbed particle thing on elastic plate surface can be scraped off, and gather in the surface of first hot plate, through the heating of first hot plate and second hot plate, can make evaporation material regasify, partial evaporation material can pass through the inclined hole and lead back and be utilized.
Preferably, the inside of the air outlet hole is fixedly connected with a material guiding elastic sheet at the inclined hole position; the inside of the air outlet hole is fixedly connected with a guide pipe at the top of the material guiding elastic sheet, and the guide pipe is communicated with the corresponding inclined hole; during operation, through setting up the guide shell fragment, after the accessory crop on elastic plate surface is scraped, can drop into the surface of guide shell fragment at first, the guide shell fragment can avoid scraping the accessory crop of leaving and directly fall into the inclined hole, simultaneously through the pipe, with the top position of the direct introduction guide shell fragment of the leading-in gas of inclined hole to the vibrations of guide shell fragment can be made to gaseous flow, promotes impurity through the surface that the guide shell fragment falls into first hot plate, accomplishes the collection to the impurity attachment of scraping.
Preferably, the inside of the inclined hole is fixedly connected with a connecting rope; the end face of one side of the connecting rope, which is close to the material guiding elastic sheet, is fixedly connected with a vibration ball; during operation, through setting up the rope that links in the inside of inclined hole, the tip that links the rope links there is the vibrations ball, when gaseous through the inclined hole, gaseous can blow the vibrations ball for the vibrations ball is constantly rocked in the bottom position of guide shell fragment, promotes the vibrations effect to the guide shell fragment.
The beneficial effects of the invention are as follows:
1. the invention adopts the laser cleaning method to pretreat the sintered NdFeB magnet to remove greasy dirt and oxide skin on the surface of the magnet, and uses inert gas to blow away the dirt cleaned by the laser in time from the surface of the magnet, thereby avoiding the secondary pollution and oxidation of the clean surface. The traditional sintered NdFeB magnet pretreatment process comprises alkaline washing oil and acid washing rust removal, the surface magnetism of the magnet can be influenced in the pretreatment process, a small amount of hydrogen ions are attached to the surface of the magnet to influence the quality of a coating, and a large amount of waste liquid can be generated in the magnet pretreatment process. The laser cleaning is a green and environment-friendly surface cleaning mode, does not need an organic solvent, does not discharge waste liquid, has less residues, does not cause environmental pollution, and can effectively remove various pollutants adsorbed on the surface of the magnet. The laser cleaning has high flexibility and good controllability, is easy to realize precise cleaning by selecting areas and positioning, and is easy to clean places which are difficult to reach or dangerous by remote control. Therefore, the laser cleaning can effectively avoid the problems of surface magnetic decline caused by the traditional magnet surface pretreatment and environmental pollution caused by the adsorption of other cleaning products such as hydrogen ions on a substrate and waste liquid, and is the most ideal choice for replacing the traditional sintered NdFeB magnet surface pretreatment.
2. According to the invention, the laser remelting technology is adopted to carry out modification treatment on the Al film deposited on the surface of the magnet, so that metallurgical bonding between the Al film and the matrix can be realized, the columnar structure of the Al film is changed, the density of the Al film is obviously improved, and the corrosion resistance of the Al film is greatly improved. Compared with the vacuum evaporation Al film, the laser remelting technology can change the growth of the columnar crystal structure of the Al film, improve the structure morphology of the Al film, ensure that the distribution of the columnar crystal structure is more uniform, reduce or even eliminate the stress between the film and the matrix, and realize the metallurgical bonding between the Al film and the matrix. The laser remelting can remove impurities and gas, and meanwhile, the tissue obtained by quenching and recrystallization has higher hardness, wear resistance and corrosion resistance, and the remelting layer has a small heat action area and has little influence on surface roughness and workpiece size. Therefore, the vacuum evaporation Al film is treated by adopting laser remelting, the density of the Al film and the binding force between the Al film and a matrix can be obviously improved, and the Al film subjected to laser remelting has more excellent corrosion resistance.
3. According to the invention, the vacuum evaporation device is adopted, the shell, the crucible and the adjusting clamp are arranged, the motor is controlled to rotate, the motor drives the rotating pressing block to rotate, so that the sintered NdFeB magnet rotates, the surface which is not subjected to vacuum evaporation is controlled to be switched downwards, the surface of the sintered NdFeB magnet is completely evaporated, the two sealing plates can enable the sintered NdFeB magnet to be in a completely sealed space, then the air inlet is controlled to guide air into cooling gas, the cooling gas can pass through the surface of the sintered NdFeB magnet and is guided out through the air outlet, the cooling of the sintered NdFeB magnet is realized, and the damage to an Al film which is subjected to vacuum evaporation is avoided when the clamping of the sintered NdFeB magnet is replaced later.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is a flow chart of the method of the present invention;
fig. 2 is a perspective view of a vacuum vapor deposition apparatus used in the present invention;
fig. 3 is a first cross-sectional view of a vacuum vapor deposition apparatus used in the present invention;
fig. 4 is a second cross-sectional view of the vacuum vapor deposition apparatus used in the present invention;
FIG. 5 is a cross-sectional view of a closure plate of the present invention;
FIG. 6 is an enlarged view of a portion of FIG. 5 at A;
FIG. 7 is an enlarged view of a portion of FIG. 6 at B;
in the figure: the device comprises a shell 1, a crucible 2, an adjusting clamp 3, a push rod 4, a motor 5, a rotating pressing block 6, a first hydraulic groove 7, a second hydraulic groove 8, a sealing plate 9, an air inlet hole 10, an air outlet hole 11, a control block 12, a spring 13, a cooling groove 14, an elastic plate 15, an elastic sheet 16, an inclined hole 17, a first heating plate 18, a second heating plate 19, a guide elastic sheet 20, a guide pipe 21, a connecting rope 22 and a vibration ball 23.
Detailed Description
The invention is further described in connection with the following detailed description in order to make the technical means, the creation characteristics, the achievement of the purpose and the effect of the invention easy to understand.
Example 1
As shown in fig. 1, (1) magnet pretreatment:
commercial sintered NdFeB magnets (trade name: 42SH, status: not magnetized) with a specification of 20×15×4mm were selected for the test. The method comprises the steps of preprocessing the surface of a sintered NdFeB magnet by a laser cleaning method to remove greasy dirt and oxide skin on the surface of the magnet, wherein the laser cleaning process parameters comprise: the laser power is 100W, the laser beam wavelength is 1064nm, the pulse width is 50ns, the laser scanning speed is 5mm/s, and the laser incident angle is 20 degrees. And (3) blowing dirt cleaned by the laser away from the surface of the magnet in time by using inert gas, so as to avoid secondary pollution and oxidation of the cleaned surface, wherein the inert gas is argon.
(2) Preparing a vacuum evaporation Al film:
and depositing a layer of Al film on the surface of the pretreated magnet by adopting a vacuum evaporation process, wherein the process parameters of the vacuum evaporation comprise the vacuum degree of 1 multiplied by 10 < -3 > Pa, the evaporation current of 2000A and the vacuum evaporation time of 50min.
(3) Laser remelting treatment:
and the laser remelting technology is adopted to carry out modification treatment on the Al film deposited on the surface of the magnet, so that the density of the Al film and the binding force between the Al film and the matrix are improved. The technological parameters of the laser remelting comprise: the laser power is 1000W, the scanning speed is 5mm/s, the spot size is 2mm, the lap joint coefficient is 5%, and inert gas is filled as shielding gas, wherein the inert gas is argon.
Comparative example 1
For comparison, an Al film was deposited on the surface of the sintered neodymium-iron-boron magnet according to steps (1) and (2) in example 1, and no laser remelting treatment was performed.
Example 2
(1) Magnet pretreatment:
commercial sintered NdFeB magnets (trade name: 42SH, status: not magnetized) with a specification of 20×15×4mm were selected for the test. The method comprises the steps of preprocessing the surface of a sintered NdFeB magnet by a laser cleaning method to remove greasy dirt and oxide skin on the surface of the magnet, wherein the laser cleaning process parameters comprise: the laser power is 1300W, the laser beam wavelength is 1064nm, the pulse width is 175ns, the laser scanning speed is 80mm/s, and the laser incident angle is 60 degrees. And (3) blowing away dirt after laser cleaning from the surface of the magnet in time by using inert gas, so as to avoid secondary pollution and oxidation of the cleaning surface, wherein the inert gas is helium.
(2) Preparing a vacuum evaporation Al film:
and depositing a layer of Al film on the surface of the pretreated magnet by adopting a vacuum evaporation process, wherein the process parameters of the vacuum evaporation comprise a vacuum degree of 3X 10 < -3 > Pa, an evaporation current of 2450A and a vacuum evaporation time of 65min.
(3) Laser remelting treatment:
and the laser remelting technology is adopted to carry out modification treatment on the Al film deposited on the surface of the magnet, so that the density of the Al film and the binding force between the Al film and the matrix are improved. The technological parameters of the laser remelting comprise: the laser power is 2000W, the scanning speed is 10mm/s, the spot size is 3.5mm, the lap joint coefficient is 12.5%, and inert gas is filled as shielding gas, wherein the inert gas is helium.
Comparative example 2
For comparison, an Al film was deposited on the surface of the sintered neodymium-iron-boron magnet according to steps (1) and (2) in example 1, and no laser remelting treatment was performed.
Example 3
(1) Magnet pretreatment:
commercial sintered NdFeB magnets (trade name: 42SH, status: not magnetized) with a specification of 20×15×4mm were selected for the test. The method comprises the steps of preprocessing the surface of a sintered NdFeB magnet by a laser cleaning method to remove greasy dirt and oxide skin on the surface of the magnet, wherein the laser cleaning process parameters comprise: the laser power is 2500W, the laser beam wavelength is 1064nm, the pulse width is 300ns, the laser scanning speed is 150mm/s, and the laser incident angle is 90 degrees. And (3) blowing away dirt after laser cleaning from the surface of the magnet in time by using inert gas, so as to avoid secondary pollution and oxidation of the cleaning surface, wherein the inert gas is helium.
(2) Preparing a vacuum evaporation Al film:
and depositing a layer of Al film on the surface of the pretreated magnet by adopting a vacuum evaporation process, wherein the process parameters of the vacuum evaporation comprise a vacuum degree of 5 multiplied by 10 < -3 > Pa, an evaporation current of 2900A and a vacuum evaporation time of 80min.
(3) Laser remelting treatment:
and the laser remelting technology is adopted to carry out modification treatment on the Al film deposited on the surface of the magnet, so that the density of the Al film and the binding force between the Al film and the matrix are improved. The technological parameters of the laser remelting comprise: the laser power is 3000W, the scanning speed is 15mm/s, the spot size is 5mm, the lap joint coefficient is 20%, and inert gas is filled as shielding gas, wherein the inert gas is helium.
Comparative example 3
For comparison, an Al film was deposited on the surface of the sintered neodymium-iron-boron magnet according to steps (1) and (2) in example 3, and no laser remelting treatment was performed.
The samples prepared in examples 1,2 and 3 and the samples prepared in comparative examples 1,2 and 3 were respectively subjected to neutral salt spray test (salt spray test conditions: test chamber temperature 36.+ -. 2 ℃ C., salt water concentration 5% by weight, continuous spray test method) and plating adhesion, and the specific results are shown in Table 1 below.
TABLE 1 salt spray test and binding force test results of samples
| Sample of | Binding force (MPa) | Salt spray test (h) |
| Example 1 | 48.7 | 289 |
| Example 2 | 50.2 | 291 |
| Example 3 | 49.6 | 288 |
| Comparative example 1 | 12.9 | 96 |
| Comparative example 2 | 13.1 | 98 |
| Comparative example 3 | 12.6 | 96 |
As can be seen from table 1, compared with comparative examples 1,2 and 3, the binding force and salt spray resistance of the samples of examples 1,2 and 3 are both significantly improved, which means that the laser cleaning method is adopted to pretreat the magnet, inert gas is adopted to blow dirt away from the surface of the magnet in time, and then the laser remelting technology is adopted to treat the Al film on the surface of the magnet, so that the density of the Al film on the surface of the magnet and the binding force between the Al film and the substrate can be significantly improved, and the corrosion resistance of the magnet is greatly improved.
Example 4
As shown in fig. 2-7, comparative example one, in which another embodiment of the present invention is: the vacuum evaporation device comprises a shell 1, a crucible 2 and an adjusting clamp 3; the crucible 2 is fixedly connected to the inner part of the shell 1 near the bottom surface of the shell 1, and the inner part of the crucible 2 is used for placing evaporation materials; an adjusting clamp 3 is arranged in the shell 1 at the top of the crucible 2; the adjusting clamp 3 comprises a push rod 4, a motor 5 and a rotary pressing block 6; the inner side surface of the shell 1 is provided with first hydraulic grooves 7, and the number of the first hydraulic grooves 7 is four; push rods 4 are slidably connected inside the four first hydraulic grooves 7; wherein the motor 5 is fixedly connected with the inside of any two adjacent push rods 4; the surfaces of the four push rods 4 are respectively and rotatably connected with a rotary pressing block 6; during operation, through the inside hydraulic pressure of two relative first hydraulic tanks 7 of control, control should push rod 4 ejecting, push rod 4 can drive and correspond rotation briquetting 6 extrusion sintering neodymium iron boron magnet, fix sintering neodymium iron boron magnet, then correspond motor 5 through control and rotate, motor 5 can drive and correspond rotation briquetting 6 rotation, rotation briquetting 6 can drive sintering neodymium iron boron magnet and rotate, make four wherein faces of sintering neodymium iron boron magnet, adjust gradually to the decurrent, be convenient for carry out the vacuum evaporation to this four faces of sintering neodymium iron boron magnet, accomplish behind the vacuum evaporation of these four faces, derive first hydraulic tank through control two other push rods 4, two push rods 4 can drive and correspond rotation briquetting 6 extrusion fixed sintering neodymium iron boron magnet, adduction original two push rods 4, control motor 5 rotates this moment, motor 5 can drive rotation briquetting 6 rotation, make sintering neodymium iron boron magnet rotate, control does not switch to decurrent two surfaces of vacuum evaporation magnet, the complete evaporation to the surface of sintering neodymium iron boron magnet is handled.
The inner surface of the shell 1 is provided with second hydraulic grooves 8 at the top and bottom positions of the adjusting clamp 3; a sealing plate 9 is slidably connected inside the second hydraulic groove 8; the top surface of the sealing plate 9 at the bottom position is provided with evenly arranged air inlets 10; the bottom surface of the sealing plate 9 positioned at the top position is provided with uniformly arranged air outlet holes 11; during operation, through setting up two shrouding 9, derive through two shrouding 9 of control and correspond and obtain second hydraulic groove 8, two shrouding 9 can make the sintered neodymium iron boron magnet be in the space of totally sealing, then control inlet port 10 air guide income cooling gas, cooling gas can be through sintered neodymium iron boron magnet surface to export through venthole 11, realized the cooling to sintered neodymium iron boron magnet, when follow-up change is tight to the clamp of sintered neodymium iron boron magnet, avoid producing the damage to the Al film of vacuum evaporation.
The inside of the air outlet hole 11 is connected with a control block 12 in a sliding way; springs 13 are fixedly connected to the tops of the control blocks 12; during operation, through setting up control block 12, and control block 12 receives the pretension pressure of spring 13, when because the inside of shell 1 is in the vacuum state, control block 12 can carry out automatic shutoff to venthole 11 under the initial state, along with inlet port 10 continuous import gas, the pressure between two shrouding 9 increases, and then control block 12 slides and extrudees spring 13 for the venthole 11 is automatic to be opened, has guaranteed that a large amount of cooling gas stops around sintering neodymium iron boron magnetism body, realizes quick cooling.
The cooling grooves 14 are formed in the positions, close to the air outlet holes 11, inside the sealing plate 9, and the cooling grooves 14 are externally connected with a cooling air source through a pipeline; the inside of the cooling groove 14 is slidably connected with an elastic plate 15, and the elastic plates 15 are fixedly connected with the bottom surfaces of the corresponding control blocks 12; elastic sheets 16 are fixedly connected between the elastic plates 15 and the bottom surfaces of the corresponding cooling grooves 14; inclined holes 17 are formed in the surface of the sealing plate 9 and close to the air outlet holes 11; the opening positions of the bottoms of the air outlet holes 11 are fixedly connected with a first heating plate 18; the bottom surfaces of the control blocks 12 are fixedly connected with a second heating plate 19; during operation, when the control block 12 moves upwards, the control block 12 can squeeze the spring 13, and simultaneously can pull the corresponding elastic plate 15, so that the elastic plate 15 is led out to correspond to the cooling tank 14, the cooling tank 14 is externally connected with a cooling air source, so that the led-out elastic plate 15 is in a cooling state, after the pressure between the two sealing plates 9 rises, air can be led into the air outlet hole 11 through the inclined hole 17, solid particles in the air are adsorbed through the elastic plate 15, preliminary purification of the exhaust air is realized, and finally, the exhaust air is completely purified through cotton, after the temperature reduction of the sintered NdFeB magnet is completed, the control block 12 is reset, under the action of the elastic plate 16, the elastic plate 15 is recycled to correspond to the cooling tank 14, and adsorbed particles on the surface of the elastic plate 15 can be scraped off and gathered on the surface of the first heating plate 18, and part of the evaporation material can be led back through the inclined hole 17 and utilized by heating of the first heating plate 18 and the second heating plate 19.
The inside of the air outlet hole 11 is fixedly connected with a material guiding elastic sheet 20 at the position of the inclined hole 17; the inside of the air outlet hole 11 is fixedly connected with a guide pipe 21 at the top position of the material guiding elastic sheet 20, and the guide pipe 21 and the corresponding inclined hole 17 are communicated with each other; during operation, through setting up the guide shell fragment 20, after the attached crop on elastic plate 15 surface is scraped, can drop into the surface of guide shell fragment 20 at first, guide shell fragment 20 can avoid scraping the attached crop of leaving and directly fall into inclined hole 17, simultaneously through pipe 21, the upper position of guide shell fragment 20 is directly introduced to the gas that will incline hole 17 the import, and the vibrations of guide shell fragment 20 can be made to the flow of gas, promote impurity through the surface that guide shell fragment 20 falls into first hot plate 18, accomplish the collection to the impurity attachment of scraping.
The inside of the inclined hole 17 is fixedly connected with a connecting rope 22; the vibration balls 23 are fixedly connected to the end face of one side of the connecting rope 22, which is close to the material guiding elastic sheet 20; during operation, through setting up the rope 22 that links in the inside of inclined hole 17, the tip that links rope 22 links has vibrations ball 23, and when gas passed through inclined hole 17, gas can blow vibrations ball 23 for vibrations ball 23 constantly rocks in the bottom position of guide shell fragment 20, promotes the vibrations effect to guide shell fragment 20.
During operation, the pair of push rods 4 are controlled to eject through controlling the internal hydraulic pressure of the two opposite first hydraulic grooves 7, the push rods 4 can drive the corresponding rotating press blocks 6 to extrude the sintered NdFeB magnet, the sintered NdFeB magnet is fixed, then the corresponding motor 5 is controlled to rotate, the motor 5 can drive the corresponding rotating press blocks 6 to rotate, the rotating press blocks 6 can drive the sintered NdFeB magnet to rotate, four surfaces of the sintered NdFeB magnet are sequentially adjusted to be in a downward direction, the four surfaces of the sintered NdFeB magnet are conveniently subjected to vacuum evaporation, after the vacuum evaporation of the four surfaces is finished, the other two push rods 4 are controlled to guide out the first hydraulic grooves 7, the two push rods 4 can drive the corresponding rotating press blocks 6 to extrude and fix the sintered NdFeB magnet, the original two push rods 4 are retracted, at the moment, the motor 5 is controlled to rotate, the motor 5 can drive the rotating press blocks 6 to rotate, the sintered NdFeB magnet is controlled to switch to be downward, and the surface of the sintered NdFeB magnet is completely evaporated; through setting two sealing plates 9, the second hydraulic groove 8 is correspondingly obtained by controlling the two sealing plates 9 to lead out, the two sealing plates 9 can enable the sintered NdFeB magnet to be in a completely sealed space, then an air inlet hole 10 is controlled to lead in cooling air, the cooling air can pass through the surface of the sintered NdFeB magnet and is led out through an air outlet hole 11, the temperature of the sintered NdFeB magnet is reduced, and damage to an Al film which is subjected to vacuum evaporation is avoided when the sintered NdFeB magnet is clamped in subsequent replacement; by arranging the control block 12, and the control block 12 is under the pre-tightening pressure of the spring 13, when the inside of the shell 1 is in a vacuum state, the control block 12 automatically seals the air outlet hole 11 in an initial state, and the pressure between the two sealing plates 9 is increased along with the continuous introduction of air into the air inlet hole 10, so that the control block 12 slides and presses the spring 13, the air outlet hole 11 is automatically opened, a large amount of cooling air is ensured to stay around the sintered NdFeB magnet, and rapid cooling is realized; by arranging the elastic plate 15 and the elastic sheet 16, when the control block 12 moves upwards, the control block 12 can squeeze the spring 13, and simultaneously pulls the corresponding elastic plate 15, so that the elastic plate 15 is led out of the corresponding cooling groove 14, as the cooling air source is externally connected to the inside of the cooling groove 14, the led-out elastic plate 15 is in a cooling state, after the pressure between the two sealing plates 9 is increased, air is led into the inside of the air outlet hole 11 through the inclined hole 17, solid particles in the air are adsorbed by the elastic plate 15, the primary purification of the exhaust air is realized, and finally, the exhaust air is completely purified through cotton, after the temperature reduction of the sintered NdFeB magnet is completed, the control block 12 is reset, under the action of the elastic sheet 16, the elastic plate 15 is recycled into the corresponding cooling groove 14, and in the recycling process, adsorbed particles on the surface of the elastic plate 15 can be scraped off and gathered on the surface of the first heating plate 18, by heating of the first heating plate 18 and the second heating plate 19, the evaporated material can be re-gasified and partially recycled through the inclined hole 17; by arranging the guide elastic sheet 20, when the accessory on the surface of the elastic plate 15 is scraped off, the accessory can firstly fall into the surface of the guide elastic sheet 20, the guide elastic sheet 20 can prevent the scraped accessory from directly falling into the inclined hole 17, meanwhile, the gas led in by the inclined hole 17 is directly led into the position above the guide elastic sheet 20 through the guide pipe 21, and the vibration of the guide elastic sheet 20 can be caused by the flow of the gas, so that the impurity can be promoted to fall into the surface of the first heating plate 18 through the guide elastic sheet 20, and the collection of the scraped impurity attachment is completed; through setting up the rope 22 that links in the inside of inclined hole 17, the tip that links rope 22 links has vibrations ball 23, and when gas passed through inclined hole 17, gas can blow vibrations ball 23 for vibrations ball 23 constantly rocks in the bottom position of guide shell fragment 20, promotes the vibrations effect to guide shell fragment 20.
The front, rear, left, right, up and down are all based on fig. 1 in the drawings of the specification, the face of the device facing the observer is defined as front, the left side of the observer is defined as left, and so on, according to the viewing angle of the person.
In the description of the present invention, it should be understood that the terms "center," "longitudinal," "lateral," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like indicate orientations or positional relationships based on the orientation or positional relationships shown in the drawings, merely to facilitate describing the present invention and simplify the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and therefore should not be construed as limiting the scope of the present invention.
The foregoing has shown and described the basic principles, principal 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, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (5)
1. A preparation method of an Al film on the surface of a sintered NdFeB magnet is characterized by comprising the following steps: the method comprises the following steps:
s1: magnet pretreatment: carrying out surface pretreatment on the sintered NdFeB magnet by adopting a laser cleaning method, and blowing dirt away from the surface of the magnet in time by using inert gas;
s2: preparing a vacuum evaporation Al film: depositing a layer of Al film on the surface of the pretreated magnet by adopting a vacuum evaporation process in a vacuum evaporation device;
s3: laser remelting treatment: carrying out modification treatment on the Al film deposited on the surface of the magnet by adopting a laser remelting technology, and improving the density of the Al film and the binding force between the Al film and a matrix;
the magnet pretreatment in the step S1 is to pretreat the surface of the sintered NdFeB magnet by a laser cleaning method so as to remove greasy dirt and oxide skin on the surface of the magnet, and the technological parameters of the laser cleaning comprise: the laser power is 100-2500W, the laser beam wavelength is 1064nm, the pulse width is 50-300 ns, the laser scanning speed is 5-150 mm/s, and the laser incident angle is 20-90 degrees; the magnet pretreatment in the step S1, the inert gas is used for timely blowing dirt after laser cleaning away from the surface of the magnet, so that the cleaned surface is prevented from being polluted and oxidized again, and the inert gas is one of argon and helium;
the S2 preparation of the vacuum evaporation Al film adopts a vacuum evaporation process to deposit a layer of Al film on the surface of the pretreated magnet, and the process parameters of the vacuum evaporation include that the vacuum degree is 1 multiplied by 10 -3 ～5×10 -3 Pa, the evaporation current is 2000-2900A, and the vacuum evaporation time is 50-80 min;
the S3 laser remelting treatment is carried out, and a laser remelting technology is adopted to carry out modification treatment on the Al film deposited on the surface of the magnet, so that the density of the Al film and the binding force between the Al film and a matrix are improved; the technological parameters of the laser remelting comprise: the laser power is 1000-3000W, the scanning speed is 5-15 mm/s, the spot size is 2-5 mm, the lap joint coefficient is 5% -20%, and inert gas is filled as shielding gas, wherein the inert gas is one of argon gas and helium gas;
the vacuum evaporation device comprises a shell (1), a crucible (2) and an adjusting clamp (3); the crucible (2) is fixedly connected to the inner part of the shell (1) close to the bottom surface of the shell (1), and the inner part of the crucible (2) is used for placing evaporation materials; an adjusting clamp (3) is arranged at the top of the crucible (2) in the shell (1); the adjusting clamp (3) comprises a push rod (4), a motor (5) and a rotating pressing block (6); the inner side surface of the shell (1) is provided with first hydraulic grooves (7), and the number of the first hydraulic grooves (7) is four; push rods (4) are slidably connected inside the four first hydraulic grooves (7); wherein the motor (5) is fixedly connected inside any two adjacent push rods (4); the surfaces of the four push rods (4) are respectively and rotatably connected with a rotary pressing block (6);
the inner surface of the shell (1) is provided with second hydraulic grooves (8) at the top and bottom positions of the adjusting clamp (3); a sealing plate (9) is slidably connected inside the second hydraulic groove (8); the top surface of the sealing plate (9) at the bottom is provided with evenly arranged air inlets (10); the bottom surface of the sealing plate (9) positioned at the top is provided with uniformly arranged air outlet holes (11).
2. The method for preparing the Al film on the surface of the sintered NdFeB magnet according to claim 1, which is characterized in that: the inside of the air outlet hole (11) is connected with a control block (12) in a sliding way; springs (13) are fixedly connected to the tops of the control blocks (12).
3. The method for preparing the Al film on the surface of the sintered NdFeB magnet according to claim 2, which is characterized in that: the cooling grooves (14) are formed in the sealing plate (9) and close to the air outlet holes (11), and the cooling grooves (14) are externally connected with a cooling air source through pipelines; the inside of the cooling groove (14) is slidably connected with an elastic plate (15), and the elastic plates (15) are fixedly connected with the bottom surfaces of the corresponding control blocks (12); elastic sheets (16) are fixedly connected between the elastic plates (15) and the bottom surfaces of the corresponding cooling grooves (14); inclined holes (17) are formed in the positions, close to the air outlet holes (11), of the surface of the sealing plate (9); the opening positions of the bottoms of the air outlet holes (11) are fixedly connected with a first heating plate (18); the bottom surfaces of the control blocks (12) are fixedly connected with a second heating plate (19).
4. The method for preparing the surface Al film of the sintered NdFeB magnet according to claim 3, wherein the method comprises the following steps: the inside of the air outlet hole (11) is fixedly connected with a material guiding elastic sheet (20) at the position of the inclined hole (17); the inside of the air outlet hole (11) is fixedly connected with a guide pipe (21) at the top position of the guide elastic sheet (20), and the guide pipe (21) and the corresponding inclined hole (17) are communicated with each other.
5. The method for preparing the Al film on the surface of the sintered NdFeB magnet according to claim 4, which is characterized in that: the inside of the inclined hole (17) is fixedly connected with a connecting rope (22); the vibration balls (23) are fixedly connected to the end face of one side of the connecting rope (22) close to the material guiding elastic sheet (20).
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